US3192102A - Pulping process - Google Patents
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- US3192102A US3192102A US216969A US21696962A US3192102A US 3192102 A US3192102 A US 3192102A US 216969 A US216969 A US 216969A US 21696962 A US21696962 A US 21696962A US 3192102 A US3192102 A US 3192102A
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- chips
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- digesting
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
- D21C1/00—Pretreatment of the finely-divided materials before digesting
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- This invention relates to a process of treating cellulose fiber-bearing materials and, more particularly, relates to an improved process of removing the non-cellulosic material therefrom by the use of a digestion process for the manufacture of paper, cellulose for synthetic fibers, and the like. 7 It is a particular object of this invention to provide a method for producing papermaking pulps from wood or other cellulosic materials by a rapid continuous process, in which from about half to nearly all of the lignin is removed. i
- a further object is the production of cellulosic pulps having a high alpha cellulose content and a low lignin and pentosan content, which is useful for the manufacture of rayon, cellophane and like products.
- Another object of the invention is the modification of existing so-called batch processes so that reaction time may be shortened, resulting in increased yield and improved quality of the resultant pulp.
- a further object of the invention is the provision of such a process that is readily adaptable for the processing of various types of lignocellulose materials and wherein effective control is obtainable as the yield and composition of the resultant pulp.
- a widening reaction zone develops, bounded on one end by the outer dimensions of the original chip, at the other end by the moving reaction interface.
- the lignin content of the chip ice is, of course, that of the original wood.
- the lignin content of the material is much lower, being determined by the time of contact, temperature and chemical concentration.
- This moving reaction interface theory is the basis for my invention. I have discovered that wood chips can be specially tailored, dimension-wise, to most efliciently meet the conditions set up by this moving interface. This socalled tailoring consists of, first, presenting the maximum possible wood surface to the initial reacting interface, where liquor comes in contact with the unreacted chip. Second, the chip is so designed that the distance which this reacting interface must travel to reach the center of the chip is reduced to a minimum.
- My invention comprises altering the chip dimensions by taking advantage of the physical weakness-of the chip caused by the grain of the wood, then adjusting the pulping conditions to fit the new chip dimensions to produce a pulp of maximum yield and quality.
- a comparatively small force is required to break a chip if the break takes place in the grain direction. This force is variable, being at a maximum with dry wood, decreasing as the chip moisture increases and reaching a minimum when the lignin, the cementing material, is softened by application of heat. Since the cellulose fibers lie in the grain direction, none of these fibers are torn by the break. Much greater force is required to cause a break across the grain and such a break will tear a high percentage of the fibers located at or near the line of breakage.
- my invention I carry out this breaking or shredding of chips in the grain direction to as small a cross-section, across the grain, as possible. However, if cross-section is reduced excessively, the chip fragment becomes so weak, physically, that cross-grain breakage takes place and mechanical fiber damage occurs.
- the aim of my invention is to carry out this breaking or splitting of the chips along the grain, maintaining the same length of the split fragments as was present in the original whole chips which are ordinarily at least about inch in length.
- 2,716,926, or other devices which will provide sufficient impact to split the chips along the grain can be used to carry outthis shredding operation.
- the size of the openings in the discharge screen through which the product falls is critical. Too small an opening increases fines, while too large an opening will produce insufiicient splitting. I have used /2 inch expanded metal successfully for such a discharge screen in hammer milling. In attrition mill, toothed rather than bar type plates should be used. In this type mill, the clearance between plates and feed rate of chips are the controlling features. For any specific disc speed and chip feed rate, there is one specific clearance which will produce the optimum size range of chip cross-section.
- This shredding operation which greatly increases wood surface and decreases the distance from the surface to the chip center, is essential to high speed, continuous pulping, which invariably involves substantially constant temperature and elimination of the warm-up period. I have found that it is also definitely beneficial in the slower, batch pulping where a warm-up period is used.
- the yields of screened pulp amounted to 40.0% for the chips from dull knives, 45% for the chips from sharp knives and 48.6% from the shredded chips.
- the screened yield from the shredded chips would have been even higher if a shorter cooking time had been used but could not be improved for the full-size chips.
- This example shows how much damage can be caused, through the dissolving of cellulose fibers, by too wide a range of chip crosssections in the same digester.
- the method used in screening shredded chips to separate them into their various cross-sectional dimensions is quite critical.
- the material must pass endwise through the screen if the screen is to be used as a measure of crosssection rather than length. Therefore, a Rotap sifter, or some similar device, must be used which will provide a bouncing as well as a shaking action so that the chips will pass endwise through the screen.
- the usual reciprocating sifter is not satisfactory, since it separates chips primarily by length along the grain.
- Chips obtained from logs will have an average moisture content within the above specified range so long as they are not subjected to special drying or presteaming procedures. Such chips are hereinafter referred to as green chips.
- the amount of surface opened up by the shredding operation is not as great as when the chips are steamed before shredding because the chips are not nearly as soft and flexible. Consequently, the ends of the shredded fragments do not broom out to expose greater surface, as do the steamed chips. Furthermore, it is notpossible to obtain the extremely slender sections, as long, as the original chips, always found in the shredded mixture from steamed chips.
- the screening after shredding and recycling of oversize can be eliminated.
- the shredding operation alone will produce processed chips considerably more uniform than the chips coming directly from the chipper and an improvement in yield and quality will result.
- screening-out and recycling of oversize should be practiced.
- My invention therefore, relates to a process which consists of subdividing green chips of fiber-bearing materials having a moisture content of from about 20% to about 50% to produce a shredded product consisting of three factions, the first (1) fraction comprising a substantial proportion, usually at least 50% by Weight or more of the total shredded product and the particles of which have at least one transverse (cross-grain) dimension of at least about 1.65 mm. and no transverse dimension greater than about 6.7 mm. the second (2) fraction comprising not more than about 5% by weight of the total shredded product and the particles of which have no transverse dimension in excess of about 1.65 mm.
- the third (3) fraction comprising at least 25% by Weight of the total shredded product and the particles of which have a transverse dimension in excess of about 6.7 mm., the lengthwise dimensions along the grain of the chips being substantially the same as the original chips.
- the particles of the (1) fraction will pass endwise through 21 Tyler Standard 3 mesh screen and will be retained on a Tyler Standard mesh screen, the (2) fraction will pass endwise through Tyler Standard 10 mesh screen and the (3) fraction will not pass endwise through a Tyler Standard 3 mesh screen.
- the shredded product preferably will then be screened to separate the particles whose transverse dimensions are in excess of 6.7 mm. However, if a lower quality product is desired, this latter screening step need not be performed.
- shredded product as used in the claims shall include either a product from which particles whose transverse dimensions are in excess of 6.7 mm. have not been removed or a product from which such particles have been removed.
- the shredded product is then digested by applying a digesting liquor of the alkaline, neutral sulfite or acid bisulfi-te type thereto and heating the shredded product and the digesting liquor to the digesting temperature as quickly as possible and holding the mixture at the digesting temperature for the period of time required to produce a pulp of the desired characteristics.
- the shredding of the chips and the subsequent digestion thereof under the conditions described hereinafter have been found to result in a higher screened yield of pulp with a shorter digestion time and the pulp has a higher degree of polymerization number, indicating better quality, than is possible with mill size chips, that is, chips passing through a screen having openings 1.0 x 2.0 inches in size.
- mill size chips that is, chips passing through a screen having openings 1.0 x 2.0 inches in size.
- the use of shredded chips provides a more uniformly softened pulp which can be fibrated with less expense than pulp formed from mill size chips. Further, the pulp from shredded chips is much brighter.
- Hardwoods and conifers can be simultaneously digested successfully in. the same digester.
- the conifer chips should be shredded to relatively small cross sections While hardwood chips should be shredded to relatively larger cross sections
- the degree of shredding will depend on the particular species of woodinvolved. The shredding is selected to compensate for the difference in the normal rate of pulping of the species involved.
- Degree of polymerization is a measure of the number of cell obiose groups in the cellulose molecule and is calculated from viscosity measurements as prescribed in TAPPI Standard No. T-230. It is generally considered to be a measure of pulp quality, the higher the number the better the quality. In the following description it is abbreviated as D.P.
- the shredded chips whose cross-grain dimensions are substantially within the range of between 1.65 and 6.7 mm., are digested with a liquor consisting essentially of sodium hydroxide alone or in combination with sodium sulphide.
- the concentration of the cooking liquor is from 20 to 55 grams per liter measured as Na O.
- the sulphidity ranges from 0 to
- the maximum temperature is between about 170 and 180 C.
- the contents of the digester are heated to maximum temperature in from 30 to 120 minutes and the contents of the digester are maintained at the maximum temperature for from 10 to 60 minutes.
- the digestion operation is then terminated by blowing the digester.
- the screened yield of pulp from a digesting operation of the type above described will normally be between about and about 52% by weight of the original wood.
- A. high yield digesting operation may be performed under the same conditions as described above except that the contents of the digester are maintained at the maximum temperature for a period of 0 to 45 minutes.
- the pulp after being discharged from the digester is then fibrated in an attrition mill or similar device.
- the total yield will normally be between about and about 65% by weight of the original wood.
- Example I Shredded slash pine chip of 4 +8 mesh size in crossgrain direction were digested in a liquor whose starting concentration was 50 g.p.l. as Na O with a sulphidity of 25%. The time to raise the contents of the digester to maximum temperature was minutes and the maximum temperature was 175 C. The liquor-to-wood ratio was 3.4: 1. The time at maximum temperature was 35 minutes. The screened yield was 47.5% of original wood and the total yield was 47.6%. The percent lignin in the pulp was 8.0% and the D.P. of the pulp was 1718.
- Mill-size chips were subjected to the same digestion conditions. The results were: screened yield 36.6%, total yield 51.9%, percent lignin in pulp 9.1 D.P. of pulp 1753.
- a further series of digesting operations for both shredded and mill size chips was conducted under the same conditions except that the times. at maximum temperature were varied from 5 to minutes for mill-size chips and from 5 to 35 minutes for shredded chips.
- a maximum screened yield of 48.2% for shredded chips was achieved at 25 minutes at maximum temperature.
- the D.P. of this pulp was 1837.
- the maximum screened yield of the mill-size chips was 40% realized at 65 minutes at maximumtemperature- The D.P. of this pulp was 1610.
- chips and liquor are fed into one end of a pressure vessel by one of several methods such as by using high compression screws, compartmented feeder valves and the like.
- the mixture is conducted through the length of the pressure vessel which is held at a constant high pressure and temperature.
- the mixture of reacted materials is discharged at the other end of the vessel through any suitable type of pressure relieving device.
- a continuous processfor digesting green shredded chips by the kraft or soda processes to produce a paper making pulp includes continuously forwarding chips whose cross-grain dimensions are substantially within the range of between 1.65 and 6.7 mm. through a digester and contacting same with a cooking liquor consisting essentially of sodium hydroxide alone or in combination with sodium sulphide.
- the concentradoubt the cooking liquor is from 20 to 55 grams per liter measured as Na O.
- the concentration of the liquor may be allowed to fall during the digestion operation or it may be maintained substantially constant, such as by adding extra liquor to the digester.
- the sulphidity of the cooking liquor ranges from to 35%.
- the contents of the digester are continuously maintained at a temperature within the range of 175 to 190 C. for a period of time ranging from 10 to 75 minutes, following which they are discharged therefrom.
- the liquor-to-wood ratio may vary between about 3.021 and about 10.0: 1. In general, the lower the liquorto-wood ratio, the higher the concentration and the lower the digesting temperature and vice versa. Thus, if the liquor-to-wood ratio is 3.0:1, the concentration should be about 50 g.p.l. as Na O and the digesting temperature should be 175 to 178 C. If the liquor-to-wood ratio is 10.0:1, the concentration can be about 20 g.p.l., as Na o and the digesting temperaturecan be about 190 C. The screened yield of pulp from this digesting operation will normally be between 45% and 52% of the original wood.
- a high yield continuous process for papermaking pulp involves the same steps as just described except that the shredded chips are maintained at the digesting temperature for a time period of from to 50 minutes and after being discharged are mechanically fioi'ated in an attrition mill or similar device.
- a continuous process for digesting shredded chips to produce a dissolving pulp containing less than 3% pentosan for making rayon, etc. involves contacting shredded chips of the size specified above with a kraft or soda cooking liquor having a concentration of 70 to 90 grams per liter measured as Na;,,() and a sulphidity of from 0 to 35%.
- the chips are maintained at a constant temperature ranging from 162 to 178 C., and are retained in the digester for a time period of from 5 to 40 minutes.
- the screened yield of pulp will be in the range of 38% to 48% of the original wood.
- the same kraft or soda cooking liquor may be used in two successive continuous digesting operations to produce from the first digesting operation a dissolving pulp and to produce from the second digestingoperation a paper-making pulp.
- shredded green chips of the size specified above are digested with a kraft or soda cooking liquor whose initial concentration is 70-90 grams per liter measured as Na O and which has a sulphidity of from O to 35%.
- the cooking temperature is con stant at between 162 and 178 C. and the cooking time is from 5 to 40 minutes.
- the liquor is expressed or drained from the pulp exiting from the first digestion operation and its concentration is then adjusted so that it contains from 20 to 55 grams per liter measured as Na O.
- the first digestion operation usually does not consume suificient of the chemicals to reduce the concentration to this value, adjustment of the concentration is effected by dilution.
- additional chemicals may be added thereto to bring it to the desired concentration.
- the liquor at a concentration of 20 to 55 grams per liter measured as Na O and a sulphidity of 0' to 35%, is then utilized to digest other shredded green chips of the size specified above in a second continuous digestion operation to produce a papermaking grade of pulp.
- the digestion temperature for the second digesting operation is constant at between 170 and 190 C. and the cooking time is to 75 minutes.
- Example 11 Shredded slash pine chips of -4 +8 mesh size in cross-grain direction were continuously digested utilizing a liquor whose initial concentration was 35 g.p.l. as Na O with a sulphidity of 25 The temperature was main- 10 tained constant at 185 C. The digesting time was 20 minutes. The results were: screened yield 45.8%, total yield 49.1%, percent lignin in pulp 10.0%, D1. of pulp 1634.
- Mill-size chips were subjected to identical digestion conditions. The results were: screened yield 182%, total yield 62.4%, percent lignin in pulp 11.5%, DP. of pulp 1703.
- a further series of digesting operations for both shredded and mill-size chips was conducted under the same conditions except that the digesting times were varied from 10 to 45 minutes for mill-size chips and from 10 to minutes for shredded chips.
- the maximum screened yield for shredded chips was 46.5% at 18 min utes cooking time and a DR of 1650.
- the maximum screened yield for mill size chips was about at a cooking time of about minutes and the DI. for this pulp was 1450.
- shredding the chips increased screened yield, decreased cooking time and improved the quality of the pulp.
- Example III Shredded slash pine chips of 4 +8 mesh size were continuously digested while maintaining the concentration of the cooking liquor substantially constant. The conditions were: concentration of liquor 20 g.p.l. as Na O; sulphidity 25%; temperature 190 C.; time 28 minutes. The results were: screened yield 42.5%; total yield 43.3%; percent lignin in pulp 7.8%, DR of pulp 1493.
- Mill-size chips were subjected to the same digestion conditions. The results were: screened yield 23.3%, total yield 58.3%; percent lignin in pulp 9.2%, DR of pulp 1614.
- a further series of continuous, constant concentration, digesting operations were carried out for shredded and mill-size chips under the same conditions except that the digestion time was varied from 15 to 90 minutes for millsize chips and was varied from 12 to 35 minutes for shredded chips.
- the maximum screened yield was about at 20 minutes cooking time, and the pulp had a DP. of about 1600.
- the maximum screened yield was about 36%, at about minutes cooking time and the pulp had a DR of about 1020.
- the cooking chemical is a mixture of sulphurous acid and a bisulphite salt of sodium, ammonium, calcium, or magnesium.
- Ammonia base was selected for the purpose of the following examples, instead of sodium, calcium or magnesium, because it is less corrosive and is less subject to decomposition at high temperature than the other salts.
- the invention includes within its scope any of the above-mentioned bisulphite salts.
- Combined S0 is defined as that amount of S0 combined with the base ammonium as bisulphite but calculated as though it were ammonium sulphite. It is only half of the S0 which would be necessary to form ammonium bisulphite with all of the ammonia present.
- the free S0 is all of the S0 present as sulphurous acid plus half of the S0 which is present as ammonium bisulphite.
- Total S0 is the sum of free and combined S0 BATCH OPERATION
- shredded chips Whose cross-grain dimensions are substantially within the range of between 1.65 and 6.7 mm, are digested with a liquor containing from 4.0% to 6.0% total S0 and 0.8% to 1.6% combined S0 (based on the weight of the liquor).
- the maximum digestion temperature is between about 148 ill and 165 C.
- the contents of the digester are heated to 1 maximum temperature in from 30 to 120 minutesand the contents of the digester are maintained at the maximum temperature for from 30 to 150 minutes.
- the screened yield of pulp from such a digesting operation will normally be between 45% and 52% of the original wood.
- a high yield digesting operation may be performed under the same conditions as described above except that the contents of the digester are maintained at the maximum temperature for a period of from 10 to 100 minutes.
- the pulp after being discharged from the digester is then fibrated in an attrition mill or smililar device- In this type of operation, the total yield will normally be between about 50% and about 70% of the original wood.
- Example IV pulp was 1899.
- Mill-size chips were subjected to the same digesting conditions except that the time at maximum temperature was 135 minutes. The results were: screened yield 39.4%, total yield 52.4%, percent lignin in pulp 5.7% and DR of pulp 1850.
- a further series of digesting operations for both shredded and mill-size chips was conducted under the same, conditions except that the digesting times were varied from to 120 minutes for shredded chips and from 0 to 180 minutes for mill-size chips.
- the maximum screened yield for shredded chips was about 50.6% at 120 minutes cooking time and the pulp had a D.P. of 1899.
- the maximum screened yield for mill-size chips was about 42% at 180 minutes cooking time and the pulp had a DR of 1659.
- a continuous process for digesting shredded chips by the acid bisulphite process includes continuously forwarding chipswhose cross-grain dimensions are substantially within the range of 1.65 and 6.7 mm. through a digester and contacting same with a cooking liquor whose concentration is from 4.0% to .60% total S0 and 0.8% to 1.6% combined S0
- the digesting temperature is constant within the range of between 148 and 165 C.
- the digesting time is between 45 and 120 minutes; The screened yield of pulp from this digestion operation will normally be between 42% and 50% of the original wood.
- a high yield continuous process involves the same steps as just described except that the shredded chips are maintained at the digesting temperature for a time period of from to 100 minutes and, after being discharged, are mechanically fibrated in'an attrition mill or a similar device.
- Example V Shredded spruce chips of 4 +8 mesh size in crossgrain direction were digested in a liquor whose starting concentration was 4.4% total S0 and 1.2% combined S0 The temperature was maintained constant at 148 C. The digesting time was 120 minutes. The results were: Screened yield 44.3%, total yield 51.2%, percent lignin in pulp 6.2%; DR of the pulp was 1682.
- Example VI Shredded spruce chips of -4 "+8 mesh size were pretreated by boiling same for 10 minutes and then cooling same in a bisulphite liquor whose concentration was 2.3% total S0 and 1.2% combined S0 The chips were then subjected to the same digesting conditions as described in Example V except that the digesting liquor has 4.6% total S0 The results were: screened yield 50%; total yield 50.9%; percent lignin in pulp 7.5%; DR of the pulp was 1740.
- the concentration of this preimpregnating solution may lie between 1.6% and 6.0% total S0 0.8% and 3.0% combined 50;.
- the shredded chips are treated by placing same in the solution while it is boiling for a short period of time such as 10 minutes, cooling rapidly to about 50 to C. and then draining the excess liquor. Vacuum impregnation and impregnation by soaking of the chips for several hours is also suitable.
- the pretreatment of the chips with the bisulphite salt will result in a substantial decrease in cooking time and, at the higher yields, more uniformly soften chips.
- the maximum digesting temperature is between about 165 and 178 C.
- the contents of the digester are brought to maximum temperature in from 30 to 90 minutes and are maintained at the maximum temperature for a period ranging from 100 to 240 minutes.
- the screened yield of a pulp from such a digesting operation will normally range from 62% to 78% of the original wood.
- the pulp, after being discharged from the digester, is then fibrated in an attrition mill or similar device.
- a continuous process for digesting shredded chips by the neutral sulphite semi-chemical process includes continuously forwarding the chips whose cross-grain dimensions are substantially within the range of 1.65 to 6.7 mm, through a digester and contacting same with a cooking liquor consisting essentially of sodium sulphite and sodium carbonate.
- the concentration or" the cooking liquor is from 20 to 75 grams Na O per liter of which from 60% to 80% is present as sodium sulphite and the remainder as sodium carbonate.
- the contents of the dig-es ter are continuously maintained at a temperature of between 185 and 200 C. for a period of 20 to 90 minutes following which the pulp is discharged therefrom.
- the pulp is then fibrated by passin same through an attrition mill or similar device.
- the total yield of the pulp normally ranges from between 62% and 78% of the original wood.
- a pretreatment of the shredded chips with cooking liquor before same are fed to the digester will bring about a reduction in the cooking time.
- Example VII Shredded eucalyptus chips of 4 +8 mesh size in cross-grain direction were continuously digested in a liquor whose concentration was 12.5% (Na O), 4 mols Na SO per mol Na CO The liquor-to-wood ratio was 7: 1. At a constant temperature of 193 C. and a cooking time of 45 minutes, the total yield was 71.3% and GE. brightness of the pulp was 37. Mill-size chips cooked under identical conditionsresulted in the same yield but With'a G.E. brightness of 20.6. The shredded chips, after cooking, were soft throughout while the mill-size chips had hard, dark centers.
- Shredded eucalyptus chips were cooked under the same conditions as in the preceding example except that they were pretreated with cooking liquor before being cooked, the pretreating consisting in submerging the chips in boiling liquor for 10 minutes, cooling the chips and the liquor to 140 F. while the chips are submerged and then draining the chips.
- the cooked chips after a cooking time of 45 minutes, had a total yield of 67.8% and a GE. brightness of 37.5.
- the cooked, pretreated chips were softer than the cooked mill-size chips.
- a process for converting chips of a cellulose fiberbearing material, such as wood, into a pulp product which consists of the steps:
- digesting the shredded product by applying thereto a digesting liquor and heating the particles and the digesting liquor to the digesting temperature as quickly as possible and holding the mixture at the digesting temperature for the period of time required to produce a pulp of the desired characteristics.
- a process for digesting a cellulose fiber-bearing material, such as Wood, with digesting chemicals to produce a pulp product including the steps:
- a process for digesting a cellulose fiber-bearing material, such as wood, with a cooking liquor to produce a pulp for paper-making purposes including the steps:
- the dimension of the chips being substantially the same and no transverse dimension greater than about 6.7; as the original chips; '10 mm., (2) not more than about 5% have no transverse cooking the shredded product in a liquor consisting esdimensions in excess of about 1.65 mm., and (3) at sentially of sodium hydroxide alone or, in combinaleast 25% have at-least one transverse dimension in tion with sodium sulphide, the liquor containing excess of about 6.7 mm., the lengthwise dimensions from 20 to 55 grams as Na O per liter and having of the chips being substantially the sameas the origia sulphidity ranging from 0 to 35%, allowing from nal chips; 30 to 120 minutes for particles and liquor to reach continuously cooking the shredded product in a liquor a maximum temperature in a range between 170 consisting essentially of sodium hydroxide alone or and 180 C., then cooking at this constant temperain combination with sodium sulphide at a constant ture for 10 to 60 minutes.
- a process for digesting cellulose fiber-bearing mateing a moisture content of from about 20% to about rial, such as wood chips, with a cooking liquor to produce a pulp for papermaking purposes including the steps:
- a shredded product consisting of particles of (2) not more than about 5% have no transverse which (1) a substantial proportion have at least one imensions in excess of about 1.65 mm., and (3) transverse dimension in excess of about 1.65 mm.
- At least 25% have at least one transverse dimension and no transverse dimension greater than about 6.7 in excess of about 6.7 mm., the lengthwise dimenmm., (2) not more than about-5% have no transsions of the chips being substantially the same as verse dimensions in excess of about 1.65 mm., and the original chips; (3) at least 25% have at least one transverse dimencooking the shredded product in a liquor consisting sion inv excess of about 6.7 mm., the lengthwise diessentially of sodium hydroxide alone or in commensious of the chips being substantially the same bination with sodium sulphide, the liquor containing as the original chips; from '20 to 55 grams as Na O per liter and having 40 continuously cooking the shredded product in a liquor a sulphidity ranging from 0 to 35%, allowing from consisting essentially of sodium hydroxide alone or 30 to 120 minutes for chips and liquor to reach a in combination with'sodium sulphide at a constant maximum temperature in a range between 170 and temperature, the liquor
- a process for digesting a cellulose fiber-bearing ma- 175 to 190 C. for a period of from 5 t minutes. terial, such as wood, with a cooking liquor to produce andthen mechanically fibrating the partially cooked a pulp for papermaking purposes including the steps: 'PaTticlfiS subdividing green chips of fiber-bearing materials hav- 50
- P Ongma C 9 (2) not more than about 5% have no transverse dicontinuously cooking the shredded product in a liquor mansions in excass of about L mm and (3) at consisting essentially Sodium hydroxidfi alone or least 25 have at least one transverse dimension in in Combination With Sodium sulphide at a constant 65 excess of about 6.7 mm., the lengthwise dimensions temperature, the liquor containing from 20 to 55 of'thechips being substantially the same as the origigrams as Na O per liter and having a sulphidity nal chips;
- the chips and liquor being cooking the shredded product in a liquor consisting maintained at a constant temperature ranging from essentially of sodium hydroxide alone or in combina- 175 to 190 C. for a period of from 10 to tion with sodium sulphide at constant temperature,
- the liquor containing from 70 to grams Na O per 7.
- a sulphidity of to 35% cooking other subdivided continuously cooking the shredded product in an acid chips of the above-mentioned size in the liquor at a bisulphite liquor containing firom 4.0% to 6.0% total constant temperature ranging between 170 and 190 S0 and 0.8% to 1.6% combined S0 the basic ion C. for a period of from to 75 minutes to produce used to form the bisulphite being selected from the a papermaking pulp. group consisting of sodium, calcium, magnesium or 10.
- a process for digesting cellulose fiber-bearing material, such as wood chips, with a cooking liquor to produce a pulp for papermaking or dissolving purposes including the steps:
- terial such as wood chips
- cooking liquor to produce a pulp for papermaking or dissolving purposes, including the steps:
- a process for digesting cellulose fiber-bearing maphite liquor containing 4.0% to 6.0% total S0 and terial, such as wood chips, with a cooking liquor to pro- 0.8% to 1.6% combined 50, the basic ion used Jerusalem a plant
- the basic ion used Jerusalem a plant
- the bisulphite being selected from the group subdividing green chips of fiber bearing materials havconsisting of sodium, calcium, magnesium or ammonium, the particles being maintained at a constant temperature in the range of between 148 and 165 C. for a period between and 120 minutes.
- a process for digesting cellulose fiber-bearing material, such as wood chips, with a cooking liquor to produce a pulp for papermaking purposes including the steps:
- a process for digesting cellulose fiber-bearing macontinuously cooking the shredded product in an acid bisulphite liquor containing from 4.0% to 6.0% total S0 and 0.8% to 1.6% combined S0 the basic terial, such as wood chips, with a cooking liquor to produce a pulp for papermaking or dissolving purposes, including the steps:
- the ion used to form the bisulphite being selected from the group consisting of sodium, calcium, magnesium or ammonium, the chips and liquor being maintained at a constant temperature in the range of 148 to 165 C. for a period bet-ween 20 and minutes and then mechanically fibrating the cooked pulp to reduce partially cooked particles to fiber.
- a process for digesting cellulose fiber-bearing material, such as wood chips, with a cooking liquor to produce a pulp for papermaking purposes including the steps:
- terial such'as wood chips with a cooking liquor to produce a pulp for papermaking purposes, including the steps: subdividing green chips of fiber-bearing materials havcontinuously cooking the shredded product in a neutral sulphite liquor containing 20 to 75 grams as N3 0 per liter, of which 60% to 80% is present as sodium suiphite, the remainder as sodium carbonate, the
- chips and liquor being held at a constant temperature ranging between 185 and 200 C. for a period between 20 and 90 minutes, then mechanically fibrating the cooked particles to reduce partially cooked particles to fiber.
- a process for digesting cellulose fiber-bearing material, such as wood chips, with a cooking liquor to produce a pulp for papermaking purposes including the steps:
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Description
United States Patent 3,192,102 PULPING PRQCESS William J. Nolan, 1029 NE. 23rd Blvd, Gainesville, Fla.
No Drawing. Filed Aug. 15, 1962, Ser. No. 216,969 The portion of the term of the patent subsequent to Sept. 15, 1976, has been disclaimed 19 Claims. (Cl. 16224) This application is a continuation-in-part of my application Serial No. 852,978, filed November 16, 1959, which in turn is a continuation-in-part of my application Serial No. 578,378, filed April 16, 1956, both now abandoned.
This invention relates to a process of treating cellulose fiber-bearing materials and, more particularly, relates to an improved process of removing the non-cellulosic material therefrom by the use of a digestion process for the manufacture of paper, cellulose for synthetic fibers, and the like. 7 It is a particular object of this invention to provide a method for producing papermaking pulps from wood or other cellulosic materials by a rapid continuous process, in which from about half to nearly all of the lignin is removed. i
A further object is the production of cellulosic pulps having a high alpha cellulose content and a low lignin and pentosan content, which is useful for the manufacture of rayon, cellophane and like products.
Another object of the invention is the modification of existing so-called batch processes so that reaction time may be shortened, resulting in increased yield and improved quality of the resultant pulp.
A further object of the invention is the provision of such a process that is readily adaptable for the processing of various types of lignocellulose materials and wherein effective control is obtainable as the yield and composition of the resultant pulp.
In the past it has been common practice in the pulping industry to allow extended periods of time (1.0-2.5 hrs. in alkaline pulping, 5.015.0 hours in acid sulphite pulping) for the cellulosic raw material and the reacting liquors to reach the maximum, or cooking, temperature and pressure. This practice has been followed because of the generally accepted but mistaken belief that it is necessary for the reacting chemical solutions to completely penetrate the wood chips, or other cellulosic material, before the temperature becomes high enough for the delignification reaction to take place. It was erroneously believed that this slow penetration period was necessary to prevent degradation and solution of the cellulose fibers While lignin was being removed.
I have found, through very extensive experimentation, that penetration of cooking liquor into wood chips or other cellulosic material does not occur before the pulping reactions take place. Rather, the reactions themselves penetrate'the material, delignifying the cellulose fibers as the react-ions move toward the centers of the chips. This penetrating reaction, or moving reaction interface, opens up tiny passages around the fibers, permitting diffusion of fresh chemical toward the reacting interface and diffusion of reaction products outward to the main body of cooking liquor. These diffusional operations are not movements of a liquid medium but, rather, are movements of ions and molecules within a liquid medium caused by differences in concentration gradient.
As this moving reaction interface moves toward the center of the wood chip, a widening reaction zone develops, bounded on one end by the outer dimensions of the original chip, at the other end by the moving reaction interface. There is a lignin gradient across this reaction zone. At the interface end, the lignin content of the chip ice is, of course, that of the original wood. At the outer end of this zone the lignin content of the material is much lower, being determined by the time of contact, temperature and chemical concentration.
This moving reaction interface theory is the basis for my invention. I have discovered that wood chips can be specially tailored, dimension-wise, to most efliciently meet the conditions set up by this moving interface. This socalled tailoring consists of, first, presenting the maximum possible wood surface to the initial reacting interface, where liquor comes in contact with the unreacted chip. Second, the chip is so designed that the distance which this reacting interface must travel to reach the center of the chip is reduced to a minimum.
Obviously, from a purely theoretical point of view, the most efiiciently tailored chip would consist of a chip made of only one whole fiber. This is impossible of accomplishment without damaging the cellulose fibers because of the very strong bond between fibers, set up by the cementing lignin. Such attempts to reduce the wood to its individual fibers, as described in Asplund Patent No. 2,388,592, Olfermanns Patent No. 2,164,040, Mason Patout No. 1,872,996, Walter Patent No. 2,454,532, Olsen Patent No. 1,979,341 and Australian Patent No. 12,149 (Asplund), cut and tear a high percentage of the cellulose fibers, resultin in reduced strength of the purified cellulose.
My invention comprises altering the chip dimensions by taking advantage of the physical weakness-of the chip caused by the grain of the wood, then adjusting the pulping conditions to fit the new chip dimensions to produce a pulp of maximum yield and quality. A comparatively small force is required to break a chip if the break takes place in the grain direction. This force is variable, being at a maximum with dry wood, decreasing as the chip moisture increases and reaching a minimum when the lignin, the cementing material, is softened by application of heat. Since the cellulose fibers lie in the grain direction, none of these fibers are torn by the break. Much greater force is required to cause a break across the grain and such a break will tear a high percentage of the fibers located at or near the line of breakage.
In my invention I carry out this breaking or shredding of chips in the grain direction to as small a cross-section, across the grain, as possible. However, if cross-section is reduced excessively, the chip fragment becomes so weak, physically, that cross-grain breakage takes place and mechanical fiber damage occurs. The aim of my invention is to carry out this breaking or splitting of the chips along the grain, maintaining the same length of the split fragments as was present in the original whole chips which are ordinarily at least about inch in length.
I have found that this shredding along the grain should be so adjusted that as much as possible of the shredded product will pass, end-wise, through a Tyler Standard 3 mesh screen and be retained on an 8 mesh screen. This indicates that the optimum range of cross-section dimen sion lies between 6.7 and 2.3 mm. Material slightly smaller in cross-section, passing 8 mesh but retained on 10 mesh (between 2.3 and 1.65 mm.) will suffer negligible cross-grain breakage and will cook to strong pulp. About 10-20% loss in tear strength has been found for the fraction between 10 and 16 mesh (1.65 to 0.99 mm). Shredded material below 0.99 mm. in cross-section suffers severe loss in tear strength when converted to pulp.
At the other extreme of size range, material larger in cross-section than 6.7 mm. will, of course, suffer no mechanical damage. However, with these larger crosssections, the path which the reaction must travel is so long that the smaller size ranges will be severely overcooked and suffer excessive chemical damage while the larger cross-sections are being cooked. In addition, in high speed, continuous pulping, these larger cross-sections will result in excessive degradation and even solution of'the outer cellulose fibers while the fibers near the chip centers are still being delignified. It can, therefore, be seen that both oversize and undersize should be kept at a minimum'for efficient cooking. I have found that hammer mills, attrition mills, such as that disclosed in Patent No. 2,716,926, or other devices which will provide sufficient impact to split the chips along the grain can be used to carry outthis shredding operation. When hammer mills are used, the size of the openings in the discharge screen through which the product falls is critical. Too small an opening increases fines, while too large an opening will produce insufiicient splitting. I have used /2 inch expanded metal successfully for such a discharge screen in hammer milling. In attrition mill, toothed rather than bar type plates should be used. In this type mill, the clearance between plates and feed rate of chips are the controlling features. For any specific disc speed and chip feed rate, there is one specific clearance which will produce the optimum size range of chip cross-section. Clearances larger than this value will result in an excessive percentage of oversize, while smaller clearance results in excessive fines and cross-grain breakage. Properly operated, either hammer mills or attrition mills should perform the shredding operation for an energy expenditure of less than 0.5 HP. days per O.D. ton of wood.
This shredding operation, which greatly increases wood surface and decreases the distance from the surface to the chip center, is essential to high speed, continuous pulping, which invariably involves substantially constant temperature and elimination of the warm-up period. I have found that it is also definitely beneficial in the slower, batch pulping where a warm-up period is used.
This application of reduction of chip cross section without decrease in chip length to the commonly practical batch pulping can be illustrated by the following example. A sample of chips was taken from a commercial kraft mill chipper whose knives were dull and, as a consequence, 33.5% of the chips resulting were large enough to be retained on a screen with in. square openings. Another sample was taken when the knives of the same chipper had been sharpened. In this chip sample, only 6.9% of the chips Were retained on the in. screen. Some of these latter chips were shredded by my process, resulting in a product, 90% of which had chip cross-sections varying between 1.65 and 6.65 mm. but whose length in the grain direction was the same as the original chips. Each of these samples was cooked by the kraft process, using identical conditions, including time. The yields of screened pulp amounted to 40.0% for the chips from dull knives, 45% for the chips from sharp knives and 48.6% from the shredded chips. The screened yield from the shredded chips would have been even higher if a shorter cooking time had been used but could not be improved for the full-size chips. This example shows how much damage can be caused, through the dissolving of cellulose fibers, by too wide a range of chip crosssections in the same digester.
This principle of chip shredding to achieve maximum surface, and minimum cross-section was first disclosed in my US. Patent No. 2,904,460, issued September 15, 1959. In this patent I disclosed a method for reducing the crosssection, across the grain, of dry chips which had been modified to avoid cross-grain breakage. In preliminary experiments I had found that the dry chips, untreated,.
were hard and brittle, offering considerable resistance to breaking along the grain. At the same time that the resistance to breaking along the grain was at a maximum, the resistanceto breaking across the grain was at a minimum because of this brittleness. As a result of this brittleness, a great deal of fiber damage was done when shredding was attempted. As an example, slash pine chips containing moisture were shredded in an attrition Percent onscreen. 0.4 21.2 19.4 11.3
The material smaller than 10 mesh, 30.7% of the total product, had suffered severe fiber damage. A part of the material between 10 and 16 mesh was broken into pieces very short in the grain direction. All of the 16 mesh fraction was either dust or very short, thin fragments.
However, when I steamed these dry, brittle chips for very short periods of time in the range of 170 p.s.i.g., the lignin cementing the fibers together became soft, resulting in very flexible chips which would separate easily along the grain. The shredded fragments were so flexible that they could be bent almost double before breaking. This flexible characteristic was retained as the chips cooled to room temperature, as long as they were not allowed to become dry.
Upon shredding these steamed chips in the same mill as just described for the dry chips, using the same clearance of 0.445 in., the following screen analysis of the product resultedzi Screenmesh 3 3 +4 -4 +8 8 +10 10 +16 16 Percent on screen. 7. 5 18. 7 50. 3 11.9 7. 5 4. 1
Upon close examination of the various screen fractions it was found that this analysis did not give the true size distribution of cross-sectional dimensions. The extreme flexibility of the fragments had left them entangled to such an extent that they interfered with each other, preventing passage through the proper screen. For example, hand sorting of the fractions disclosed that, of the material held on 3 mesh, only 12.5% was actually large enough in cross-section that it would not pass 6 mesh; 25% would go through 6 mesh but not through 8 mesh; 25.9% would pass through 8 mesh but not through 10 mesh; 36.6% would pass through 10 mesh. It can be seen, therefore, that screen analysis cannot provide a true picture of crosssectional size when the chips are softened by presteaming before shredding.
The method used in screening shredded chips to separate them into their various cross-sectional dimensions is quite critical. The material must pass endwise through the screen if the screen is to be used as a measure of crosssection rather than length. Therefore, a Rotap sifter, or some similar device, must be used which will provide a bouncing as well as a shaking action so that the chips will pass endwise through the screen. The usual reciprocating sifter is not satisfactory, since it separates chips primarily by length along the grain.
Subsequent to my disclosure in US. Patent 2,904,460, I have discovered that non-prestearned chips containing from about 20% to 50% by weight of moisture can be shredded reasonably well if proper precautions are taken. Chips obtained from logs will have an average moisture content within the above specified range so long as they are not subjected to special drying or presteaming procedures. Such chips are hereinafter referred to as green chips. The amount of surface opened up by the shredding operation is not as great as when the chips are steamed before shredding because the chips are not nearly as soft and flexible. Consequently, the ends of the shredded fragments do not broom out to expose greater surface, as do the steamed chips. Furthermore, it is notpossible to obtain the extremely slender sections, as long, as the original chips, always found in the shredded mixture from steamed chips.
However, the shredding of green chips, if it can be done Without excessive mechanical damage, offers two great advantages over the presteamed shredding. First, the presteaming operation is costly, probably almost as expensive as the cooking itself because the same type pressure vessel must be used. In this presteaming, part of the pentosan in the wood is reacted and removed by the steaming operation. Second, the bulky character'of the presteamed, shredded product, mentioned previously as a characteristic which prevents accurate screen analysis, will not permit the loading of nearly as much shredded chips in the digester as when conventional chips are used, causing serious curtailment in production. Green chips shredded without presteaming, on the other hand, have the same packing characteristics as conventional chips.
It is true that, in the shredding of green chips Without presteaming, the wood is much more subject to mechanical damage by cross-grain breakage than is the presteamed wood. It the shredding is carried out to the same degree, that is, to the point where practically all the shredded product will pass endwise through a 3 mesh screen, much more cross-grain breakage will occur with the green chips. Furthermore, the amount of this damage from shredding will increase as the chips dry out. It has been pointed out earlier that the chips become more brittle as they become dry. The following example shows how much more damage is done as chips become dry. The untreated chips were shredded, as in previous examples, in the attrition mill with a plate clearance of 0.445 in.
Considering the percentage of material passing mesh as a measure of fiber damage, 26.7% of the wood containing 45% moisture was damaged, either slightly or seriously, while the wood containing 10% moisture was damaged to the extent of 30.7%. In addition, an examination of the acceptably shredded fraction, that material passing 3 mesh and retained on 10 mesh, showed that the dry (10% moisture) material had also suifered some dam age. The long, slender pieces of the dry shreds showed damage along the surface parallel to the grain. This surface was rough, with indentations where tiny fragments had broken away, caused by impact on the brittle chips. Thus, even the acceptably shredded fraction of the dry chips suffered more fiber damage than the corresponding fraction of the moist chips.
A comparison of these data for the shredding of untreated chips with the similar data listed earlier for presteamed chips at the same attrition mill clearance of 0.445 in. shows that the fraction smaller than 10 mesh is extremely low for the presteamed chips, 11.6%. As stated earlier, even this 11.6% of material of very small crosssection has suffered very little cross-grain breakage because of its great flexibility.
It thus becomes apparent that untreated green chips, regardless of the amount of natural moisture they contain, cannot be successfully shredded to the extent that all of the shredded product will pass 3 mesh. So much crossgrain breakage occurs that more mechanical damage is done than the chemical damage which is avoided in the digester.
However, I have found that the property of the shredded untreated green chips to screen easily into screen fractions having sharply defined cross-sectional dimensions can be used to create a product in which most of the material will pass endwise through a 3 mesh screen but will not contain an excessive fraction smaller than 10 mesh. If
d the clearaiice of the attrition mill is increased, the shredded particles increase in cross-section and the fraction which is smaller in cross-section than 10 mesh becomes smaller. The following tabulation shows how these cross-sectional size ranges change with attrition mill clearance, using green chips containing 45% moisture.
P1 t Percentage held on each screen (based on original wood) a e clearance (in.) 3 -3 +4 4 +8 8 +10 -l0 +16 16 mesh mesh mesh mesh mesh mesh 0. 0 9. 7 is. s 18.0 16. 3 10. 4 22. 2 28. 3 36.0 6. 4 4. 5 2. 7 35. 6 27. 4 27. 8 5. 3 2. 8 1. 1
When the shredded products are passed over a 3 mesh screen, using a vibrating motion which will up-end the chips on the screen so that they pass endwise through the openings whereby the oversized particles are removed,
the analyses of the screened products become:
Percentage held of each screen (based only on particles -3 mesh size or smaller) Plate clearance mesh mesh mesh mesh mesh mesh The oversize material, amounting to 35.6% of the original wood in the case of 0.971 plate clearance, can be returned to the attrition mill, mixed with fresh chips for reshredding. This can be done economically since the cost of shredding is extremely low.
It can thus be seen that a wide range or" screen analyses can be attained in the shredded product, depending on how much fine, mechanically damaged material can be tolerated in the product. This process reguires the installation of adequate screening equipment in addition to the shredding equi ment. However, the total cost of operations will be much less than steaming the chips before shredding and a good control of cross-sectional size range can be obtained.
In some instances, especially in batch pulping, the screening after shredding and recycling of oversize can be eliminated. The shredding operation alone will produce processed chips considerably more uniform than the chips coming directly from the chipper and an improvement in yield and quality will result. However, if maximum improvement is to be realized, screening-out and recycling of oversize should be practiced.
The fundamental purpose of this chip shredding is to tailor the shape of the wood chips to best fit the kinetic laws of pulping which I have found to be true. As was pointed out earlier the ideal cross-sectional dimensions of the Wood for most efficient cooking by the alkaline, neutral or acid processes should consist of particles only about one fiber thick. Such pulping conditions as liquor concentration and temperature could be made quite severe without damaging the fibers because the time required to delignify a single fiber would be very short. Since the individual fibers could be removed from the cooking zone immediately after they have lost their protective covering of lignin, degradation and dissolution of cellulose could almost be eliminated.
However, the information just presented showed that about the best cross-sectional reduction without serious mechanical damage that can be attained on chips that have not been presteamed will lie in the size range between 1.65 and 6.7 mm. It is obvious that reduction to this size range will not result in delignification without at least some degradation and dissolution of cellulose. As long as the chip cross-sections are several fibers thick, the outer fiberwill be delignified and be vulnerable to degradation while the inner fibers are being delignified. What I have discovered is that tailoring the chips to this cross-section range of 1.65 to 6.7 mm., then adjusting such cooking conditions asliquor concentration, temperature and time to best fit this attainable range of chip cross sections, will result in improved yield and quality in batch pulping; will permit high speed, continuous pulping to produce pulps of good yield and quality, not attainable if this tailoring of chip cross-sections is not carried out.
My invention, therefore, relates to a process which consists of subdividing green chips of fiber-bearing materials having a moisture content of from about 20% to about 50% to produce a shredded product consisting of three factions, the first (1) fraction comprising a substantial proportion, usually at least 50% by Weight or more of the total shredded product and the particles of which have at least one transverse (cross-grain) dimension of at least about 1.65 mm. and no transverse dimension greater than about 6.7 mm. the second (2) fraction comprising not more than about 5% by weight of the total shredded product and the particles of which have no transverse dimension in excess of about 1.65 mm. and the third (3) fraction comprising at least 25% by Weight of the total shredded product and the particles of which have a transverse dimension in excess of about 6.7 mm., the lengthwise dimensions along the grain of the chips being substantially the same as the original chips. Stated different- 1y the particles of the (1) fraction will pass endwise through 21 Tyler Standard 3 mesh screen and will be retained on a Tyler Standard mesh screen, the (2) fraction will pass endwise through Tyler Standard 10 mesh screen and the (3) fraction will not pass endwise through a Tyler Standard 3 mesh screen. The shredded product preferably will then be screened to separate the particles whose transverse dimensions are in excess of 6.7 mm. However, if a lower quality product is desired, this latter screening step need not be performed. The term shredded product as used in the claims shall include either a product from which particles whose transverse dimensions are in excess of 6.7 mm. have not been removed or a product from which such particles have been removed. The shredded product is then digested by applying a digesting liquor of the alkaline, neutral sulfite or acid bisulfi-te type thereto and heating the shredded product and the digesting liquor to the digesting temperature as quickly as possible and holding the mixture at the digesting temperature for the period of time required to produce a pulp of the desired characteristics.
For soda, kraft and acid bisulphite digestion operations, the shredding of the chips and the subsequent digestion thereof under the conditions described hereinafter have been found to result in a higher screened yield of pulp with a shorter digestion time and the pulp has a higher degree of polymerization number, indicating better quality, than is possible with mill size chips, that is, chips passing through a screen having openings 1.0 x 2.0 inches in size. For neutral sulphite semichemical digestion operations, the use of shredded chips provides a more uniformly softened pulp which can be fibrated with less expense than pulp formed from mill size chips. Further, the pulp from shredded chips is much brighter.
Hardwoods and conifers can be simultaneously digested successfully in. the same digester. The conifer chips should be shredded to relatively small cross sections While hardwood chips should be shredded to relatively larger cross sections The degree of shredding will depend on the particular species of woodinvolved. The shredding is selected to compensate for the difference in the normal rate of pulping of the species involved.
Degree of polymerization is a measure of the number of cell obiose groups in the cellulose molecule and is calculated from viscosity measurements as prescribed in TAPPI Standard No. T-230. It is generally considered to be a measure of pulp quality, the higher the number the better the quality. In the following description it is abbreviated as D.P.
KRAFT OR SODA PROCESS :BA'DCH OPERATION In kraft or soda batch digestion operations, according to the invention, the shredded chips, whose cross-grain dimensions are substantially within the range of between 1.65 and 6.7 mm., are digested with a liquor consisting essentially of sodium hydroxide alone or in combination with sodium sulphide. The concentration of the cooking liquor is from 20 to 55 grams per liter measured as Na O. The sulphidity ranges from 0 to The maximum temperature is between about 170 and 180 C. The contents of the digester are heated to maximum temperature in from 30 to 120 minutes and the contents of the digester are maintained at the maximum temperature for from 10 to 60 minutes.
The digestion operation is then terminated by blowing the digester. The screened yield of pulp from a digesting operation of the type above described will normally be between about and about 52% by weight of the original wood.
A. high yield digesting operation may be performed under the same conditions as described above except that the contents of the digester are maintained at the maximum temperature for a period of 0 to 45 minutes. The pulp after being discharged from the digester is then fibrated in an attrition mill or similar device. In this type of operation, the total yield will normally be between about and about 65% by weight of the original wood.
Example I Shredded slash pine chip of 4 +8 mesh size in crossgrain direction were digested in a liquor whose starting concentration was 50 g.p.l. as Na O with a sulphidity of 25%. The time to raise the contents of the digester to maximum temperature was minutes and the maximum temperature was 175 C. The liquor-to-wood ratio was 3.4: 1. The time at maximum temperature was 35 minutes. The screened yield was 47.5% of original wood and the total yield was 47.6%. The percent lignin in the pulp was 8.0% and the D.P. of the pulp was 1718.
Mill-size chips were subjected to the same digestion conditions. The results were: screened yield 36.6%, total yield 51.9%, percent lignin in pulp 9.1 D.P. of pulp 1753.
A further series of digesting operations for both shredded and mill size chips was conducted under the same conditions except that the times. at maximum temperature were varied from 5 to minutes for mill-size chips and from 5 to 35 minutes for shredded chips. A maximum screened yield of 48.2% for shredded chips was achieved at 25 minutes at maximum temperature. The D.P. of this pulp was 1837. The maximum screened yield of the mill-size chips was 40% realized at 65 minutes at maximumtemperature- The D.P. of this pulp was 1610. Thus, shredding increased screened yield, decreased cooking time, and improved the quality of the ul p p CONTINUOUS OPERATION In continuouspulping operations, chips and liquor are fed into one end of a pressure vessel by one of several methods such as by using high compression screws, compartmented feeder valves and the like. The mixture is conducted through the length of the pressure vessel which is held at a constant high pressure and temperature. The mixture of reacted materials is discharged at the other end of the vessel through any suitable type of pressure relieving device.
A continuous processfor digesting green shredded chips by the kraft or soda processes to produce a paper making pulp, according to invention, includes continuously forwarding chips whose cross-grain dimensions are substantially within the range of between 1.65 and 6.7 mm. through a digester and contacting same with a cooking liquor consisting essentially of sodium hydroxide alone or in combination with sodium sulphide. The concentradoubt the cooking liquor is from 20 to 55 grams per liter measured as Na O. The concentration of the liquor may be allowed to fall during the digestion operation or it may be maintained substantially constant, such as by adding extra liquor to the digester. The sulphidity of the cooking liquor ranges from to 35%. The contents of the digester are continuously maintained at a temperature within the range of 175 to 190 C. for a period of time ranging from 10 to 75 minutes, following which they are discharged therefrom.
The liquor-to-wood ratio may vary between about 3.021 and about 10.0: 1. In general, the lower the liquorto-wood ratio, the higher the concentration and the lower the digesting temperature and vice versa. Thus, if the liquor-to-wood ratio is 3.0:1, the concentration should be about 50 g.p.l. as Na O and the digesting temperature should be 175 to 178 C. If the liquor-to-wood ratio is 10.0:1, the concentration can be about 20 g.p.l., as Na o and the digesting temperaturecan be about 190 C. The screened yield of pulp from this digesting operation will normally be between 45% and 52% of the original wood.
A high yield continuous process for papermaking pulp involves the same steps as just described except that the shredded chips are maintained at the digesting temperature for a time period of from to 50 minutes and after being discharged are mechanically fioi'ated in an attrition mill or similar device.
A continuous process for digesting shredded chips to produce a dissolving pulp containing less than 3% pentosan for making rayon, etc., involves contacting shredded chips of the size specified above with a kraft or soda cooking liquor having a concentration of 70 to 90 grams per liter measured as Na;,,() and a sulphidity of from 0 to 35%. The chips are maintained at a constant temperature ranging from 162 to 178 C., and are retained in the digester for a time period of from 5 to 40 minutes. The screened yield of pulp will be in the range of 38% to 48% of the original wood.
The same kraft or soda cooking liquor may be used in two successive continuous digesting operations to produce from the first digesting operation a dissolving pulp and to produce from the second digestingoperation a paper-making pulp. According to such a procedure, in the first digestion operation shredded green chips of the size specified above are digested with a kraft or soda cooking liquor whose initial concentration is 70-90 grams per liter measured as Na O and which has a sulphidity of from O to 35%. The cooking temperature is con stant at between 162 and 178 C. and the cooking time is from 5 to 40 minutes. The liquor is expressed or drained from the pulp exiting from the first digestion operation and its concentration is then adjusted so that it contains from 20 to 55 grams per liter measured as Na O. Ordinarily, since the first digestion operation usually does not consume suificient of the chemicals to reduce the concentration to this value, adjustment of the concentration is effected by dilution. However, it will be understood that if the liquor after the first digestion operation is below the desired concentration, additional chemicals may be added thereto to bring it to the desired concentration. The liquor, at a concentration of 20 to 55 grams per liter measured as Na O and a sulphidity of 0' to 35%, is then utilized to digest other shredded green chips of the size specified above in a second continuous digestion operation to produce a papermaking grade of pulp. The digestion temperature for the second digesting operation is constant at between 170 and 190 C. and the cooking time is to 75 minutes.
Example 11 Shredded slash pine chips of -4 +8 mesh size in cross-grain direction were continuously digested utilizing a liquor whose initial concentration was 35 g.p.l. as Na O with a sulphidity of 25 The temperature was main- 10 tained constant at 185 C. The digesting time was 20 minutes. The results were: screened yield 45.8%, total yield 49.1%, percent lignin in pulp 10.0%, D1. of pulp 1634.
Mill-size chips were subjected to identical digestion conditions. The results were: screened yield 182%, total yield 62.4%, percent lignin in pulp 11.5%, DP. of pulp 1703.
A further series of digesting operations for both shredded and mill-size chips was conducted under the same conditions except that the digesting times were varied from 10 to 45 minutes for mill-size chips and from 10 to minutes for shredded chips. The maximum screened yield for shredded chips was 46.5% at 18 min utes cooking time and a DR of 1650. The maximum screened yield for mill size chips was about at a cooking time of about minutes and the DI. for this pulp was 1450. Again, shredding the chips increased screened yield, decreased cooking time and improved the quality of the pulp.
Example III Shredded slash pine chips of 4 +8 mesh size were continuously digested while maintaining the concentration of the cooking liquor substantially constant. The conditions were: concentration of liquor 20 g.p.l. as Na O; sulphidity 25%; temperature 190 C.; time 28 minutes. The results were: screened yield 42.5%; total yield 43.3%; percent lignin in pulp 7.8%, DR of pulp 1493.
Mill-size chips were subjected to the same digestion conditions. The results were: screened yield 23.3%, total yield 58.3%; percent lignin in pulp 9.2%, DR of pulp 1614.
A further series of continuous, constant concentration, digesting operations were carried out for shredded and mill-size chips under the same conditions except that the digestion time was varied from 15 to 90 minutes for millsize chips and was varied from 12 to 35 minutes for shredded chips. For shredded chips, the maximum screened yield was about at 20 minutes cooking time, and the pulp had a DP. of about 1600. For millsize chips the maximum screened yield was about 36%, at about minutes cooking time and the pulp had a DR of about 1020.
ACID BISUIJPH ITE PROCESS In acid bisulphite digestion operations, the cooking chemical is a mixture of sulphurous acid and a bisulphite salt of sodium, ammonium, calcium, or magnesium. Ammonia base was selected for the purpose of the following examples, instead of sodium, calcium or magnesium, because it is less corrosive and is less subject to decomposition at high temperature than the other salts.
However, the invention includes within its scope any of the above-mentioned bisulphite salts.
The nomenclature utilized in the following examples, namely, total, free and combined S0 follows the accepted terms of the sulphite pulping literature. Combined S0 is defined as that amount of S0 combined with the base ammonium as bisulphite but calculated as though it were ammonium sulphite. It is only half of the S0 which would be necessary to form ammonium bisulphite with all of the ammonia present. The free S0 is all of the S0 present as sulphurous acid plus half of the S0 which is present as ammonium bisulphite. Total S0 is the sum of free and combined S0 BATCH OPERATION In batch digesting operations according to the acid bisulphite process, shredded chips, Whose cross-grain dimensions are substantially within the range of between 1.65 and 6.7 mm, are digested with a liquor containing from 4.0% to 6.0% total S0 and 0.8% to 1.6% combined S0 (based on the weight of the liquor). The maximum digestion temperature is between about 148 ill and 165 C. The contents of the digester are heated to 1 maximum temperature in from 30 to 120 minutesand the contents of the digester are maintained at the maximum temperature for from 30 to 150 minutes. The screened yield of pulp from such a digesting operation will normally be between 45% and 52% of the original wood.
A high yield digesting operation may be performed under the same conditions as described above except that the contents of the digester are maintained at the maximum temperature for a period of from 10 to 100 minutes. The pulp after being discharged from the digester is then fibrated in an attrition mill or smililar device- In this type of operation, the total yield will normally be between about 50% and about 70% of the original wood.
Example IV pulp was 1899.
Mill-size chips were subjected to the same digesting conditions except that the time at maximum temperature was 135 minutes. The results were: screened yield 39.4%, total yield 52.4%, percent lignin in pulp 5.7% and DR of pulp 1850.
A further series of digesting operations for both shredded and mill-size chips was conducted under the same, conditions except that the digesting times were varied from to 120 minutes for shredded chips and from 0 to 180 minutes for mill-size chips. The maximum screened yield for shredded chips was about 50.6% at 120 minutes cooking time and the pulp had a D.P. of 1899. The maximum screened yield for mill-size chips was about 42% at 180 minutes cooking time and the pulp had a DR of 1659.
Two further series of digesting operations were performed for both shredded and mill-size chips in which the time to raise the material to the cooking temperature for both types of chips was, respectively, 360 minutes and 540 minutes. In each case, it was found that shredded chips achieved a higher screened yield more rapidly and the resultant pulp had a higher D.P. than did the mill-size chips.
CONTINUOUS OPERATION A continuous process for digesting shredded chips by the acid bisulphite process, according to the invention, includes continuously forwarding chipswhose cross-grain dimensions are substantially within the range of 1.65 and 6.7 mm. through a digester and contacting same with a cooking liquor whose concentration is from 4.0% to .60% total S0 and 0.8% to 1.6% combined S0 The digesting temperature is constant within the range of between 148 and 165 C. The digesting time is between 45 and 120 minutes; The screened yield of pulp from this digestion operation will normally be between 42% and 50% of the original wood.
It isbeneficial to preimpregnate the shredded chips with a dilutevbisulphite salt solution with no excess sulphurous acid. The concentration of this preimpregnation solution is between 0.8% and 1.6% combined S0 and 1.6% to 3.2% total S0 The shredded chips are treated by placing same in the solution while it is boiling for a short period of time, such as minutes, cooling rapidly to about 50 to 65 C. and then draining the excess liquor. Vacuum impregnation and soaking of the chips for several hours are also suitable. The pre treatment of the chips with the bisulphite salt will result 12 in a substantial increase in the screened yield of the pulp and also a slightly increased D.P.
A high yield continuous process involves the same steps as just described except that the shredded chips are maintained at the digesting temperature for a time period of from to 100 minutes and, after being discharged, are mechanically fibrated in'an attrition mill or a similar device.
Example V Shredded spruce chips of 4 +8 mesh size in crossgrain direction were digested in a liquor whose starting concentration was 4.4% total S0 and 1.2% combined S0 The temperature was maintained constant at 148 C. The digesting time was 120 minutes. The results were: Screened yield 44.3%, total yield 51.2%, percent lignin in pulp 6.2%; DR of the pulp was 1682.
Example VI Shredded spruce chips of -4 "+8 mesh size were pretreated by boiling same for 10 minutes and then cooling same in a bisulphite liquor whose concentration was 2.3% total S0 and 1.2% combined S0 The chips were then subjected to the same digesting conditions as described in Example V except that the digesting liquor has 4.6% total S0 The results were: screened yield 50%; total yield 50.9%; percent lignin in pulp 7.5%; DR of the pulp was 1740.
BISULPHITE PRGCESS In this variation of the acid bisulphite process, free sulphurous acid is eliminated,'the cooking chemical being only the bisulphite salt of ammonia, sodium, calcium or magnesium. The pulping reaction is slower than for acid bisulphite pulping but pentosan in the pulp is conserved because acid hydrolysis is reduced to a minimum by the pH of the liquor, usually in the range of 5.0 to 6.0.
A continuous process for digesting shredded chips by the bisulphite process, acoording to the invention, in-
cludes continuously forwarding chips whose cross-grain dimensions are substantially within the range of 1.65 and 6.7 mm. through a digester and contacting same with a cooking liquor whose concentration is from 3.0% to 8.0% total S0 and 1.5% to 4.0% combined S0 The digesting temperature is constant within the range of between 148 and 180 'C. The digesting time is between and 180 minutes. The total yield of pulp from this digestion operation will normally be between 48% and 72% of the original wood. At the higher yields a fibration treatment of the cooked chips is necessary to reduce the soft chip fragments to fibers.
It is beneficial to preimpregnate the shredded chips with a bisulphite salt solution, not necessarily as high in concentration as that of the cooking liquor itself. The concentration of this preimpregnating solution may lie between 1.6% and 6.0% total S0 0.8% and 3.0% combined 50;. The shredded chips are treated by placing same in the solution while it is boiling for a short period of time such as 10 minutes, cooling rapidly to about 50 to C. and then draining the excess liquor. Vacuum impregnation and impregnation by soaking of the chips for several hours is also suitable. The pretreatment of the chips with the bisulphite salt will result in a substantial decrease in cooking time and, at the higher yields, more uniformly soften chips.
NEUTRAL SULPHITE. SEMI-CHEMICAL PROCESS BATCH OPERATION In batch digestion operations according to the neutral sulphite chemical process, the shredded chips whose crossgrain dimensions are substantially between the range of 1.65 and 6.7 mm. are digested with a liquor consisting essentially of a mixture containing sodium sulphite and sodium carbonate. The concentration of the cooking liquor is from 20 to grams per liter measured as N320,
stresses of which 60% to 80% is present as sodium sulphite and the remainder is sodium carbonate. The maximum digesting temperature is between about 165 and 178 C. The contents of the digester are brought to maximum temperature in from 30 to 90 minutes and are maintained at the maximum temperature for a period ranging from 100 to 240 minutes. The screened yield of a pulp from such a digesting operation will normally range from 62% to 78% of the original wood. The pulp, after being discharged from the digester, is then fibrated in an attrition mill or similar device.
A continuous process for digesting shredded chips by the neutral sulphite semi-chemical process includes continuously forwarding the chips whose cross-grain dimensions are substantially within the range of 1.65 to 6.7 mm, through a digester and contacting same with a cooking liquor consisting essentially of sodium sulphite and sodium carbonate. The concentration or" the cooking liquor is from 20 to 75 grams Na O per liter of which from 60% to 80% is present as sodium sulphite and the remainder as sodium carbonate. The contents of the dig-es ter are continuously maintained at a temperature of between 185 and 200 C. for a period of 20 to 90 minutes following which the pulp is discharged therefrom. The pulp is then fibrated by passin same through an attrition mill or similar device. The total yield of the pulp normally ranges from between 62% and 78% of the original wood.
A pretreatment of the shredded chips with cooking liquor before same are fed to the digester will bring about a reduction in the cooking time.
Example VII Shredded eucalyptus chips of 4 +8 mesh size in cross-grain direction were continuously digested in a liquor whose concentration was 12.5% (Na O), 4 mols Na SO per mol Na CO The liquor-to-wood ratio was 7: 1. At a constant temperature of 193 C. and a cooking time of 45 minutes, the total yield was 71.3% and GE. brightness of the pulp was 37. Mill-size chips cooked under identical conditionsresulted in the same yield but With'a G.E. brightness of 20.6. The shredded chips, after cooking, were soft throughout while the mill-size chips had hard, dark centers.
Shredded eucalyptus chips were cooked under the same conditions as in the preceding example except that they were pretreated with cooking liquor before being cooked, the pretreating consisting in submerging the chips in boiling liquor for 10 minutes, cooling the chips and the liquor to 140 F. while the chips are submerged and then draining the chips. The cooked chips, after a cooking time of 45 minutes, had a total yield of 67.8% and a GE. brightness of 37.5. Mill-size chips, treated identically, had a total yield of 69.7% and a GE. brightness of 26.7. The cooked, pretreated chips were softer than the cooked mill-size chips.
While a variety of specific examples have been given, it will be understood that the invention is not limited to the conditions set forth therein but includes all conditions falling within the scope of the appended claims.
What is claimed is:
v 1. A process for converting chips of a cellulose fiberbearing material, such as wood, into a pulp product, which consists of the steps:
subdividing green chips of fiber-bearing materials having a moisture content of from about to about 50% by shredding the chips along the grain to produce a shredded product consisting of particles of which 1) a substantial proportion have at least one transverse dimension in excess of about 1.65 mm. and no transverse dimension greater than about 6.7 mm., (2) not more than about 5% have no transverse dimensions in excess of about 1.65 mm, and (3) at least have at least one transverse dimeni sion in excess of about 6.7 mm, the lengthwise dimensions of the chips being substantially the same as the original chips;
digesting the shredded product by applying thereto a digesting liquor and heating the particles and the digesting liquor to the digesting temperature as quickly as possible and holding the mixture at the digesting temperature for the period of time required to produce a pulp of the desired characteristics.
2. A process according to claim 1, in which the shredded product is screened, prior to application thereto of the digestion liquor, to remove the particles whose transverse dimensions are in excess of about 6.7 mm. and recycling these particles through the subdivision step.
3. A process for digesting a cellulose fiber-bearing material, such as Wood, with digesting chemicals to produce a pulp product, including the steps:
subdividing green chips of fiber-bearing materials having a moisture content of from about 20% to about 50% by shredding the chips along the grain to pro duce a shredded product consisting of particles of which (1) a substantial proportion have at least one transverse dimension in excess of about 1.65 mm. and no transverse dimension greater than about 6.7 mm, (2) not more than about 5% have no transverse dimensions in excess of about 1.65 mm., and (3) at least 25% have at least one transverse dimension in excess of about 6.7 mm., the lengthwise dimensions of the chips being substantially the same (c) digesting chemicalsacid bisulphite solution concentration4.06.0% total S0 84.6%
combined S0 time to maximum temperatureless than about 120 minutes time at maximum tcrnperature'less than about 120 minutes maximum temperaturel48178 C. (d) digesting chemicals-neutral sulphite solution concentration-2045 grams Na O per liter, 6080% sodium sulphite, balance sodium carbonate time to maximum temperatureless than about minutes time at maximum temperatureless than about 240 minutes maximum temperature-165400 C.
whereby the particles are rapidly digested.
4. A process for digesting a cellulose fiber-bearing material, such as wood, with a cooking liquor to produce a pulp for paper-making purposes, including the steps:
subdividing green chips of fiber-bearing materials having a moisture content of from about 20% 'to about 50% by shredding the chips along the grain to 1.5 produce a shredded product consisting of particles of which (1) a substantial proportion have at least one transverse dimension in excess of about 1.65 mm. and no transverse dimension greater than about 6.7
50% by shredding the chips along the grain to produce a shredded product consisting of particles of which (1) a substantial proportion have at least one transverse dimension in excess of about 1.65 mm. and
. a; the manufacture of rayon, cellulose films and the like, including the steps:
subdividing green chips of fiber-bearing materials'having a moisture content of from about 20% to about mm., (2) not more than about have no trans- 5 50% by shredding the chips along the grain to proverse dimensions in excess of about 1.65 mm., and duce a shredded product consisting of particles of (3) at least 25% have at least one transverse dimenwhich (1) a substantial proportion have at least one sion in excess of about 6.7 'mm., the lengthwise transverse dimension in excess of about 1.65 mm. dimension of the chips being substantially the same and no transverse dimension greater than about 6.7; as the original chips; '10 mm., (2) not more than about 5% have no transverse cooking the shredded product in a liquor consisting esdimensions in excess of about 1.65 mm., and (3) at sentially of sodium hydroxide alone or, in combinaleast 25% have at-least one transverse dimension in tion with sodium sulphide, the liquor containing excess of about 6.7 mm., the lengthwise dimensions from 20 to 55 grams as Na O per liter and having of the chips being substantially the sameas the origia sulphidity ranging from 0 to 35%, allowing from nal chips; 30 to 120 minutes for particles and liquor to reach continuously cooking the shredded product in a liquor a maximum temperature in a range between 170 consisting essentially of sodium hydroxide alone or and 180 C., then cooking at this constant temperain combination with sodium sulphide at a constant ture for 10 to 60 minutes. temperature, the liquor containing from 70 to 90 5. A process for digesting cellulose fiber-bearing magramsi-Na O perliter and having a sulphidity rangterial, such as wood chips, with a cooking liquor to ing from 0 to 35%, the particles and liquor being produce a pulp for paper-making purposes, including maintained at a constant temperature ranging from the steps: 162 to 178 C. fora period of from 5 to 40 minutes.
subdividing green chips of fiber-bearing materials hav- 8. A process for digesting cellulose fiber-bearing mateing a moisture content of from about 20% to about rial, such as wood chips, with a cooking liquor to produce a pulp for papermaking purposes, including the steps:
subdividing green chips 0t fiber-bearing materials having a moisture content of from about 20% to about 50% by shredding the chips along the grain to prono transverse dimension greater than about 6.7 mm., duce a shredded product consisting of particles of (2) not more than about 5% have no transverse which (1) a substantial proportion have at least one imensions in excess of about 1.65 mm., and (3) transverse dimension in excess of about 1.65 mm. at least 25% have at least one transverse dimension and no transverse dimension greater than about 6.7 in excess of about 6.7 mm., the lengthwise dimenmm., (2) not more than about-5% have no transsions of the chips being substantially the same as verse dimensions in excess of about 1.65 mm., and the original chips; (3) at least 25% have at least one transverse dimencooking the shredded product in a liquor consisting sion inv excess of about 6.7 mm., the lengthwise diessentially of sodium hydroxide alone or in commensious of the chips being substantially the same bination with sodium sulphide, the liquor containing as the original chips; from '20 to 55 grams as Na O per liter and having 40 continuously cooking the shredded product in a liquor a sulphidity ranging from 0 to 35%, allowing from consisting essentially of sodium hydroxide alone or 30 to 120 minutes for chips and liquor to reach a in combination with'sodium sulphide at a constant maximum temperature in a range between 170 and temperature, the liquor containing from 20 to 55 180 C., then cooking at this constant temperature grams Na O per liter and having a sulphidity rangfor 0 to minutes and then mechanically defibering A5 ing fr m 0 to 35 the particles and liquor being the partially cooked chips to pulp, maintained at a constant temperature ranging from 6. A process for digesting a cellulose fiber-bearing ma- 175 to 190 C. for a period of from 5 t minutes. terial, such as wood, with a cooking liquor to produce andthen mechanically fibrating the partially cooked a pulp for papermaking purposes, including the steps: 'PaTticlfiS subdividing green chips of fiber-bearing materials hav- 50 A process for utilizing the same liquor for digesting ing a moisture content of from about 20% to about 50% by shredding the chips along the grain to produce a shredded product consisting of particles of which (1) a substantial proportion have at least one transverse dimension in excess of about 1.65 mm. and no transverse dimension greater than about 6.7 mm., (2) not more than about 5% have no transverse dimensions in excess of about 1.65 mm., and (3) at least 25% have at least one transverse dimencellulose fiber-bearing material, such as wood chips, to
produce two grades ofpulp, the first containing less than 3% pentosan to be used for the manufacture of, rayon,
cellulose films and the like, the other to be used for papermaking purposes, including the steps:
subdividing green chips of fiber-bearing materials having a moisture content of from about 20% to 50% by shredding the chips along the grain to produce a shredded product consisting of particles of which (1) a substantial proportion have at least one transzigfi z ig g gl i zx zfg g gg verse dimension in excess of about 1.65 mm. and no h 1 y transverse dimension greater than'about 6.7 mm
P Ongma C 9 (2) not more than about 5% have no transverse dicontinuously cooking the shredded product in a liquor mansions in excass of about L mm and (3) at consisting essentially Sodium hydroxidfi alone or least 25 have at least one transverse dimension in in Combination With Sodium sulphide at a constant 65 excess of about 6.7 mm., the lengthwise dimensions temperature, the liquor containing from 20 to 55 of'thechips being substantially the same as the origigrams as Na O per liter and having a sulphidity nal chips;
ranging from 035%, the chips and liquor being cooking the shredded product in a liquor consisting maintained at a constant temperature ranging from essentially of sodium hydroxide alone or in combina- 175 to 190 C. for a period of from 10 to tion with sodium sulphide at constant temperature,
minutes. the liquor containing from 70 to grams Na O per 7. A process for digesting cellulose fiber-bearing mateliter and having a sulphidity ranging from O to 35 rial, such as wood, with a cooking liquor to produce a the chips and liquor being maintained at a constant pulp containing less than 3% pentosan, to be used for 75 temperature ranging from 162- to 178 for a period of from 5 to 40 minutes to produce a dissolving pulp, separating the liquor from the dissolving pulp and adjusting the concentration of said liquor so that it contains from 20 to 55 grams Na O per liter and has 18 and (3) at least 25% have at least one transverse dimension in excess of about 6.7 mm., the length- -wise dimensions of the chips being substantially the same as the original chips;
a sulphidity of to 35%; cooking other subdivided continuously cooking the shredded product in an acid chips of the above-mentioned size in the liquor at a bisulphite liquor containing firom 4.0% to 6.0% total constant temperature ranging between 170 and 190 S0 and 0.8% to 1.6% combined S0 the basic ion C. for a period of from to 75 minutes to produce used to form the bisulphite being selected from the a papermaking pulp. group consisting of sodium, calcium, magnesium or 10. A- process for digesting cellulose fiber-bearing ma- 10 ammonium, the chips and liquor being maintained at a constant temperature between 148 and 165 C. for a period between 45 and 120 minutes.
13. A process for digesting cellulose fiber-bearing material, such as wood chips, with a cooking liquor to produce a pulp for papermaking or dissolving purposes, including the steps:
terial, such as wood chips, with a cooking liquor to produce a pulp for papermaking or dissolving purposes, including the steps:
subdividing green chips of fiber bearing materials having a moisture content of from about 20% to about 50% by shredding the chips along the grain to produce a shredded product consisting of particles of which (1) a substantial proportion have at least one transverse dimension in excess of about 1.65 mm.
ing a moisture content of from about to 50% by shredding the chips along the grain to produce a shredded product consisting of particles of which (1) a substantial proportion have at least one transverse subdividing green chips of fiber-bearing materials having a moisture content of from about 20% to about 50% by shredding the chips along the grain to proand no transverse dimension greater than about 6.7 20 duce a shredded product consisting of particles off mm., (2) not more than about 5% have no transwhich (1) a substantial proportion have at least one verse dimensions in excess of about 1.65 mm., and transverse dimension in excess of about 1.65 mm. (3) at least have at least one transverse dimenand no transverse dimension greater than about 6.7 sion in excess of about 6.7 mm., the lengthwise dimm., (2) not more than about 5% have no transmensions of the chips being substantially the same 25 verse dimensions in excess of about 1.65 mm., and as the original chips;' (3) at least 25% have at least one transverse dicooking the shredded product by a batch, acid bisulmension in excess of about 6.7 mm., the lengthwise phite process in a liquor containing from 4.0% to dimensions of the chips being substantially the same 6.0% total S0 and 0.8% to 1.6% combined S0 as the original chips; the basic ion used to form the bisulphite being seimpregnating the shredded product with a dilute bilected from the group consisting of sodium, calcium, sulphite solution whose basic ion is selected from magnesium or ammonium, allowing from 30 to 120 the group consisting of sodium, calcium, magnesium minutes for particles and liquor to reach a maximum or ammonium, the concentration of this impregnattemperature of between 148 and 165 C., then cooking solution being between 0.8% and: 1.6% coming at this constant temperature for from 30 to 150 bined S0 1.6% to 3.2% total S0 continuously minutes. cooking the impregnated particles in an acid bisul- 131. A process for digesting cellulose fiber-bearing maphite liquor containing 4.0% to 6.0% total S0 and terial, such as wood chips, with a cooking liquor to pro- 0.8% to 1.6% combined 50,, the basic ion used duce a pulp for papermaking purposes, including the steps: to form the bisulphite being selected from the group subdividing green chips of fiber bearing materials havconsisting of sodium, calcium, magnesium or ammonium, the particles being maintained at a constant temperature in the range of between 148 and 165 C. for a period between and 120 minutes.
14. A process for digesting cellulose fiber-bearing material, such as wood chips, with a cooking liquor to produce a pulp for papermaking purposes, including the steps:
dimension in excess of about 1.65 mm. and no trans- 45 'verse dimension greater than about 6.7 mm., (2) not more than about 5% have no transverse dimensions in excess of about 1.65 mm., and (3) at least 25% have at least one transverse dimension in excess of subdividing green chips of fiber-bearing materials having a moisture content of from about 20% to about about 6.7 mm., the lengthwise dimensions of the chips 50%' .by shredding the chips along the grain to probeing substantially the same as the original chips; duce a shredded product consisting of particles of cooking the shredded product by a batch, acid bisul-f which (*1) a substantial proportion have at least one phite process in a liquor containing from 4.0% to transverse dimension in excess of about l|.6'5 mm. 6.0% total S0 and 0.8% to 1.6% combined S0 and no transverse dimension greater than about 6.7 the basic ion used to form the bisulphite being semm., (2) not more than about 5% have no transverse lected from the group consisting of sodium, calcium, dimensions in excess of about 1.65 mm., and (3) magnesium or ammonium, allowing from 30 to 120 at least 25 have at least one transverse dimenminutes for chips and liquor to reach a maximum sion in excess of about"6.7 mm., the lengthwise ditemperature between 148 and 165 C., then cooking mensions of the chips being substantially the same at this constant temperature for from 10 to 100 minas the original chips;
utes and then mechanically fibrating the cooked pulp to reduce partially cooked particles to fiber. 12. A process for digesting cellulose fiber-bearing macontinuously cooking the shredded product in an acid bisulphite liquor containing from 4.0% to 6.0% total S0 and 0.8% to 1.6% combined S0 the basic terial, such as wood chips, with a cooking liquor to produce a pulp for papermaking or dissolving purposes, including the steps:
subdividing green chips of fiber-bearing materials having a moisture content oif from about 20% to about 50% by shredding the chips along the grain to produce a shredded product consisting of particles of which (1) a substantial proportion have at least one transverse dimension in excess of about 1.65 mm. and no transverse dimension greater than about 6.7 mm., (2) not more than about 5% have no transverse dimensions in excess of about 1 .65 mm.,
ion used to form the bisulphite being selected from the group consisting of sodium, calcium, magnesium or ammonium, the chips and liquor being maintained at a constant temperature in the range of 148 to 165 C. for a period bet-ween 20 and minutes and then mechanically fibrating the cooked pulp to reduce partially cooked particles to fiber.
- 15. A process for digesting cellulose fiber-bearing material, such as wood chips, with a cooking liquor to produce a pulp for papermaking purposes, including the steps:
subdividing green chips of fiber-bearing materials havh.. r. M
1% ing a moisture content of from about 20% to about 50% by shredding the chips along the grain to produce a shredded product consisting of particles of which ('1) a substantial proportion have at least one transverse dimension in excess of about 1.65
mm. and no transverse dimension greater than p as and 178 C. in from 30 to 90 minutes, this maximum temperature then being maintained constant for a period between 100 and 240 minutes and then mechanically fibrating the cooked particles to reduce partially cooked particles to pulp. 18. A process for digesting cellulose fiber-bearing maabout 6.7 mm., (2) not more than about 5% have no transverse dimensions in excess of about 1.65 mm., and (3) a-tleast 25% have at least one transterial, such as wood chips, with a cooking liquor to produce a pulp for papermaking purposes, including the steps:
minutes.
16. A process for digesting cellulose fiber-bearing ma- VeYse dimension in excess of about the 10 subdividing green chips of fiber-bearing materials havlengthwise dimensions of the chips being substaning a moisture content of from about 20% to about tiany the Same as the Original p 50% by shreddingthe chips along the grain to procontimlollsly Cooking [the Shredded Product in a duce a shredded product consisting of particles of sulphite liquor Containing from 310% 83% total which (1) a substantial proportion have at least one 2 and combined 2, the basic 15 transverse dimension in excess of about 1.65 mm. ion usgd to form {he bisulphite Salt being Selficted and no transverse dimension greater than about 6.7 from the gfollpiconsis'ting of gmm., (2) not more than about 5% have no trans- 1165mm and ammonium; the Chips and liquor verse dimensions inexcess of about 1.65 mm., and maintained ata constant temperature in the range (3) at least 25% h at least one transverse p 0f C for a P betwefin 45 and 180 mension in excess of about 6.7 mm., the lengthwise dimensions of the chips being substantially the same as the original chips;
terial, such'as wood chips with a cooking liquor to produce a pulp for papermaking purposes, including the steps: subdividing green chips of fiber-bearing materials havcontinuously cooking the shredded product in a neutral sulphite liquor containing 20 to 75 grams as N3 0 per liter, of which 60% to 80% is present as sodium suiphite, the remainder as sodium carbonate, the
ing a moisture content of from about 2.0% to about 50% by shredding the chips along the grain to produce a shredded product consisting of particles of which (1) a substantial proportion have at least one transverse dimension in excess of about 1.65 mm.
chips and liquor being held at a constant temperature ranging between 185 and 200 C. for a period between 20 and 90 minutes, then mechanically fibrating the cooked particles to reduce partially cooked particles to fiber.
and no transverse dimension greater than about 6.7 mm., (2) not more than about 5% have no transverse dimensions in excess of about 1.65 mm., and (3) at least 25% have at least one transverse dimensionin excess of about 6.7 mm., the lengthwise dimensions 00S the chips being substantially the same as the original chips;
impregnating the shredded product with a dilute bisulphite solution whose basic ion is selected from 40 the group consisting of sodium, calcium, magnesium and ammonium, the concentration of the impregnating solution being between 0.8% and 3.0% combined S0 1.6% and. 6.0% total S0 continuously cooking the impregnated particles in a bisulphite liquor containing from 3.0% to 8.0% total S0 and 1.5% and 4.0% combined S0 the basic ion used to formthe bisulphite salt being selected from the groupconsisting of sodium, calcium, magnesium and ammonium, the chips and liquor being maintained at a constant temperature in the range of 148 and 180 C. for a period between 30 and 150 minutes.
17. A process for digesting cellulose fiber-bearing material, such as wood chips, with a cooking liquor to produce a pulp for papermaking purposes, including the steps:
subdividing green chips of fiber-bearing materials having a moisture content of from about 20% to about 50% by shredding the chips along the grain to produce a shredded product consisting of particles of which (1) a substantial proportion have at least one 19. A process for digesting cellulose fiber-bearing material, such as wood chips, with a cooking liquor to produce a pulp for papermaking purposes, including the steps: 7
subdividing green chips of fiber-bearing materials having a moisture content of from about 20% to about 50% by shredding the chips along the grain to produce a shredded product consisting of particles of which (1) a substantial proportion have at least one transverse dimension in excess of about 1.65 mm. and no transverse dimension greater than about 6.7 mm., (2) not more than about 5% have no transverse dimensions in excess of about 1.65 mm., and (3) at least 25% have at least one transverse dimension in excess of about 6.7 mm., the lengthwise dimensions of the chips being substantially the same as the original chips;
impregnating the shredded product with cooking liquor containing 20 to grams Na O per liter, of which 60% to is present as sodium sulphite, and the remainder as sodium carbonate, draining ofi excess impregnating liquor after impregnation; cooking the impregnated particles in cooking liquor similar to the impregnating liquor at constant temperature in the range of 180 to 200 C. for a period between 20 and minutes and then mechanically fibrating the cooked particles to reduce partially cooked particles 7 to pulp.
60 References Cited by the Examiner UNITED STATES PATENTS transverse dimension in excess of. about 1.65 mm. 1,203,511 /16 Embrce 162-23 and no transverse dimension greater than about 6.7 2,904,460 9/ Nolan 15223 mm., .(2) not more than about 5% have no trans- FOREIGN PA verse dimensions in excess of about 1.65 mm., and 5 3 9 0 5 /33 France (3) at least 25 have at least one transverse dimension in excess of about 6.7 mm., the lengthwise dimensions of the chips being substantially'the same as the original chips;
cooking the shredded product by a batch, neutral. sul- 7 phite semichemical process in a liquor containing 20 to 75 grams as Na O per liter, of which 60% to 80% is present as sodium sulphite, the remainder as sodium carbonate, the chips and liquor being brought to a maximum temperature ranging between 165 55 OTHER REFERENCES Hagglund: Significance of Chip Sizes in Sulphite Cooking, C. A;, 1941;CA 36, 6013.1 1
Montigny: Investigation of Physics-Chemical Factors Which Influence Sulfite Cooking, Forest Service Bulletin No. 87, Dept. of Interior Canada, page 33 relied on. DONALLH. SYLVESTER, Primary Examiner. MORRIS O. WOLK,WILLIAM B. KNIGHT,
Examiners.
Claims (1)
1. A PROCESS FOR CONVERTING CHIPS OF A CELLULOSE FIBERBEARING MATERIAL, SUCH AS WOOD, INTO A PULP PRODUCT, WHICH CONSISTS OF THE STEPS: SUBDIVIDING GREEN CHIPS OF FIBER-BEARING MATERIALS HAVING A MOISTURE CONTENT OF FROM ABOUT 20% TO ABOUT 50% BY SHREDDING THE CHIPS ALONG THE GRAIN TO PRODUCE A SHREDDED PRODUCT CONSISTING OF PARTICLES OF WHICH (1) A SUBSTANTIAL PROPORTION HAVE AT LEAST ONE TRANSVERSE DIMENSION IN EXCESS OF ABOUT 1.65 MM. AND NO TRANSVERSE DIMENSION GREATER THAN ABOUT 6.7 MM., (2) NOT MORE THAN ABOUT 5% HAVE NO TRANSVERSE DIMENSIONS IN EXCESS OF ABOUT 1.65 MM., AND (3) AT LEAST 25% HAVE AT LEAST ONE TRANSVERSE DIMENSION IN EXCESS OF ABOUT 6.7 MM., THE LENGTHWISE DIMENSIONS OF THE CHIPS BEING SUBSTANTIALLY THE SAME AS THE ORIGINAL CHIPS; DIGESTING THE SHREDDED PRODUCT BY APPLYING THERETO A DIGESTING LIQUOR AND HEATING THE PARTICLES AND THE DIGESTING LIQUOR TO THE DIGESTING TEMPERATURE AS QUICKLY AS POSSIBLE AND HOLDING THE MIXTURE AT THE DIGESTING TEMPERATURE FOR THE PERIOD OF TIME REQUIRED TO PRODUCE A PULP OF THE DESIRED CHARACTERISTICS.
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US (1) | US3192102A (en) |
Cited By (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3607618A (en) * | 1967-11-06 | 1971-09-21 | Process Dev Corp | Wood-pulping process |
US4087317A (en) * | 1975-08-04 | 1978-05-02 | Eucatex S.A. Industria E Comercio | High yield, low cost cellulosic pulp and hydrated gels therefrom |
US4113553A (en) * | 1976-02-05 | 1978-09-12 | Mo Och Domsjo Aktiebolag | Sodium sulfide pulping with hydrogen sulfide generation |
US4869783A (en) * | 1986-07-09 | 1989-09-26 | The Mead Corporation | High-yield chemical pulping |
US20020098267A1 (en) * | 2000-10-23 | 2002-07-25 | The Procter & Gamble Co. | Filled snacks |
US20020106441A1 (en) * | 2000-10-23 | 2002-08-08 | Wong Vincent York-Leung | Low-fat nut spread composition and process for making the same |
US6743458B2 (en) | 2000-10-23 | 2004-06-01 | The Procter + Gamble Co. | Reduced fat lipid-based fillings |
US6793956B2 (en) | 2000-10-23 | 2004-09-21 | The Procter & Gamble Co. | Low-moisture, reduced fat, lipid-based fillings |
US20060200357A1 (en) * | 2005-02-23 | 2006-09-07 | International Business Machines (Ibm) Corporation | Policy based data shredding for storage controller |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US1203511A (en) * | 1916-06-03 | 1916-10-31 | Royal B Embree | Process of producing pulp for paper or the like. |
FR830048A (en) * | 1936-11-28 | 1938-07-19 | Halbzellstoff Ind Ag F | Beech cellulose manufacturing process |
US2904460A (en) * | 1953-07-22 | 1959-09-15 | Control Acting For The Univers | Continuous pulping process |
-
1962
- 1962-08-15 US US216969A patent/US3192102A/en not_active Expired - Lifetime
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US1203511A (en) * | 1916-06-03 | 1916-10-31 | Royal B Embree | Process of producing pulp for paper or the like. |
FR830048A (en) * | 1936-11-28 | 1938-07-19 | Halbzellstoff Ind Ag F | Beech cellulose manufacturing process |
US2904460A (en) * | 1953-07-22 | 1959-09-15 | Control Acting For The Univers | Continuous pulping process |
Cited By (11)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3607618A (en) * | 1967-11-06 | 1971-09-21 | Process Dev Corp | Wood-pulping process |
US4087317A (en) * | 1975-08-04 | 1978-05-02 | Eucatex S.A. Industria E Comercio | High yield, low cost cellulosic pulp and hydrated gels therefrom |
US4113553A (en) * | 1976-02-05 | 1978-09-12 | Mo Och Domsjo Aktiebolag | Sodium sulfide pulping with hydrogen sulfide generation |
US4869783A (en) * | 1986-07-09 | 1989-09-26 | The Mead Corporation | High-yield chemical pulping |
US20020098267A1 (en) * | 2000-10-23 | 2002-07-25 | The Procter & Gamble Co. | Filled snacks |
US20020106441A1 (en) * | 2000-10-23 | 2002-08-08 | Wong Vincent York-Leung | Low-fat nut spread composition and process for making the same |
US6720021B2 (en) | 2000-10-23 | 2004-04-13 | The Procter + Gamble Co. | Process for making a low-fat nut spread composition |
US6743458B2 (en) | 2000-10-23 | 2004-06-01 | The Procter + Gamble Co. | Reduced fat lipid-based fillings |
US6793956B2 (en) | 2000-10-23 | 2004-09-21 | The Procter & Gamble Co. | Low-moisture, reduced fat, lipid-based fillings |
US20060200357A1 (en) * | 2005-02-23 | 2006-09-07 | International Business Machines (Ibm) Corporation | Policy based data shredding for storage controller |
US7739462B2 (en) * | 2005-02-23 | 2010-06-15 | International Business Machines Corporation | Policy based data shredding for storage controller |
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