CN105256626A - Mulberry bark chemi-mechanical pulp as well as preparation method and application thereof - Google Patents
Mulberry bark chemi-mechanical pulp as well as preparation method and application thereof Download PDFInfo
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- WYMDDFRYORANCC-UHFFFAOYSA-N 2-[[3-[bis(carboxymethyl)amino]-2-hydroxypropyl]-(carboxymethyl)amino]acetic acid Chemical group OC(=O)CN(CC(O)=O)CC(O)CN(CC(O)=O)CC(O)=O WYMDDFRYORANCC-UHFFFAOYSA-N 0.000 claims description 7
- VBIXEXWLHSRNKB-UHFFFAOYSA-N ammonium oxalate Chemical compound [NH4+].[NH4+].[O-]C(=O)C([O-])=O VBIXEXWLHSRNKB-UHFFFAOYSA-N 0.000 claims description 7
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- 238000006243 chemical reaction Methods 0.000 claims description 7
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 7
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Abstract
The invention discloses mulberry bark chemi-mechanical pulp as well as a preparation method and application thereof, and belongs to the technical field of paper pulp and paper products. The method comprises the following steps: preparing a sample and carrying out primary defibering; (2), carrying out primary pickling; (3), carrying out secondary pickling; (4) carrying out secondary defibering; (5), carrying out primary stewing; (6), carrying out secondary stewing; (7), carrying out primary acid washing; (8), grinding to obtain pulp; (9), carrying out secondary acid washing; (10), carrying out chelating treatment; (11), carrying out acid treatment; (12), carrying out primary bleaching; (13) carrying out secondary bleaching; (14) obtaining the mulberry bark chemi-mechanical pulp. With the adoption of the method, the efficiency and effects of removing lignin and pectin from mulberry bark fibers are high. Meanwhile, the damage to the mulberry bark fibers is less and the fibers have excellent comprehensive properties of relatively high whiteness, high mechanical property and better fibrillating degree.
Description
Art
The present invention relates to a kind of mulberry root bark pulp and preparation method thereof, particularly relate to a kind of mulberry skin chemi-mechanical pulp and preparation method and purposes, belong to paper pulp and paper products technical field.
Background technology
Mulberry tree is deciduous tree or shrub.Mulberry skin peels from mulberry branch, and ramulus mori phloem fiber accounts for 26% ~ 30% of full bar gross weight.Be different from the bast of other wood types, it is low that mulberry skin has content of lignin, the feature that pectin content is high.
The mulberry fibre extracted from mulberry skin is that a kind of toughness is strong, the natural green fiber of good mechanical performance, is mainly used in weaving or pulping and paper-making.Mulberry fibre carries out blending with the fiber such as cotton, numb, can obtain the yarn that brute force is high, ABRASION RESISTANCE good, good hygroscopicity, easy dyeing, wrinkle resistance are good.Be raw material papermaking with mulberry fibre, the advantages such as the mulberry paper obtained possesses solid and flexible, tender, insect protected, pulling force is strong, colour-fast, water absorbing force is strong, are mainly used in the aspect such as the mounting of calligraphy and painting, wrapping bank note, umbrella processed, packaging, firecrackers processed.In addition, be also used in the cultural Publishing such as print money, system fan, book printing.
The present stage research of mulberry fibre focuses mostly in weaving, and technique relative maturity, the exploitation of Related product is also carried out ruly, the especially exploitation of blended yarn.Research for pulping and paper-making aspect is then less, and technology is not mature enough, and the exploitation of Related product is few especially.
The shortcoming such as less and technology is immature at the Study and appliance of pulping and paper-making for mulberry fibre, the present invention with mulberry skin for raw material, chemical pulping and mechanical feedback are combined, give full play to the respective advantage of chemistry and machinery, remove the lignin in mulberry skin raw material and pectin substance, isolate mulberry fibre, preparation mulberry skin chemi-mechanical pulp.The mulberry skin chemi-mechanical pulp made, may be used for manufacture paper with pulp hand-made paper and machine-made paper, coordinates china picture-character paper of manufacturing paper with pulp, wrapping paper, cheque paper etc. with other paper pulp, be applied to packaging, the print reproduction of ancient books painting and calligraphy etc.
Summary of the invention
The invention provides a kind of preparation method and technique of mulberry skin chemi-mechanical pulp.Preparation method of the present invention is, chemical method and mechanical means is effectively combined, and plays the respective advantage of chemical action and mechanism and complementary synergy, makes mulberry skin chemi-mechanical pulp.
The manufacturing process steps of mulberry skin chemi-mechanical pulp of the present invention is as follows:
(1) sample prepares and once discongests that---------(4) secondary is discongested, and------(6) are secondary boiled, and------------------(12) once bleach---bleaching of (13) secondary---, and (14) obtain mulberry skin chemi-mechanical pulp to (10) chelation treatment to (8) defibrination to (5) once boiling in (11) acid treatment in (9) white picking in (7) pickling in (3) secondary pickling in (2) picklings.
(1) sample prepares and once discongests, and by without scraping blue or green dry mulberry skin, be cut into certain length 3 ~ 5cm, width 2 ~ 3cm, in running water, soak time is after 4 ~ 10 weeks, then once discongests in defiberizing machine.Discongesting concentration is 1% ~ 5%.
(2) picklings, the mulberry skin after step (1) being processed soaks in sulfuric acid solution, constantly rubs while immersion, evenly acid-treated to ensure, adopts 40 object filter cloth bag tap water to pH to 7.
Once soaking acid-treated condition is, sulfuric acid concentration 2g/L during pickling discongests mulberry skin absolute dry mass: the mass ratio 1:15 of water in a pickling, temperature 70 C, time 6Omin, and every 5min rubs once, normal pressure.
(3) secondary pickling, soaks the mulberry skin solid after step (2) picklings and constantly rubs in sulfuric acid solution, evenly acid-treated to ensure, then adopts 40 object filter cloth bag tap water to pH to 7.
Secondary soaks acid-treated condition, sulfuric acid concentration 2g/L, mulberry skin absolute dry mass after a pickling: the mass ratio 1:15 of water in secondary pickling, temperature 70 C, time 120min, and every 5min rubs once, normal pressure.
(4) secondary is discongested, and the mulberry skin solid after step (3) secondary pickling also being filtered is discongested in defiberizing machine; Discongesting revolution is 20000 ~ 40000 turns, preferably discongests revolution and is preferably 30000 turns.
(5) once boiling, the mulberry skin after being discongested by step (4) secondary carries out boiling in sodium hydroxide solution, after boiling, washs with running water, after washing, adopts 40 object filter cloth bag tap water to pH to 7.
The process conditions of once boiling are, the concentration of sodium hydroxide solution is 5g/L ~ 20g/L, normal pressure, temperature 100 DEG C, liquor ratio (secondary discongest after mulberry skin absolute dry mass: the quality of water in sodium hydroxide solution) be 1:20, time 2 ~ 10h.
Preferred process conditions are, the concentration of sodium hydroxide solution is 15g/L, and the time is 6h.Under preferred processing condition, the yield that gained is slightly starched is 37.8%, the Kappa number of paper pulp is 20.8, and the residual gum content of paper pulp is 7.19%.
(6) secondary boiled, gained solids crude slurry after step (5) once boiling is carried out secondary boiled in sodium hydroxide solution, and adds tertiary sodium phosphate, ammonium oxalate; After secondary boiled, wash with running water, after washing, adopt 40 object filter cloth bag tap water to pH to 7.
Secondary boiled process conditions are, the concentration of sodium hydroxide solution is 10g/L ~ 20g/L, tertiary sodium phosphate consumption is once boiling and filters 1% ~ 7% of gained solids crude slurry, ammonium oxalate is 1g/L ~ 3g/L, normal pressure, temperature 100 DEG C, liquor ratio (once boiling also filters gained solids crude slurry absolute dry mass: the quality of water in sodium hydroxide solution) is 1:15, time 1 ~ 3h.
Preferred process conditions are, the concentration of sodium hydroxide solution is 15g/L, and tertiary sodium phosphate consumption is 3%, and ammonium oxalate consumption is 2g/L, and liquor ratio is 1:15, and temperature is 100 DEG C, and pressure is normal pressure, and digestion time is 1.5h.
Under preferred processing condition, the yield that gained is slightly starched is 94.33%, and the Kappa number of paper pulp is 16.0, and the residual gum content of paper pulp is 3.04%.
Compared with once boiling, after secondary boiled, Kappa number, the residual gum content of paper pulp all reduce further.
(7) pickling, carry out pickling by the paper pulp after secondary boiled for step (6); Acid washing conditions is sulfuric acid concentration is 2g/L, liquor ratio (secondary boiled and filter after paper pulp absolute dry mass: the quality of water in sulfuric acid) be 1:20, normal temperature and pressure washing 5min; After pickling, adopt 40 object filter cloth bag tap water to pH to 7.
(8) defibrination, carries out defibrination process by the mulberry skin after step (7) pickling.After defibrination terminates, adopt 260 object filter cloth bags by pulp concentrating and washing.
Refining process condition is, defibrination mass concentration is 1.0% ~ 5.0%, and refining pressure is 0.25MPa, and the defibrination time is 20min ~ 60min.
Preferred refining process condition is, refining concentration is 1.5%, and the defibrination time is 40min.The beating degree of gained paper pulp is 31 ° of SR.
By under preferred defibrination condition, gained paper pulp is copied into paper.The tightness of paper is 0.23 μm, and tensile index is 33.6N.m/g, and tear index is 600mN.m
2/ g, whiteness is 44.5%, and the L value of color is 79.6, a* be 1.83, b* is 13.19.
(9) white picking, carries out pickling by the paper pulp after step (8) defibrination also washing.Acid washing conditions is sulfuric acid concentration is 2g/L, and liquor ratio (step (8) defibrination also washs rear paper pulp absolute dry mass: the quality of water in sulfuric acid) is 1:20, normal temperature and pressure washing 5min.After pickling terminates, adopt 260 object filter cloth bag running water that paper pulp is washed till pH to 7.
(10) chelation treatment, carries out chelation treatment with chelating agent to the paper pulp after step (9) white picking.Chelating agent is DPTA, DPTA quality consumption is 0.2% of the absolute dried paper pulp after white picking, and the temperature of chelation treatment is 90 DEG C, and the time is 60min, ensures that chelatropic reaction is even.After chelation treatment, be 7 by pulp washing to pH with running water in 260 object filter cloth bags.
(11) acid treatment, carries out acid treatment by the paper pulp after step (10) chelation treatment; Adopt sulfuric acid to process, sulfuric acid mass percent concentration is 2%, and the temperature of process is 70 DEG C, and the time is 40min, ensures acid-treated uniformity.After acid treatment, be 7 by pulp washing to pH with running water in (260 object) filter cloth bag.
(12) bleach, bleached by the paper pulp after step (11) acid treatment, first, paper pulp sodium metasilicate carries out preliminary treatment, and the consumption of preferred sodium metasilicate is 3% of the paper pulp absolute dry mass after acid treatment; Then, bleach paper pulp with hydrogen peroxide bleaching and NaOH, the consumption of hydrogen peroxide is 2.0% ~ 4.0% of the paper pulp absolute dry mass after acid treatment, and it is 9 ~ 11 that NaOH is used for adjust pH.After bleaching, be 7 by pulp washing to pH with running water in (260 object) filter cloth bag.
Bleaching method is divided into once bleaching and bleaching in stages two kinds.Compared with a bleaching method, although total consumption of bleaching agent is identical, during due to bleaching in stages, the concentration of every section of bleaching agent and the concentration of NaOH all lower, little to the destruction of paper pulp, and the whiteness of paper pulp is higher.Therefore, preferred bleaching method is bleaching in stages, and total consumption of hydrogen peroxide is 3.0%.
When adopting bleaching in stages, the process conditions of every section of bleaching are identical, contribute to simplifying whitening procedure, do not reduce pulp quality.Therefore, the process conditions of every section of bleaching are starch dense 6%, hydrogen peroxide use 1.0% ~ 2.0%, temperature 95 DEG C, time 10 ~ 20min.
Preferred every sectional bleaching process condition is that starching dense is 6%, and temperature is 95 DEG C, and first paragraph bleaching time is 15min and hydrogen peroxide use is 1.5%.
Under optimum condition, the whiteness of gained paper pulp is 78%, and the L value of color is 95.43, a* be 0.27, b* is 4.15.
The effect of several process and object be respectively:
1, sample prepares and once discongests is that mulberry skin raw material is cut into certain length, and adopts the method for machinery, be conducive to the crust getting rid of mulberry skin raw material, mulberry fibre raw material mix becomes more loose, makes mulberry fibre raw material be applicable to the needs of pickling and boiling, to obtain reasonable thick slurry.
2, soaking acid-treated object is, the crust of the mulberry fibre raw material of removing open structure.The pickling mode that can adopt is pickling and gradation pickling once.Gradation pickling process, contributes to removing more crust, to boiling subsequently advantageously, improves cooking effect.
3, secondary is discongested and is, further by the mechanism of defiberizing machine, makes the structure of mulberry fibre raw material more loose, when being conducive to boiling subsequently, the diffusion of boiling reagent in mulberry fibre raw material, improves lignin and pectin generation chemical reaction, is conducive to removing lignin and pectin.
4, the effect of boiling is, the mulberry fibre raw material loosened by structure comparison, under the chemical action of boiling reagent, carries out chemical reaction with lignin and pectin, get rid of lignin and pectin, destroy the connection between mulberry fibre, and destroy the epidermis of mulberry skin further, obtain thick mulberry root bark pulp.At this moment mulberry root bark pulp is also owing to making mulberry fibre remain certain contact containing part lignin and pectin, but the contact between mulberry fibre is weaker.The effect of this step Major Basic chemical reagent, so be chemical method.The mode of boiling is divided into once boiling and repeatedly boiling.Repeatedly boiling is adopted to contribute to while minimizing chemical reagent is to the destruction of fiber, can better defibre.
5, defibrination is by thick mulberry root bark pulp, adopts mechanical system to process further.Thick mulberry root bark pulp under the effect of mechanical force, through tearing, conquassation, friction etc. effect, reach the object separated further.This step mainly mechanism.Mechanism makes mulberry fibre obtain separation, and the contact between mulberry fibre weakens further in the effect of mechanical force, and the mulberry root bark pulp mulberry fibre obtained has certain longitudinal wire-dividing broom purification and horizontal fracture.Through this mechanical treatment, what obtain is thin mulberry root bark pulp.
6, twice pickling is arranged in the front and back of defibrination respectively, can remove cleaner by the crust of mulberry fibre by pickling.
What 7, bleaching adopted is hydrogen peroxide bleaching, is divided into once bleaching and bleaching in stages.Before employing hydrogen peroxide is bleached, need to adopt acid treatment and chelating agent process, heavy-metal ion removal, eliminate heavy metal ion to the impact of hydrogen peroxide bleaching.Adopt hydrogen peroxide to carry out bleaching to thin mulberry root bark pulp further, paper pulp is subject to the oxidation of hydrogen peroxide, removes remaining lignin and pectin further, obtains mulberry skin chemi-mechanical pulp.
Present invention also offers process conditions and the preferred processing condition thereof of mulberry skin chemi-mechanical pulp.As everyone knows, the character of process conditions to final paper pulp of chemical action and mechanism produces conclusive effect.
Chemical treatment comprises digestion process and bleaching.The process conditions of boiling and the process conditions of bleaching all decide the degree removing lignin and pectin, affect the performance of paper pulp.
Mechanical treatment comprises discongests process and defibrination process.Discongest and mulberry skin raw material mix is loosened, so that boiling reagent and bleaching agent easily permeate, be convenient to the removal of reagent to lignin and pectin.Defibrination is the effect utilizing mechanical force, through tearing, conquassation, friction etc. physical action, further fiber separation is come, and the fibrillatings such as longitudinal wire-dividing broom purification and surface area occur and exposes more hydroxyl, contribute to improving adhesion when fiber becomes paper between fiber, improve the performance of paper.
The purposes of mulberry skin chemi-mechanical pulp that the present invention makes adopts ancient method copy paper mode to manufacture paper with pulp mulberry paper, as china picture-character paper, as the carrier copied of ancient books painting and calligraphy.Mulberry root bark pulp can also with other paper pulp, as drawing paper of plagiarizing a book joined by Chinese alpine rush slurry, reed pulp, bamboo pulp, rice straw pulp, wood pulp etc., for collotype printing, serigraphy, ink jet printing, the creation that mode of printing carries out the print culture art work such as to stencil.Mulberry root bark pulp can also be used for the repair process of damaged historical relic ancient books.
The beneficial effect that the present invention has is, the efficiency that preparation method removes lignin and pectin to mulberry fibre is high and effective.Meanwhile, less to the damage of mulberry fibre, fiber has the large and good excellent comprehensive performance of fibrillating degree of the higher and mechanical property of whiteness.Such as, the fibrillating degree of mulberry fibre is higher, then the mechanical property that to become the large and folding number of the pulling force of paper many etc. excellent.The whiteness of mulberry paper slurry is higher, then become the whiteness of paper higher, less dirt count.Boiling reagent hydrogen peroxide and other chemical levels of employing are less, and process is gentle, and carrying capacity of environment is less.The bleaching agent adopted is hydrogen peroxide, is environment-friendly type bleaching agent, belongs to Green Chemistry, non-environmental-pollution.Therefore, preparation method of the present invention, meets the requirement of Modern Green environmental protection.Mulberry skin chemi-mechanical pulp of the present invention has many-sided extensive use.
Detailed description of the invention
By following specific embodiment, the invention will be further described.Following specific descriptions are for the ease of understanding the present invention, are not for limiting the scope of the invention.
Its manufacturing process steps of mulberry skin chemi-mechanical pulp of the present invention is:
(1) sample prepares and once discongests that---------(4) secondary is discongested, and------(6) are secondary boiled, and------------------(12) once bleach---bleaching of (13) secondary---, and (14) obtain mulberry skin chemi-mechanical pulp to (10) chelation treatment to (8) defibrination to (5) once boiling in (11) acid treatment in (9) white picking in (7) pickling in (3) secondary pickling in (2) picklings.
The object of manufacturing process steps and effect:
1, sample prepares.Peel mulberry skin (without scraping blue or green process) from branch air-dry through exposure in sunshine, the sample being cut into 3 ~ 5cm length and width, 2 ~ 3cm with fruittree shear is for subsequent use.Then said sample to be soaked in the running water of normal temperature 6 weeks, to take out the cleaning through 4 ~ 8 times, the pectin analyzed in the middle part of mulberry skin is cleaned.The sample of 3 ~ 5cm length and width, 2 ~ 3cm both can ensure that mulberry skin comes unstuck smoothly, can not affect again the performance of prepared slurry.Soak and the part pectin in mulberry skin within 6 weeks, can be made to precipitate in water, thus the indirect efficiency promoting boiling and come unstuck.
2, discongest.Discongesting before boiling is the surface area in order to increase mulberry skin, cooking liquor is penetrated between every bundle fiber and goes, thus the efficiency that raising boiling is come unstuck.Discongesting after bleaching is for copy paper is prepared, make fiber can evenly be dispersed in water.
3, pickling.Before boiling is come unstuck, carry out pickling process removal unit can divide pectin and lignin, next material making wherein other hydrolyzed pectins do not removed become molecular weight lower, the preliminary treatment of last pickling can also be that most exocuticle is separated with bast, indirectly improves the efficiency that soda boiling is come unstuck, removed the peel.But when it should be noted that the excessive concentration when pickling, also can bring cellulolytic side effect, therefore want the concentration of attentional manipulation pickling.
4, wash.All clean with water after pickling, boiling, bleaching, pickling, effect is that the sample of acid-forming base returns back to neutrality, and each cleaning all first cleans one time with the warm water of 50 DEG C, then rubs limit with waterside from the beginning and clean 3 ~ 5 times.Complete in the sack that the filter cloth being 40 in mesh when cleaning after pickling, boiling is made, completing in the sack that the filter cloth being 260 in mesh during cleaning after pickling, bleaching is made, is take away the impurity such as tiny exocuticle, dust cleaning while by the object of filter cloth cleaning.The filter cloth order number selected after two pickling, bleaching is different from the former, be then because the rear fiber of making beating shortens to attenuate, if clean by 240 object meshes, then fiber can run off between mesh again.With pH test paper, washing lotion is measured during cleaning, when filtrate pH value is 7, complete cleaning.During cleaning wherein after first time boiling, removal of impurities is carried out to material originally, pick out larger for remove by alkali lye bifurcated, location of necrosis impurity.
5, boiling.Boiling can remove remaining most of pectin and lignin in mulberry skin, makes fiber become more soft, thinner.The present invention adopts secondary boiled mode to carry out, and first time boiling can slough most of pectin and lignin, adds digesting assistant and further deviate from pectin and lignin during second time boiling.
6, defibrination.Major part of coming unstuck in the mulberry skin of boiling is removed, but sticks on a small quantity between fiber in addition, cannot be removed by the mode of boiling, so remove the pectin of remnants and outer flaw-piece in the mode of mechanical jordaning.Meanwhile, under the effect of shearing force, length and the fineness of fiber all make moderate progress, and are conducive to the carrying out of next step bleaching.
7, pickling.The residual alkali after pickling can neutralize making beating, fiber adhered to makes it reach neutral, can remove the coloring matter that fiber adsorbs simultaneously.
8, bleach.The present invention adopts the method for two-part hydrogen peroxide bleaching, and the object of bleaching removes the coloring matter affecting fibre whiteness and optical property.Under the condition that bleaching agent hydrogen peroxide use is identical, the number of times increasing bleaching can make the whiteness of fiber promote to some extent.
In technical process of the present invention, the consumption of chemical reagent is less, causes environmental pollution less, and energy consumption and water consume less.
Embodiment 1
The manufacturing process steps of mulberry skin chemi-mechanical pulp is:
(1) sample prepares and once discongests that---------(4) secondary is discongested, and------(6) are secondary boiled, and------------------(12) once bleach---bleaching of (13) secondary---, and (14) obtain mulberry skin chemi-mechanical pulp to (10) chelation treatment to (8) defibrination to (5) once boiling in (11) acid treatment in (9) white picking in (7) pickling in (3) secondary pickling in (2) picklings.
The technological process of mulberry skin chemi-mechanical pulp is:
(1) sample prepares and once discongests.After being dried by the mulberry skin peeled from ramulus mori, be cut into the mulberry leather strap of 3 ~ 5cm length and width, 1 ~ 2cm, soak 6 weeks with running water.Then, the mulberry skin after immersion is put into defiberizing machine to discongest.Discongesting concentration is 2.5%, discongests revolution 30000 turns.
(2) picklings.Liquor ratio is 1:15, and sulfuric acid concentration is 2g/L, and temperature is 70 DEG C, time 6Omin, and every 5min rubs once, normal pressure.
(3) secondary pickling.Liquor ratio is 1:15, and sulfuric acid concentration is 2g/L, and temperature is 70 DEG C, time 120min, and every 5min rubs once, normal pressure.
(4) secondary is discongested.Discongesting concentration is 2.5%, and discongesting revolution is 30000 turns.
(5) once boiling.The concentration of sodium hydroxide solution is 15g/L, and liquor ratio (absolute dried paper pulp quality: the quality of water) is 1:20, and boiling temperature is 100 DEG C, and pressure is normal pressure, and the time is 6h.Under preferred processing condition, the yield that gained is slightly starched is 37.8%, the Kappa number of paper pulp is 20.8, and the residual gum content of paper pulp is 7.19%.
(6) secondary boiled.The concentration of sodium hydroxide solution is 15g/L, and 3% tertiary sodium phosphate consumption is 3%, and ammonium oxalate is 2g/L liquor ratio is 1:15, and temperature is 100 DEG C, and pressure is normal pressure, and digestion time is 1.5h.Under preferred processing condition, the yield that gained is slightly starched is 94.33%, and the Kappa number of paper pulp is 16.0, and the residual gum content of paper pulp is 3.04%.
(7) pickling.Sulfuric acid concentration is 2g/L, and liquor ratio is 1:20, normal temperature and pressure washing 5min.
(8) defibrination.Refining concentration is 1.5%, and refining pressure is 0.25MPa, and the defibrination time is 40min.The beating degree of gained paper pulp is 31 ° of SR.
By under preferred defibrination condition, gained paper pulp is copied into paper.The tightness of paper is 0.23 μm, and tensile index is 33.6N.m/g, and tear index is 600mN.m
2/ g, whiteness is 44.5%, and the L value of color is 79.6, a* be 1.83, b* is 13.19.
(9) white picking.Sulfuric acid concentration is 2g/L, and liquor ratio is 1:20, normal temperature and pressure washing 5min.
(10) chelation treatment.Chelating agent is DPTA, DPTA quality consumption is 0.2%, and the temperature of chelation treatment is 90 DEG C, and the time is 60min.
(11) acid treatment.Sulfuric acid concentration is 2%, and the temperature of process is 70 DEG C, and the time is 40min.
(12) bleach.Adopt two sections of bleaching methods, every sectional bleaching process condition is, starching dense is 6%, and temperature is 95 DEG C, and first paragraph bleaching time is 15min and hydrogen peroxide use is 1.5%.
The whiteness of gained paper pulp is 78%, and the L value of color is 95.43, a* be 0.27, b* is 4.15, beating degree 39 ° of SR.
By mulberry skin chemi-mechanical pulp obtained under above-mentioned processing step and process conditions, manufacture paper with pulp into paper, and mulberry paper performance is tested.
By the mulberry skin chemi-mechanical pulp prepared, be configured to suspension, with 30g/m with the concentration of 0.5%
2, 45g/m
2, 60g/m
2, 75g/m
2, 90g/m
2quantitatively on handsheet machine, carry out handsheet.The mechanical property and the optical property that measure paper are as shown in table 1.
The impact of table 1 quantitatively on mulberry paper performance
Along with quantitative increase, the tightness of paper, whiteness, ageing-resistant brightness (absolute value) decline, and the performance change such as suction range, expansion and contraction, tightness, dirt count, moisture are little.The whiteness of paper depends primarily on the whiteness of paper pulp used.Because used is same bleaching mulberry root bark pulp, so the whiteness of paper is more or less the same.It is the index representing whiteness change before and after paper aging that ageing-resistant brightness declines, and changing little reason and Paper White Degree, to change little reason the same.
What what the dirt count of paper was measured is paper surface was macroscopic has with paper color the spot significantly distinguished, relevant with the spot of paper surface.Dust thing in same paper pulp is dispersed in paper pulp uniformly.Quantitatively large paper sheet thickness is large, although dust thing quantity increases relatively, have a lot of impurity cover by surface fiber, be not dispersed in paper surface, cause dirt count to be more or less the same.
Expansion and contraction depends primarily on hemicellulose level in paper pulp, beating degree height and applying glue, adds factors such as filling out.Because mulberry root bark pulp used is same, and do not add fill out, applying glue, therefore expansion and contraction change is little.Suction range depends primarily on the structure of the character of fiber, the beating degree of paper pulp and paper, therefore also change is little.Be quantitatively 30g/m
2tensile index, the tearability of mulberry paper are lower than high quantitative mulberry paper.This is because quantitative too low time, mulberry paper evenness is poor to be caused.
Embodiment 2
Adopt the mulberry skin oar of embodiment 1 gained and other paper pulp to join to copy, paper of manufacturing paper with pulp.
1, mulberry skin chemi-mechanical pulp and lincaraboard paper
Mulberry skin chemi-mechanical pulp embodiment 1 prepared mixes, with 30g/m according to different percentage composition from Straw Pulp
2quantitatively on handsheet machine, carry out handsheet, measure paper performance.
The conceptual design of table 2 mulberry skin chemi-mechanical pulp and lincaraboard paper
| Sequence number | Mulberry root bark pulp (%) | Straw Pulp (%) |
| 1 | 60 | 40 |
| 2 | 70 | 30 |
| 3 | 80 | 20 |
| 4 | 90 | 10 |
| 5 | 100 | 0 |
The performance of table 3 mulberry skin chemi-mechanical pulp and lincaraboard paper
As shown in Table 3, along with the raising of Straw Pulp ratio, the whiteness of joining copy paper reduces gradually.This is because low than mulberry skin chemi-mechanical pulp of the whiteness of Straw Pulp, along with the lifting of Straw Pulp ratio, the whiteness of joining copy paper promotes naturally to some extent.Tightness aspect, 4 groups of difference of adding Straw Pulp are little; Do not add wheat straw fiber group and be starkly lower than interpolation group.This is because wheat straw fiber is thin, short, the gap can interted between mulberry fibre when copy paper, therefore paper seems closely knit.
Along with the increase of Straw Pulp ratio, tensile index first increases rear reduction.This is because mulberry skin chemi-mechanical pulp plays backbone to paper strength, Straw Pulp is filled between mulberry fibre, the effect played bonding and strengthen.After Straw Pulp ratio arrives more than 30%, the intensity of paper is caused to reduce to the mulberry root bark pulp content reduction that intensity is a mainstay.Tearability reduces along with the increase of Straw Pulp content.This is because tearability increases along with the increase of fibre length, Straw Pulp fibre length is shorter than mulberry fibre, and the ratio increasing Straw Pulp makes the average length of joining papermaking reduce, thus reduces the tearability of paper.Because the ageing-resistant performance of Straw Pulp fiber is not as mulberry skin chemical machinery pulp fibres, therefore lifting Straw Pulp makes ageing-resistant brightness drop-out value increase than regular meeting.
Along with the rising of Straw Pulp ratio, suction range slightly reduces, this is because the water imbibition of wheat straw fiber is poorer than mulberry fibre.Along with the lifting of Straw Pulp ratio, the expansion and contraction of paper slightly promotes.This is because expansion and contraction is subject to the impact of hemicellulose level and beating degree.The beating degree of Straw Pulp and hemicellulose level are a little more than mulberry root bark pulp.Dirt count can increase along with the lifting of Straw Pulp content, is because the impurity contained by Straw Pulp is more than mulberry root bark pulp.Take mechanical property as primary evaluation index, in conjunction with other performances, comprehensively think sequence number 4, it is relatively best that namely mulberry skin chemi-mechanical pulp content is 90%, Straw Pulp content joins the properties of copy paper when being 10%.
2, mulberry skin chemi-mechanical pulp and softwood pulp are joined copy paper and are opened
Mulberry skin chemi-mechanical pulp embodiment 1 prepared mixes, with 30g/m according to different percentage composition from softwood pulp
2quantitatively on handsheet machine, carry out handsheet, measure paper performance.
Table 4 mulberry skin chemi-mechanical pulp and softwood pulp join the conceptual design that copy paper is opened
Table 5 mulberry skin chemi-mechanical pulp and softwood pulp join the performance that copy paper is opened
As shown in Table 5, along with the raising of softwood pulp ratio, the whiteness of joining copy paper promotes to some extent, and the tightness change of paper is little.This is because the whiteness of softwood pulp is than the height of mulberry skin chemi-mechanical pulp, along with the lifting of softwood pulp ratio, the whiteness of joining copy paper promotes naturally to some extent.
Along with the increase of softwood pulp ratio, tensile index increase slightly increases.This is because mulberry skin chemi-mechanical pulp and softwood pulp intert mutually, play the effect of enhancing.But because mulberry fibre and needle-leaved wood fibre is all wider, long, this humidification is also not obvious.Tearability increases along with the increase of softwood pulp content.This is because tearability increases along with the increase of fibre length, needle-leaved wood fibre length is greater than mulberry fibre length, and the ratio increasing softwood pulp makes the average length of joining papermaking increase, thus improves the tearability of paper.
Because the ageing-resistant performance of softwood pulp fiber is similar to mulberry skin chemical machinery pulp fibres, therefore the change of ageing-resistant brightness drop-out value is little.Along with the lifting of softwood pulp ratio, suction range slightly promotes.Reason is that the beating degree of softwood pulp is the 39 ° SRs of 19 ° of SR lower than mulberry skin chemi-mechanical pulp.Along with the lifting of softwood pulp ratio, the expansion and contraction of paper slightly declines.This is because expansion and contraction is by the impact of beating degree, softwood pulp beating degree is lower than mulberry root bark pulp.Dirt count can reduce along with the lifting of softwood pulp content, is because softwood pulp impurities is less than mulberry root bark pulp.Take mechanical property as primary evaluation index, in conjunction with other performances, comprehensively think sequence number 8, it is relatively best that namely mulberry skin chemi-mechanical pulp content is 80%, softwood pulp content joins the properties of copy paper when being 20%.Comparison mulberry skin chemi-mechanical pulp and Straw Pulp, softwood pulp are joined copy paper and are opened, the tensile index of mulberry skin chemi-mechanical pulp and lincaraboard paper, dirt count, expansion and contraction join copy paper Zhang Yaogao than mulberry root bark pulp and softwood pulp, and tearability, suction range, whiteness to join than mulberry root bark pulp and softwood pulp the paper copied low.
3, mulberry skin chemi-mechanical pulp and Straw Pulp and softwood pulp are joined copy paper and are opened
Mulberry skin chemi-mechanical pulp embodiment 1 prepared mixes, with 30g/m according to different percentage composition from Straw Pulp and softwood pulp
2quantitatively on handsheet machine, carry out handsheet, measure paper performance.
Table 6 mulberry skin chemi-mechanical pulp and Straw Pulp softwood pulp starch the conceptual design of joining copy paper and opening
Table 7 mulberry skin chemi-mechanical pulp and Straw Pulp and softwood pulp join the performance that copy paper is opened
As shown in Table 7, during softwood pulp content height, the whiteness of joining copy paper is higher.During Straw Pulp content height, tensile index is higher.Tearability increases along with the increase of fibre length, therefore increases along with the increase of softwood pulp content.Suction range reduces along with the increase of beating degree, and expansion and contraction raises along with the rising of beating degree.
Dirt count reduces, because Straw Pulp impurity content > mulberry root bark pulp > softwood pulp along with the increase of softwood pulp content.Along with the lifting of mulberry root bark pulp constant concentration, each performance change scope reduces gradually.Take mechanical property as primary evaluation index, in conjunction with other performances, comprehensively think sequence number 14, the properties of joining copy paper when namely mulberry root bark pulp content is 70%, Straw Pulp content is 10%, softwood pulp content is 20% is relatively best.
Embodiment 3
First, mulberry skin chemi-mechanical pulp embodiment 1 prepared is manufactured paper with pulp mulberry paper; Then, mulberry skin chemi-mechanical pulp and Straw Pulp, softwood pulp (mulberry skin chemi-mechanical pulp content is 70%, Straw Pulp content is 10%, softwood pulp content be 20%) are joined copy paper and opened; By mulberry paper, join and copy mulberry paper and commercially available paper performance compares.
Table 8 mulberry paper, join the performance comparison of copying mulberry paper and commercially available rice paper
As shown in Table 8, join and copy mulberry paper and commercially available rice paper properties is all more or less the same, and meet the requirement of china picture-character paper industry standard.Join bigger than commercially available rice paper of dirt count copying mulberry paper, tensile index, tearability are apparently higher than commercially available rice paper.Join the function admirable of copying mulberry paper, but dirt count needs to improve further.
Embodiment 4
In embodiment 3 three kind of a paper is printed.
Table 9 raw material and printing equipment
Technological process: join ink → printing
1, ink is joined
Owing to stenciling the ink that ink used is water color ink, variable concentrations, controlled by the addition of deionized water.
2, print
The ink prepared is put into disc, picks with ink brush and beat on version uniformly afterwards, then the paper got ready is laid in above version, finally brush one times the paper back of the body in the horizontal direction with bristle brush, take paper off, picture and text have just been transferred to above paper, so far complete wholely to stencil flow process.
The concentration of ink affects ink in the diffusion velocity of paper surface, the definition of printed matter and stereovision.Mass colour is had nothing in common with each other for the printing effect impact of the different piece such as picture, word.When ink concentration is low, greatly, halation effect is now good for the radius that ink spread at paper surface, but printing precision and definition low.When black moderate concentration, precision and the definition of printed matter are better, and the word in printed matter is clear, picture stereovision is good.When black excessive concentration, the pressure stenciled is less, and cause ink all to transfer on paper from version, printed matter is unintelligible, and without stereovision, and the ink at word place obviously lacks.
Join that to copy mulberry paper best for the printing effect stenciled, to commercially available rice paper to stencil effect similar, be that definition or stereovision are all relatively good.With regard to printing effect, join and copy mulberry paper and be better than mulberry paper.
Mulberry skin chemi-mechanical pulp of the present invention can be joined copy paper with other paper pulp except Straw Pulp, softwood pulp and be opened.
Mulberry skin chemi-mechanical pulp of the present invention and comprise its paper, can adopt the various mode of printings except stenciling, also can adapt to the printing of multiple inks.
Usefulness of the present invention, the purposes such as mulberry skin chemi-mechanical pulp of the present invention, can adopt the manual methods such as method, machine paper method, dry method of paper-making method of manufacturing paper with pulp to carry out shaping, and gained paper products have painting and calligraphy, packaging, printing, false proof, Gu Pin is imitated.
It is apparent to those skilled in the art that above-described embodiment just illustrating this patent, do not form the restriction to this patent.Can make improvements as required, combine, sub-combination and conversion, all improvement, combination, sub-combination, conversion and equivalence are replaced, and are all incorporated in the scope of appended claim.
Claims (10)
1. a preparation method for mulberry skin chemi-mechanical pulp, is characterized in that, comprises the following steps:
Sample prepares and once discongests; (2) picklings; (3) secondary pickling; (4) secondary is discongested; (5) once boiling; (6) secondary boiled; (7) pickling; (8) defibrination; (9) white picking; (10) chelation treatment; (11) acid treatment; (12) once bleach; (13) secondary bleaching; (14) mulberry skin chemi-mechanical pulp is obtained.
2., according to the method for claim 1, it is characterized in that, specific as follows:
(1) sample prepares and once discongests, and by without scraping blue or green dry mulberry skin, be cut into certain length 3 ~ 5cm, width 2 ~ 3cm, in running water, soak time is after 4 ~ 10 weeks, then once discongests in defiberizing machine;
(2) picklings, the mulberry skin after step (1) being processed soaks in sulfuric acid solution, constantly rubs while immersion, evenly acid-treated to ensure, adopts 40 object filter cloth bag tap water to pH to 7;
(3) secondary pickling, soaks the mulberry skin solid after step (2) picklings and constantly rubs in sulfuric acid solution, evenly acid-treated to ensure, then adopts 40 object filter cloth bag tap water to pH to 7;
(4) secondary is discongested, and the mulberry skin solid after step (3) secondary pickling also being filtered is discongested in defiberizing machine;
(5) once boiling, the mulberry skin after being discongested by step (4) secondary carries out boiling in sodium hydroxide solution, after boiling, washs with running water, after washing, adopts filter cloth bag tap water to pH to 7;
(6) secondary boiled, gained solids crude slurry after step (5) once boiling is carried out secondary boiled in sodium hydroxide solution, and adds tertiary sodium phosphate, ammonium oxalate; After secondary boiled, wash with running water, after washing, adopt filter cloth bag tap water to pH to 7;
(7) pickling, carry out pickling by the paper pulp after secondary boiled for step (6); Acid washing conditions is sulfuric acid concentration is 2g/L, and liquor ratio is 1:20, normal temperature and pressure washing 5min; After pickling, adopt 40 object filter cloth bag tap water to pH to 7;
(8) defibrination, carries out defibrination process by the mulberry skin after step (7) pickling, after defibrination terminates, adopts filter cloth bag by pulp concentrating and washing;
(9) white picking, the paper pulp after step (8) defibrination also washing is carried out pickling, and acid washing conditions is sulfuric acid concentration is 2g/L, and liquor ratio is 1:20, normal temperature and pressure washing 5min; After pickling terminates, adopt filter cloth bag running water that paper pulp is washed till pH to 7;
(10) chelation treatment, carries out chelation treatment with chelating agent to the paper pulp after step (9) white picking; Chelating agent is DPTA, ensures that chelatropic reaction is even; After chelation treatment, be 7 by pulp washing to pH with running water in filter cloth bag;
(11) acid treatment, carries out acid treatment by the paper pulp after step (10) chelation treatment; Adopt sulfuric acid to process, after acid treatment, be 7 by pulp washing to pH with running water in filter cloth bag;
(12) bleach, bleached by the paper pulp after step (11) acid treatment, first, paper pulp sodium metasilicate carries out preliminary treatment; Then, bleach paper pulp with hydrogen peroxide bleaching and NaOH, the consumption of hydrogen peroxide is 2.0% ~ 4.0% of the paper pulp absolute dry mass after acid treatment, and it is 9 ~ 11 that NaOH is used for adjust pH; After bleaching, be 7 by pulp washing to pH with running water in filter cloth bag.
3. according to the method for claim 2, it is characterized in that, step (2) is once soaked acid-treated condition and is, sulfuric acid concentration 2g/L during pickling, discongests mulberry skin absolute dry mass: the mass ratio 1:15 of water in a pickling, temperature 70 C, time 6Omin, and every 5min rubs once, normal pressure;
Step (3) secondary soaks acid-treated condition, sulfuric acid concentration 2g/L, mulberry skin absolute dry mass after a pickling: the mass ratio 1:15 of water in secondary pickling, temperature 70 C, time 120min, and every 5min rubs once, normal pressure;
The process conditions of step (5) once boiling are, the concentration of sodium hydroxide solution is 5g/L ~ 20g/L, normal pressure, temperature 100 DEG C, and liquor ratio is 1:20, time 2 ~ 10h;
The secondary boiled process conditions of step (6) are that the concentration of sodium hydroxide solution is 10g/L ~ 20g/L, and tertiary sodium phosphate consumption is once boiling and filters 1% ~ 7% of gained solids crude slurry, ammonium oxalate is 1g/L ~ 3g/L, normal pressure, temperature 100 DEG C, liquor ratio is 1:15, time 1 ~ 3h;
Step (8) refining process condition is, defibrination mass concentration is 1.0% ~ 5.0%, and refining pressure is 0.25MPa, and the defibrination time is 20min ~ 60min;
Step (10) chelating agent is DPTA, DPTA quality consumption is 0.2% of the absolute dried paper pulp after white picking, and the temperature of chelation treatment is 90 DEG C, and the time is 60min, ensures that chelatropic reaction is even;
Step (11) sulfuric acid mass percent concentration is 2%, and the temperature of process is 70 DEG C, and the time is 40min, ensures acid-treated uniformity;
The consumption of step (12) sodium metasilicate is 3% of the paper pulp absolute dry mass after acid treatment.
4. according to the method for claim 3, it is characterized in that, step (12) bleaching method is divided into once bleaching and bleaching in stages two kinds; When adopting bleaching in stages, the process conditions of every section of bleaching are identical, contribute to simplifying whitening procedure, do not reduce pulp quality.Therefore, the process conditions of every section of bleaching are starch dense 6%, hydrogen peroxide use 1.0 ~ 2.0%, temperature 95 DEG C, time 10 ~ 20min.
5. according to the method for claim 4, it is characterized in that, every sectional bleaching process condition is, starching dense is 6%, and temperature is 95 DEG C, and first paragraph bleaching time is 15min and hydrogen peroxide use is 1.5%.
6. according to the method for claim 4, it is characterized in that, the concentration of step (5) sodium hydroxide solution is 15g/L, and the time is 6h.
7. according to the method for claim 4, it is characterized in that, the concentration of step (6) sodium hydroxide solution is 15g/L, tertiary sodium phosphate consumption is 3%, and ammonium oxalate consumption is 2g/L, and liquor ratio is 1:15, temperature is 100 DEG C, and pressure is normal pressure, and digestion time is 1.5h.
8. according to the method for claim 4, it is characterized in that, step (11) sulfuric acid mass percent concentration is 2%, and the temperature of process is 70 DEG C, and the time is 40min, ensures acid-treated uniformity.
9. according to the mulberry skin chemi-mechanical pulp that the either method of claim 1-9 prepares.
10. the purposes of the mulberry skin chemi-mechanical pulp prepared according to the either method of claim 1-9: adopt ancient method copy paper mode to manufacture paper with pulp mulberry paper; Drawing paper of plagiarizing a book is joined with other paper pulp; For the repair process of damaged historical relic ancient books.
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