CN101032820A - Method for liquefying wood - Google Patents
Method for liquefying wood Download PDFInfo
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- CN101032820A CN101032820A CNA2007100036747A CN200710003674A CN101032820A CN 101032820 A CN101032820 A CN 101032820A CN A2007100036747 A CNA2007100036747 A CN A2007100036747A CN 200710003674 A CN200710003674 A CN 200710003674A CN 101032820 A CN101032820 A CN 101032820A
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Abstract
The timber liquefying method is to mixing timber with solvent in the presence of acid catalyst and under timber liquefying condition, with the timber accounting for not less than 30 wt% of the 1 wt% concentration water solution of NaOH as the extractant. The present invention has mild timber liquefying condition, reduced solvent consumption, greatly reduced liquefied residue rate, environment friendship and other advantages. The timber liquefying product is used for preparing adhesive, foamed polyurethane plastic, molded phenolic plastic and other polymer material.
Description
Technical field
The invention relates to a kind of method for liquefying wood.
Background technology
Timber can not be processed by modes such as heating, pressurizations as plastics, metal and glass as the natural macromolecular material of a kind of indissoluble, infusibility, so the reprocessing of timber and degree of depth utilization are subjected to certain restriction.Discovering afterwards, the product after Wood liquefied has thermal fluidity, can be used as the raw material of multiple novel high polymer materials such as adhesive, polyurethane foam plastics, phenolic molding compound plastics, fiber and carbon fiber, thereby widen the application of timber.Wood liquefied main finger is with the reaction of organic solvents such as wood materials and phenol, polyalcohol, cyclic carbonate, liquefaction reaction takes place under acidic catalyst, base catalyst even catalyst-free condition, making cellulose, hemicellulose and lignin macromolecules degradation in the timber is the liquid substance with certain reactivity, become a kind of new Biodegradable high-molecular raw material, thereby be used for preparation such as macromolecular materials such as adhesive, moulding material, polyurethane foams.
Present liquifying method mainly contains two classes: the HTHP liquefaction method of timber and the timber low-temperature liquefaction method under catalyst action.No matter be HTHP liquefaction method or low-temperature liquefaction method, all be the timber raw material to be pulverized the back directly liquefy at present with organic solvents such as phenol, polyalcohol or cyclic carbonates.Because HTHP liquefaction method need be carried out, and is not easy to operate, and need to consume a large amount of energy under 240-270 ℃ high temperature and high pressure condition, therefore at present mostly tend to adopt the low-temperature liquefaction method of catalyst.Be used for Wood liquefied catalyst and be divided into acidic catalyst and base catalyst, because acidic catalyst is better than base catalyst to Wood liquefied catalytic effect, therefore the research of the liquefaction under acid condition is more relatively.
Although the employing acid catalyst can be with Wood liquefied, the problem that adopts acidic catalyst to exist is: the acidity of catalyst is strong more, and the liquefaction effect is good more, and is also serious more to the corrosion of equipment.For example make catalyst with the concentrated sulfuric acid, Wood liquefied carry out more thorough, the liquefied residue rate is lower, can be low to moderate 1%.But sulfuric acid is serious to equipment corrosion, the local charing and the phenomenon of being fuming can occur in the liquefaction process, also can cause environmental pollution.Therefore generally do not recommend at present to adopt sulfuric acid to make catalyst.
And when adopting phosphoric acid, phosphoric acid be a kind of in strong acid, compare with the concentrated sulfuric acid, the liquefaction effect of phosphoric acid slightly a little less than, the residue rate is higher." Forestry Studies in China " 6 (3) for example: 50-54 studies Wood liquefied effect phosphoric acid in the presence of phenol, found that in condensing temperature to be that 160 ℃, liquefying time are that 2.0 hours, liquor ratio (solvent and timber weight ratio) are 3.5, catalyst amount is that the residue rate of Chinese China fir is up to more than 16.0% under the 6 weight % conditions of timber weight.When adopting the ethanedioic acid organic acid, less to the influence of equipment and environment, but the liquefied residue rate is very high when using ethanedioic acid to make catalyst at normal pressure, generally between 45-72%.Those skilled in the art will know that, must be no more than 17 weight % as the residue content in the Wood liquefied product of the raw material of multiple novel high polymer materials such as adhesive, phenolic molding compound plastics, fiber and carbon fiber, otherwise must macromolecular materials such as adhesive will can be used to just after the residue filtering in the liquefaction products make, and residue content is low more, and is favourable more to subsequent reactions such as multiple novel high polymer material such as preparation adhesive, phenolic molding compound plastics, fiber and carbon fibers.Though in condensing temperature is that 180 ℃, liquefying time are under the optimal conditions of the 8 weight % that 2.5 hours, liquor ratio (solvent and timber weight ratio) are 4.5, catalyst amount is timber weight, adopts phosphoric acid does catalyst can obtain littler residue rate.Even but under above-mentioned optimal conditions, the residue rate of Chinese China fir is still up to more than 5.6%.And higher condensing temperature, liquor ratio (solvent and timber weight ratio) can increase Wood liquefied cost undoubtedly greatly, and especially the phenols price is higher.Reduce Wood liquefied cost, especially reduce Wood liquefied used solvent load, become the key point of Wood liquefied technology.Thereby the method for liquefying wood of prior art can't be realized gentle liquefaction condition, low residue rate and less liquor ratio simultaneously.
Summary of the invention
The objective of the invention is to realize the shortcoming of gentle liquefaction condition, low residue rate and less liquor ratio simultaneously, a kind of method for liquefying wood that can realize gentle liquefaction condition, low residue rate and less liquor ratio simultaneously is provided in order to overcome timber normal pressure liquifying method of the prior art.
In order to solve the aforementioned problems in the prior, the present inventor has carried out a large amount of research, the result is surprised to find that, the timber that adopts 1 weight %NaOH aqueous solution the extractives content to be not less than 30 weight % liquefies, can reduce the liquefaction difficulty greatly, solve the problem that the residue rate is low and the liquefaction condition gentleness can not get both in the prior art thus.And the waste wood behind the cultivation Poria cocos promptly can be used as the present invention is the timber that 1 weight %NaOH aqueous solution the extractives content is not less than 30 weight %, thereby solved the problem that Wood liquefied condition is relatively harsher, solvent load is big on the one hand, also found new outlet on the other hand for the waste wood behind the cultivation Poria cocos.
Method for liquefying wood provided by the invention is included under the acidic catalyst existence and under the Wood liquefied reaction condition, and timber is contacted with solvent, and wherein, described timber is the timber that 1 weight %NaOH aqueous solution the extractives content is not less than 30 weight %.
According to method provided by the invention, adopt 1 weight %NaOH aqueous solution the extractives content to be not less than the raw material of the timber of 30 weight % as liquefaction reaction, can make Wood liquefied mild condition, reduce solvent load and reduce residue rate after Wood liquefied greatly, as making catalyst with ethanedioic acid, condensing temperature is 150 ℃, liquefying time is 2.0 hours, liquor ratio (solvent and timber weight ratio) is 3 o'clock, the liquefied residue rate of the normal material of masson pine (1 weight %NaOH aqueous solution the extractives content is 12.89%) is 66.2%, reduces to 6.9% and 1 weight %NaOH aqueous solution the extractives content is 62.29% the liquefied residue rate of masson pine brown rot material under similarity condition.That is to say, adopt method provided by the invention to reduce Wood liquefied requirement, greatly reduced the liquefaction difficulty of timber, guaranteed higher Wood liquefied efficient under the same conditions, reduced the liquefied residue rate catalyst activity.The method according to this invention, lower liquor ratio and more weak acid can obtain higher Wood liquefied efficient.In addition, method provided by the invention also has advantages such as raw material sources are abundant, environmental protection.The Wood liquefied product that adopts method provided by the invention to obtain can be directly used in multiple novel high polymer materials such as preparation adhesive, polyurethane foam plastics, phenolic molding compound plastics, fiber and carbon fiber.
The specific embodiment
According to method provided by the invention, although being not less than the timber of 30 weight %, 1 weight %NaOH aqueous solution the extractives content all can realize purpose of the present invention, but the high more timber of 1 weight %NaOH aqueous solution the extractives content, the objective of the invention is favourable more to realization, because 1 weight %NaOH aqueous solution the extractives content can reflect the degree that raw material is rotten, rotten to a certain extent in the timber, reflect that especially cellulose degradation becomes micromolecular degree in the timber.With regard to present discovery, the impossible infinite height of 1 weight %NaOH aqueous solution the extractives content especially can not reach 100 weight %, generally the highest can only reaching about 80 weight % in the timber but because in fact.Therefore, under the preferable case, described concentration is that 1 weight %NaOH aqueous solution the extractives content is 30-80 weight %, more preferably 50-80 weight %.
The timber that described 1 weight %NaOH aqueous solution the extractives content is not less than 30 weight % can obtain by the whole bag of tricks, for example, can be commercially available, and also can obtain by existing prepared in various methods, for example obtains by biodegradable method.Described biodegradable method for example can be the method for the various peckiness fungies of existing cultivation.Usually, the method for the various peckiness fungies of existing cultivation comprises that bacterial classification inoculation with brown rot fungus to timber, cultivates and can obtain required brown rot fungus under this fungi growth condition.The purpose of said method is in order to obtain brown rot fungus, and will be discarded as the dote of cultivating behind the brown rot fungus bacterial classification, and this has caused the great wasting of resources undoubtedly.The inventor finds, use the timber after the above-mentioned cultivation brown rot fungus to liquefy, not only can reduce Wood liquefied difficulty greatly, make and adopt weak acid also can obtain extremely low residue rate as catalyst, but also, make it by the useless treasured that becomes for the dote behind the cultivation bacterial classification has found new outlet.1 weight %NaOH aqueous solution the extractives content of the timber after the above-mentioned cultivation brown rot fungus generally is not less than 30 weight %, concrete content with the growth conditions of time of inoculation, brown rot fungus with the different of brown rot fungus bacterial classification and slightly different, but all in above-mentioned scope.Therefore, the 1 weight %NaOH aqueous solution the extractives content of the present invention wood powder that generally is not less than 30 weight % is for cultivating the wood powder after the brown rot fungus.Described brown rot fungus is that the full pore fungi of the red plan shelf fungus of Poria cocos fungi, rose, erythema cheese bacteria, hedge limit lenzites bacteria, continuous rotten transverse hole fungus, oak Daedalea, bright red sulphur look gorgeous pore fungi, thick black shelf fungus, birch, applewood shelf fungus, white bracket fungus, yellowish pink bolt bacterium, fomitopsis pinicola, fragrant sticking gill fungus, gloeophyllum sepiarum, the gorgeous pore fungi of sulphur, the dark pore fungi of loose China fir, fan covers cheese bacteria, ungulate cheese bacteria, one or more in Antrodia, rare hardwood layer pore fungi and the special-shaped bolt bacterium in vain.The method of described cultivation brown rot fungus has been conventionally known to one of skill in the art, and for example, CN1732761A discloses a kind of method of cultivating the Poria cocos fungi.Generally, above-mentioned 1 weight %NaOH aqueous solution the extractives content be not less than 30 weight % timber can by bacterium culture medium provide.
Described timber can be existing various biodegradable timber, for example can be in softwood plant such as China fir, larch, Japanese red pine, the masson pine one or more, can also be in broadleaf plant such as robur, Manchurian ash, eucalyptus, birch and the poplar one or more.
In order to make reaction be easy to carry out and to make the reaction that obtains homogeneous inside and outside the timber, described timber is preferably the wood powder of timber through obtaining after pulverizing, and for example can be that particle diameter is no more than 4 millimeters wood powder particle.Can be wood powder behind 4 millimeters the sieve by timber is crossed mesh size through the wood powder that obtains after pulverizing.More preferably water content is no more than the dried wood powder particle of gas of 12 weight %.
The present invention under the Wood liquefied condition and acidic catalyst in the presence of, there is no particular limitation for condition that timber is contacted with solvent and concrete operations, described acidic catalyst can be a various acidic catalyst of the prior art, for example can be various inorganic acids and/or organic acid or its solution, described inorganic acid for example can be one or more in sulfuric acid, hydrochloric acid, phosphoric acid, the nitric acid, and described organic acid for example can be one or more in ethanedioic acid, formic acid, acetate, malonic acid, succinic acid, benzene sulfonic acid, the benzoic acid.Because the used timber of the present invention is the timber that 1 weight %NaOH aqueous solution the extractives content is not less than 30 weight %, even therefore use relatively low, the also relatively low weak acid of catalytic activity to the corrosive power of equipment, also can obtain the promptly lower residue rate of higher liquefied fraction, therefore, comprehensive liquefied fraction and the corrosive power of equipment considered, catalyst of the present invention are preferably acid more weak phosphoric acid, in the ethanedioic acid one or both.Consumption to described acidic catalyst is not particularly limited, and can be the conventional acid catalyst amount, for example can be the 3-10 weight % of weight of solvent.Because the timber that the present invention uses 1 weight %NaOH aqueous solution the extractives content to be not less than 30 weight % carries out Wood liquefied reaction as raw material, therefore can use catalyst, for example can use the acidic catalyst of weight of solvent 0.5-10 weight % than conventional method for liquefying wood less amount.
Described solvent can be the conventional all kinds of solvents that uses in this area, for example can be in phenol, o-cresol, m-cresol, p-cresol, catechol, resorcinol, hydroquinones, 1,2,3,-thrihydroxy-benzene, phloroglucin, hydroxyquinol, alpha-Naphthol, betanaphthol, bisphenol-A, the Bisphenol F one or more.Generally speaking, higher solvent is favourable to improving Wood liquefied rate, and the present inventor had such experiment experience, under the identical situation of other conditionally complete, the residue rate of 20 gram timber being carried out liquefaction reaction in 100 gram solvents is well below the residue rate of 50 gram timber in 100 gram solvents.But the content of solvent is big more, and required quantity of solvent is also big more, and corresponding production cost is also high more, and in subsequent reactions, if quantity of solvent is too big, may need to remove partial solvent, and this has further increased operational sequence undoubtedly.Comprehensive production cost and residue rate consider that the weight ratio that the amount of described solvent is preferably solvent and timber is 0.5-4: 1, and 0.5-3 more preferably: 1.
The temperature of described liquefaction reaction can be the conventional liquefaction reaction temperature of using in this area.Because the timber that the present invention uses 1 weight %NaOH aqueous solution the extractives content to be not less than 30 weight % carries out Wood liquefied reaction as raw material, therefore described liquefaction reaction temperature can be than the lower temperature of conventional liquefaction reaction temperature, for example can be 100-180 ℃, more preferably 120-160 ℃.The time of liquefaction reaction can be the Wood liquefied reaction time of routine, because the present invention adopts 1 weight %NaOH aqueous solution content to be not less than the timber of 30 weight %, therefore, the time of liquefaction reaction can the used liquefying time of more conventional method for liquefying wood shorten greatly, for example, can foreshorten to 10-180 minute.
Adopt method provided by the invention can obtain the Wood liquefied product that the residue rate is lower than 15 weight %, especially can obtain the residue rate and be low to moderate 2.2% masson pine liquefaction products, this liquefaction products need not to separate residue or other step and can directly applying to fully in the subsequent handlings such as multiple novel high polymer material such as preparation adhesive, phenolic molding compound plastics, fiber and carbon fiber wherein.The performance that the Wood liquefied product that employing is obtained by method for liquefying wood of the present invention makes multiple novel high polymer materials such as adhesive, phenolic molding compound plastics, fiber and carbon fiber meets national standard fully, for example, the bonding strength of 3 layers of poplar plywood of the compressed with adhesive that the Wood liquefied product that employing is obtained by method for liquefying wood of the present invention makes meets the requirement of I class glued board in the GB/T 9846.3-2004 standard fully up to 1.6 MPas.
The following examples will the present invention is further illustrated.
Embodiment 1
This embodiment is used to illustrate method for liquefying wood provided by the invention.
The masson pine powder (by 0.9 millimeter mesh screen aperture) that with 20 grams, 1 weight %NaOH aqueous solution the extractives content is 62.29 weight % is that the phosphoric acid of 85 weight % joins in 500 milliliters of there-necked flasks that agitator, thermometer and reflux condensing tube are housed with 40 gram phenol and 3.2 gram concentration, there-necked flask immersed in the oil bath be heated to 150 ℃ in advance stirring reaction 120 minutes, and obtained Wood liquefied product.Described masson pine collecting location is Yuexi County, Anhui and Pingxiang sun village, the discarded masson pine brown rot timber after cultivating about 10 months Poria cocos of gathering of Poria cocos fungi under 25-30 ℃, relative air humidity 60-80% damp condition that is provided by Poria cocos plantation family.
Calculate residue rate after Wood liquefied by following method: the gained product is filtered with Toyo GA100 glass filter paper with methyl alcohol dilution back under vacuum, the filtrate of fully washing until new washing with methyl alcohol becomes colorless, the gained filter residue is weighed after dry 24 hours in 105 ℃ of drying boxes, and the percentage of filter residue weight and timber weight is the residue rate after Wood liquefied.Among this embodiment, the residue rate after Wood liquefied is 2.2%.
Comparative Examples 1
This Comparative Examples is used to illustrate the method for liquefying wood of prior art.
Carry out Wood liquefied according to the method identical with embodiment 1, different is, masson pine timber is the normal material of masson pine in Yuexi County, Anhui and the collection of Pingxiang sun village, the 1 weight %NaOH aqueous solution the extractives content of this masson pine is 12.89 weight %, according to the method for embodiment 1 calculate Wood liquefied after the residue rate be 26.2%.
Embodiment 2
This embodiment is used to illustrate method for liquefying wood provided by the invention.
Carry out Wood liquefiedly according to the method identical with embodiment 1, different is, masson pine timber is that 1 weight %NaOH aqueous solution the extractives content is the timber of 70.07 weight %, according to the method for embodiment 1 calculate Wood liquefied after the residue rate be 1.3%.Described masson pine collecting location is Yuexi County, Anhui and Pingxiang sun village, by Poria cocos plantation family provide at the masson pine brown rot timber of cultivating under 25-30 ℃, relative air humidity 60-80% damp condition after 15 week of Poria cocos fungi, top layer Poria cocos mycelia and foreign material were removed in the back.
Embodiment 3
This embodiment is used to illustrate method for liquefying wood provided by the invention.
Carry out Wood liquefiedly according to the method identical with embodiment 1, different is, masson pine timber is that 1 weight %NaOH aqueous solution the extractives content is the timber of 54.01 weight %, according to the method for embodiment 1 calculate Wood liquefied after the residue rate be 3.37%.Described masson pine collecting location is Yuexi County, Anhui and Pingxiang sun village, by Poria cocos plantation family provide at the masson pine brown rot timber of cultivating under 25-30 ℃, relative air humidity 60-80% damp condition after 11 week of Poria cocos fungi, top layer Poria cocos mycelia and foreign material were removed in the back.
Embodiment 4
This embodiment is used to illustrate method for liquefying wood provided by the invention.
Carry out Wood liquefiedly according to the method identical with embodiment 1, different is, masson pine timber is that 1 weight %NaOH aqueous solution the extractives content is the timber of 36.34 weight %, according to the method for embodiment 1 calculate Wood liquefied after the residue rate be 10.4%.Described masson pine collecting location is Yuexi County, Anhui and Pingxiang sun village, by Poria cocos plantation family provide at the masson pine brown rot timber of cultivating under 25-30 ℃, relative air humidity 60-80% damp condition after 7 week of Poria cocos fungi, top layer Poria cocos mycelia and foreign material were removed in the back.
Embodiment 5
This embodiment is used to illustrate method for liquefying wood provided by the invention.
Carry out Wood liquefied according to the method identical with embodiment 1, different is, adding 60 gram phenol and 4.8 gram ethanedioic acids, to replace 40 gram phenol and 3.2 gram concentration be the phosphoric acid of 85 weight %, according to the method for embodiment 1 calculate Wood liquefied after the residue rate be 6.9%.
Comparative Examples 2
This Comparative Examples is used to illustrate the method for liquefying wood of prior art.
Carry out Wood liquefied according to the method identical with embodiment 5, different is, masson pine timber is the normal material of masson pine in Yuexi County, Anhui and the collection of Pingxiang sun village, the 1 weight %NaOH aqueous solution the extractives content of this masson pine is 12.89 weight %, according to the method for embodiment 1 calculate Wood liquefied after the residue rate be 66.2%.
Embodiment 6
This embodiment is used to illustrate method for liquefying wood provided by the invention.
Carry out Wood liquefiedly according to the method identical with embodiment 1, different is, the addition of phenol is 10 grams, according to the method for embodiment 1 calculate Wood liquefied after the residue rate be 14.8%.
Embodiment 7
This embodiment is used to illustrate method for liquefying wood provided by the invention.
Carry out Wood liquefiedly according to the method identical with embodiment 5, different is, the temperature of liquefaction reaction is 120 ℃, according to the method for embodiment 1 calculate Wood liquefied after the residue rate be 14.5%.
Embodiment 8
This embodiment is used to illustrate method for liquefying wood provided by the invention.
Carry out Wood liquefiedly according to the method identical with embodiment 5, different is, the time of liquefaction reaction is 30 minutes, according to the method for embodiment 1 calculate Wood liquefied after the residue rate be 12.5%.
Embodiment 9
This embodiment is used to illustrate method for liquefying wood provided by the invention.
Carry out Wood liquefied according to the method identical with embodiment 2, different is, 1 weight %NaOH aqueous solution the extractives content is that the masson pine of 70.07 weight % is that the poplar of 71.21 weight % replaces by 1 weight %NaOH aqueous solution the extractives content, according to the method for embodiment 1 calculate Wood liquefied after the residue rate be 1.6%.Described poplar is for infecting 5 months removal mycelia and the poplar brown rot material behind the foreign material according to GB/T 13942.1-92 at the continuous rotten transverse hole fungus that is subjected to of prepared in laboratory.
Comparative Examples 3
This Comparative Examples is used to illustrate the method for liquefying wood of prior art.
Carry out Wood liquefied according to the method identical with embodiment 9, different is, 1 weight %NaOH aqueous solution the extractives content is that the poplar of 71.21 weight % is the normal material of poplar of the same breed of same place collection, 1 weight %NaOH aqueous solution the extractives content of this poplar is 19.25%, according to the method for embodiment 1 calculate Wood liquefied after the residue rate be 27.5%.
Embodiment 10
Following embodiment is used to illustrate the application performance of the Wood liquefied product that adopts method acquisition provided by the invention.
The Wood liquefied product that embodiment 1 is prepared is cooled to room temperature rapidly, and adding sodium hydrate aqueous solution and the 62 gram concentration that 51 gram concentration are 20 weight % then under stirring condition is the formalin of 37 weight %, reacts 1 hour down at 60 ± 2 ℃ afterwards; Continue reaction 1 hour down at 85 ± 2 ℃ again, be cooled to 40 ℃ then rapidly, obtain thermosetting liquefaction products resin.
With above-mentioned liquefaction products resin, peanut hull meal and curing agent Na
2CO
3Mixed by weight 100: 7: 3, obtain wood adhesive.As adhesive preparation 3 layers of poplar plywood (millimeter (wide) * 1.6,270 millimeters (length) * 270 millimeter (thick)), the technological parameter of preparation glued board is with the gained wood adhesive: resin added 125 gram/square metre (single faces); Pressure 1.3 MPas of colding pressing, 10 minutes time; Hot pressing pressure 1.3 MPas, 4 minutes time.According to the requirement of GB/T 17657-1999 " Test methods of evaluating the properties of woodbased panels and surface decorated woodbased panels " I class glued board, detect the bonding strength and the wood-breaking rate of gained poplar plywood.Found that bonding strength and wood-breaking rate are respectively 1.62 MPas and 85%, satisfy national I class glued board requirement (bonding strength 〉=0.7 MPa).
Embodiment 11
Following embodiment is used to illustrate the application performance of the Wood liquefied product that adopts method acquisition provided by the invention.
The Wood liquefied product of embodiment 1 preparation is cooled to 80 ℃ rapidly, adding 20 gram concentration then under stirring condition is the formalin of 37 weight %, reacted 1.5 hours down at 95-100 ℃ afterwards, be cooled to 40 ℃ then rapidly, obtain thermoplasticity liquefaction products resin.
Above-mentioned thermoplasticity liquefaction products resin is first 50 ℃ of following decompression distillation (vacuum is-0.1 MPa) 1 hour, and then, obtain solid shape thermoplasticity liquefaction products resin 180 ℃ of following decompression distillation (vacuum-0.1 MPa) 1 hour.The gained resin all is ground into subparticle by 0.28 millimeter screen cloth diameter.Performance according to " phenolic resins and application thereof " (Huang Farong, Jiao Yangsheng chief editor, Chemical Industry Press, 2003) above-mentioned resin of check.Found that free phenol content is 5 weight % in the resin, moisture is 2.5 weight %, and gel time is 70 seconds.
Claims (10)
1, a kind of method for liquefying wood, this method is included under the acidic catalyst existence and under the Wood liquefied reaction condition, timber is contacted with solvent, it is characterized in that, described timber is the timber that 1 weight %NaOH aqueous solution the extractives content is not less than 30 weight %.
2, method according to claim 1, wherein, 1 weight %NaOH aqueous solution the extractives content of described timber is 30-80 weight %.
3, method according to claim 1, wherein, the timber that described 1 weight %NaOH aqueous solution the extractives content is not less than 30 weight % is for cultivating the timber after the brown rot fungus.
4, method according to claim 3, wherein, described brown rot fungus is that the full pore fungi of the red plan shelf fungus of Poria cocos fungi, rose, erythema cheese bacteria, hedge limit lenzites bacteria, continuous rotten transverse hole fungus, oak Daedalea, bright red sulphur look gorgeous pore fungi, thick black shelf fungus, birch, applewood shelf fungus, white bracket fungus, yellowish pink bolt bacterium, fomitopsis pinicola, fragrant sticking gill fungus, gloeophyllum sepiarum, the gorgeous pore fungi of sulphur, the dark pore fungi of loose China fir, fan covers cheese bacteria, ungulate cheese bacteria, one or more in Antrodia, rare hardwood layer pore fungi and the special-shaped bolt bacterium in vain.
5, method according to claim 1, wherein, the weight ratio of described solvent and timber is 0.5-4: 1.
6, method according to claim 5, wherein, described solvent is one or more in phenol, o-cresol, m-cresol, p-cresol, catechol, resorcinol, hydroquinones, 1,2,3,-thrihydroxy-benzene, phloroglucin, hydroxyquinol, alpha-Naphthol, betanaphthol, bisphenol-A, the Bisphenol F.
7, method according to claim 1, wherein, described acidic catalyst is the 0.5-10 weight % of weight of solvent.
8, according to claim 1 or 7 described methods, wherein, described acidic catalyst is one or more in phosphoric acid, hydrochloric acid, sulfuric acid, nitric acid, formic acid, acetate, ethanedioic acid, malonic acid, succinic acid, benzene sulfonic acid, benzoic acid or its solution.
9, method according to claim 1, wherein, described timber is that particle diameter is no more than 4 millimeters wood powder particle.
10, method according to claim 1, wherein, the condition of described Wood liquefied reaction comprises that reaction temperature is 100-180 ℃, the reaction time is 10-180 minute.
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| CNB2007100036747A CN100537164C (en) | 2006-12-30 | 2007-01-23 | Method for liquefying wood |
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| CN200610172295.6 | 2006-12-30 | ||
| CN200610172295 | 2006-12-30 | ||
| CNB2007100036747A CN100537164C (en) | 2006-12-30 | 2007-01-23 | Method for liquefying wood |
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| CN101032820A true CN101032820A (en) | 2007-09-12 |
| CN100537164C CN100537164C (en) | 2009-09-09 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101396838B (en) * | 2008-10-31 | 2010-06-09 | 中国林业科学研究院林产化学工业研究所 | Wood liquefier and method for preparing surfactant using liquidated wood |
| CN102463614A (en) * | 2010-11-09 | 2012-05-23 | 中国林业科学研究院木材工业研究所 | Rapid liquefying method for wood |
| CN102528879A (en) * | 2012-01-06 | 2012-07-04 | 四川农业大学 | Building wood planking recycling method |
| CN102617818A (en) * | 2012-04-10 | 2012-08-01 | 北京林业大学 | Preparation method of biological oil modified phenolic resin for foaming |
| CN103289310A (en) * | 2013-06-13 | 2013-09-11 | 北京林业大学 | Wood liquefied substance foamed material and preparation method thereof |
| CN110280189A (en) * | 2019-06-24 | 2019-09-27 | 长安大学 | A kind of rapid liquefying method of Poplar Powder |
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2007
- 2007-01-23 CN CNB2007100036747A patent/CN100537164C/en not_active Expired - Fee Related
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101396838B (en) * | 2008-10-31 | 2010-06-09 | 中国林业科学研究院林产化学工业研究所 | Wood liquefier and method for preparing surfactant using liquidated wood |
| CN102463614A (en) * | 2010-11-09 | 2012-05-23 | 中国林业科学研究院木材工业研究所 | Rapid liquefying method for wood |
| CN102463614B (en) * | 2010-11-09 | 2014-10-01 | 中国林业科学研究院木材工业研究所 | Rapid liquefying method for wood |
| CN102528879A (en) * | 2012-01-06 | 2012-07-04 | 四川农业大学 | Building wood planking recycling method |
| CN102528879B (en) * | 2012-01-06 | 2015-03-11 | 四川农业大学 | Building wood planking recycling method |
| CN102617818A (en) * | 2012-04-10 | 2012-08-01 | 北京林业大学 | Preparation method of biological oil modified phenolic resin for foaming |
| CN103289310A (en) * | 2013-06-13 | 2013-09-11 | 北京林业大学 | Wood liquefied substance foamed material and preparation method thereof |
| CN103289310B (en) * | 2013-06-13 | 2015-04-15 | 北京林业大学 | Wood liquefied substance foamed material and preparation method thereof |
| CN110280189A (en) * | 2019-06-24 | 2019-09-27 | 长安大学 | A kind of rapid liquefying method of Poplar Powder |
| CN110280189B (en) * | 2019-06-24 | 2022-03-15 | 长安大学 | Rapid liquefaction method of poplar powder |
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