CN104988783A - Pulping method of reed organic solvent slurry by pre-extracting hemicellulose and product thereof - Google Patents
Pulping method of reed organic solvent slurry by pre-extracting hemicellulose and product thereof Download PDFInfo
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- CN104988783A CN104988783A CN201510433913.7A CN201510433913A CN104988783A CN 104988783 A CN104988783 A CN 104988783A CN 201510433913 A CN201510433913 A CN 201510433913A CN 104988783 A CN104988783 A CN 104988783A
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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
- D21C3/00—Pulping cellulose-containing materials
- D21C3/20—Pulping cellulose-containing materials with organic solvents or in solvent environment
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0057—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid beta-D-Xylans, i.e. xylosaccharide, e.g. arabinoxylan, arabinofuronan, pentosans; (beta-1,3)(beta-1,4)-D-Xylans, e.g. rhodymenans; Hemicellulose; Derivatives thereof
-
- 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
- D21C1/02—Pretreatment of the finely-divided materials before digesting with water or steam
-
- 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
- D21C9/00—After-treatment of cellulose pulp, e.g. of wood pulp, or cotton linters ; Treatment of dilute or dewatered pulp or process improvement taking place after obtaining the raw cellulosic material and not provided for elsewhere
- D21C9/02—Washing ; Displacing cooking or pulp-treating liquors contained in the pulp by fluids, e.g. wash water or other pulp-treating agents
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- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Wood Science & Technology (AREA)
- Paper (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention relates to a pulping method of a reed organic solvent slurry by pre-extracting hemicellulose and a product thereof. The method includes: reed preparation, prehydrolysis, solid-liquid separation and washing, and pulp preparation by a high boiling alcohol solvent method from residues. The method can obtain a reed pulp and a reed extracting liquid which can be used for preparation of saccharide compounds or ethanol. Compared with the reed raw material which is not subjected to hemicellulose extraction by hydrolysis, the Kappa number of the slurry obtained under the same pulping conditions is reduced by 5-8 units after the reed is subjected to prehydrolysis. By prehydrolysis to extract hemicellulose before pulping, the problem of high sugar content in a high boiling alcohol solvent recovery system can be solved, and effective utilization of all components of wood biomass raw materials also can be realizes, so that the added value of a byproduct is improved, and the economic costs of high boiling solvent alcohol pulping are balanced.
Description
Technical field
The present invention relates to Chemical Engineering, reed pulping process field, reed organic solvent slurry pulping process being specifically related to a kind of preextraction hemicellulose and products thereof.
Background technology
The timber resources of China extremely lacks, and paper making raw material bottleneck is particularly thorny.Reed is a kind of important non-wood papermaking raw material, has higher cost performance.Therefore, the scientific and reasonable problem utilizing the non-wood materials such as reed can solve China's paper making raw material deficiency.
Organic solvent pulping is a kind of free of contamination free pulping method, and high boiling solvent (hbs) slurrying belongs to the category of organosolv pulping method.Document 1 bagasse high boiling solvent method slurrying pre-test--" Chinese papermaking " 06 phase in 2008, document 2 height alcohol method (HBS method) of boiling prepares yellow pulp and lignin--and " Min Jiang institute journal " 02 phase in 2003 reports bagasse and straw and adopts BDO to be that the height of boiling solvent boils alcohol pulping process.Although reed and bagasse, straw belongs to non-wood material together, and growth characteristics and raw material mix are not identical, and therefore their slurrying behavior difference is larger.Particularly reed is extracted after hemicellulose through prehydrolysis, and the lignin structure of reed residue compared with reed raw material, has had very large change with reactivity worth, also have impact on the slurrying behavior of reed residue and the performance of reed pulp after preextraction hemicellulose.
In high boiling solvent (hbs) digestion process, under the heat effect of solvent, the hemicellulose of plant material is degraded, and the residual sugar of generation is dissolved in raffinate.Boiling raffinate contains height and to boil the derivative etc. of alcohol, low molecule quality lignin, hemicellulose carbohydrate and sugar.From the raffinate of high boiling solvent (hbs) pulping and digesting, isolate large molecular mass lignin ratio be easier to, but low molecule quality lignin is a large difficult point with being separated of carbohydrate.
Hemicellulose is dissolved in slurrying raffinate, not only bad for the process of raffinate, but also due to the dissolving of sugar, makes the viscosity of raffinate high, adds the energy consumption of high boiling solvent (hbs) separation and recovery system.
In recent years, the New York State University of the U.S. proposes the technology of comprehensive forestry biomass refinery plant.Its core technology is that traditional kraft pulp mills is transformed, before slurrying, with weakly acidic pH, acidity or alkaline aqueous solution, prehydrolysis is carried out to wood chip, extract part hemicellulose and be translated into ethanol and saccharide compound again, produce various chemicals further, pretreated wood chip obtains slurry paper product by chemical pulping, achieve effective utilization of lignocellulosic material each component, economic and social benefit is better than simple slurrying.
The hemicellulose level of reed is 20%-25%, and Main Ingredients and Appearance is poly-pentose, is wood sugar, xylo-oligosaccharide, xylitol, one of optimum feed stock of arabinose and ethanol.At present, reed or prepare paper pulp merely, or the simple sugar that extracts prepares saccharide compound or ethanol.The target product of these two kinds of modes of production is single, deficiency in economic performance.Also do not starch the reed comprehensive utilization technique scheme of considering every possible angle by extracting hemicellulose and preparing organic solvent at present.
Summary of the invention
One of technical problem to be solved by this invention is to provide a kind of reed prehydrolysis to extract the technique of hemicellulose.Make pre-hydrolyzed solution can Appropriate application, do not affect again follow-up reed pulp performance.
Two of technical problem to be solved by this invention is to provide a kind of reed residue of preextraction hemicellulose the high alcohol method pulping process that boils.
Three of technical problem to be solved by this invention is to provide the product of the reed organic solvent slurry adopting above-mentioned preextraction hemicellulose obtained by pulping process, comprises reed extract and reed pulp.
thisinvent the purposes that four of technical problem to be solved is to provide above-mentioned reed extract and reed organic solvent slurry product.
The present invention solves the problems of the technologies described above taked technical scheme: the high alcohol method pulping technique that boils of a kind of reed of preextraction hemicellulose, comprises the steps:
(1) reed dry and wet stock preparation, reed uniform cut, through winnowing machine removing lightweight dust, the fine impurities such as silt, reed marrow is screened out again through rotary strainer, finally by dust removal machine removing reed leaf, reed film etc., there is provided length 20-40mm, the reed sheet of qualification rate more than 85% is through the further removal of impurities of water washing, and the reed mass dryness fraction after dehydration is not less than 35%;
(2) prehydrolysis: carry out in digester, water is as the Extraction solvent of hemicellulose.Process conditions are: to clean over dry reed raw material, solid-to-liquid ratio is 1: 3 ~ 7, is warming up to 150 ~ 190 DEG C, is incubated 30 ~ 240 minutes at this temperature, hydrolysis endpoint pH is 2.5 ~ 4.5, and controlled hydrolysis process and hydrolysate are to pentose sugar concentration≤40% of extract;
(3) solid-liquor separation and washing, collects filtrate and obtains extract, collect residue for subsequent use;
(4) the high alcohol legal system of boiling of reed residue is for paper pulp;
(5) reed pulp washing after boiling.
On the basis of such scheme, in step (3), the hydrolysate of continuous squeezing mode to step (2) is adopted to carry out solid-liquor separation and multistage counter current washing (carrying out multistage counter current washing with filtered fluid and clear water), collect dense filtrate and obtain extract, collect residue for subsequent use.
Continuous squeezing mode and multistage counter current washing technology adopt known and disclosed technical scheme, it can be screw extrusion, roll press or vacuum filtration etc., the first paragraph washing of second segment filtrate and squeezing, second segment the 3rd section of filtrate washing and squeezing, the rest may be inferred, final stage clear water washing and squeezing, collect the dense filtrate of first paragraph and obtain extract, collect final stage residue for subsequent use.
On the basis of such scheme, in step (4), reed residue puts into digester boiling, the butanediol amount adopted is butanediol: water=40% ~ 60% (percent by volume), liquor ratio is reed residue: liquid=1: 4 ~ 10 (kg/l), boiling temperature 160 ~ 200 DEG C, temperature retention time 60 ~ 180min, reed is fully dissolved, obtains paper pulp.
On the basis of such scheme, reed pulp washing after boiling in step (4).First wash with butanediol, cleaning solution is the concentration prepared by liquor ratio 1: 7 ~ 9 is the butanediol of 50% ~ 60% (volume ratio), and wash temperature is 50 DEG C-60 DEG C.Then clear water wash clean is used at normal temperatures and pressures.
Adopt the product of reed organic solvent slurry obtained by pulping process of above-mentioned preextraction hemicellulose, for getting the raw materials ready through the reed of step (1) to (3), the reed extract that obtains of prehydrolysis and solid-liquor separation, to over dry reed raw material, reed pentose recovery rate is 20% ~ 40%, extracting liquid pH value is 2.5 ~ 4.5, and component comprises xylo-oligosaccharide, wood sugar, arabinose, glucose, lignin, furfural, uronic acid and acetic acid.
For the purposes of above-mentioned reed extract product, known and disclosed technology can be adopted to the further process of extract and following process, as acid hydrolysis, decolouring, depickling, concentrated, purification, ion-exchange, dehydration, hydrogenation synthesis, biofermentation, enzyme hydrolysis, chromatography, ultrafiltration, crystallization and spraying dry etc., make wood sugar, xylo-oligosaccharide, xylitol further, the products such as arabinose, also can make ethanol and other fermented product by acid hydrolysis, concentrated, purification, biofermentation, distillation.
Adopt the product of reed organic solvent slurry obtained by pulping process of above-mentioned preextraction hemicellulose, for the reed obtained to (5) through step (1) is slightly starched, to over dry reed raw material, unscreened yield is 48 ~ 55%, and thick slurry Kappa number is 29 ~ 35.
For the purposes of above-mentioned thick slurry product, adopt known and disclosed technology, as washing, screening and bleaching etc. slightly will starch the obtained bleach chemical pulp of processing further.
Beneficial effect of the present invention is: be not hydrolyzed extract hemicellulose reed raw material compared with, reed is after prehydrolysis, and under identical Pulping conditions, the Kappa number of gained slurry reduces 5-8 unit.Pulping efficiency after prehydrolysis process obviously improves.
Hemicellulose extract component comprises xylo-oligosaccharide, wood sugar, arabinose, glucose, lignin, furfural, uronic acid and acetic acid etc., but the content of the non-saccharide foreign organic matters such as the furfural in extract and lignin is low, extract may be used for the preparation of the food additives such as xylo-oligosaccharide, wood sugar, xylitol, arabinose and ethanol and chemical products.
Before slurrying, carry out prehydrolysis extract hemicellulose, the hemicellulose extracted can be used for preparing saccharide compound or ethanol, and pretreated reed residue is used for the production of paper pulp.This technology path, can reduce the difficult point that in high boiling solvent (hbs) recovery, sugared content is high, can realize again effectively utilizing at the multicomponent of pulping process Wooden Biomass raw material, improve the added value of byproduct, balance high boiling solvent (hbs) slurrying financial cost.
Detailed description of the invention
Below in conjunction with embodiment, the present invention will be further described, it should be understood that these embodiments only for the object of illustration, never limit the scope of the invention.
Embodiment 1
(1) reed dry and wet stock preparation, reed uniform cut, through winnowing machine removing lightweight dust, the fine impurities such as silt, reed marrow is screened out again through rotary strainer, finally by dust removal machine removing reed leaf, reed film etc., there is provided length 20-40mm, the reed sheet of qualification rate more than 85% is through the further removal of impurities of water washing, and the reed mass dryness fraction after dehydration is not less than 35%.
(2) prehydrolysis: carry out in digester, process conditions are: to over dry reed raw material, and solid-to-liquid ratio is 1: 4, and hydrolysis temperature is 160 DEG C, and pressure is the saturated vapour pressure under relevant temperature, and temperature retention time is 180 minutes, and hydrolysis endpoint pH is 4.3.
(3) solid-liquor separation and washing, collect filtrate and obtain extract, reed pentose recovery rate is 35.6%.Three sections of vacuum filters are adopted to carry out solid-liquor separation and countercurrent washing to hydrolysate, the first paragraph washing of second segment filtrate and squeezing, second segment the 3rd section of filtrate washing and squeezing, 3rd section washes with water and squeezes, the dense filtrate of collecting first paragraph obtains extract, collect the 3rd section of residue for pulping by cooking, residue mass dryness fraction is not less than 35%.
(4) the high alcohol method pulping by cooking that boils of reed residue: to over dry reed residue, the butanediol amount adopted is butanediol: water=60% (percent by volume), liquor ratio is reed raw material: liquid=1: 6, be rapidly heated, boiling temperature 190 DEG C, temperature retention time 60min, makes reed fully dissolve, obtains paper pulp.
(5) wash: first wash with butanediol, wash with the butanediol solution of 50% (volume ratio), liquor ratio 1:7, wash temperature is 60 DEG C.Then clear water wash clean is used at normal temperatures and pressures.Reed unscreened yield 53%, Kappa number 33.
Embodiment 2
(1) reed dry and wet stock preparation, with embodiment 1.
(2) prehydrolysis: carry out in digester, process conditions are: to over dry reed raw material, and solid-to-liquid ratio is 1: 5, and hydrolysis temperature is 170 DEG C, and pressure is the saturated vapour pressure under relevant temperature, and temperature retention time is 60 minutes, and hydrolysis endpoint pH is 4.1.
(3) solid-liquor separation and washing, collects filtrate and obtains extract: reed pentose recovery rate is 36.5%, and method of operating is with embodiment 1.
(4) reed residue pulping by cooking: to over dry reed residue, the butanediol amount adopted is butanediol: water=60% (percent by volume), liquor ratio is reed raw material: liquid=1: 5 (kg/l), be rapidly heated, boiling temperature 180 DEG C, temperature retention time 80min, makes reed fully dissolve, obtains paper pulp.
(5) wash: first wash with butanediol, wash with the butanediol solution of 60% (volume ratio).Wash temperature is 60 DEG C, liquor ratio 1:8.Then clear water wash clean is used at normal temperatures and pressures.Reed unscreened yield 52%, Kappa number 31.
Embodiment 3
(1) reed dry and wet stock preparation, with embodiment 1.
(2) prehydrolysis: carry out in digester, process conditions are: to over dry reed raw material, and solid-to-liquid ratio is 1: 6, and hydrolysis temperature is 180 DEG C, and pressure is the saturated vapour pressure under relevant temperature, and temperature retention time is 40 minutes, and hydrolysis endpoint pH is 3.8.
(3) solid-liquor separation and washing, collect filtrate and obtain extract, reed pentose recovery rate is 37.3%, and concrete operation method is with embodiment 1.
(4) reed residue pulping by cooking: to over dry reed residue, the butanediol amount adopted is butanediol: water=50% (percent by volume), liquor ratio is reed raw material: liquid=1: 5 (kg/l), be rapidly heated, boiling temperature 180 DEG C, temperature retention time 60min, makes reed fully dissolve, obtains paper pulp.
(5) wash: first wash with butanediol, wash with the butanediol solution of 50% (volume ratio).Wash temperature is 50 DEG C, liquor ratio 1:8.Then clear water wash clean is used at normal temperatures and pressures.Reed unscreened yield 51%, Kappa number 32.
Claims (6)
1. the pulping process of the reed organic solvent slurry of preextraction hemicellulose, is characterized in that: sequentially comprise the steps:
(1) reed dry and wet stock preparation, provides length 20-40mm, qualification rate >=85%, and mass dryness fraction is not less than the reed sheet of 35%;
(2) prehydrolysis: carry out in digester, water is as the Extraction solvent of hemicellulose, and process conditions are: to clean over dry reed raw material, solid-to-liquid ratio is 1: 3 ~ 7, be warming up to 150 ~ 190 DEG C, be incubated 30 ~ 240 minutes at this temperature, hydrolysis endpoint pH is 2.5 ~ 4.5;
(3) solid-liquor separation and washing, collect filtrate and obtain extract, its component comprises xylo-oligosaccharide, wood sugar, arabinose, glucose, lignin, furfural, uronic acid and acetic acid, and to over dry reed raw material, reed pentose recovery rate is 20 ~ 40%;
(4) reed residue of preextraction hemicellulose puts into digester boiling, the butanediol amount adopted is butanediol: water=40% ~ 60% (percent by volume), liquor ratio is reed residue: liquid=1: 4 ~ 10 (kg/l), boiling temperature 160 ~ 200 DEG C, temperature retention time 60 ~ 180min, reed is fully dissolved, obtains paper pulp;
(5) reed pulp washing after boiling, the butanediol of cleaning solution for by the concentration of liquor ratio 1: 7 ~ 9 preparation being 50% ~ 60% (volume ratio), wash temperature is 50 DEG C-60 DEG C, first washes with butanediol, then uses clear water wash clean at normal temperatures and pressures.
2. preextraction hemicellulose according to claim 1
'sreed organic solvent slurry pulping process, is characterized in that: in step (3), adopts the product of continuous squeezing mode to step (2) to carry out solid-liquor separation, collects filtrate and obtains extract, collect residue for subsequent use.
3. adopt the reed extract product obtained by preparation method of the reed organic solvent slurry of the preextraction hemicellulose described in claim 1 or 2, it is characterized in that: be the reed extract obtained through step (1) to (3), to over dry reed raw material, reed pentose recovery rate is 20 ~ 40%, extracting liquid pH value is 2.5 ~ 4.5, and component comprises xylo-oligosaccharide, wood sugar, arabinose, glucose, lignin, furfural, uronic acid and acetic acid.
4. for the purposes of reed extract product according to claim 3, it is characterized in that: described reed extract is used for the preparation of wood sugar, xylo-oligosaccharide, xylitol, arabinose or ethanol.
5. adopt the reed obtained by preparation method of the slurry of the reed organic solvent described in claim 1 ~ 2 slightly to starch product, it is characterized in that: for the reed obtained to (5) through step (1) is slightly starched, to initial over dry reed raw material, the yield that reed is slightly starched is 48-55%, and thick slurry Kappa number is 29-35.
6. slightly starch the purposes of product for reed according to claim 5, it is characterized in that: described reed slightly starches the preparation for bleach chemical pulp.
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| CN106012654A (en) * | 2016-06-11 | 2016-10-12 | 苏州思创源博电子科技有限公司 | Preparation method for high-quality paper pulp |
| CN108842008A (en) * | 2018-07-11 | 2018-11-20 | 北京林业大学 | A kind of method that the hydro-thermal acidolysis of slurrying pre-hydrolyzed solution prepares xylo-oligosaccharide solution |
| CN111945453A (en) * | 2020-08-18 | 2020-11-17 | 何建设 | Preparation method of loofah sponge dissolving pulp |
| CN112064394A (en) * | 2020-09-10 | 2020-12-11 | 大连工业大学 | Method for obtaining high-purity cellulose and modified lignin by preprocessing reed |
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| CN106012654A (en) * | 2016-06-11 | 2016-10-12 | 苏州思创源博电子科技有限公司 | Preparation method for high-quality paper pulp |
| CN108842008A (en) * | 2018-07-11 | 2018-11-20 | 北京林业大学 | A kind of method that the hydro-thermal acidolysis of slurrying pre-hydrolyzed solution prepares xylo-oligosaccharide solution |
| CN111945453A (en) * | 2020-08-18 | 2020-11-17 | 何建设 | Preparation method of loofah sponge dissolving pulp |
| CN112064394A (en) * | 2020-09-10 | 2020-12-11 | 大连工业大学 | Method for obtaining high-purity cellulose and modified lignin by preprocessing reed |
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| CN104988783B (en) | 2017-03-08 |
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