CN104988783B - Pulping process of phragmites communiss organic solvent slurry of preextraction hemicellulose and products thereof - Google Patents
Pulping process of phragmites communiss organic solvent slurry of preextraction hemicellulose and products thereof Download PDFInfo
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- CN104988783B CN104988783B CN201510433913.7A CN201510433913A CN104988783B CN 104988783 B CN104988783 B CN 104988783B CN 201510433913 A CN201510433913 A CN 201510433913A CN 104988783 B CN104988783 B CN 104988783B
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- phragmites communiss
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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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- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
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- General Health & Medical Sciences (AREA)
- Molecular Biology (AREA)
- Biochemistry (AREA)
- 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 present invention relates to pulping process of phragmites communiss organic solvent slurry of preextraction hemicellulose and products thereof.Method includes：Phragmites communiss are got the raw materials ready；Prehydrolysis；Solid-liquor separation and washing；Residue high boiling alcohol method prepares paper pulp.Said method obtains reed pulp and the phragmites communiss extracting solution that can prepare saccharide compound or ethanol.Compared with not hydrolyzing the phragmites communiss raw material extracting hemicellulose, after prehydrolysis, under identical Pulping conditions, the Kappa number of gained slurry reduces 58 units to phragmites communiss.Carry out prehydrolysis and extract hemicellulose before slurrying, the high difficult point of sugared content in high boiling solvent (hbs) recovery system can be reduced, can achieve each component effectively utilizes of Wooden Biomass raw material again, improve the added value of side-product, the Financial cost of balance high boiling solvent (hbs) slurrying.
Description
Technical field
The present invention relates to Chemical Engineering, phragmites communiss pulping process field are and in particular to a kind of phragmites communiss of preextraction hemicellulose
Organic solvent slurry pulping process and products thereof.
Background technology
The timber resources of China extremely lacks, and paper making raw material bottleneck is particularly thorny.Phragmites communiss are that a kind of important non-timber is made
Paper material, has higher cost performance.Therefore, the non-wood material such as scientific and reasonable utilization phragmites communiss can solve China's paper making raw material
Not enough problem.
Organic solvent pulping is a kind of free of contamination free pulping method, and high boiling solvent (hbs) slurrying belongs to organic solvent system
The category of paste-making method.Document 1 bagasse high boiling solvent method slurrying pre-test --《Chinese papermaking》06 phase in 2008, document 2 height boiling
Alcohol method（HBS method）Prepare yellow pulp and lignin --《Min Jiang institute journal》02 phase in 2003 reports bagasse and Caulis et Folium Oryzae is adopted
The high boiling alcohol pulping process being steaming and decocting solvent with 1,4- butanediol.Although phragmites communiss and bagasse, Caulis et Folium Oryzae belongs to non-wood material together, raw
Long feature and raw material mix differ, and therefore their slurrying behavior difference is larger.Particularly phragmites communiss extract half through prehydrolysis
After cellulose, the lignin structure of reed residue compared with phragmites communiss raw material, has very big change, also have impact on pre- carrying with reactivity worth
Take the slurrying behavior of reed residue and the performance of reed pulp after hemicellulose.
In high boiling solvent (hbs) digestion process, under the heat effect of solvent, the hemicellulose of plant material is degraded, and produces
Raw residual sugar is dissolved in residual liquid.Steaming and decocting residual liquid contains high boiling alcohol, low molecule quality lignin, hemicellulose saccharide and sugar
Derivant etc..Isolate macromole quality lignin to be easier from the residual liquid of high boiling solvent (hbs) pulping and digesting, but, low molecule
It is a big difficult point that quality lignin is separated with saccharide.
Hemicellulose is dissolved in slurrying residual liquid, not only bad for the process of residual liquid, but also due to sugared dissolving, makes residual
The viscosity of liquid is high, increased 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 skill
Art is traditional kraft pulp mills transformation, carries out pre- water with weakly acidic pH, acidity or alkaline aqueous solution to wood chip before slurrying
Solution, extracts part hemicellulose and is translated into ethanol and saccharide compound again, produce various chemicals further, pre- place
Wood chip after reason obtains slurry paper product it is achieved that the effectively utilizes of lignocellulosic material each component, warp by chemical pulping
Ji and social benefit are than simple slurrying more preferably.
The hemicellulose level of phragmites communiss is 20%-25%, and Main Ingredients and Appearance is poly-pentose, is xylose, oligomeric xylose, xylitol,
One of optimum feed stock of arabinose and ethanol.At present, phragmites communiss or prepare paper pulp merely, or the simple sugar that extracts prepares saccharide
Compound or ethanol.The target product of both modes of production is single, deficiency in economic performance.There is presently no and will extract hemicellulose
With the phragmites communiss comprehensive utilization technique scheme preparing organic solvent slurry comprehensive consideration.
Content of the invention
The technique that one of the technical problem to be solved is to provide a kind of phragmites communiss prehydrolysis to extract hemicellulose.
So that pre-hydrolyzed solution can be rationally utilized, and do not affect follow-up reed pulp performance.
The two of the technical problem to be solved are to provide a kind of reed residue height boiling of preextraction hemicellulose
Alcohol method pulping process.
The three of the technical problem to be solved are to provide the phragmites communiss using above-mentioned preextraction hemicellulose organic
The product obtained by pulping process starched by solvent, including phragmites communiss extracting solution and reed pulp.
The four of the technical problem to be solved are to provide above-mentioned phragmites communiss extracting solution and phragmites communiss organic solvent slurry to produce
The purposes of product.
The present invention solves above-mentioned technical problem and is adopted the technical scheme that：A kind of phragmites communiss height boiling of preextraction hemicellulose
Alcohol method pulping technique, comprises the steps：
(1) phragmites communiss dry and wet stock preparation, phragmites communiss uniform cut, removes lightweight dust through winnower, then screens out mud through rotary strainer
The fine impurities such as sand, reed marrow, last removing dust machine removes Folium Phragmitis, reed film etc., provides length 20-40mm, qualification rate is more than 85%
Reed piece through the further remove impurity of water washing, the phragmites communiss mass dryness fraction after dehydration is not less than 35%；
(2) prehydrolysis：Digester is carried out, water is as the Extraction solvent of hemicellulose.Process conditions are：To clean
Over dry phragmites communiss raw material, solid-to-liquid ratio be 1: 3～7, be warming up to 150～190 DEG C, at this temperature be incubated 30～240 minutes, hydrolysis
Endpoint pH is 2.5～4.5, controls hydrolysis process and hydrolyzate to pentose sugar concentration≤40% of extracting solution；
(3) solid-liquor separation and washing, collects filtrate and extracting solution is obtained, collect residue standby；
(4) reed residue high boiling alcohol method prepares paper pulp；
(5) reed pulp washing after steaming and decocting.
On the basis of such scheme, in step (3), using continuous squeezing mode, the hydrolyzate of step (2) is carried out
Solid-liquor separation and multistage counter current washing (carrying out multistage counter current with filtrate and clear water to wash), collect dense filtrate and extracting solution are obtained,
Collect residue standby.
Continuous squeezing mode and multistage counter current washing technology adopt known and disclosed technical scheme, can be that spiral squeezes
Pressure, roll press or vacuum filter etc., first paragraph wash with second segment filtrate and squeezes, second segment washed with the 3rd section of filtrate with
Squeezing, the rest may be inferred, and final stage is washed with clear water and squeezes, and collects the dense filtrate of first paragraph and extracting solution is obtained, collect last
Section residue is standby.
On the basis of such scheme, in step (4), reed residue puts into steaming and decocting in digester, the butanediol amount of employing
For butanediol: water=40%～60% (percent by volume), liquor ratio is reed residue: liquid=1: 4～10 (kg/l), steaming and decocting temperature
160～200 DEG C of degree, temperature retention time 60～180min, so that phragmites communiss is fully dissolved, obtain paper pulp.
On the basis of such scheme, reed pulp washing after steaming and decocting in step (4).First washed with butanediol, cleaning mixture is
The butanediol being 50%～60% (volume ratio) by the concentration that liquor ratio 1: 7～9 is prepared, wash temperature is 50 DEG C -60 DEG C.Then exist
Clear water wash clean is used under normal temperature and pressure.
Product obtained by pulping process is starched using the phragmites communiss organic solvent of above-mentioned preextraction hemicellulose, is through step
(1) the phragmites communiss extracting solution that the phragmites communiss to (3) are got the raw materials ready, prehydrolysis and solid-liquor separation obtain, to over dry phragmites communiss raw material, phragmites communiss pentose carries
Rate is taken to be 20%～40%, extracting liquid pH value is 2.5～4.5, and component includes oligomeric xylose, xylose, arabinose, glucose, wood
Quality, furfural, alduronic acid and acetic acid.
Extract the purposes of liquid product for above-mentioned phragmites communiss, process further and following process to extracting solution can adopt
Known and disclosed technology, such as acid hydrolysis, decolouring, deacidification, concentration, purification, ion exchange, dehydration, hydrogenation synthesis, biology are sent out
Ferment, enzyme hydrolysiss, chromatographic separation, ultrafiltration, crystallization and spray drying etc., make xylose, oligomeric xylose, xylitol further, I
The products such as primary sugar are it is also possible to make ethanol and other fermented product by acid hydrolysis, concentration, purification, biofermentation, distillation.
Product obtained by pulping process is starched using the phragmites communiss organic solvent of above-mentioned preextraction hemicellulose, is through step
(1) the phragmites communiss unscreened stock obtaining to (5), to over dry phragmites communiss raw material, unscreened yield is 48～55%, and unscreened stock Kappa number is 29～35.
For the purposes of above-mentioned unscreened stock product, using known and disclosed technology, such as wash unscreened stock, screen and bleach etc.
It is processed further bleach chemical pulp is obtained.
Beneficial effects of the present invention are：With do not hydrolyze extract hemicellulose phragmites communiss raw material compared with, phragmites communiss after prehydrolysis,
Under identical Pulping conditions, the Kappa number of gained slurry reduces 5-8 unit.Prehydrolysis process the pulping efficiency after being obviously improved.
Hemicellulose extract component includes oligomeric xylose, xylose, arabinose, glucose, lignin, furfural, alduronic acid
With acetic acid etc., but the content of the non-saccharide foreign organic matter such as the furfural in extracting solution and lignin is low, and extracting solution can be used for oligomeric wood
The food additive such as sugar, xylose, xylitol, arabinose and ethanol and the preparation of chemical products.
Carry out prehydrolysis and extract hemicellulose before slurrying, the hemicellulose extracting can be used for preparing saccharide compound or
Ethanol, pretreated reed residue is used for the production of paper pulp.This technology path, can reduce sugar during high boiling solvent (hbs) reclaims
The high difficult point of content, may be implemented in the multicomponent effectively utilizes of pulping process Wooden Biomass raw material again, improves the attached of side-product
Value added, balance high boiling solvent (hbs) slurrying Financial cost.
Specific embodiment
With reference to embodiment, the present invention will be further described it should be understood that these embodiments are only used for illustration
Purpose, be in no way intended to limit protection scope of the present invention.
Embodiment 1
(1) phragmites communiss dry and wet stock preparation, phragmites communiss uniform cut, removes lightweight dust through winnower, then screens out mud through rotary strainer
The fine impurities such as sand, reed marrow, last removing dust machine removes Folium Phragmitis, reed film etc., provides length 20-40mm, qualification rate is more than 85%
Reed piece through the further remove impurity of water washing, the phragmites communiss mass dryness fraction after dehydration is not less than 35%.
(2) prehydrolysis：Digester is carried out, process conditions are：To over dry phragmites communiss raw material, solid-to-liquid ratio is 1: 4, hydrolysis temperature
Spend for 160 DEG C, pressure is the saturated vapour pressure under relevant temperature, temperature retention time is 180 minutes, hydrolysis endpoint pH is 4.3.
(3) solid-liquor separation and washing, collects filtrate and extracting solution is obtained, and phragmites communiss pentose extraction ratio is 35.6%.Using three sections
Vacuum filter carries out solid-liquor separation and countercurrent washing to hydrolyzate, and first paragraph is washed with second segment filtrate and squeezes, second
Section is washed with the 3rd section of filtrate and is squeezed, and the 3rd section washes with water and squeeze, and the dense filtrate collecting first paragraph is obtained extracting solution, receives
Collect the 3rd section of residue for pulping by cooking, residue mass dryness fraction is not less than 35%.
(4) reed residue high boiling alcohol method pulping by cooking：To over dry reed residue, the butanediol amount of employing is butanediol: water
=60% (percent by volume), liquor ratio is phragmites communiss raw material: liquid=1: 6, it is rapidly heated, 190 DEG C of boiling temperature, temperature retention time
60min, makes phragmites communiss fully dissolve, obtains paper pulp.
(5) wash：First washed with butanediol, washed with the butanediol solution of 50% (volume ratio), liquor ratio 1:7, wash temperature
For 60 DEG C.Then use clear water wash clean at normal temperatures and pressures.Phragmites communiss unscreened yield 53%, Kappa number 33.
Embodiment 2
(1) phragmites communiss dry and wet stock preparation, with embodiment 1.
(2) prehydrolysis：Digester is carried out, process conditions are：To over dry phragmites communiss raw material, solid-to-liquid ratio is 1: 5, hydrolysis temperature
Spend for 170 DEG C, pressure is the saturated vapour pressure under relevant temperature, temperature retention time is 60 minutes, hydrolysis endpoint pH is 4.1.
(3) solid-liquor separation and washing, collects filtrate and extracting solution is obtained：Phragmites communiss pentose extraction ratio is 36.5%, operational approach
With embodiment 1.
(4) reed residue pulping by cooking：To over dry reed residue, the butanediol amount of employing is butanediol: water=60% (body
Long-pending percentage ratio), liquor ratio is phragmites communiss raw material: liquid=1: 5 (kg/l), is rapidly heated, 180 DEG C of boiling temperature, temperature retention time
80min, makes phragmites communiss fully dissolve, obtains paper pulp.
(5) wash：First washed with butanediol, washed with the butanediol solution of 60% (volume ratio).Wash temperature is 60 DEG C, liquid
Ratio 1:8.Then use clear water wash clean at normal temperatures and pressures.Phragmites communiss unscreened yield 52%, Kappa number 31.
Embodiment 3
(1) phragmites communiss dry and wet stock preparation, with embodiment 1.
(2) prehydrolysis：Digester is carried out, process conditions are：To over dry phragmites communiss raw material, solid-to-liquid ratio is 1: 6, hydrolysis temperature
Spend for 180 DEG C, pressure is the saturated vapour pressure under relevant temperature, temperature retention time is 40 minutes, hydrolysis endpoint pH is 3.8.
(3) solid-liquor separation and washing, collects filtrate and extracting solution is obtained, and phragmites communiss pentose extraction ratio is 37.3%, concrete operations
Method is with embodiment 1.
(4) reed residue pulping by cooking：To over dry reed residue, the butanediol amount of employing is butanediol: water=50% (body
Long-pending percentage ratio), liquor ratio is phragmites communiss raw material: liquid=1: 5 (kg/l), is rapidly heated, 180 DEG C of boiling temperature, temperature retention time
60min, makes phragmites communiss fully dissolve, obtains paper pulp.
(5) wash：First washed with butanediol, washed with the butanediol solution of 50% (volume ratio).Wash temperature is 50 DEG C, liquid
Ratio 1:8.Then use clear water wash clean at normal temperatures and pressures.Phragmites communiss unscreened yield 51%, Kappa number 32.
Claims (6)
1. preextraction hemicellulose phragmites communiss organic solvent slurry pulping process it is characterised in that：Sequentially comprise the steps：
(1) phragmites communiss dry and wet stock preparation, provides length 20-40mm, qualification rate >=85%, mass dryness fraction is not less than 35% reed piece；
(2) prehydrolysis：Digester is carried out, water as the Extraction solvent of hemicellulose, process conditions is：To clean over dry
Phragmites communiss 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, hydrolyzes terminal pH
It is worth for 2.5～4.5；
(3) solid-liquor separation and washing, collects filtrate and extracting solution is obtained, its component includes oligomeric xylose, xylose, arabinose, Portugal
Grape sugar, lignin, furfural, alduronic acid and acetic acid, to over dry phragmites communiss raw material, phragmites communiss pentose extraction ratio is 20～40%；
(4) reed residue of preextraction hemicellulose puts into steaming and decocting in digester, and the butanediol amount of employing is butanediol: water=
40%～60% (percent by volume), liquor ratio is reed residue: liquid=1: 4～10 (kg/l), 160～200 DEG C of boiling temperature,
Temperature retention time 60～180min, makes phragmites communiss fully dissolve, obtains paper pulp；
(5) reed pulp washing after steaming and decocting, cleaning mixture is the concentration by liquor ratio 1: 7～9 preparation is 50%～60% (volume ratio)
Butanediol, wash temperature be 50 DEG C -60 DEG C, first washed with butanediol, then use clear water wash clean at normal temperatures and pressures.
2. preextraction hemicellulose according to claim 1 phragmites communiss organic solvent slurry pulping process it is characterised in that：Step
Suddenly, in (3), solid-liquor separation is carried out using continuous squeezing mode to the product of step (2), collects filtrate and extracting solution is obtained, collect residual
Slag is standby.
3. adopt obtained by the preparation method of phragmites communiss organic solvent slurry of preextraction hemicellulose described in claim 1 or 2
Phragmites communiss extract liquid product it is characterised in that：It is the phragmites communiss extracting solution obtaining through step (1) to (3), to over dry phragmites communiss raw material, reed
Reed pentose extraction ratio is 20～40%, and extracting liquid pH value is 2.5～4.5, and component includes oligomeric xylose, xylose, arabinose, Portugal
Grape sugar, lignin, furfural, alduronic acid and acetic acid.
4. be directed to claim 3 described in phragmites communiss extract liquid product purposes it is characterised in that：Described phragmites communiss extracting solution is used for
The preparation of xylose, oligomeric xylose, xylitol, arabinose or ethanol.
5. adopt the phragmites communiss unscreened stock product obtained by preparation method of the phragmites communiss organic solvent slurry described in claim 1～2, it is special
Levy and be：It is the phragmites communiss unscreened stock obtaining through step (1) to (5), to initial over dry phragmites communiss raw material, the yield of phragmites communiss unscreened stock is 48-
55%, unscreened stock Kappa number is 29-35.
6. be directed to claim 5 described in phragmites communiss unscreened stock product purposes it is characterised in that：Described phragmites communiss unscreened stock is used for bleaching
The preparation of 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 |
| ES2915174B2 (en) * | 2020-12-18 | 2023-01-04 | Instituto Nac De Investigacion Y Tecnologia Agraria Y Alimentaria Inia | PROCEDURE FOR OBTAINING REINFORCED PACKAGING PAPER |
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| ZA75370B (en) * | 1974-02-15 | 1976-01-28 | H Funk | Method of treating bagasse |
| CN101613970B (en) * | 2009-06-09 | 2012-10-03 | 上海士林纤维材料有限公司 | Method for preparing bagasse dissolving pulp and pre-extracting hemicellulose and product thereof |
| CN101701429B (en) * | 2009-10-26 | 2011-06-29 | 昆明理工大学 | Method for improving yield and viscosity of gum wood pulp under condition of stewing mild sulfate |
| US9371612B2 (en) * | 2011-02-22 | 2016-06-21 | Andritz Inc. | Method and apparatus to produce pulp using pre-hydrolysis and Kraft cooking |
| CN102995475B (en) * | 2012-11-16 | 2014-09-03 | 昆明理工大学 | Extraction method of bagasse cellulose |
| CN103711017B (en) * | 2014-01-06 | 2016-05-11 | 海宁朗赛纤维科技有限公司 | A kind ofly prepare the method for cellulose and lignin as solvent normal pressure ultrasonic wave is auxiliary taking the height alcohol that boils |
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