CN102585247B - A kind of method utilizing lignocellulose residue from enzymatic hydrolysis to prepare lignosulfonates - Google Patents
A kind of method utilizing lignocellulose residue from enzymatic hydrolysis to prepare lignosulfonates Download PDFInfo
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- CN102585247B CN102585247B CN201210011668.7A CN201210011668A CN102585247B CN 102585247 B CN102585247 B CN 102585247B CN 201210011668 A CN201210011668 A CN 201210011668A CN 102585247 B CN102585247 B CN 102585247B
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Abstract
The present invention relates to a kind of method utilizing lignocellulose residue from enzymatic hydrolysis to prepare lignosulfonates, it is to the acid hydrolysis residue obtained after lignocellulosic material diluted acid method pretreatment, enzymolysis is carried out with cellulase and xylanase, obtain residue from enzymatic hydrolysis, with bisulfite method digesting technoloy, residue from enzymatic hydrolysis is carried out steaming and decocting, sulfonation again, prepare lignin sulfonic acid product salt.The inventive method improves the utilization rate of lignocellulosic material, has preferable economic and social benefit.
Description
Technical field
The invention belongs to biological fermentation engineering field, specifically, relate to one and utilize wooden
Cellulase hydrolysis residue prepares the method for lignosulfonates.
Background technology
Lignocellulosic sources is Renewable resource the abundantest on the earth, according to measuring and calculating gross annual output
Amount up to 150,000,000,000 tons, accumulates and stores up huge biomass energy.China is a large agricultural country,
The annual production of crop material (such as Caulis et Folium Oryzae, straw etc.) is the hugest (to be produced per year up to 700,000,000 tons of left sides
The right side, is equivalent to 500,000,000 tons of mark coals), according to statistics, current straw utilization rate 33%, but pass through
Utilize after certain technical finesse only accounts for 2.6%, and remaining major part is intended only as fuel etc. directly
Utilizing, DEVELOPMENT PROSPECT is boundless.If can be by a part therein for lignocellulosic sources
It is converted into chemicals or the energy, huge economic and social benefit will be produced.Traditional is wooden
Cellulose resource utilization ways is more single, and in addition to going back field, main utilization ways is combustion
Burn, gasify and hydrolyze.
At present for the utilization of lignocellulose, applying more is to be former with lignocellulose
Material, hydrolyzes hemicellulose therein and cellulosic component, prepares sugar alcohol product or fermenting and producing
Ethanol and other organic acid product.Industrial lignin by fibrous raw material, pulping process and
The impact of the factors such as extracting method, physicochemical properties differ greatly, and typically have acid hydrolysis wood
Quality, alkali lignin, lignosulfonates, enzyme hydrolysis lignin etc..Enzyme hydrolysis lignin
Owing to there is higher activity close to initial wood mass procatarxis.The hemicellulose of lignocellulose
And cellulosic component be utilized after can produce substantial amounts of hydrolytic residue, the lignin of the overwhelming majority
Component still remains wherein, if not being used, will result in significant wastage.Therefore, further
The hydrolytic residue Development and Production lignin sulfonic acid salt product utilizing lignocellulose is the most necessary.
Summary of the invention
It is an object of the invention to provide one, to utilize lignocellulose residue from enzymatic hydrolysis to prepare wooden
The method of element sulfonate.
Lignocellulose residue from enzymatic hydrolysis can use sulfite cooking to prepare lignin sulfonic acid
Product salt.The purpose of sulphite steaming and decocting is by wooden with raw material of sulfite liquor
Element effect, generates lignin sulfonic acid and lignosulfonates, thus realizes dividing of raw material components
From.During sulfite cooking, whole physical-chemical reaction is broadly divided into two kinds of works
With.The first act as cooking liquor to the infiltration of raw material and sulfonation, and the second act as reaction
The dissolution of product and raw material are separated into threadiness paper pulp.Two kinds of effects occur, not simultaneously
Well-separated.Cooking liquor had both relied on the diffusion of cooking liquor itself and former to the infiltration of raw material
The capillarity of material, raises also by way of digestion process pressure and forces to penetrate into.Cooking liquor
Penetrate into after raw material, main with the lignin generation sulfonating reaction generation lignosulphonic acid in raw material or
Lignosulphonates, are referred to as sulfonated lignin, are dissolved in acid solution.
Of the present invention lignocellulose residue from enzymatic hydrolysis is utilized to prepare lignosulfonates
Method, comprises the following steps:
(1) diluted acid method pretreatment: under diluted acid, cryogenic conditions, lignocellulosic material is entered
Row pretreatment, solid-liquid separation, obtain acid hydrolysis residue；
(2) enzymolysis: utilize cellulase and xylanase that acid hydrolysis residue is carried out enzymolysis,
Remove major part cellulose and remaining hemicellulose, obtain residue from enzymatic hydrolysis；
(3) steaming and decocting, sulfonation: use bisulfite method digesting technoloy that residue from enzymatic hydrolysis is entered
Row steaming and decocting, sulfonation, prepare lignosulfonates.
Above-mentioned steps also include steaming and decocting, sulfonation after product concentrate after be spray-dried,
Obtain lignosulfonates powder product.
Described lignocellulosic material can be corn cob, corn straw, wheat stalk, height
Fine strain of millet straw, cotton stalk, soybean stalks, sunflower straw, Semen Sesami straw, peanut straw,
One or more in rape stalk, sweet potato vine and rice straw.
Wherein, in described step (1), diluted acid Cold pretreatment condition is: acid concentration
0.1%～2.0%, liquid-solid ratio 10～4: 1, temperature 100～150 DEG C, the time 10～180min；
Acid hydrolysis residue component is: content of cellulose: 40%～70%, hemicellulose level:
1%～15%, Kelly Clarkson content of lignin: 15%～30%, content of ashes: 1%～5%.
In described step (1), described acid can be in sulphuric acid, hydrochloric acid, phosphoric acid, formic acid
One；Dry substance concentration can regulate to 15%-18% by adding water.
In described step (2), cellulase consumption is 10～30FPIU/ gram of substrate, and wood is poly-
Carbohydrase consumption is 10～30FPIU/ gram of substrate.
In described step (2), enzymatic hydrolysis condition is: pH 4.5～5.2, rotating speed
50～200r/min, temperature is at 46～50 DEG C, and enzymolysis time is 24～72h.
Klason lignin content >=40% in residue from enzymatic hydrolysis.
In described step (3), residue from enzymatic hydrolysis water use regulation becomes concentration of substrate to be 5%～20%
Slurry, add sealed reactor after sodium sulfite, be warming up to temperature required beginning timing.
In described step (3), sodium sulfite quality and residue from enzymatic hydrolysis mass ratio during steaming and decocting
It is 1%～20%.
In described step (3), steaming and decocting, sulfonating conditions be: reaction temperature is 120～180
DEG C, the response time is 1～10h.
The present invention, with lignocellulose residue from enzymatic hydrolysis as raw material, uses bisulfite method to steam
Boil technique and prepare lignin sulfonic acid product salt, improve in lignocellulose for fermentation production process
In utilization rate to lignocellulosic material, it is achieved that recycling of industrial waste, reduce
Cost, is also significant in terms of reducing water environment pollution, has significant economy
Benefit and social benefit.The pH value when pH value of the inventive method enzyme hydrolysis and steaming and decocting relatively connects
Closely, residue from enzymatic hydrolysis can directly carry out steaming and decocting without regulation pH, technique is simple, it is simple to behaviour
Make.
Detailed description of the invention
Following example are used for illustrating the present invention, but are not limited to the scope of the present invention.?
In the case of present invention spirit and essence, to the inventive method, step or condition institute
The amendment made or replacement, belong to the scope of the present invention.If not specializing, in embodiment
The conventional means that technological means used is well known to those skilled in the art.
Embodiment 1
1.5kg corn cob joins in 9kg dilution heat of sulfuric acid, sulfuric acid concentration 1.2%, 118 DEG C
Under the conditions of steaming and decocting 120min.Reaction uses cloth bag centrifuge to carry out solid-liquid separation after terminating,
To acid hydrolysis residue.Acid hydrolysis residue adds in the reactor of band stirring, and add water regulation dry
Concentration, to 16%, regulates pH to 4.8, temperature 50 C, adds cellulase (20FPIU/
Gram cellulose) and xylanase (15FPIU/ gram of cellulose), speed of agitator 200r/min,
Using cloth bag centrifuge to carry out solid-liquid separation after enzymolysis 48h, filtrate is stand-by, filtering residue i.e. enzyme water
Solve residue, be used for preparing lignosulfonates.During steaming and decocting, concentration of substrate is 20%, sulfurous acid
Hydrogen sodium quality and residue from enzymatic hydrolysis mass ratio are 10%, and reaction temperature is 160 DEG C, during reaction
Between be 5h.It is 1.89mmol/CLS that reaction detects sulfonation degree after terminating, spray dried after concentration
Dry obtain yellowish-brown sodium lignin sulfonate powder product.After measured, sodium lignin sulfonate diminishing
Rate is 10.47%, meets the country of efficient retarding and water reducing agent in " concrete admixture " qualified
Product standard (GB8076-1997).
Embodiment 2
1.5kg corn straw joins in 15kg dilution heat of sulfuric acid, sulfuric acid concentration 0.8%,
Steaming and decocting 90min under the conditions of 125 DEG C.Reaction uses cloth bag centrifuge to carry out solid-liquid and divide after terminating
From, obtain acid hydrolysis residue.Acid hydrolysis residue enters in the reactor of band stirring, and the regulation that adds water is dry
Substrate concentration, to 18%, regulates pH to 5.1, temperature 49 DEG C, adds cellulase
(15FPIU/ gram of cellulose) and xylanase (20FPIU/ gram of cellulose), speed of agitator
150r/min, uses cloth bag centrifuge to carry out solid-liquid separation after enzymolysis 36h, filtrate is stand-by,
Filtering residue i.e. residue from enzymatic hydrolysis is used for preparing lignosulfonates.During steaming and decocting, concentration of substrate is
10%, sodium sulfite quality and residue from enzymatic hydrolysis mass ratio are 20%, and reaction temperature is
140 DEG C, the response time is 2h.It is 1.37mmol/CLS that reaction detects sulfonation degree after terminating,
It is spray-dried after concentration and obtains dark brown sodium lignin sulfonate powder product.After measured, wooden
Element sodium sulfonate water-reducing rate is 10.62%, meets retardation setting high efficiency diminishing in " concrete admixture "
The national certified products standard (GB8076-1997) of agent.
Embodiment 3
Wheat stalk 1.5kg joins in 10.5kg dilution heat of sulfuric acid, sulfuric acid concentration 2.0%,
Steaming and decocting 150min under the conditions of 105 DEG C.Reaction uses cloth bag centrifuge to carry out solid-liquid and divide after terminating
From, obtain acid hydrolysis residue.Acid hydrolysis residue enters in the reactor of band stirring, and the regulation that adds water is dry
Substrate concentration, to 15%, regulates pH to 4.6, temperature 48 DEG C, adds cellulase
(10FPIU/ gram of cellulose) and xylanase (30FPIU/ gram of cellulose), speed of agitator 50
R/min, uses cloth bag centrifuge to carry out solid-liquid separation after enzymolysis 72h, filtrate is stand-by, filtering residue
I.e. residue from enzymatic hydrolysis is used for preparing lignosulfonates.During steaming and decocting, concentration of substrate is 5%, sulfurous
Acid hydrogen sodium quality is 15% with residue from enzymatic hydrolysis mass ratio, and reaction temperature is 150 DEG C, reaction
Time is 3h.It is 1.76mmol/CLS that reaction detects sulfonation degree after terminating, and sprays after concentration
It is dried to obtain dark brown sodium lignin sulfonate powder product.After measured, sodium lignin sulfonate subtracts
Water rate is 11.29%, meets country's conjunction of efficient retarding and water reducing agent in " concrete admixture "
Lattice product standard (GB8076-1997).
Embodiment 4
1.5kg rice straw joins in 6kg dilute hydrochloric acid solution, concentration of hydrochloric acid 2.0%, and 100
Steaming and decocting 180min under the conditions of DEG C.Reaction uses cloth bag centrifuge to carry out solid-liquid separation after terminating,
Obtain acid hydrolysis residue.Acid hydrolysis residue adds in the reactor of band stirring, and the regulation that adds water is dry
Substrate concentration, to 16%, regulates pH to 4.5, temperature 50 C, adds cellulase
(30FPIU/ gram of cellulose) and xylanase (10FPIU/ gram of cellulose), speed of agitator
180r/min, uses cloth bag centrifuge to carry out solid-liquid separation after enzymolysis 24h, filtrate is stand-by,
Filtering residue i.e. residue from enzymatic hydrolysis, is used for preparing lignosulfonates.During steaming and decocting, concentration of substrate is
5%, sodium sulfite quality and residue from enzymatic hydrolysis mass ratio are 1%, and reaction temperature is 120
DEG C, the response time is 10h.It is 1.58mmol/CLS that reaction detects sulfonation degree after terminating, dense
It is spray-dried after contracting and obtains yellowish-brown sodium lignin sulfonate powder product.After measured, lignin
Sodium sulfonate water-reducing rate is 10.98%, meets efficient retarding and water reducing agent in " concrete admixture "
National certified products standard (GB8076-1997).
Embodiment 5
1.5kg broomcorn straw joins in 15kg dilute phosphoric acid solution, phosphoric acid concentration 2%, and 150
Steaming and decocting 90min under the conditions of DEG C.Reaction uses cloth bag centrifuge to carry out solid-liquid separation after terminating,
Obtain acid hydrolysis residue.Acid hydrolysis residue enters in the reactor of band stirring, and the regulation dry that adds water is dense
Degree, to 14%, regulates pH to 5.2, temperature 47 DEG C, adds cellulase (20FPIU/ gram
Cellulose) and xylanase (20FPIU/ gram of cellulose), speed of agitator 100r/min, enzyme
Using cloth bag centrifuge to carry out solid-liquid separation after solving 36h, filtrate is stand-by, filtering residue i.e. enzyme hydrolysis
Residue is used for preparing lignosulfonates.During steaming and decocting, concentration of substrate is 13%, sodium sulfite
Quality and residue from enzymatic hydrolysis mass ratio are 17%, and reaction temperature is 180 DEG C, and the response time is
1h.It is 1.37mmol/CLS that reaction detects sulfonation degree after terminating, and is spray-dried after concentration
To dark brown sodium lignin sulfonate powder product.After measured, sodium lignin sulfonate water-reducing rate is
10.31%, meet the national certified products mark of efficient retarding and water reducing agent in " concrete admixture "
Accurate (GB8076-1997).
Embodiment 6
Soybean stalks 1.5kg joins in 9kg dilute hydrochloric acid solution, concentration of hydrochloric acid 2.0%, and 121
Steaming and decocting 140min under the conditions of DEG C.Reaction uses cloth bag centrifuge to carry out solid-liquid separation after terminating,
Obtain acid hydrolysis residue.Acid hydrolysis residue enters in the reactor of band stirring, and the regulation dry that adds water is dense
Degree, to 17%, regulates pH to 4.7, temperature 46 DEG C, adds cellulase (10FPIU/ gram
Cellulose) and xylanase (25FPIU/ gram of cellulose), speed of agitator 80r/min, enzymolysis
Using cloth bag centrifuge to carry out solid-liquid separation after 60h, filtrate is stand-by, and filtering residue i.e. enzyme hydrolysis is residual
Slag is used for preparing lignosulfonates.During steaming and decocting, concentration of substrate is 15%, sodium sulfite matter
Amount and residue from enzymatic hydrolysis mass ratio are 8%, and reaction temperature is 170 DEG C, and the response time is 8h.
It is 6.83mmol/CLS that reaction detects sulfonation degree after terminating, and is spray-dried and obtains deeply after concentration
Brown sodium lignin sulfonate powder product.After measured, sodium lignin sulfonate water-reducing rate is 11.73
%, meets the national certified products standard of efficient retarding and water reducing agent in " concrete admixture "
(GB8076-1997)。
Although, the most with a general description of the specific embodiments the present invention is made
Detailed description, but on the basis of the present invention, it can be made some modifications or improvements, this
Will be apparent to those skilled in the art.Therefore, without departing from present invention spirit
On the basis of these modifications or improvements, belong to the scope of protection of present invention.
Claims (8)
1. utilize the method that lignocellulose residue from enzymatic hydrolysis prepares lignosulfonates,
Comprise the following steps:
(1) diluted acid method pretreatment: under diluted acid, cryogenic conditions, lignocellulosic material is carried out
Pretreatment, solid-liquid separation, obtain acid hydrolysis residue；In step (1), described diluted acid low temperature
Pretreatment condition is: acid concentration 0.1%～2.0%, diluted acid and the volume mass of lignocellulose
Ratio is 10～4: 1, temperature 100～150 DEG C, the time 90～180min；
(2) enzymolysis: utilize cellulase and xylanase that acid hydrolysis residue is carried out enzymolysis, from
The heart, filtration, filtrate is stand-by, filtering residue i.e. residue from enzymatic hydrolysis；In step (2), described fiber
Element enzyme dosage is 10～30FPIU/g substrates, and xylanase consumption is 10～30FPIU/g substrates；
Enzymatic hydrolysis condition is: pH 4.5～5.2, rotating speed 50～200r/min, temperature 46～50 DEG C, enzyme
The solution time 24～72h；
(3) steaming and decocting, sulfonation: use bisulfite method that residue from enzymatic hydrolysis is carried out steaming and decocting, sulphur
Change, prepare lignosulfonates.
2. the method for claim 1, it is characterised in that in step (1), described wooden
Cellulosic material be corn cob, corn straw, wheat stalk, broomcorn straw, cotton stalk,
Soybean stalks, sunflower straw, Semen Sesami straw, peanut straw, rape stalk, sweet potato vine and
One or more in rice straw.
3. the method for claim 1, it is characterised in that also include
(4) it is spray-dried after the product after steaming and decocting, sulfonation being concentrated, obtains lignin
Sulfonate powder product.
4. the method for claim 1, it is characterised in that in step (1), described acid
For the one in sulphuric acid, hydrochloric acid, phosphoric acid, formic acid, by adding water, dry substance concentration is regulated extremely
15%-18%.
5. the method for claim 1, it is characterised in that in step (1), described sour water
Solve residue component as follows: content of cellulose: 40%～70%, hemicellulose level: 1%～
15%, Kelly Clarkson content of lignin: 15%～30%, content of ashes: 1%～5%.
6. the method as described in claim 1-4 is arbitrary, it is characterised in that in step (2), institute
State in residue from enzymatic hydrolysis, Klason lignin content >=40%.
7. the method as described in claim 1-4 is arbitrary, it is characterised in that in step (3), steams
When boiling, residue from enzymatic hydrolysis mass percent is 5%～20%, sodium sulfite and residue from enzymatic hydrolysis
Mass ratio is 1%～20%.
8. the method as described in claim 1-4 is arbitrary, it is characterised in that in step (3), institute
State steaming and decocting, sulfonating reaction condition is: temperature 120～180 DEG C, and the response time is 1～10h.
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| CN105061779B (en) * | 2015-08-17 | 2017-07-21 | 湖州长盛化工有限公司 | A kind of preparation of modified sodium lignosulfonate |
| CN106317417A (en) * | 2016-08-19 | 2017-01-11 | 管天球 | Method for preparing sodium lignin sulfonate with camellia oleifera shells |
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| CN109251700A (en) * | 2018-07-05 | 2019-01-22 | 北京林业大学 | Multi-functional wooden cellulase hydrolysed ferment residue filler, preparation method and applications |
| CN109503859B (en) * | 2018-12-06 | 2021-04-27 | 齐鲁工业大学 | Method for preparing sodium lignosulfonate with high sulfonation degree by using wheat straws |
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| CN1264985C (en) * | 2003-12-18 | 2006-07-19 | 中国科学院理化技术研究所 | Process for preparing phenol and toluene from lignin by utilizing straw plants |
| CN101608192B (en) * | 2009-07-22 | 2012-04-04 | 安徽丰原发酵技术工程研究有限公司 | Method for producing succinic acid employing corn cob |
| CN101619332B (en) * | 2009-08-13 | 2012-05-23 | 安徽丰原发酵技术工程研究有限公司 | Method for efficiently saccharifying bagasse |
| CN102001841B (en) * | 2010-11-08 | 2012-05-30 | 福州大学 | Preparation method of zymolytic lignin modified water reducing agent |
| CN102140174B (en) * | 2011-03-08 | 2014-01-29 | 延边石岘白麓纸业股份有限公司 | Preparation method for lignosulfonate |
| CN102268139B (en) * | 2011-05-30 | 2013-08-14 | 中国科学院理化技术研究所 | Resin additive and preparation method and use thereof |
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