CN110130135A - A kind of method of acetic acid sodium sulfite collaboration preprocessing lignocellulose raw material - Google Patents
A kind of method of acetic acid sodium sulfite collaboration preprocessing lignocellulose raw material Download PDFInfo
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- CN110130135A CN110130135A CN201910451933.5A CN201910451933A CN110130135A CN 110130135 A CN110130135 A CN 110130135A CN 201910451933 A CN201910451933 A CN 201910451933A CN 110130135 A CN110130135 A CN 110130135A
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- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P19/00—Preparation of compounds containing saccharide radicals
- C12P19/02—Monosaccharides
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- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P19/00—Preparation of compounds containing saccharide radicals
- C12P19/14—Preparation of compounds containing saccharide radicals produced by the action of a carbohydrase (EC 3.2.x), e.g. by alpha-amylase, e.g. by cellulase, hemicellulase
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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
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P2201/00—Pretreatment of cellulosic or lignocellulosic material for subsequent enzymatic treatment or hydrolysis
Abstract
A kind of method of acetic acid sodium sulfite collaboration preprocessing lignocellulose raw material, it is pretreatment medium with acetic acid, alkaline sodium sulfite, collaboration pretreatment is carried out using high temperature oil bath pan and high temperature high pressure sterilizing pot, the following steps are included: S1: weighing raw material powder and put into reaction flask, acetic acid solution is added, it is put into high temperature oil bath pan and reacts after mixing, obtain dry powders A through cooling, suction filtration, washing, low temperature drying after the reaction was completed；S2: weighing powders A and be put into reaction flask, adds alkaline sodium sulfite solution, is put into high temperature high pressure sterilizing pot and reacts after mixing, obtains preprocessing lignocellulose raw material through cooling, suction filtration, washing, low temperature drying after the reaction was completed.The present invention is that pretreatment medium carries out collaboration pretreatment using high pressure oil bath pan and high temperature high pressure sterilizing pot, the quantum of output of cellulose obviously increases after pretreatment using different heat treatment temperatures with acetic acid and alkaline sodium sulfite.
Description
Technical field
The invention belongs to the matrix technology field of cellulose-containing material more particularly to a kind of collaboration of acetic acid sodium sulfite are pre-
The method for handling lignocellulosic material.
Background technique
China's timber biological matter yield is very high, but China's timber biological matter resource utilization is very low, biomass resource
Comprehensive utilization technique is also immature.Thermo-chemical treatment is the committed step that lignocellulosic biomass conversion is energy.Cellulose
It can be effectively utilized, and the saccharification of hemicellulose is also changed.Thermochemical treatment is to realize renewable wooden biological energy source
The committed step that cellulose efficiently utilizes in source and hemicellulose saccharification is converted.Difficulty can be quickly removed by preprocessing process
Molten lignin or the physico separation for realizing the hemicellulose in cell wall, so that the polysaccharide in plant cell wall passes through chemistry
It decomposes, increases lignocellulosic quantum of output.
Currently, since preprocessing method of raw materials and technological parameter not enough optimize, so that preprocessing process is complicated, when consuming
Between it is long, quantity of solvent is big, and economic cost is high, and carrying capacity of environment is also larger.Therefore, Wooden Biomass pretreatment is advanced optimized
Method, science use simple and easy, economical and efficient preprocess method, are the main sides of Wooden Biomass material energy conversion
To.Efficient and convenient pre-treatment solvents, optimization pretreatment time point and temperature parameter are selected, and effectively carries out preprocessing process
Operation is the main path for improving pretreatment efficiency and reducing cost.
Summary of the invention
It is an object of that present invention to provide a kind of acetic acid sodium sulfite collaboration preprocessing lignocellulose raw material method,
It is pretreatment medium with acetic acid and sodium hydroxide, sodium sulfite, makes full use of the collaboration of acetic acid and sodium hydroxide, sodium sulfite
Effect carries out the basic material property improvement of material, destroys the barrier of lignin, solves since the cladding bring of lignin is pre-
Processing difficulty is big, the low problem for the treatment of effeciency.
To achieve the above object, the present invention is achieved by following scheme:
A kind of method of acetic acid sodium sulfite collaboration preprocessing lignocellulose raw material is with acetic acid, alkaline sodium sulfite
Medium is pre-processed, carries out collaboration pretreatment using high temperature oil bath pan and high temperature high pressure sterilizing pot, comprising the following steps:
S1: weighing 12-15 parts of raw material powders and put into reaction flask, and it is molten to add the acetic acid that solid-liquid ratio is 1:8-12g/ml
Liquid tightens reaction bottle cap after mixing, is put into high temperature oil bath pan, and the temperature setting of high temperature oil bath pan is 165-175
DEG C, the hot operation time is 25-35min, takes out reaction flask after the reaction was completed, is cooled to room temperature, by the dirty solution in reaction flask
Body pours into suction funnel, using distilled water filtering and washing, cleans and filters repeatedly, until extracting liquid shows neutral out, in low temperature
Oven dried obtains dry powders A；
S2: weighing 10-12 parts of powders As and be put into reaction flask, adds the alkaline sulfurous acid that solid-liquid ratio is 1:8-12g/ml
Sodium solution tightens reaction bottle cap after mixing, is put into high temperature high pressure sterilizing pot, the temperature setting of high temperature high pressure sterilizing pot
At 118-122 DEG C, working time 55-65min takes out after the reaction was completed, is cooled to room temperature, by the dirty solution in reaction flask
Body pours into suction funnel, using distilled water filtering and washing, then cleans and filters repeatedly, low until extracting liquid shows neutral out
Temperature drying, obtains preprocessing lignocellulose raw material.
Further, acetic acid pretreatment temperature is set as 170 DEG C in step S1, and the processing time is 30min, hydrogen in step S2
Sodium oxide molybdena and sodium sulfite treatment temperature are 121 DEG C, and the processing time is 60min.
Further, step S1, the temperature of low temperature drying is 40-50 DEG C in S2 and S3, and the moisture content of powder is small after drying
In 10%.
Further, raw material powder is paulownia powder, and paulownia are broken into wood shavings, are ground into after dry with pulverizer tiny
The sieve of 80 mesh is crossed after graininess, raw material powder is made less than 10% in 40-50 DEG C of low temperature drying to moisture content.
Further, the mass concentration of acetic acid solution is 3-4.5%.
Further, the mass concentration of acetic acid solution is 4%.
Further, it is 3.5-5% sodium sulfite and 0.8-1.5% hydrogen-oxygen that alkaline sulfurous acid solution, which is containing mass concentration,
Change the mixed solution of sodium.
Further, alkaline sulfurous acid solution is the mixing for being 4% sodium sulfite and 1% sodium hydroxide containing mass concentration
Solution.
The beneficial effects of the present invention are:
The present invention is that pretreatment medium utilizes high temperature using different heat treatment temperatures with acetic acid, alkaline sodium sulfite
Oil bath pan and high temperature high pressure sterilizing pot carry out collaboration pretreatment, and the quantum of output of cellulose obviously increases after pretreatment.With acetic acid,
Alkaline sodium sulfite is pretreatment medium, and acetic acid, acting synergistically for alkaline sodium sulfite is made full use of to carry out the basic material of material
Property improvement, destroy the barrier of lignin, solve due to lignin cladding bring pretreatment difficulty it is big, low efficiency
Problem.Acetic acid, alkaline sodium sulfite collaboration pretreatment paulownia, heating are carried out using high temperature oil bath pan and high temperature high pressure sterilizing pot
Temperature is stably and controllable, and can get the pretreating effect of higher fiber cellulose content and enzymolysis process glucose yield, easy to operate
Safety, the cellulose rate of recovery is high, at low cost, economic and environment-friendly, is better than single solvent.
Detailed description of the invention
Fig. 1 is the method that the present invention implements the acetic acid provided, alkaline sodium sulfite collaboration preprocessing lignocellulose raw material
Flow chart；
Fig. 2 is the different pretreatments infrared spectrogram that the present invention implements the paulownia provided；
Fig. 3 is that the present invention implements the enzyme gradient comparison glucose and xylan hydrolysis variation of yield variation diagram that provide；
Fig. 4 be the present invention implement provide 48h and 72h under the conditions of, bis- generation of 30fpu enzymatic treatment paulownia raw cellulose and
Xylan variation of yield figure.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts it is all its
Its embodiment, shall fall within the protection scope of the present invention.
Embodiment 1
A kind of method of acetic acid sodium sulfite collaboration preprocessing lignocellulose raw material, comprising the following steps:
S1: weighing 12g raw material powder and put into reaction flask, adds the acetic acid solution that solid-liquid ratio is 1:10g/ml, mixing
Reaction bottle cap is tightened after uniformly, is put into high temperature oil bath pan, the temperature setting of high temperature oil bath pan is 170 DEG C, when hot operation
Between be 30min, take out reaction flask after the reaction was completed, be cooled to room temperature, the turbid liquid in reaction flask is poured into suction funnel,
It using distilled water filtering and washing, cleans and filters repeatedly, until extraction liquid shows neutral is done in low temperature oven dried
Dry powders A；
S2: weighing 10g powders A and be put into reaction flask, and it is molten to add the alkaline sodium sulfite that solid-liquid ratio is 1:10g/ml
Liquid tightens reaction bottle cap after mixing, is put into high temperature high pressure sterilizing pot, and the temperature of high temperature high pressure sterilizing pot is set in 121
DEG C, working time 60min takes out after the reaction was completed, is cooled to room temperature, and the turbid liquid in reaction flask is poured into suction filtration leakage
Then bucket is cleaned and is filtered repeatedly, until extracting liquid shows neutral out, low temperature drying is obtained pre- using distilled water filtering and washing
Handle lignocellulosic material.
Embodiment 2
A kind of method of acetic acid sodium sulfite collaboration preprocessing lignocellulose raw material, comprising the following steps:
S1: weighing 15g raw material powder and put into reaction flask, adds the acetic acid solution that solid-liquid ratio is 1:12g/ml, mixing
Reaction bottle cap is tightened after uniformly, is put into high temperature oil bath pan, the temperature setting of high temperature oil bath pan is 165 DEG C, when hot operation
Between be 25min, take out reaction flask after the reaction was completed, be cooled to room temperature, the turbid liquid in reaction flask is poured into suction funnel,
It using distilled water filtering and washing, cleans and filters repeatedly, until extraction liquid shows neutral is done in low temperature oven dried
Dry powders A；
S2: weighing 12g powders A and be put into reaction flask, and it is molten to add the alkaline sodium sulfite that solid-liquid ratio is 1:12g/ml
Liquid tightens reaction bottle cap after mixing, is put into high temperature high pressure sterilizing pot, and the temperature of high temperature high pressure sterilizing pot is set in 118
DEG C, working time 55min takes out after the reaction was completed, is cooled to room temperature, and the turbid liquid in reaction flask is poured into suction filtration leakage
Then bucket is cleaned and is filtered repeatedly, until extracting liquid shows neutral out, low temperature drying is obtained pre- using distilled water filtering and washing
Handle lignocellulosic material.
Embodiment 3
S1: weighing 12g raw material powder and put into reaction flask, adds the acetic acid solution that solid-liquid ratio is 1:10g/ml, mixing
Reaction bottle cap is tightened after uniformly, is put into high temperature oil bath pan, the temperature setting of high temperature oil bath pan is 165 DEG C, when hot operation
Between be 25min, take out reaction flask after the reaction was completed, be cooled to room temperature, the turbid liquid in reaction flask is poured into suction funnel,
It using distilled water filtering and washing, cleans and filters repeatedly, until extraction liquid shows neutral is done in low temperature oven dried
Dry powders A；
S2: weighing 10g powders A and be put into reaction flask, and it is molten to add the alkaline sodium sulfite that solid-liquid ratio is 1:10g/ml
Liquid tightens reaction bottle cap after mixing, is put into high temperature high pressure sterilizing pot, and the temperature of high temperature high pressure sterilizing pot is set in 118
DEG C, working time 55min takes out after the reaction was completed, is cooled to room temperature, and the turbid liquid in reaction flask is poured into suction filtration leakage
Then bucket is cleaned and is filtered repeatedly, until extracting liquid shows neutral out, low temperature drying is obtained pre- using distilled water filtering and washing
Handle lignocellulosic material.
Embodiment 4
S1: weighing 15g raw material powder and put into reaction flask, adds the acetic acid solution that solid-liquid ratio is 1:10g/ml, mixing
Reaction bottle cap is tightened after uniformly, is put into high temperature oil bath pan, the temperature setting of high temperature oil bath pan is 170 DEG C, when hot operation
Between be 30min, take out reaction flask after the reaction was completed, be cooled to room temperature, the turbid liquid in reaction flask is poured into suction funnel,
It using distilled water filtering and washing, cleans and filters repeatedly, until extraction liquid shows neutral is done in low temperature oven dried
Dry powders A；
S2: weighing 12g powders A and be put into reaction flask, and it is molten to add the alkaline sodium sulfite that solid-liquid ratio is 1:10g/ml
Liquid tightens reaction bottle cap after mixing, is put into high temperature high pressure sterilizing pot, and the temperature of high temperature high pressure sterilizing pot is set in 121
DEG C, working time 30min takes out after the reaction was completed, is cooled to room temperature, and the turbid liquid in reaction flask is poured into suction filtration leakage
Then bucket is cleaned and is filtered repeatedly, until extracting liquid shows neutral out, low temperature drying is obtained pre- using distilled water filtering and washing
Handle lignocellulosic material.
Comparative test
Taking the embodiment of the present invention 1 is experimental group 1, i.e., wooden using acetic acid, sodium sulfite and sodium hydroxide collaboration pretreatment
Cellulosic material obtains pretreated lignocellulosic material I.
Experimental group 2: lignocellulosic material II without any processing；
Experimental group 3: using acetic acid treatment lignocellulosic material, weigh 12g raw material powder and put into reaction flask, then plus
Enter the acetic acid solution that solid-liquid ratio is 1:10g/ml, tightens reaction bottle cap after mixing, be put into high temperature oil bath pan, high temperature oil
The temperature setting of bath is 170 DEG C, and the hot operation time is 30min, takes out reaction flask after the reaction was completed, is cooled to room temperature,
Turbid liquid in reaction flask is poured into suction funnel, using distilled water filtering and washing, cleans and filters repeatedly, until extraction
Liquid shows neutral obtains preprocessing lignocellulose raw material III in low temperature oven dried；
Experimental group 4: acetic acid and sodium sulfite preprocessing lignocellulose raw material are used, 10g powders A is weighed and is put into reaction
In bottle, the alkaline sodium sulfite solution that solid-liquid ratio is 1:10g/ml is added, reaction bottle cap is tightened after mixing, is put into height
In warm cannery retort, the temperature of high temperature high pressure sterilizing pot is set in 121 DEG C, and working time 60min takes after the reaction was completed
Out, it is cooled to room temperature, the turbid liquid in reaction flask is poured into suction funnel, using distilled water filtering and washing, then repeatedly
Cleaning and suction filtration, until extracting liquid shows neutral out, low temperature drying obtains preprocessing lignocellulose raw material IV.
The product obtained to above-mentioned 4 groups of experiments is analyzed:
1, structure table is carried out to pretreatment sample by FTIR spectrum, thermogravimetric analysis, scanning electron microscope
Sign, the variation of cellulose, hemicellulose, content of lignin before and after analysis sample pretreatment.
(1) the above-mentioned 4 groups products tested are carried out to the Image Acquisition of FTIR infrared spectroscopy, test equipment uses
Nicolet FTIR IS10, test wavelength range are 400~4000cm-1, spectral resolution 32cm-1, scanning times 64
It is secondary.The big component fibre element of paulownia three, hemicellulose and lignin, are changed in the content of the ingredient after pretreatment, because
This can show the infrared absorpting light spectra centainly changed in different wave bands, as shown in Figure 2.
The present invention is based on the Infrared spectra adsorption functional group ownership in each chemical composition change of paulownia after pretreatment, thermogravimetrics
The variation of analysis raw material degradation temperature and rate and the map observed of scanning electron microscope judge cellulose and half fiber
The composition transfer of dimension element and lignin.Larger change also occurs for functional group's ownership situation by bamboo wood under the conditions of different disposal
Change, for the ease of comparing, the present invention by the corresponding functional group of main band value in infrared spectroscopy stacking chart be summarized in table 1 to
Table 3:
The corresponding functional group in 1 cellulosic absorbent peak of table
The corresponding functional group of 2 hemicellulose absorption peak of table
The corresponding functional group in 3 lignin absorption peak of table
The map comprehensive change of cellulose, hemicellulose, lignin, the characteristic absorption peak 2924cm of cellulose-1With
3412cm-1.Hemicellulose is different from other compositions and is characterized in 1740 cm-1C=O on neighbouring acetyl group and carboxyl stretches
Contracting vibration absorption peak.1640cm-1Place is the conjugation aryl ketones C=O stretching vibration of lignin carbonyl, be can be seen that from spectrogram, pre- to locate
Manage the 1740cm of raw material-1And 1640cm-1The absorption peak of appearance becomes unobvious after by different pretreatments, says
After bright pretreatment, hemicellulose is degraded.In 1640cm-1The wave band of neighbouring absorption peak, pretreated feedstock map becomes
Suddenly, illustrate that content of lignin is reduced.
Cellulose is the straight chain high-molecular compound being made of D-Glucose base, and the infrared-sensitive group of cellulose is
Hydroxyl；Cellulose has a free hydroxyl on C4, has special X ray spectra.Hemicellulose is two or more
Monosaccharide composition inhomogenous glycan, containing acetyl group, the infrared-sensitives group such as hydroxyl, lignin this base benzene alkane passes through ether
The aromatic polymer compound that key and carbon-carbon bond are formed by connecting contains methoxyl group CH2O, hydroxyl, carbonyl C=in molecule
The a variety of infrared ray responsive groups of O, double bond C=O and phenyl ring etc..
By Fig. 1 it can be concluded that paulownia pretreatment front and back functional group content is changed, and different processing mode variations
Degree it is different, content of cellulose totally increases after pre-processing as seen from the figure, and the content of hemicellulose and lignin is
Decline, and acetic acid and the pretreating effect of alkaline sodium sulfite collaboration are best.
(2) TGA/DSC3 type thermogravimetric heating differential analysis instrument is selected, regards protective gas with nitrogen, protection air-flow amount is set as
20mL/min, 10 DEG C/min of heating rate, the range of pyrolysis reaction temperature are 50~600 DEG C.
The thermal stability analysis of pretreatment front and back paulownia, the highest big plain pyrolysis temperature of timber three is lignin, and paulownia are pre-
Thermal stability reduces after processing.By control compared to discovery, the corresponding temperature of biggest quality loss rate of paulownia heat-treated wood
Degree is all declined, and illustrates that pre-processing material shortens the time for reaching biggest quality loss rate, to illustrate wood after pyrolysis
The content of quality reduces.
(3) scanning electron microscope that scanning electron microscope is S3400 using number, operating voltage are 5.00KV object lens distance
It is amplified to for 10.1mm and starts to observe after 3000 times and focus, click preservation after finding suitable target.
The overscanning electron microscope atlas analysis of pretreatment front and back paulownia, can be found that the observation of sample surfaces pre-
The different disengaging degree to paulownia lignin portion with preprocess method before and after the processing pass through comparison picture discovery pretreatment
The preceding cellulose without the smooth growth strip in discovery surface, it is pretreated to be found, illustrate pretreatment departing from being wrapped in fibre
Lignin on dimension element.
2, the standard method according to (NREL) of U.S. Department of Energy is come cellulose in 4 groups of experimental products measuring, wooden
Element, the content of xylan are as shown in table 4 below:
The chemical constituent variation of sample under the conditions of 4 different pretreatments of table
From table 4, it can be seen that significant changes, and different processing has occurred in paulownia pretreatment front and back Main chemical component
Each component content that mode obtains is different, and identical point is that the content of cellulose after handling dramatically increases trend, lignin
Content is reduced, and containing for hemicellulose is reduced, wherein under three kinds of pretreatment ambient conditions, acetic acid and alkaline sodium sulfite collaboration
Pretreating effect it is best.
3, by 4 groups of experimental products at 50 degrees Celsius, revolving speed is tested are as follows: 240r/min makes enzyme hydrolysis sample: using 10,
20,30 (FPU/g DM) CTEC2 bis- generations enzymes comparison different as 3 kinds of concentration gradients.Select 48h and 72h as enzyme hydrolysis
Time point is analyzed.
The yield of sugar fermentation during the enzyme hydrolysis of cellulose is the important indicator for evaluating pretreating effect superiority and inferiority,
It is most direct index.Later cellulase hydrolysis effect is pre-processed in order to verify sodium sulfite collaboration under acetic acid and alkaline condition
Fruit, the present invention comparison different as 3 kinds of concentration gradients using 10,20,30 (FPU/g DM) CTEC2 bis- generations enzymes.Select 48h
It is analyzed with 72h as the time point of enzyme hydrolysis.Analyze the following Fig. 3 and Fig. 4 of result:
As can be seen from figs. 3 and 4 cellulose hydrolyzation effect significantly improves after pretreatment, especially acetic acid and alkaline condition
Hydrolysis effect is more preferably after lower sodium sulfite collaboration processing.
And two generation enzyme effects of three kinds of contents all achieve the purpose that enzymatic hydrolysis pretreatment paulownia raw material, but two generations of 30fpu
Enzymatic treatment reaches 72.05 to the best glucose yield of paulownia+acetic acid+alkaline sodium sulfite pretreated feedstock effect, and wood is poly-
Sugared yield reaches 77.80%.
It is former paulownia to be pre-processed to paulownia+acetic acid+alkaline sodium sulfite in 48 hours and 72h under the degradation of 30fpu bis- generations enzyme
The effect promoting of material is little, and bis- generation of 30fpu enzymatic treatment paulownia+pretreated paulownia raw material of acetic acid+alkaline sodium sulfite used is most
68.88% is reached to save time enzymolysis time glucose yield, xylan yield reaches 73.48%.
In conclusion the present invention is pretreatment medium with acetic acid, sodium sulfite and sodium hydroxide, at different heat
Temperature is managed, carries out collaboration pretreatment using high pressure oil bath pan and high temperature high pressure sterilizing pot, to mainization of paulownia pretreatment front and back
It learns component to be studied, passes through ftir analysis and thermogravimetric analysis and scanning electron microscope collaboration inspection
Test the variation of bamboo wood chemical constituent before and after the processing.The result shows that: the quantum of output of cellulose obviously increases cellulose after pretreatment
Changing rule of the yield under different processing ambient conditions is that acetic acid and alkaline sodium sulfite cooperate with treatment effect the brightest
Aobvious, followed by sodium sulfite and acetic acid collaboration processing are finally only acetic acid treatments.(NREL's) of foundation U.S. Department of Energy
Standard method is real come the enzyme hydrolysis for measuring cellulose in pretreated paulownia, lignin, the content of xylan and cellulose
The quantum of output for testing cellulose after can absolutely proving present invention pretreatment obviously increases.
In the description of this specification, the description meaning of reference term " one embodiment ", " example ", " specific example " etc.
Refer to that specific features described in conjunction with this embodiment or example, structure, material live feature and be contained at least one reality of the invention
It applies in example or example.In the present specification, schematic expression of the above terms are not necessarily referring to identical embodiment or show
Example.Moreover, particular features, structures, materials, or characteristics described can be in any one or more embodiment or examples
In can be combined in any suitable manner.
Present invention disclosed above preferred embodiment is only intended to help to illustrate the present invention.There is no detailed for preferred embodiment
All details are described to the greatest extent, also do not limit the specific embodiment that the invention is only.It obviously, can according to the content of this specification
It makes many modifications and variations.These embodiments are chosen and specifically described to this specification, is in order to better explain the present invention
Principle and practical application, so that skilled artisan be enable to better understand and utilize the present invention.The present invention is only
It is limited by claims and its full scope and equivalent.
Claims (8)
1. a kind of method of acetic acid sodium sulfite collaboration preprocessing lignocellulose raw material, which is characterized in that sub- with acetic acid, alkalinity
Sodium sulphate is pretreatment medium, carries out collaboration pretreatment using high temperature oil bath pan and high temperature high pressure sterilizing pot, specifically includes following
Step:
S1: weighing 12-15 parts of raw material powders and put into reaction flask, adds the acetic acid solution that solid-liquid ratio is 1:8-12g/ml, mixes
Reaction bottle cap is tightened after closing uniformly, is put into high temperature oil bath pan, the temperature setting of high temperature oil bath pan is 165-175 DEG C, high temperature
Working time is 25-35min, takes out reaction flask after the reaction was completed, is cooled to room temperature, and the turbid liquid in reaction flask is poured into pumping
Funnel is filtered, using distilled water filtering and washing, cleans and filters repeatedly, until extraction liquid shows neutral is obtained in low temperature oven dried
To dry powders A；
S2: weighing 10-12 parts of powders As and be put into reaction flask, and it is molten to add the alkaline sodium sulfite that solid-liquid ratio is 1:8-12g/ml
Liquid tightens reaction bottle cap after mixing, is put into high temperature high pressure sterilizing pot, and the temperature of high temperature high pressure sterilizing pot is set in 118-
122 DEG C, working time 55-65min takes out after the reaction was completed, is cooled to room temperature, and the turbid liquid in reaction flask is poured into pumping
Funnel is filtered, using distilled water filtering and washing, then cleans and filters repeatedly, until extracting liquid shows neutral out, low temperature drying is obtained
Preprocessing lignocellulose raw material.
2. a kind of method of acetic acid sodium sulfite collaboration preprocessing lignocellulose raw material according to claim 1, special
Sign is that acetic acid pretreatment temperature is set as 170 DEG C in step S1, and the processing time is 30min, sodium hydroxide and Asia in step S2
Sodium sulphate treatment temperature is 121 DEG C, and the processing time is 60min.
3. a kind of method of acetic acid sodium sulfite collaboration preprocessing lignocellulose raw material according to claim 1, special
Sign is that the temperature of low temperature drying is 40-50 DEG C in step S1 and S2, and the moisture content of powder is less than 10% after drying.
4. a kind of method of acetic acid sodium sulfite collaboration preprocessing lignocellulose raw material according to claim 1, special
Sign is that raw material powder is paulownia powder, and paulownia are broken into wood shavings, are ground into mistake after tiny graininess with pulverizer after dry
Raw material powder is made less than 10% in the sieve of 80 mesh, 40-50 DEG C of low temperature drying to moisture content.
5. a kind of method of acetic acid sodium sulfite collaboration preprocessing lignocellulose raw material according to claim 1, special
Sign is that the mass concentration of acetic acid solution is 3-4.5%.
6. a kind of method of acetic acid sodium sulfite collaboration preprocessing lignocellulose raw material according to claim 5, special
Sign is that the mass concentration of acetic acid solution is 4%.
7. a kind of method of acetic acid sodium sulfite collaboration preprocessing lignocellulose raw material according to claim 1, special
Sign is, alkaline sulfurous acid solution is containing mass concentration be 3.5-5% sodium sulfite and 0.8-1.5% sodium hydroxide mixing
Solution.
8. a kind of method of acetic acid sodium sulfite collaboration preprocessing lignocellulose raw material according to claim 7, special
Sign is, alkaline sulfurous acid solution is containing mass concentration be 4% sodium sulfite and 1% sodium hydroxide mixed solution.
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Cited By (2)
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|---|---|---|---|---|
| CN110540604A (en) * | 2019-10-12 | 2019-12-06 | 西藏天虹科技股份有限责任公司 | Method for extracting conic gymnadenia rhizome polysaccharide |
| CN112694629A (en) * | 2021-01-04 | 2021-04-23 | 湖南科技大学 | Method for preparing biodegradable transparent film by using waste wood biomass |
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| CN104830928A (en) * | 2015-05-15 | 2015-08-12 | 江南大学 | Pretreatment method of lignocellulose by using microwave-assisted alkaline sodium sulfite |
| CN106283788A (en) * | 2016-08-03 | 2017-01-04 | 内蒙古科技大学 | A kind of for the chemical-biological pulping process with non-wood material |
| CN108330723A (en) * | 2017-12-28 | 2018-07-27 | 潍坊友容实业有限公司 | A method of extracting cellulose using the false indigo of salt-soda soil plantation |
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| CN101535561A (en) * | 2006-11-03 | 2009-09-16 | 纳尔科公司 | Method and composition for improving fiber quality and process efficiency in mechanical pulping |
| CN104342466A (en) * | 2013-08-09 | 2015-02-11 | 中国石油天然气股份有限公司 | Combined pretreatment method of lignocellulose raw material |
| CN104830928A (en) * | 2015-05-15 | 2015-08-12 | 江南大学 | Pretreatment method of lignocellulose by using microwave-assisted alkaline sodium sulfite |
| CN106283788A (en) * | 2016-08-03 | 2017-01-04 | 内蒙古科技大学 | A kind of for the chemical-biological pulping process with non-wood material |
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| CN110540604A (en) * | 2019-10-12 | 2019-12-06 | 西藏天虹科技股份有限责任公司 | Method for extracting conic gymnadenia rhizome polysaccharide |
| CN112694629A (en) * | 2021-01-04 | 2021-04-23 | 湖南科技大学 | Method for preparing biodegradable transparent film by using waste wood biomass |
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