CN108179646A - With the method for plant fiber material production xylose, high-boiling alcohol lignin and fiber - Google Patents
With the method for plant fiber material production xylose, high-boiling alcohol lignin and fiber Download PDFInfo
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- CN108179646A CN108179646A CN201810009684.XA CN201810009684A CN108179646A CN 108179646 A CN108179646 A CN 108179646A CN 201810009684 A CN201810009684 A CN 201810009684A CN 108179646 A CN108179646 A CN 108179646A
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- xylose
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21B—FIBROUS RAW MATERIALS OR THEIR MECHANICAL TREATMENT
- D21B1/00—Fibrous raw materials or their mechanical treatment
- D21B1/04—Fibrous raw materials or their mechanical treatment by dividing raw materials into small particles, e.g. fibres
- D21B1/12—Fibrous raw materials or their mechanical treatment by dividing raw materials into small particles, e.g. fibres by wet methods, by the use of steam
- D21B1/30—Defibrating by other means
- D21B1/36—Explosive disintegration by sudden pressure reduction
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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
- D21C1/00—Pretreatment of the finely-divided materials before digesting
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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
- D21C11/00—Regeneration of pulp liquors or effluent waste waters
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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
- 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
- D21C9/10—Bleaching ; Apparatus therefor
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- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Mechanical Engineering (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention discloses the method with plant fiber material production xylose, high-boiling alcohol lignin and fiber, solve in the prior art that traditional paper industry is merely with cellulose, the problem of other ingredients waste and pollute environment.After extracting xylose from plant fiber material using steam explosion method, high-boiling alcohol lignin is extracted from the material after extraction xylose for the method for the present invention, finally by the material after extraction lignin for papermaking or dissolving fiber.Present invention process is simple, easy to operate, can fully extract cellulose, lignin and the hemicellulose in plant fiber material respectively and efficiently use, take full advantage of raw material, while reduce the pollution to environment.
Description
Technical field
The invention belongs to chemical industry and field of papermaking, and in particular to plant fiber material production xylose, high-boiling alcohol lignin
And the method for fiber.
Background technology
Main component is cellulose, lignin, hemicellulose (poly-pentose) in bamboo and stalk, and tradition is for papermaking.
But traditional pulping process causes CR Critical environmental pollution, main cause is paper making raw material using unreasonable.Particularly China
Slurrying using bamboo and stalk as raw material, wherein account for raw material half non-cellulose raw material and whole industrial chemicals as waste
It exhausts.Non-cellulose part fails to make full use of in raw material, wastes, and also causes certain environmental pollution.
(1) the application of cellulose
Plant fiber material is widely used in the various aspects of industrial and agricultural production, as textile enterprise's plant fiber woven fabric should
With；Ecological feed ecological fertilizer raw materials for production；High-grade packing case raw materials for production；The mess-tin raw materials for production of available for export；Papermaking
Industry；Energy industry；Food industry；Industrial chemicals, construction material etc..Plant fiber has fabulous in following many years
Development prospect and wide selling market.
Usually it is used for papermaking, cotton price persistently sharp rose in recent years, and downstream textile industry cost pressure increases severely, and led to
It crosses and improves the use ratio of cotton substitute to alleviate selection of the cost pressure as numerous producers.Dissolving pulp can produce viscose
Fiber substitutes other fibers, and paper grade (stock) chemical wood pulp and dissolving pulp production technology are substantially similar, and part papermaking enterprise will at present
Chemical pulp production line is converted into timber dissolving pulp production line, and profitability is substantially improved, by market extensive concern.
Dissolving pulp belongs to the refined stock of high-purity, mainly for the production of viscose artificial silk, nitrocellulose, acetate fiber, glass
The products such as glass paper, carboxymethyl cellulose.The raw material for preparing dissolving pulp is mainly cotton linter and timber, due to cotton linter price and
Supply the factors such as unstable, cotton linter pulp is replaced by part wood pulp at present, compared with cotton linter pulp, wood pulp have preferably and
Uniform viscose processing performance, particularly filtrability of viscose energy.Non-timber is used to prepare dissolving pulp and also receives significant attention at present,
Such as bamboo wood, straw, cotton stalk, wheat straw etc..Have been used to production fiber, non-woven fabrics etc..
Different from paper grade (stock) pulp, dissolving pulp does not require the form and intensity of pulp fibers, but fiber is gathered
Right and chemical composition, particularly alpha-cellulose content and whiteness have higher requirement.Dissolving pulp rank is generally with alpha-cellulose
Content divides, and alpha-cellulose content is rudimentary dissolving pulp less than 90%, be intermediate dissolving pulp between 90%~95%,
And it is advanced dissolving pulp more than 95%.
(2) the application of hemicellulose (poly-pentose)
Hemicellulose is by being hydrolyzed to xylose in stalk, and xylose is a kind of important industrial chemicals, the conduct in food, beverage
Industrially by xylose hydro-reduction, crystalline xyhose alcohol is obtained after crystallized for non-caloric sweetener.Xylitol is human body carbohydate metabolism
Normal intermediate, be also widely present, be particularly present in the plants such as veterinary antibiotics, mushroom in nature, but content compared with
It is low, it is directly expensive from Nature inorganic bone xylitol, therefore the production method of commodity xylitol both at home and abroad, it is to use containing wood
The plant material of glycan, such as corncob, bagasse, birch, northern factory are concentrated mainly on Shandong Province, use corncob for
Raw material, therefore cause corncob there is lack of raw materials, it need to be from the long-distance allocation and transportation in other provinces.We can utilize the poly-pentose in bamboo or stalk
(hemicellulose) steam blasting is hydrolyzed to xylose, and Xylose produces furfural or is hydrogenated into xylitol.
(3) the application of lignin
Another main component is lignin in stalk, and sulfonated lignin into sodium lignin sulfonate (wooden sodium) product is shallow
Yellow (brown) free mobility powder, soluble easily in water, chemical property is stablized, and long-term sealed storage does not decompose.Lignin series
Product is a kind of surfactant.But there is presently no the pure lignin of the quality of production for the country.
In order to solve environmental pollution and many researchers of hemicellulose and lignin in raw material be made full use of to carry out half
Cellulose extraction prepares the extraction of xylose and lignin；If patent No. 201010136130.X is from hemicellulose acid hydrolysis liquid
Separating-purifying xylose, method (57) of the arabinose invention are related to one kind separating-purifying wood from hemicellulose acid hydrolysis liquid
The step of method of sugar, arabinose, separating-purifying, is as follows：(1) hemicellulose hydrolysate for obtaining direct sour water solution is through electricity
Dialysis, membrane filtration concentration pretreatment, high purity water progress deoxidation, filtering are spare；(2) by pretreatment hemicellulose hydrolysate into
Enter moving bed imitation chromatogram separation facility to be detached, two kinds of out-feed liquids are obtained after separation；(3) two kinds of out-feed liquids are dropped with multiple-effect
Film evaporator concentration, decrease temperature crystalline obtain xylose, arabinose product.
" the organic solvent purifying element potash lignin just delivered through Yang Yiqin, Li Zhong knowable to retrieval《Nanjing Forestry University is learned
Report》2000,24 (5) 14-16 exist since traditional papermakingization is limited to, its lignin are made to be influenced by structure, and safety
Difference.
Patent No. CN1424459 " method that high boiling solvent (hbs) prepares cellulose and lignin " is although solve fine in raw material
The problem of dimension element and process conditions of lignin separation, but also there are Batch Process, equipment is huge.More than patent is also only sharp
With lignin in plant fiber material, and there is no solve for hemicellulose extraction and application.Early in 2009, China was more than just
The U.S. becomes the first producing country of world's paper products.According to statistics, the first three quarters in 2012, China's production of paper products amount are 86,940,000
Ton.However, also there is secret worry in the behind of industry fast development.High energy consumption, high pollution and excess capacity, become and shroud in paper industry
The dark clouds that can't get rid of on the crown.Paper industry faces transition.
Therefore it provides a kind of production method, it can be fully by cellulose, lignin and the hemicellulose in plant fiber material
The reasonable compositions such as element utilize, and become those skilled in the art's urgent problem to be solved.
Invention content
Present invention solves the technical problem that it is：Offer produces xylose, high-boiling alcohol lignin and fiber with plant fiber material
Method, solve the problem of that traditional paper industry wastes merely with the other ingredients of cellulose and pollutes environment in the prior art.
The technical solution adopted by the present invention is as follows：
Method of the present invention with plant fiber material production xylose, high-boiling alcohol lignin and fiber, using steam explosion
After method extracts xylose from plant fiber material, high-boiling alcohol lignin is extracted from the material after extraction xylose, will finally be carried
The material after lignin is taken for papermaking or dissolving fiber.
Further, the plant fiber material be selected from bamboo, timber, reed, hybrid giant napier, wheat straw, straw, corn stalk,
One kind of cotton stalk, bagasse.
Further, xylose is extracted from plant fiber material using steam explosion method and specifically includes following steps：
Step 1：Plant fiber material, into devillicate machine, is treated as filiform after dedusting is washed；
Step 2：Material after sub-wire enters hot water washer, is measured with 4-6 times, 80 DEG C of continuous washings of hot water adverse current；By water
Soluble substance comes out (including carbohydrate), with coking during gas explosion-proof, deepens product color；Water-solubility impurity is eliminated simultaneously,
Improve xylose quality.
Step 3：After material after step 2 is washed is drained away the water, into steam explosion device, steam explosion device closing is taken out true
Sky is to 80-90KPa, and it is 130-160 DEG C to then pass to and be steam heated to temperature, reusable heat pressurized with compressed air to 1.4-
3.0MPa, processing time 1-5min make the segmentation of the tissues such as lignin, cellulose, hemicellulose and sugar chain detach and by big portion
It is xylose to divide hemicellulose degradation；
Step 4：Material after step 3 processing enters separator, steam is made to be detached with solid fiber, the object after degassing
Material is made into the slurry of aqueous 70-80wt% through mixer, then enters extractor after highly concentrated mill is levigate by fiber, with 8-12 times
Amount, 65-85 DEG C of hot water Continuous Countercurrent Extraction obtain mixing monosaccharide extracting solution；
Step 5：Fiber after extraction xylose, which enters in continuous pipe type hydrolyzer, to be hydrolyzed, and the condition of the hydrolysis is：
Solid-liquid mass ratio 1：4-6 uses sulfuric acid as catalyst, and the dosage of the catalyst is 0.2-1.5wt%, hydrolysis temperature 100-
110 DEG C, residence time 20-60min；The hydrolysis reactant come out by tubular reactor is detached through centrifuge, obtained clear liquid
Merge with the mixing monosaccharide extracting solution in step 4, obtain mixed extract；
Step 6：Mixed extract in step 5 is concentrated into 10-15wt% containing xylose using film.
Further, it extracts high-boiling alcohol lignin from the material after extraction xylose and specifically includes following steps：
Step A：Material after extraction xylose is added in into butanediol aqueous solution, measures containing for catalyst sulfuric acid after mixing
Amount, insufficient section are added to 2wt%, to ensure being normally carried out for reaction；
Step B：The material for having adjusted catalyst content is entered in flow reactor, is warming up to 180-220 DEG C, pressure dimension
It holds in 1.6-2.0MPa and is kept for 20-40 minutes, be then cooled to 100 DEG C, mixture is discharged；
Step C：The reactant discharged in step B is filtered, filter residue is washed successively with butanediol aqueous solution, then uses 40-60
DEG C warm water washs 1 time, and cleaning solution with filtrate is merged, mixed solution is obtained, filter residue is dried, obtain crude fibre, due to it is aforementioned respectively
The processing of portion's technique, hemicellulose, lignin almost all extract in cellulose, and the bleaching of cellulose is also easier to carry out,
Reduce the dosage of bleaching agent simultaneously；
Step D：Mixed solution in step C is added into water, stirs, there is lignin precipitation, is filtered, filter cake is washed with hot water
Afterwards, it is dry, obtain lignin, filtrate use continuous film to be concentrated into the volumetric concentration of butanediol as 75-85%, with recycling.
Further, the water leached in the step 3 is returned again to after precipitation process after step 2 washs the sub-wire
Material.
Further, the volumetric concentration of butanediol is 75-85% in butanediol aqueous solution in the step B and step C, institute
The mass ratio for stating the material after xylose is extracted in step B and butanediol aqueous solution is 1：4-6.
Further, in the step C, butanediol aqueous solution and 50 DEG C of warm water of 5 times of amounts that filter residue is measured successively with 3 times are washed
It washs.
Further, in the step D, mixed solution is placed in settling tank, adds the water of 3-5 times of volume, is stirred,
There is lignin precipitation, filter, after filter cake is washed with 60-70 DEG C of hot water, freeze-drying obtains lignin.
Further, ultrafiltration is obtained after the filtrate in step D being removed the impurity such as resin, pigment using continuous ultrafiltration film
Liquid, then ultrafiltrate is concentrated with NF membrane, it is 80% to take off moisture and be concentrated to the volumetric concentration of butanediol, you can re-circulation makes
With；With film concentration instead of traditional evaporation and concentrating, the energy is saved, reduces operating cost.
Further, in step D, water is penetrated using continuous film concentration, returns to the precipitation for lignin and washing.
Compared with prior art, the invention has the advantages that：
Present invention process is simple, easy to operate, can be fully by cellulose, lignin and the half fiber in plant fiber material
Dimension element extracts respectively to be efficiently used, and takes full advantage of raw material, while reduce the pollution to environment.
The present invention is using Steam explosion treatment raw material, and since its action time is short, energy density is high and concentrates, steam point
Son can be penetrated between the macromoleculars such as cellulose and lignin, inside plant tissues structure is destroyed, so as to complete lignin, fibre
The segmentation separation and hemicellulose for tieing up the tissues such as element, hemicellulose and sugar chain are largely converted into xylose.Lignin and fiber
Element is detached using high boiling alcohol, obtains high-boiling alcohol lignin (HBSL) and cellulose.
The high income of xylose, high-boiling alcohol lignin obtained by method using the present invention, purity is good, and can realize continuous
The industrial production of change, water, the butanediol generated in production process etc. recycles, while production cost is reduced,
The pollution to environment can also be reduced.
Due to the processing of aforementioned each portion's technique, hemicellulose, lignin almost all extract in cellulose, cellulose
Bleaching be also easier to carry out, while reduce the dosage of bleaching agent.
Lignin, cellulose, the poly-pentose in plant fiber material are extracted effectively respectively using the method for the present invention
Utilization.It is not only able to increase profit and tax revenue, and can increase farmers' income, solves the problem of employing the population, improve agricultural and sideline production
Therefore the utility value of product, there is good economic benefit and social benefit.Meet national energy-saving consumption reduction and changing rejected material to useful resource
The circular economy industrial policy of the sustainable development utilized.
Description of the drawings
Process flow chart of the attached drawing 1 for the present invention.
Specific embodiment
The invention will be further described with embodiment for explanation below in conjunction with the accompanying drawings, and mode of the invention includes but not only limits
In following embodiment.
Embodiment 1
As shown in Figure 1, the method using bamboo production xylose, high-boiling alcohol lignin and fiber is present embodiments provided,
Specifically include following steps：
Raw bamboo into devillicate machine, becomes 1-2mm filiforms, then row cuts into 2-4cm long after dedusting is washed.After sub-wire
Material enters hot water washer, is washed with 4 times of amounts, 80 DEG C of hot water continuous flow upstreams.After bamboo silk after washing drains away the water, into vapour
Quick-fried machine.The water of bleeding is after precipitation process, for washing the material after sub-wire.Steam explosion device closing is evacuated to 80KPa,
It is 145 DEG C, then be forced into 2.2MPa with 145 DEG C of hot compressed airs to then pass to and be steam heated to temperature, and processing time 3min makes
The segmentation of the tissues such as lignin, cellulose, hemicellulose and sugar chain detaches and is xylose by most of hemicellulose degradation.Steam explosion
Material afterwards enters separator, and steam is made to be detached with solid fiber, and the bamboo silk after degassing is made into aqueous 70wt%'s through mixer
Slurry, then enter equipment for continuous extraction after highly concentrated mill is levigate by fiber, with 12 times of amounts, 85 DEG C of hot water Continuous Countercurrent Extractions, mixed
Close monosaccharide extracting solution.
Still there is the undegradable hemicellulose of 30-40% in fiber after extraction xylose, make it into continuous pipe type hydrolysis
It is hydrolyzed in device, the condition of hydrolysis is：Solid-liquid mass ratio 1：5, sulfuric acid is used as catalyst, and the dosage of catalyst is
0.3wt%, hydrolysis temperature is 110 DEG C, residence time 20min.The hydrolysis reactant come out by tubular reactor is through centrifuge
Separation, obtained clear liquid merge with xylose extracting solution, obtain mixed extract；15wt% containing xylose is concentrated into using film.
Material after extraction xylose and the butanediol aqueous solution of 80% volumetric concentration are pressed into solid-liquid mass ratio 1：After 4 mixing,
The content of catalyst sulfuric acid is measured, and complements to 2wt%, is then entered in stainless steel flow reactor with the flow of 2t/h, so
After heat to 200 DEG C, pressure maintains 1.6-2.0MPa and is kept for 20 minutes, is then cooled to 100 DEG C, mixture is arranged
Go out.
Mixture after reaction is filtered, cellulose is made to be detached with solution.It is first dense with 3 times of 80% volume on wash engine
The butanediol aqueous solution washing filter residue of degree is primary, then is washed 2 times with 50 DEG C of warm water of 5 times of amounts, dries, obtains crude fibre, this is thick
Cellulose is processed further for papermaking or dissolving pulp.Cleaning solution with filtrate is merged, obtains mixed solution.Mixed solution is placed in
In settling tank, add in the cold water of 4 times of volumes at room temperature and stirring, a large amount of high-boiling alcohol lignin can Precipitations；It will contain
The mixed solution decompression for having precipitation filters, and wash filter cake with 70 DEG C of hot water, will be adsorbed in butanediol therein and clean up, then
Decompression filters, and is finally freeze-dried filter cake, obtains the HBSL of brown powder.
Filtered filtrate using continuous ultrafiltration film is removed, ultrafiltrate is obtained after resin, the impurity such as pigment, then by ultrafiltration
Liquid is concentrated with NF membrane, take off moisture be concentrated to butanediol volumetric concentration be 80%, you can recirculate use.Film concentration production
Raw penetrates water, returns to the precipitation for lignin and washing.
Embodiment 2
As shown in Figure 1, the method using wheat straw production xylose, high-boiling alcohol lignin and fiber is present embodiments provided,
Specifically include following steps：
Wheat straw, into devillicate machine, becomes 2-4mm filiforms after dedusting is washed.Material after sub-wire enters hot water washer,
It is washed with 6 times of amounts, 80 DEG C of hot water continuous flow upstreams.After material after washing drains away the water, into continuous steam explosion machine.The water warp of bleeding
After precipitation process, for washing the material after sub-wire.Steam explosion device closing is evacuated to 90KPa, steam is then passed to and adds
Heat to temperature is 160 DEG C, then is forced into 3MPa, processing time 5min with 160 DEG C of hot compressed airs, makes lignin, cellulose, half
The segmentation of the tissues such as cellulose and sugar chain detaches and is xylose by most of hemicellulose degradation.Subsequently into separator, make steaming
Vapour is detached with solid fiber, and the wheat straw silk after degassing is made into the slurry of aqueous 80wt% through mixer, then is ground through highly concentrated by fiber
Enter equipment for continuous extraction after levigate, with 12 times of amounts, 65 DEG C of hot water Continuous Countercurrent Extractions, obtain mixing monosaccharide extracting solution.
Still there is the undegradable hemicellulose of 30-40% in wheat straw fiber after extraction xylose, make it into continuous pipe type
It is hydrolyzed in hydrolyzer, the condition of hydrolysis is：Solid-liquid mass ratio 1：6, sulfuric acid is used as catalyst, and the dosage of catalyst is
1.5wt%, hydrolysis temperature is 100 DEG C, residence time 20min.The hydrolysis reactant come out by tubular reactor is through centrifuge
Separation, obtained clear liquid with mixing monosaccharide extracting solution merge, obtain mixed extract；Mixed extract is concentrated to containing using film
Xylose 15wt%.
Material after extraction xylose and the butanediol aqueous solution of 80% volumetric concentration are pressed into solid-liquid mass ratio 1：After 6 mixing,
The content of catalyst sulfuric acid is measured, and complements to 2wt%, subsequently into flow reactor, then heats to 180 DEG C,
Pressure maintains 1.6-2.0MPa and is kept for 30 minutes, is then cooled to 100 DEG C, mixture is discharged.
Mixture after reaction is filtered, cellulose is made to be detached with solution.It is first dense with 3 times of 80% volume on wash engine
The butanediol aqueous solution washing filter residue of degree is primary, then is washed 2 times with 50 DEG C of warm water of 5 times of amounts, dries, obtains crude fibre, this is thick
Cellulose is processed further for papermaking or dissolving pulp.Cleaning solution with filtrate is merged, obtains mixed solution.Mixed solution is placed in
In settling tank, add in the cold water of 5 times of volumes at room temperature and stirring, a large amount of high-boiling alcohol lignin can Precipitations；It will contain
The mixed solution decompression for having precipitation filters, and wash filter cake with 70 DEG C of hot water, will be adsorbed in butanediol therein and clean up, then
Decompression filters, and is finally freeze-dried filter cake, obtains the HBSL of brown powder.
Filtered filtrate using continuous ultrafiltration film is removed, ultrafiltrate is obtained after resin, the impurity such as pigment, then by ultrafiltration
Liquid is concentrated with NF membrane, take off moisture be concentrated to butanediol volumetric concentration be 80%, you can recirculate use.Film concentration production
Raw penetrates water, returns to the precipitation for lignin and washing.
Embodiment 3
The present embodiment is comparative example.
The present embodiment uses application No. is the methods of embodiment 1 in 201710117536.5 patent application document to extract wood
Sugar.
Embodiment 4
The present embodiment is comparative example.
The present embodiment is wooden using the method extraction high boiling alcohol of embodiment 1 in 201710914414.9 patent application document
Plain (HBSL).
The results are shown in table below for xylose obtained by implementation 1-3.
| Serial number | Xylose rate % | Appearance | Purity |
| Embodiment 1 (present invention) | 91 | Micro- Huang | 99% |
| Embodiment 2 (present invention) | 91.5 | Micro- Huang | 98.5% |
| Embodiment 3 (comparative example) | 89 | It is yellowish | 97% |
Using xylose made from the method for the present invention, conversion ratio, appearance and purity are superior to comparative example.
The results are shown in table below by the HBSL of 1,2 and 4 gained of embodiment.
| Serial number | Appearance | Yield % | Purity % |
| Embodiment 1 (present invention) | Brown ceramic powder | 98 | 98.5 |
| Embodiment 2 (present invention) | Brown ceramic powder | 97.8 | 97.8 |
| Embodiment 4 (comparative example) | Brown ceramic powder | 95 | 95 |
Comparative example is superior to using the yield and pure love degree of HBSL made from the method for the present invention.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art is in the technical scope of present disclosure, the change or replacement that can readily occur in,
It should be covered by the protection scope of the present invention.The present invention expands to any new feature disclosed in the present specification or any
The step of new combination and any new method or process disclosed or any new combination.
Claims (10)
1. with the method for plant fiber material production xylose, high-boiling alcohol lignin and fiber, which is characterized in that using steam explosion method from
After extracting xylose in plant fiber material, then high-boiling alcohol lignin is extracted from the material after extraction xylose, it finally will extraction
Material after lignin is for papermaking or dissolving fiber.
2. the method according to claim 1 with plant fiber material production xylose, high-boiling alcohol lignin and fiber, special
Sign is, the plant fiber material is selected from bamboo, timber, reed, hybrid giant napier, wheat straw, straw, corn stalk, cotton stalk, bagasse
It is a kind of.
3. the method according to claim 2 with plant fiber material production xylose, high-boiling alcohol lignin and fiber, special
Sign is that extracting xylose from plant fiber material using steam explosion method specifically includes following steps：
Step 1：Plant fiber material, into devillicate machine, is treated as filiform after dedusting is washed；
Step 2：Material after sub-wire enters hot water washer, is measured with 4-6 times, 80 DEG C of continuous washings of hot water adverse current；It will be water-soluble
Substance comes out, and to prevent coking during steam explosion, deepens product color；
Step 3：After material after step 2 is washed is drained away the water, into steam explosion device, steam explosion device closing is evacuated to
80-90KPa, it is 130-160 DEG C to then pass to and be steam heated to temperature, reusable heat pressurized with compressed air to 1.4-3.0MPa, place
Time 1-5min is managed, the segmentation of the tissues such as lignin, cellulose, hemicellulose and sugar chain is made to detach and by most of hemicellulose
It is degraded to xylose；
Step 4：Material after step 3 processing enters separator, and steam is made to be detached with solid fiber, the material warp after degassing
Mixer is made into the slurry of aqueous 70-80wt%, then enters extractor after highly concentrated mill is levigate by fiber, is measured with 8-12 times, 65-
85 DEG C of hot water Continuous Countercurrent Extractions obtain mixing monosaccharide extracting solution；
Step 5：Fiber after extraction xylose, which enters in continuous pipe type hydrolyzer, to be hydrolyzed, and the condition of the hydrolysis is：Solid-liquid
Mass ratio 1：4-6 uses sulfuric acid as catalyst, and the dosage of the catalyst is 0.2-1.5wt%, hydrolysis temperature 100-110
DEG C, residence time 20-60min；The hydrolysis reactant come out by tubular reactor is detached through centrifuge, obtained clear liquid and step
Mixing monosaccharide extracting solution in rapid 4 merges, and obtains mixed extract；
Step 6：Mixed extract in step 5 is concentrated into 10-15wt% containing xylose using film.
4. the method according to claim 3 with plant fiber material production xylose, high-boiling alcohol lignin and fiber, special
Sign is that extracting high-boiling alcohol lignin from the material after extraction xylose specifically includes following steps：
Step A：Material after extraction xylose is added in into butanediol aqueous solution, measures the content of catalyst sulfuric acid after mixing,
Insufficient section is added to 2wt%, to ensure that reaction is normally carried out；
Step B：The material for having adjusted catalyst content is entered in flow reactor, is warming up to 180-220 DEG C, pressure maintains
1.6-2.0MPa is simultaneously kept for 20-40 minutes, is then cooled to 100 DEG C, mixture is discharged；
Step C：The reactant discharged in step B is filtered with centrifuge, filter residue uses butanediol aqueous solution countercurrent washing successively, then
It is washed 1 time with 40-60 DEG C of warm water, cleaning solution with filtrate is merged, mixed solution is obtained, filter residue is dried, obtain crude fibre；
Step D：Mixed solution in step C is added into water, stirs, there is lignin precipitation, is filtered, after filter cake is washed with hot water, is done
It is dry, obtain lignin, filtrate uses continuous film to be concentrated into the volumetric concentration of butanediol as 75-85%, to recycle.
5. the method according to claim 4 with plant fiber material production xylose, high-boiling alcohol lignin and fiber, special
Sign is that the water leached in the step 3 returns again to step 2 after precipitation process and washs the material after the sub-wire.
6. the method according to claim 5 with plant fiber material production xylose, high-boiling alcohol lignin and fiber, special
Sign is, the volumetric concentration of butanediol is 75-85% in butanediol aqueous solution in the step B and step C, in the step B
The mass ratio for extracting the material after xylose and butanediol aqueous solution is 1：4-6.
7. the method according to claim 6 with plant fiber material production xylose, high-boiling alcohol lignin and fiber, special
Sign is, in the step C, butanediol aqueous solution and 50 DEG C of warm water of 5 times of amounts that filter residue is measured successively with 3 times wash.
8. the method according to claim 7 with plant fiber material production xylose, high-boiling alcohol lignin and fiber, special
Sign is, in the step D, mixed solution is placed in settling tank, adds the water of 3-5 times of volume, and stirring has lignin analysis
Go out, filter, after filter cake is washed with 60-70 DEG C of hot water, freeze-drying obtains lignin.
9. the method according to claim 8 with plant fiber material production xylose, high-boiling alcohol lignin and fiber, special
Sign is, the filtrate in step D using continuous ultrafiltration film is removed, ultrafiltrate is obtained after the impurity such as resin, pigment, then by ultrafiltration
Liquid is concentrated with NF membrane, take off moisture be concentrated to butanediol volumetric concentration be 80%, you can recirculate use.
10. the method according to claim 9 with plant fiber material production xylose, high-boiling alcohol lignin and fiber,
It is characterized in that, in step D, water is penetrated using continuous film concentration, returns to the precipitation for lignin and washing.
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