CN102061323B - Comprehensive utilization process of wood cellulose - Google Patents

Comprehensive utilization process of wood cellulose Download PDF

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CN102061323B
CN102061323B CN2010105384847A CN201010538484A CN102061323B CN 102061323 B CN102061323 B CN 102061323B CN 2010105384847 A CN2010105384847 A CN 2010105384847A CN 201010538484 A CN201010538484 A CN 201010538484A CN 102061323 B CN102061323 B CN 102061323B
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slag
xylogen
liquid
oligosaccharide
xylo
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CN102061323A (en
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肖林
高永保
陈小刚
覃树林
张茜
赵海涛
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SHANDONG LONGLIVE BIO-TECHNOLOGY Co Ltd
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SHANDONG LONGLIVE BIO-TECHNOLOGY Co Ltd
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E50/00Technologies for the production of fuel of non-fossil origin
    • Y02E50/10Biofuels, e.g. bio-diesel

Abstract

The invention discloses a comprehensive utilization process of wood cellulose, which comprises the processes of comprehensive treatment, oligosaccharide preparation, lignin preparation, fiber ethanol preparation and the like. The invention has the advantages of decomposing a biomass macromolecular natural compact structure by using a high-pressure instant steam exploding technology, being beneficial to the separation and the extraction of the lignin, the cellulose and the cellulose, reducing the consumption of the energy sources and the materials, such as acid, alkali, heat, catalyst and the like for preprocessing, reducing the emission of pollutants and lightening the pollution of the environment. Secondly, the cogeneration of oligosaccharide and lignin realizes the comprehensive utilization of the energy sources, especially the application of the steam exploding technology ensures that the quality of the two products of the oligosaccharide and the lignin is greatly improved and the yield is greatly increased; and alcohol and the lignin of production fuels of sugar residues can be extracted irrespective of the order.

Description

The comprehensive utilization process of one kind of plant lignocellulose
Technical field
The present invention relates to the comprehensive utilization process of a kind of plant lignocellulose, relating in particular to plant lignocelluloses such as corn cob, stalk, straw is raw material, adopt the instantaneous steam explosion technology of high pressure to carry out raw materials pretreatment, utilize the prozyme technology to prepare high-quality function sugar (wood sugar, xylo-oligosaccharide), the residue waste residue is produced macromolecular material (enzymolysis xylogen) earlier, further production of cellulosic ethanol again, waste liquid is back to production for the production of marsh gas power generation, finally realizes the comprehensive utilization process of the high added value of resource.
Background technology
Current, energy problem has been the subject matter that various countries, the world today face in evolution, has become the tempo of restriction world economy and has influenced one of principal element of regional stability.In China, along with rapid economy development, the structural inconsistency of Energy resources supply and demand further shows especially out, and the shortage of Energy resources will become one of principal element of the economy upgrading of restriction China and great-leap-forward development; Simultaneously, because the unreasonable and related infrastructure construction of the industrial structure falls behind, the problem that the city that a large amount of industrial refuses and domestic refuse cause and rural production and living environment worsen also further displays.Therefore, day by day under the outstanding dual background, the clean comprehensive utilization industry development of biomass material faces opportunities and challenges at Energy resources critical shortage and ecological environment problem.
China is a large agricultural country, is again the country that petroleum resources enrich inadequately.It is the important assurance that we implement the strategy of sustainable development that the biomass resource of China's abundant is fully also efficiently utilized.Yet along with the fast development of economy, environmental destruction day is serious, and human simultaneously environmental consciousness constantly promotes, and the high-quality conversion of biomass industry of clean shows advantage.But at present, in China, for the processing of biomass material exist utilization ratio low, do not fully utilize, pollute defectives such as big, be badly in need of a kind of technology of comprehensive utilization of the high added value that can realize resource.
Summary of the invention
At above-mentioned prior art, the invention provides the comprehensive utilization process of a kind of plant lignocellulose, it can be realized comprehensive utilization, and pollute little the utilization ratio height of biomass material.
The present invention is achieved by the following technical solutions:
The present invention utilizes the instantaneous steam explosion technology of high pressure pretreating raw material, handles the explosion thing with zymolysis technique and prepares high-purity oligoxylose, cellulose ethanol and xylogen, and its particular content is as follows:
(1) handles
(1) steam explosion: biomass material is crushed to below 10 orders, carries out steam explosion, blasting condition is: burstpressures 1.5Mpa~3.5Mpa, and blasting time is 30s~120s;
(2) size mixing: after vapour was quick-fried, resulting material is pressed solid (butt) liquid (water) than 1: prepared burden (5~8), and regulating pH is 3.0~7.0, stirs, for enzymolysis is prepared;
(3) enzymolysis: in the above-mentioned material that finishes of sizing mixing, add 10IU/g~20IU/g zytase, carry out enzymolysis and obtain raw sugar liquid, 30 ℃~70 ℃ of hydrolysis temperatures; Enzymolysis time 4~20 hours, behind the enzymolysis, xylo-oligosaccharide purity reaches more than 80%;
(4) slag liquid separates: after enzymolysis finishes, carry out slag liquid and separate, obtain liquid glucose and sugared slag, wherein, in the liquid glucose, the liquid glucose solid substance accounts for 2%~8% of total mass; Water content is 60%~80% in the sugar slag; Liquid glucose is for the preparation of xylo-oligosaccharide, and sugared slag is for the preparation of xylogen and cellulose ethanol, and waste liquid, waste residue after the preparation can be used for marsh gas power generation.
The step of described preparation xylo-oligosaccharide is as follows:
(2) preparation xylo-oligosaccharide
(1) purifies: utilize gac that liquid glucose is decoloured, utilize ion exchange resin to adsorb to remove salt in the liquid glucose impurity that grades, material is purified; After decolouring, the absorption, printing opacity is regulated pH to 3~7 more than 70%;
(2) nanofiltration: the liquid glucose that above-mentioned purification is good is purified the nanofiltration condition with existing nanofiltration equipment: 20~40 ℃ of temperature, and sugar concentration 15%~30%, pH 3~7; After the nanofiltration, the content of xylo-oligosaccharide reaches more than 95%;
(3) concentrate: the liquid glucose after the nanofiltration is concentrated, obtain the xylo-oligosaccharide finished product.
The step of described preparation xylogen is as follows:
(3) preparation xylogen
(1) batching: with sugared slag and process water according to solid-to-liquid ratio 1: prepare burden (5~8), and adding sodium hydroxide, to regulate basicity be 1%~8%, stirs;
(2) extract: under stirring condition the above-mentioned material for preparing is warming up to 50 ℃~100 ℃, insulation was extracted 1~5 hour, made the abundant stripping of xylogen;
(3) slag liquid separates: after said extracted finishes, carry out slag liquid and separate, obtain rugose wood cellulose solution and xylogen slag, the water content of xylogen slag is 60%~80%, for the preparation of cellulose ethanol;
(4) sedimentation: the rugose wood cellulose solution is warming up to 50 ℃~100 ℃, and it is 2~7 that adding hydrochloric acid is regulated its pH, makes it abundant sedimentation;
(5) separating, washing: the xylogen that above-mentioned sedimentation is good separates, and the water flushing, obtains high Vinsol wet feed, and its water content is 60%~80%;
(6) air stream drying: xylogen wet feed pneumatic drier drying namely gets xylogen.
The step of described preparation cellulose ethanol is as follows:
(4) preparation cellulose ethanol
(1) batching: with sugared slag or xylogen slag and process water according to solid-to-liquid ratio 1: prepare burden (5~9), adds yeast 1Kg/T-10Kg/T;
(2) wine fermentation: above-mentioned prepared materials is fermented, as follows:
The fermentation initial stage: temperature is 36 ± 1 ℃ during the activation yeast, and the time is 30min; Bud ratio %: 〉=18%; Mortality ratio %:<1%; Acidity (titre): 3.5~4.0%;
Ferment latter stage: outward appearance sugar :≤0.5BX; Total acid :≤0.3%; Volatile acid :≤0.1g/100ml (in rare wine sample); Residual total reducing sugar :≤0.8g/100ml (anthrone method); Ventilation: 70~120m3/h intermittent aeration;
(3) distillation: the distillation of fermentation back, namely obtain cellulose ethanol, parameter is as follows:
Thick tower: admission pressure 0.04~0.06MPa; Mash is gone into the tower temperature: 65~70 ℃; 110~112 ℃ of column bottom temperatures; 95 ± 1 ℃ of tower top temperatures;
Smart tower: admission pressure 0.03~0.07MPa; 110~112 ℃ of column bottom temperatures; Temperature is 83~87 ℃ in the tower; 80~82 ℃ of cat head temperature.
In the described step () (1), biomass material is that main components such as corn cob, stalk or straw are the raw material of plant lignocellulose.
Simmer down in the described step (two) (3): when producing the xylo-oligosaccharide slurry, be concentrated to more than 70%, namely; When producing Icing Sugar, be concentrated to 30%~35%, spraying drying then, namely;
The condition of concentrating is as follows:
Pressure: an effect 〉=0.02Mpa; Two effect 〉=0.04Mpa; Triple effect 〉=0.07Mpa;
Temperature: one imitates 〉=90 ℃; Two imitate 〉=70 ℃; Triple effect 〉=50 ℃;
Drying conditions is: interior temperature: 80-100 ℃ of tower; Negative pressure 0.5-10Pa.
In the described step (three) (6), the parameter of air stream drying is as follows: 100 ℃~150 ℃ of inlet temperature, 50 ℃~80 ℃ of air outlet temperatures.
More than related solid-to-liquid ratio be mass ratio, related water content, percentage concentration etc. are mass percent.
The product leading indicator that the present invention produces is:
Xylo-oligosaccharide content 50%~90%, printing opacity 70%~99% (420~430nm, 1~5cm cuvette), pH 3~7;
Lignin molecule amount 500~3000Da, residual sugar 0.5%~8%, yield 10%~30%, ash content 0.1%~8%.
Beneficial effect of the present invention is as follows: utilize the quick-fried technology of the instantaneous vapour of high pressure to untie the high molecular natural imporosity of biomass, be conducive to xylogen, Mierocrystalline cellulose, cellulosic separation and Extraction, reduce the consumption that is used for pretreated acid, alkali, heat, catalyzer equal energy source, material, reduce the discharging of pollutent, the pollution that alleviates environment.Secondly, xylo-oligosaccharide and xylogen coproduction have realized the quick-fried The Application of Technology of comprehensive utilization, particularly vapour that can be former, and the quality of two kinds of products is promoted significantly, and yield improves greatly; The sugar slag produces alcohol fuel and xylogen can be in no particular order.
The present invention adopts the instantaneous steam explosion technology of high pressure that biomass material is carried out pre-treatment, having substituted pretreatment modes such as former high temperature, high pressure, acid, alkali, catalyzer fully unties former natural structure, because also not adding other impurity without the long-time high temperature of mistake, autoclaving, so alleviated the pressure in processes such as later stage extraction, purifications.Not only reduced the consumption of raw and auxiliary material, reduced the discharging of pollutent, and fully untied because of the adding and the former natural structure that do not have other pre-treatment impurity, the quality of product further promotes, and yield further improves.
Embodiment
The present invention is further illustrated below in conjunction with embodiment.
Embodiment 1: comprehensive utilization plant lignocellulose is produced xylo-oligosaccharide, xylogen and cellulose ethanol, and step is as follows:
(1) preparation xylo-oligosaccharide
(1) steam explosion: biomass material (corn cob) is crushed to 20 orders; Blasting condition is: burstpressures 2.0Mpa, and blasting time is 60s;
(2) size mixing: prepare burden at 1: 6 by solid-to-liquid ratio, regulating pH is 3.5, stirs, for enzymolysis is prepared;
(3) enzymolysis: add the zytase of 20IU/g in the material that finishes to sizing mixing, carry out enzymolysis and obtain raw sugar liquid, 50 ℃ of hydrolysis temperatures, enzymolysis time 8 hours; Xylo-oligosaccharide content 82%;
(4) slag liquid separates: carry out slag liquid after enzymolysis finishes and separate, obtain liquid glucose and sugared slag, liquid glucose is for the preparation of xylo-oligosaccharide, and sugared slag is for the preparation of xylogen and cellulose ethanol, and wherein, the liquid glucose solid substance is 5%; Sugar slag water content is 73%.
(5) purify: utilize gac that liquid glucose is decoloured, utilize ion exchange resin to adsorb to remove salt in the liquid glucose impurity that grades, material is purified; After decolouring, the purification, printing opacity is regulated pH to 4.0 more than 80%;
(6) nanofiltration: the liquid glucose that above-mentioned purification is good is purified with nanofiltration equipment, and the content of xylo-oligosaccharide is reached more than 97%; The nanofiltration condition is: 35 ℃ of temperature; Sugar concentration 18%; PH4.0;
(7) concentrate: solid substance is concentrated to 35%; Temperature: one imitates 〉=90 ℃; Two imitate 〉=70 ℃; Triple effect 〉=50 ℃;
(8) spraying drying: the xylo-oligosaccharide spraying drying after will concentrating namely obtains the xylo-oligosaccharide Icing Sugar; Spraying drying condition: temperature in the tower: 90~95 ℃; Negative pressure 3Pa.
(2) preparation xylogen
(1) batching: sugared slag and process water are prepared burden according to solid-to-liquid ratio at 1: 7, regulate basicity 1% with sodium hydroxide, stir;
(2) extract: under stirring condition the above-mentioned material for preparing is warming up to 75 ℃, insulation was extracted 3 hours, made the abundant stripping of xylogen;
(3) slag liquid separates: after said extracted finishes, carry out slag liquid and separate, obtain rugose wood cellulose solution and xylogen slag, wherein, xylogen slag water content is 60%;
(4) sedimentation: the rugose wood cellulose solution is warming up to 70 ℃, and it is 5 that adding hydrochloric acid is regulated its pH, makes it abundant sedimentation, for centrifuge washing is prepared;
(5) centrifuge washing: the xylogen that above-mentioned sedimentation is good separates, and the water flushing, obtains high Vinsol wet feed, water content 75%.
(6) air stream drying: xylogen wet feed pneumatic drier drying namely gets lignin product, 120 ℃~125 ℃ of inlet temperature, 60 ℃~70 ℃ of air outlet temperatures.
(3) preparation cellulose ethanol
(1) batching: sugared slag and process water are prepared burden according to solid-to-liquid ratio at 1: 7, add yeast 2Kg/T bag and cellulase solution 10IU/g;
(2) wine fermentation: above-mentioned prepared materials is fermented, as follows:
The fermentation initial stage: temperature is 36 ± 1 ℃ during the activation yeast, and the time is 30min; Bud ratio %: 〉=18%; Mortality ratio %:<1%; Acidity (titre): 3.5~4.0%;
Ferment latter stage: outward appearance sugar :≤0.5BX; Total acid :≤0.3%; Volatile acid :≤0.1g/100ml (in rare wine sample); Residual total reducing sugar :≤0.8g/100ml (anthrone method); Ventilation: 70~120m3/h intermittent aeration;
(3) distillation: the distillation of fermentation back, namely obtain cellulose ethanol, parameter is as follows:
Thick tower: admission pressure 0.04~0.06MPa; Mash is gone into the tower temperature: 69 ℃; 111.4 ℃ of column bottom temperatures; 95 ± 1 ℃ of tower top temperatures;
Smart tower: admission pressure 0.03~0.07MPa; 111.5 ℃ of column bottom temperatures; Temperature is 85 ℃ in the tower; 81.5 ℃ of cat head temperature.
The present invention utilizes the high-purity oligoxylose of aforesaid method production and xylogen leading indicator to be:
Xylo-oligosaccharide content 96.5%, printing opacity 80%, pH 4.2;
Lignin molecule amount 1600, residual sugar 2.0%, yield 17%, ash content 2.0%;
The ethanol index meets GB.
Embodiment 2: comprehensive utilization plant lignocellulose is produced xylo-oligosaccharide, xylogen and cellulose ethanol, and step is as follows:
(1) preparation xylo-oligosaccharide
(1) steam explosion: biomass material (stalk) is crushed to 20 orders; Blasting condition is: burstpressures 2.5Mpa, and blasting time is 90s;
(2) size mixing: prepare burden at 1: 7 by solid-to-liquid ratio, regulating pH is 3.8, stirs, for enzymolysis is prepared;
(3) enzymolysis: add the 20IU/g zytase in the material that finishes to sizing mixing, carry out enzymolysis and obtain raw sugar liquid; 50 ℃ of hydrolysis temperatures; Enzymolysis time 12 hours; Behind the enzymolysis, xylo-oligosaccharide content 87%;
(4) slag liquid separates: carry out slag liquid after enzymolysis finishes and separate, obtain liquid glucose and sugared slag, liquid glucose is for the preparation of xylo-oligosaccharide, and sugared slag is for the preparation of xylogen and cellulose ethanol; Wherein, the liquid glucose solid substance is 5.6%; Sugar slag water content is 72.3%;
(5) purify: utilize gac that liquid glucose is decoloured, utilize ion exchange resin to adsorb to remove salt in the liquid glucose impurity that grades, material is purified; After decolouring, the purification, printing opacity is regulated pH to 4.3 more than 80%;
(6) nanofiltration: the liquid glucose that above-mentioned purification is good is purified with nanofiltration equipment, and the content of xylo-oligosaccharide is reached more than 97%; Nanofiltration condition: 35 ℃ of temperature; Sugar concentration 17.8%; PH4.25;
(7) concentrate: solid substance is concentrated to 35%; The condition of concentrating: pressure: an effect 〉=0.02Mpa; Two effect 〉=0.04Mpa; Triple effect 〉=0.07Mpa; Temperature: one imitates 〉=90 ℃; Two imitate 〉=70 ℃; Triple effect 〉=50 ℃;
(8) spraying drying: the xylo-oligosaccharide spraying drying after will concentrating namely obtains the xylo-oligosaccharide Icing Sugar; Spraying drying condition: temperature in the tower: 90~95 ℃; Negative pressure 3Pa.
(2) preparation xylogen
(1) batching: sugared slag and process water are prepared burden according to solid-to-liquid ratio at 1: 8, and regulating basicity with sodium hydroxide is 3%, stirs;
(2) extract: under stirring condition the material for preparing is warming up to 75 ℃, insulation was extracted 3 hours, made the abundant stripping of xylogen;
(3 slag liquid separate: carry out the separation of slag liquid after extracting end, obtain rugose wood cellulose solution and xylogen slag, wherein, xylogen slag water content is 60%;
(4) sedimentation: the rugose wood cellulose solution is warming up to 70 ℃, and it is 5 that adding hydrochloric acid is regulated its pH, makes it abundant sedimentation, for centrifuge washing is prepared;
(5) centrifuge washing: the xylogen that above-mentioned sedimentation is good separates, and the water flushing, obtains high Vinsol wet feed, water content 74%;
(6) air stream drying: xylogen wet feed pneumatic drier drying, namely obtain lignin product, wherein, 120 ℃~125 ℃ of inlet temperature, 60 ℃~70 ℃ of air outlet temperatures.
(3) preparation cellulose ethanol
(1) batching: sugared slag and process water are prepared burden according to solid-to-liquid ratio at 1: 7, add yeast 4Kg/T and cellulase solution 12IU/g;
(2) wine fermentation: above-mentioned prepared materials is fermented, as follows:
The fermentation initial stage: temperature is 36 ± 1 ℃ during the activation yeast, and the time is 30min; Bud ratio %: 〉=18%; Mortality ratio %:<1%; Acidity (titre): 3.7~4.0%;
Ferment latter stage: outward appearance sugar :≤0.5BX; Total acid :≤0.3%; Volatile acid :≤0.1g/100ml (in rare wine sample); Residual total reducing sugar :≤0.8g/100ml (anthrone method); Ventilation: 70~120m 3/ h intermittent aeration;
(3) distillation: the distillation of fermentation back, namely obtain cellulose ethanol, parameter is as follows:
Thick tower: admission pressure 0.04~0.06MPa; Mash is gone into the tower temperature: 69 ℃; 111.4 ℃ of column bottom temperatures; 95 ± 1 ℃ of tower top temperatures;
Smart tower: admission pressure 0.03~0.07MPa; 111.5 ℃ of column bottom temperatures; Temperature is 85 ℃ in the tower; 81.5 ℃ of cat head temperature.
Utilize high-purity oligoxylose and the xylogen leading indicator of aforesaid method production to be:
Xylo-oligosaccharide content 96.7%, printing opacity 84%, pH 4.2;
Lignin molecule amount 1600, residual sugar 1.8%, yield 17%, ash content 2.0%;
The ethanol index meets GB.
Embodiment 3: comprehensive utilization plant lignocellulose is produced xylo-oligosaccharide, xylogen and cellulose ethanol, and step is as follows:
(1) preparation xylo-oligosaccharide:
(1) steam explosion: biomass material (straw) is crushed to 20 orders, and it is quick-fried to carry out vapour, and blasting condition is: burstpressures 2.0Mpa, and blasting time is 60s;
(2) size mixing: prepare burden at 1: 6 by solid-to-liquid ratio, regulating pH is 3.5, stirs, for enzymolysis is prepared;
(3) enzymolysis: add the 11IU/g zytase in the material that finishes to sizing mixing, carry out enzymolysis and obtain raw sugar liquid; 50 ℃ of hydrolysis temperatures; Enzymolysis time 8 hours; Behind the enzymolysis, xylo-oligosaccharide content is 89%;
(4) slag liquid separates: carry out slag liquid after enzymolysis finishes and separate, obtain liquid glucose and sugared slag, liquid glucose is for the preparation of xylo-oligosaccharide, and sugared slag is for the preparation of xylogen and cellulose ethanol, and wherein, the liquid glucose solid substance is 5%; Sugar slag water content is 73%.
(5) purify: utilize gac that liquid glucose is decoloured, utilize ion exchange resin to adsorb to remove salt in the raw sugar liquid impurity that grades, material is purified; After decolouring, the purification, printing opacity is regulated pH to 4.0 more than 80%;
(6) nanofiltration: the liquid glucose that above-mentioned purification is good is purified with nanofiltration equipment, and xylo-oligosaccharide content is reached more than 97%; Nanofiltration condition: 35 ℃ of temperature; Sugar concentration 18%; PH4.0;
(7) concentrate: solid substance is concentrated to 35%; The condition of concentrating: pressure: an effect 〉=0.02Mpa; Two effect 〉=0.04Mpa; Triple effect 〉=0.07Mpa; Temperature: one imitates 〉=90 ℃; Two imitate 〉=70 ℃; Triple effect 〉=50 ℃;
(8) spraying drying: the xylo-oligosaccharide spraying drying after will concentrating namely obtains the xylo-oligosaccharide Icing Sugar; Spraying drying condition: interior temperature: 90-95 ℃ of tower; Negative pressure 3Pa.
(2) preparation xylogen
(1) batching: sugared slag and process water are prepared burden according to solid-to-liquid ratio at 1: 7, and regulating basicity with sodium hydroxide is 2.8%, stirs;
(2) extract: under stirring condition the material for preparing is warming up to 75 ℃, insulation was extracted 2 hours, made the abundant stripping of xylogen;
(3) slag liquid separates: carry out the separation of slag liquid after extracting end, obtain rugose wood cellulose solution and xylogen slag, wherein, xylogen slag water content is 60%;
(4) sedimentation: the rugose wood cellulose solution is warming up to 70 ℃, and it is 5 that adding hydrochloric acid is regulated its pH, makes it abundant sedimentation, for centrifuge washing is prepared;
(5) centrifuge washing: the xylogen that sedimentation is good separates, and the water flushing, obtains high Vinsol wet feed, water content 77%.
(6) air stream drying: xylogen wet feed pneumatic drier drying, namely obtain lignin product, wherein, 120 ℃~125 ℃ of inlet temperature, 60 ℃~70 ℃ of air outlet temperatures.
(3) preparation cellulose ethanol
(1) batching: sugared slag and process water are prepared burden according to solid-to-liquid ratio at 1: 7, and yeast is pressed 3Kg/T and is added, and cellulase is pressed 13IU/g and added;
(2) wine fermentation: above-mentioned prepared materials is fermented, as follows:
The fermentation initial stage: temperature is 36 ± 1 ℃ during the activation yeast, and the time is 30min; Bud ratio %: 〉=18%; Mortality ratio %:<1%; Acidity (titre): 3.5~4.2%;
Ferment latter stage: outward appearance sugar :≤0.5BX; Total acid :≤0.3%; Volatile acid :≤0.1g/100ml (in rare wine sample); Residual total reducing sugar :≤0.8g/100ml (anthrone method); Ventilation: 100m3/h intermittent aeration;
(3) distillation: the distillation of fermentation back, namely obtain cellulose ethanol, parameter is as follows:
Thick tower: admission pressure 0.04~0.06MPa; Mash is gone into the tower temperature: 68 ℃; 111.1 ℃ of column bottom temperatures; 95 ± 1 ℃ of tower top temperatures;
Smart tower: admission pressure 0.03~0.07MPa; 111.5 ℃ of column bottom temperatures; Temperature is 85 ℃ in the tower; 81.5 ℃ of cat head temperature.
Utilize high-purity oligoxylose and the xylogen leading indicator of aforesaid method production to be:
Xylo-oligosaccharide content 96.9%, printing opacity 89%, pH 4.7;
Lignin molecule amount 1600, residual sugar 1.9%, yield 17.4%, ash content 1.8%;
The ethanol index meets company standard.

Claims (3)

1. the comprehensive utilization process of a kind of plant lignocellulose is characterized in that, may further comprise the steps:
(1) handles
(1) steam explosion: biomass material is crushed to below 10 orders, carries out steam explosion, blasting condition is: burstpressures 1.5Mpa~3.5Mpa, and blasting time is 30s~120s;
(2) size mixing: after vapour is quick-fried, to resulting material by solid-to-liquid ratio 1:(5~8) prepare burden, regulating pH is 3.0~3.8, stirs;
(3) enzymolysis: add the zytase of 10IU/g~20IU/g in the above-mentioned material that finishes of sizing mixing, carry out enzymolysis and obtain raw sugar liquid, 30 ℃~50 ℃ of hydrolysis temperatures; Enzymolysis time 4~20 hours, behind the enzymolysis, xylo-oligosaccharide content is more than 80%;
(4) slag liquid separates: after enzymolysis finishes, carry out slag liquid and separate, obtain liquid glucose and sugared slag, wherein, in the liquid glucose, the liquid glucose solid substance accounts for 2%~8% of total mass; Water content is 60%~80% in the sugar slag; Liquid glucose is for the preparation of xylo-oligosaccharide, and sugared slag is for the preparation of xylogen and cellulose ethanol;
(2) preparation xylo-oligosaccharide
(1) purifies: utilize gac that liquid glucose is decoloured, utilize ion exchange resin to adsorb to remove impurity in the liquid glucose, material is purified; After decolouring, the absorption, printing opacity is regulated pH to 3~7 more than 70%;
(2) nanofiltration: the liquid glucose that above-mentioned purification is good is purified with nanofiltration equipment, the nanofiltration condition: 20~40 ℃ of temperature, sugar concentration 15%~30%, pH3~7; After the nanofiltration, the content of xylo-oligosaccharide reaches more than 95%;
(3) concentrate: the liquid glucose after the nanofiltration is concentrated, obtain the xylo-oligosaccharide finished product;
(3) preparation xylogen
(1) batching: with sugared slag and process water according to solid-to-liquid ratio 1:(5~8) prepare burden, adding sodium hydroxide, to regulate basicity be 1%~8%, stirs;
(2) extract: under stirring condition the above-mentioned material for preparing is warming up to 50 ℃~100 ℃, insulation was extracted 1~5 hour, made the abundant stripping of xylogen;
(3) slag liquid separates: after said extracted finishes, carry out slag liquid and separate, obtain rugose wood cellulose solution and xylogen slag, the water content of xylogen slag is 60%~80%;
(4) sedimentation: the rugose wood cellulose solution is warming up to 50 ℃~100 ℃, and it is 2~5 that adding hydrochloric acid is regulated its pH, makes it abundant sedimentation;
(5) separating, washing: the xylogen that above-mentioned sedimentation is good separates, and the water flushing, obtains high Vinsol wet feed, and its water content is 60%~80%;
(6) air stream drying: xylogen wet feed pneumatic drier drying namely gets xylogen;
(4) preparation cellulose ethanol
(1) batching: with sugared slag or xylogen slag and process water according to solid-to-liquid ratio 1:(5~9) prepare burden, add yeast 1Kg/T-10Kg/T and cellulase solution, the addition of described cellulase solution is 10IU/g, 12IU/g or 13IU/g;
(2) wine fermentation: above-mentioned prepared materials is fermented;
(3) distillation: the distillation of fermentation back namely obtains cellulose ethanol;
In the described step () (1), biomass material is corn cob, stalk or straw;
Simmer down in the described step (two) (3): when producing the xylo-oligosaccharide slurry, be concentrated to more than 70%, namely; When producing Icing Sugar, be concentrated to 30%~35%, spraying drying then, namely; The condition of concentrating is as follows:
Pressure: an effect 〉=0.02Mpa; Two effect 〉=0.04Mpa; Triple effect 〉=0.07Mpa;
Temperature: one imitates 〉=90 ℃; Two imitate 〉=70 ℃; Triple effect 〉=50 ℃;
Drying conditions is: interior temperature: 80-100 ℃ of tower; Negative pressure 0.5-10Pa;
In the described step (three) (6), the parameter of air stream drying is as follows: 100 ℃~150 ℃ of inlet temperature, 50 ℃~80 ℃ of air outlet temperatures.
2. the comprehensive utilization process of a kind of plant lignocellulose according to claim 1, it is characterized in that: in the described step (four) (2), processing parameter is as follows:
The fermentation initial stage: temperature is 36 ± 1 ℃ during the activation yeast, and the time is 30min; Bud ratio %: 〉=18%; Mortality ratio %:<1%; Acidity: 3.5~4.0%;
Ferment latter stage: outward appearance sugar :≤0.5BX; Total acid :≤0.3%; Volatile acid :≤0.1g/100ml; Residual total reducing sugar :≤0.8g/100ml; Ventilation: 70~120m 3/ h intermittent aeration.
3. the comprehensive utilization process of a kind of plant lignocellulose according to claim 1, it is characterized in that: in the described step (four) (3), processing parameter is as follows:
Thick tower: admission pressure 0.04~0.06MPa; Mash is gone into the tower temperature: 65~70 ℃; 110~112 ℃ of column bottom temperatures; 95 ± 1 ℃ of tower top temperatures;
Smart tower: admission pressure 0.03~0.07MPa; 110~112 ℃ of column bottom temperatures; Temperature is 83~87 ℃ in the tower; 80~82 ℃ of cat head temperature.
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