A method of producing cellulose, lignin and xylose by biomass materials

Refines the method for producing cellulose, lignin and preparing a biomass material

technical field

The invention relates to bio-engineering technical field of a refines the method for producing cellulose, lignin and preparing a biomass material. Background recycling process are comprises a on the carbon dioxide synthetic circulation of the fibre of the article, the modifying, wherein a way of the solar, stored in the renewable formed on the biosphere carbon, wherein carbon cycle's important ring is. Composition is formed with a flange to the branch pipe and agricultural straw to the wheat straw, rice straw and corn stalk, and grass and such awn grass. The material comprising a cellulose, hemicellulose and lignin crosslinking, bonded form the dense made of different materials, 5-9% of the separating and employs. The same dissociation of the biomass material is one of textile for the technical bottlenecks. The breakthrough of the technical obstacle of each biofuel and production efficiency, the stretching the source via the amount of raw material is comes, wherein the plastic and polylactic acid resin and bottom of competitive power.

To the literature and discovery of current technology, china concentration of 02145150. 8, names is of a method of composition according to reducible monosaccharide the invention, proposed the following technical solution: And the composition as raw material, using the dilute acid and catalyst, a hydrolyzed in 100-20 (TC the temperature range, is of the fermentation monosaccharide, which are the same method of using the inorganic acid hydrolysis biomass and concentrate acid hydrolysis process, in amounts wherein the viscosity in the spent acid is of recycled or the recycling factor is low, the waste and waste liquid withdrawal is high, without using environment-friendly the shortcoming. The target of the invention is suitable cap is in the current when the insufficiency, wherein by a biomass material air the production method of cellulose, and lignin xylose, and to achieve the component with a biomass material. The full use, and for the emission of wastewater and waste liquid, the additional environment-friendly.

The invention is dark the following technical solution to achieve, the invention is a hemicellulose according to the reducible preparing a low boiling point organic acid in biomass material, wherein a suspension via the cellulose and lignin, wherein by using organic solvent grading the cellulose, and lignin xylose and lower polyxylose, and recovery the organic acid and organic solvent used.

The invention specifically comprises the following steps of warps (1) biomass material smashing one of 8-64, the concentration of 20-100% (v/v) and low boiling point organic acid, comprising a liquid-solid to (w/v) 1:2 to 20, a is at one of 20-120'C, the biomass material to the disintegrating xylose and lower polyxylose, wherein the cellulosic or lignocellulosic liquefies, comprising cooling, the liquefaction composition is 18 to 35. CENTIGRADE;

(2) Is 2-10 times The biomass liquefaction of the cooling the Drawing body ^l organic solvent, an, making settles is 2-12 hours, wherein the deposited separating is; and deposited separating and washing, wherein to the cellulosic non-stereotypia drying, cellulose deposited mother liquor support is used; (3) When the cellulose the precipitation mother liquor distillation, installed according the volatilized organic material of organic acid and production, wherein the gas mother liquor cooling to 18-35'C, settles is 2-12 hours, wherein the deposited separating is; and deposited separating and washing, and obtaining the xylose and lower polyxylose drying, xylose and lower polyxylose deposited mother liquor support is used; ; (4) Distillation installed above the xylose and organic solvent and polyxylose deposited mother liquor, of the deposited separated in the gas mother liquor wherein the drying the lignin.

The biomass material is selected, the woody of raw material to the flange abandoned soil in the image is trim the branch pipe and second raw material to the agricultural wheat straw like rice straw and corn stalk, and herbaceous raw material to the weed's of grass awn and collecting of planter and so on one or several kinds of application. <p> the invention can recycle the organic acid and organic solvent in the production process the circulation of a, the production process without, waste gas exhausting and waste water discharge, wherein the environmentally-friendly green production technology; and full supply is a biomass material producing cellulose, and lignin xylose and lower polyxylose product, without the production. The cellulosic wood, and xylose and lower polyxylose invention is prepared from the following raw materials according to The process Jiankang agent, and chemical industry, and energy product, the cellulosic product is a preparation of the opening of non-stereotypia, easy to control the 歩 of 卩 the metal; The lignin product purity of the high (cellulose and withdrawal content of less than 2%, w/w), easy to control the 歩 to the other chemical raw material and finally the product,The invention is further adapted for containing the other woody device and vertical into of hemicellulose, cellulose and lignin the processing method of herbaceous raw material.

Detailed described of illustrated embodiments

The dryer according embodiment of the invention claims a detail: The embodiment and invention technical solution of the out of the water, and given the detailed is method for operating process, and invention's protected scope is the is restricted in the following embodiment.

Wherein the fibres without the amount of test concrete conditions as follows, customary according to the field US renewable energy source laboratory developing the standard biomass analysis method (NREL Used Analytical Steps, LAPs (NREL laboratory analysis method, downloading: websitehttp: Www1 '. eere. energy, gov /biomass/analytical_procedures.html; the Determination of Sugars, Byproducts, and Degradation Which the Mass Of The Samples, Araie Sluiter, 2006 ", Analysis Recycling Process Team Scraper (2005), Analytical Used, The NREL (} of a liquid grading is sampled sugar, the analysis by-product degradation and product, Amie Sluiter, 2006, parsing recycling process study team, In Laboratory Analysis Method (2005) Editions, US field renewable energy source laboratory) and Feed Structure of Carbohydrates and Lignin the Biomass, Amie Sluiter, 2006, Analysis Recycling Process Team, (Used Analytical The Scraper (2005), NREL, (of the biomass determining structure of carbohydrate and lignin, Amie Sluiter, 2006, parsing recycling process study team, In Laboratory Analysis Method (2005) Editions, US field renewable energy source laboratory)}; AThe reduction original state of sugar is 3,5 to dinitrosalicylic acid (3,5-dinitro-alicylic, DNS) and reaction redox wherein the alkali and pot in a reduction of the sugar the reduction) by one or more of red monofilament is 3 to 5 of nitro groups Of Yangsuan, the deep colour and reduction of the sugar in the same concentration range in the position] the refining, using the glucose as the standard, wherein the sugar in which of the actual product of, to a reduction of the sugars weighing the number of 0.9 means.

The embodiment 1 from the wheat straw for preparing and lower polyxylose, cellulose and lignin of Mai Jiegan crush to 64 meshes of bolters, the name of lg is disposed on the circular flask, and is trifluoroacetic acid, 8mi the sealing cover, a sand - 60 degrees and arranging, the recooling to 18 degrees, and adding 80ml isoamyl with intensive mixing, settles 12 hours separating generated, the deposited separating and washing, wherein the non-stereotypia cellulose 0.46g drying, distills the cellulose deposited mother liquor to collect the mass 75-85'C recycling trifluoroacetic acid, a 115-125'C the mass to produce the acetic acid of fibre production, wherein the collection of the cellulose deposited mother liquor cooling to 1 '- settles, 12 hours separating generated, depositing, andWashing, obtained by the xylose and lower polyxylose 0.15g drying, distills the xylose and lower polyxylose deposited mother liquor collect the 125-135'C the mass isoamyl alcohol, obtained, wherein the hue of the solid separating of the gas mother liquor separator is 0 22g. .

The embodiment of 2 Mai Jiegan to crush 8 to bolters of the wheat straw for preparing and lower polyxylose, cellulose and xylogen, the name of lg is disposed on the circular flask, and is trifluoroacetic acid, 4ml the sealing cover, in 75t; The sand bath temperature, 6h the recooling to 25 ' CENTIGRADE, and then 20 ml amyl alcohol intensive mixing, settles 6 hours separating generated, the deposited separating and washing, wherein the non-stereotypia cellulosic material 0.43g drying, distills the cellulose deposited mother liquor to collect 75-85. THE mass recycling trifluoroacetic acid, a 115-125'C the mass to reduction the midwifery the material composition producing acetic acid, wherein the cellulose deposited mother liquor and distilling to cool to 25 ' - settles, 6 hours separating generated, wherein the deposited separating and washing, and obtaining the xylose and lower polyxylose 0.20g drying, distills the xylose and lower polyxylose deposited mother liquor collect the 132-142'C the mass amyl alcohol, obtained, wherein the hue of the solid separating of the gas mother liquor separator is 0 25g. .

The embodiment 3 from the corn straw for preparing and lower polyxylose, cellulose and lignin of the corn straw crush to 8 meshes of bolters, the name of lg is disposed on the circular flask, and is trifluoroacetic acid, 2ml caps and a sealing, and 8h to 80 of the sand C), the recooling to 3 (TC, then adding 20 ml of isopropanol and intensive mixing, settles 2 hours separating generated; of the cellulose non-stereotypia the precipitation separating and washing drying 0. 48g, distills the cellulose deposited mother liquor to collect the mass 75-85'C recycling trifluoroacetic acid, wherein the fibre is distillation, wherein the deposited mother liquor cooling to 35 degrees, settles 12 hours separating generated, wherein the precipitation separating and washing,Thousand of the xylose and lower polyxylose is 0. 25g, distills the xylose and lower polyxylose deposited mother liquor collect the mass 78-88'C the isopropanol and a, the mass 115-125'C to reduction the midwifery the material composition producing acetic acid, wherein of the solid separating, the wood 0.22g the gas mother liquor in dry.

The embodiment 4 of straw for preparing and lower polyxylose, cellulose and lignin of straw crush to 16 meshes of bolters, the name of lg is disposed on the circular flask, then adding 20% concentrations of the methylsulfonic acid 12ml, a sealing cover, and lh to 120 of the sand C), the recooling to 35TC, then adding 36 ml octyl with intensive mixing, settles 6 hours separating generated, obtained, non-stereotypia cellulose 0.38g the depositing and washing and drying, distills the cellulose deposited mother liquor to collect the mass 115-125'C to reduction the midwifery the material composition producing acetic acid, a 150-17 (TC the mass to recycle of the methylsulfonic acid, wherein the cellulose deposited mother liquor gas is cooled to 35 degrees, and settles6 Hours separating slurries, obtained, the xylose and lower polyxylose 0.26g the depositing and washing and drying, distills the xylose and lower polyxylose deposited mother liquor collect the 190-200'C the mass octyl alcohol, drying, wood 0.26g the gas mother liquor separator for separating.

The embodiment 5) is poplar for preparing wood xylose and lower polyxylose, cellulose and lignin in the poplar or wood chip crush to 16 meshes of bolters, the name of lg is disposed on the circular flask, wherein the concentrations 60%) is methylsulfonic acid 15ml, a sealing cover, and 4h at after-cooling (2 TC the sand bath to 30 ', C is 45 ml heptanol intensive mixing weight, settles 4 hours separating generated, 0.1-0.25, obtained non-stereotypia cellulosic material 0.45g the depositing and washing and drying, distills the cellulose deposited mother liquor to collect the mass 115-125'C to reduction the midwifery the material composition producing acetic acid, a 150-175. The C-SHAPED mass, is agent in which methylsulfonic acid, wherein the cellulose deposited mother liquor and distilling cooling to 35 ' - settles, 6 hours separating generated, 0.1-0.25 of the xylose and lower polyxylose the precipitation separating and washing drying 0. 17g, distills the xylose and lower polyxylose deposited mother liquor a 170-180t: The mass the heptanol, drying, wood 0.24g the gas mother liquor separator for separating.

The embodiment 6 from locust for preparing wood xylose and lower polyxylose, cellulose and lignin in the locust or wood chip crush to 64 meshes of bolters, the name of lg is disposed on the circular flask, wherein the trifluoroacetic acid, 20ml the sealing cover, and 8h after-cooling of 70 ' - the sand bath to 18 degrees, and 60 ml two or more wherein the intensive mixing, settles 12 hours separating generated, obtained, non-stereotypia cellulose 0.53g the depositing and washing and drying, distills the cellulose deposited mother liquor to collect the mass 75-85'C recycling trifluoroacetic acid, wherein the gas, wherein the cellulosic deposited mother liquor cooling to 18 ' - settles, 12 hours separating generated, obtained by the preparing the precipitation separating and washing and dryingThe polyxylose 0. 17g, distills the xylose and lower polyxylose deposited mother liquor collect the 95-105'C the mass dioxane a, the mass 115-125'C to reduction the midwifery the material composition producing acetic acid; and lignin the gas mother liquor separator for separating 0 24g. .

The embodiment 7 from a eucalyptus wood for preparing and lower polyxylose, cellulose and lignin is a eucalyptus wood chip crush to 32 meshes of bolters, the name of lg is disposed on the circular flask, wherein the trifluoroacetic acid, 7ml the sealing cover, and arranging in after-cooling 45 ' OF the sand bath to 20 degrees, and 50ml 2 of the weight of 1 of butyl with intensive mixing, settle for 12 h after wherein the generated, obtained, non-stereotypia cellulose A sediment the separating washing and drying. 58g, distills the cellulose deposited mother liquor to collect the mass 75-85'C recycling trifluoroacetic acid, a 115-125 is: Acetic acid mass of the production, wherein the gas, wherein the cellulose deposited mother liquor cooling to 20 ' - settles, 10 hours separating generated, obtained by the xylose and lower polyxylose O.i: Gram the depositing and washing and drying, distills the xylose and lower polyxylose deposited mother liquor a oven. The C-SHAPED mass installed 2 to 1 of the acrylic alcohol, wherein the collection White Poplar which of the solid printing, drying 0.25g lignin.

The embodiment 8 from soft grass for preparing and lower polyxylose, cellulose and lignin of the soft grass crush to 16 meshes of bolters, the name of lg is disposed on the circular flask, wherein the trifluoroacetic acid, 2ml the sealing cover, and arranging in after-cooling 85 ' OF the sand bath to 25 degrees, and 20 ml propanol intensive mixing weight, settles 4 hours separating generated, obtained, non-stereotypia cellulose 0.38g the depositing and washing and drying, distills the cellulose deposited mother liquor to collect 75-85 "" mass OF the trifluoroacetic acid, wherein the cellulose deposited mother liquor and distilling cooling to 25 ' CENTIGRADE, the standing IO to a slurries, wherein the precipitation separating and washing, andThe position for preparing and lower polyxylose 0.26g, the collection xylose and lower polyxylose deposited mother liquor collect the mass 95-105'C recycling propanol, a 115-125X: The acetic acid mass of the production, 0.1-0.25 drying is A lignin the gas mother liquor separator for separating 18g. .

The embodiment of 9 bagasse for preparing and lower polyxylose, cellulose and lignin in the high-efficiency crush to 8 meshes of bolters, the name of lg is disposed on the circular flask, wherein the trifluoroacetic acid, 7ml the sealing cover, and 10h after-cooling of 75 ' - the sand bath to 30 degrees, and 35 ral and intensive mixing weight, settles 2 hours separating generated, obtained, non-stereotypia cellulose 0.42g the depositing and washing and drying, distills the cellulose deposited mother liquor to collect 75-85X: The mass recycling trifluoroacetic acid, wherein the cellulose deposited mother liquor and distilling cooling to 18 ' - settles, 10 hours separating generated, obtained by the xylose and lower polyxylose 0.22g the depositing and washing and drying, distills the xylose and lower polyxylose deposited mother liquor a 75-85t: The mass the ethanol, a 115-125'C the mass to reduction the midwifery the material composition producing acetic acid; and lignin the gas mother liquor separator for separating 0 20g. .

The embodiment 10) is sorghum straw for preparing and lower polyxylose, cellulose and lignin component is sorghum the straw crush to 8 meshes of bolters, the name of lg is disposed on the circular flask, wherein the three used man acetic acid 5ml, a sealing cover, and 10 h after-coolings of 75 ' - the sand bath to 30 degrees, 35 and 3 ml of methyl acrylic l- with intensive mixing weight, settles for 2 h after wherein the generated, obtained, non-stereotypia cellulose 0.48g the depositing and washing and drying, distills the cellulose deposited mother liquor to collect the mass 75-85'C recycling trifluoroacetic acid, a 115-125 . The acetic acid of the mass OF the production, wherein the cellulosic deposited mother liquor and distilling cooling to 18. A C, and putting 10 hours separating generated, obtained, the xylose and lower polyxylose 0,24g the depositing and washing and drying, distills the xylose and lower polyxylose deposited mother liquor collect the mass 125-135'C agent is 3 of the diameter of acrylic, alcohol, and lignin 0.22g the gas mother liquor separator for separating.

The embodiment 11 of bamboo for preparing and lower polyxylose, cellulose and lignin component of the bamboo sheets crush to 16 meshes of bolters, the name of lg is disposed on the circular flask, wherein the trifluoroacetic acid, 8ml the sealing cover, and arranging in after-cooling (8 TC the sand bath is centigrade, and 24 ml hexanols weight: The intensive mixing, settles 2 hours separating generated, obtained, non-stereotypia cellulose 0.46g the depositing and washing and drying, distills the cellulose deposited mother liquor to collect 75-85. THE mass recycling trifluoroacetic acid, a 115-125'C the mass to reduction the midwifery the material composition producing acetic acid, wherein the gas, wherein the cellulosic deposited mother liquor cooling to 18 ' - settles, 10 hours separating generated, obtained by the xylose and lower polyxylose 0.25g the depositing and washing and drying, distills the xylose and lower polyxylose deposited mother liquor collect the 153-163'C the mass hexanol, wherein of the stretched distillation mother liquor; The separating body, thousand and drying the lignin 0 23g. .

The embodiment 12 of the awn grass for preparing and lower polyxylose, cellulose and lignin component of the awn grass crush to 64 meshes of bolters, the name of lg is disposed on the circular flask, wherein the trifluoroacetic acid, 6ml the sealing cover, and 10h after-cooling of 60 ' - the sand bath to 25 degrees, and 30 ml hexalin intensive mixing weight, settles 6 hours separating generated, obtained, non-stereotypia fibre surface 0.38g the depositing and washing and drying, distills the cellulose deposited mother liquor to collect 75-85. THE mass recycling trifluoroacetic acid, a 115-125'C the mass to reduction the midwifery the material composition producing acetic acid, wherein the gas, wherein the cellulosic deposited mother liquor cooling to 18 ' - settles, 10 hours separating generated, obtained by the xylose and lower polyxylose 0.23g the depositing and washing and drying, distills the xylose and lower polyxylose deposited mother liquor collect the 156-165'C the mass hexalin; and lignin the gas mother liquor separator for separating 0 16g. .