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CN1515578A - Method for extracting xylose and xylitol from straw of crops - Google Patents

Method for extracting xylose and xylitol from straw of crops Download PDF

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Publication number
CN1515578A
CN1515578A CNA031108520A CN03110852A CN1515578A CN 1515578 A CN1515578 A CN 1515578A CN A031108520 A CNA031108520 A CN A031108520A CN 03110852 A CN03110852 A CN 03110852A CN 1515578 A CN1515578 A CN 1515578A
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China
Prior art keywords
xylitol
crop straw
raw material
agricultural crop
hydrolytic decomposition
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Pending
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CNA031108520A
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Chinese (zh)
Inventor
郑庆义
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Di Yuli
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Di Yuli
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Publication date
Application filed by Di Yuli filed Critical Di Yuli
Priority to CNA031108520A priority Critical patent/CN1515578A/en
Publication of CN1515578A publication Critical patent/CN1515578A/en
Pending legal-status Critical Current

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Abstract

The method for extracting xylose and xylitol from crop straw and stalk includes the following steps: using crop straw and stalk as raw material, pulverizing raw material, adding water whose added quantity is 4-6 times raw material weight, steaming for 1.5-2.5 hr. at 125-135 deg.C, washing for 3-5 times by using hot water with 75-85 deg.C, adding acid solution whose concentration is 0.65-0.75% and added quantity is 2-4 times raw material weight, making hydrolysis treatment at 105-115 deg.C until the xylose concentration is reached to 8-10%, filtering and decolouring by adopting resin, adopting ion-exchange resin to make ion-exchange treatment, making evaporation and concentration treatment under the condition of that pressure is 0.09 MPa and temp. is less than or equal to 75 deg.C, cooling to 60 deg.C and spray-drying so as to obtain the invented product.

Description

From agricultural crop straw, extract the method for wood sugar and Xylitol
(1), affiliated field
What the present invention relates to is a kind of method of utilizing of agricultural crop straw, specifically a kind of method of extracting the effective ingredient in the agricultural crop straw.
(2), background technology
The main chemical of agricultural crop straw is Mierocrystalline cellulose, pentosan, xylogen etc.The content of each Chemical Composition is different in the different agricultural crop straws.But the total amount of above-mentioned three kinds of materials remains on about 70% substantially.Along with science and technology development, the method for utilizing of multiple kinds of crops stalk has appearred.Wherein utilizing agricultural crop straw to extract wood sugar and Xylitol is exactly wherein a kind of.But the existing method of utilizing agricultural crop straw to extract wood sugar and Xylitol exists multiple weak point, be mainly reflected in: 1, not only cellulose, pentosan, xylogen etc. have the composition that utilize to be worth in the agricultural crop straw, also contain compositions such as protein, starch, fat, pectin, pigment, metal ion, inorganic salt, tannin and chemical fertilizer and agricultural chemicals, the existing method of utilizing, these compositions can not be removed, the quality of the product that obtains is low, production cost is high.2, owing to compositions such as starch can not be removed, starch at high temperature can change into glucose and influence the quality of wood sugar, so what existent method adopted all is the low temperature hydrolysis method, not only hydrolysis effect is poor, speed is slow, and the acid solution that must add high density just can be hydrolyzed, bring the handling problem of acid solution in the hydrolyzed solution so again, after hydrolysis, must carry out neutralizing treatment thus, increased cost.3, hydrolysis can not be carried out continuously, and efficient is low.And adopt the activated carbon decolorizing cost high.
(3), summary of the invention
The object of the present invention is to provide a kind of quality of wood sugar and xylitol products that can make to improve greatly, the method for from agricultural crop straw, extracting wood sugar and Xylitol that production cost reduces greatly.The object of the present invention is achieved like this: be raw material with the agricultural crop straw; With raw material pulverizing, add raw material weight 4-6 water doubly, under 125-135 ℃ of temperature boiling 1.5-2.5 hour; With 75-85 ℃ hot wash 3-5 time; Adding raw material weight 2-4 concentration doubly is the acid solution of 0.65-0.75%, in the processing that is hydrolyzed of 105-115 ℃ of temperature, reaches 8-10% to xylose concentration; Filter; Adopt resin to decolour; Adopt ion exchange resin to carry out ion exchange treatment; Carrying out evaporation concentration under at 0.09Mpa, smaller or equal to 75 ℃ condition handles; Be cooled to 60 ℃, spraying drying obtains xylose product.Method of the present invention can also comprise like this some technical characterictics: 1, after hydrolysis to wherein feeding high pressure hydrogen.Make wood sugar change into Xylitol.2, described agricultural crop straw is a corn cob.3, described hydrolysis treatment is that the continuous hydrolysis that carries out in 3-4 the placed in-line hydrolytic decomposition pot is handled, raw material after wash the river flowing from Guizhou Province through Hunan into Dongting Lake joins elementary hydrolytic decomposition pot earlier and once is being transported to the next stage hydrolytic decomposition pot, hydrolyzed solution is from final stage hydrolytic decomposition pot upwards one-stage hydrolysis jar revolution successively, and the hydrolyzed solution of drawing from elementary hydrolytic decomposition pot enters the filtration operation.4, described filtration is that vacuum suction filter combines with flame filter press.The total content of Mierocrystalline cellulose, pentosan, xylogen etc. is about 70% in the various agricultural crop straws, but the content of various concrete compositions is distinguished to some extent in the different agricultural crop straws.Though Gu the multiple kinds of crops stalk all can be used as the raw material that extracts wood sugar and Xylitol, the resulting effect of different agricultural crop straws can be different.The content of pentosan can reach a new horizontal 5-40% in the corn cob, and in the rice husk, straw the content of pentosan only 22% and 19%, so the present invention is with the preferred feedstock of corn cob as extraction wood sugar and Xylitol.High-temperature water boiling of the present invention and high temperature washing step, the protein, starch, fat, pectin, pigment, metal ion, inorganic salt, tannin and the chemical fertilizer that are contained in the agricultural crop straw and the residue of agricultural chemicals etc. can be removed extracting the useless or disadvantageous material of wood sugar and Xylitol, particularly removed starch wherein, avoided that starch changes into glucose in the process of separating, be convenient to adopt the hydrolysis process of high temperature, low acid concentration; Adopted high temperature, low acidity continuous hydrolysis technology, the percent hydrolysis of pentosan improved greatly, reduced the loss of wood sugar, improved the extraction yield of wood sugar, particularly omitted after the hydrolysis in and operation, simplified technology, reduced cost, reduced environmental pollution; The present invention adopts resin decolorization, resin ion-exchange, reduced in other extracting method in and operation; Adopted spray-dired drying means, taken away moisture content with cleaning exsiccant hot blast, obtained the tiny xylose product of particle, crystallization velocity is fast, can save crystallization time more than 30 hours.The present invention improves quality product by optimized choice, allotment to extraction process greatly, and the wood sugar purity that obtains can reach more than 90%, and does not wherein contain glucose, and the wood sugar standard can meet international standards.The wood sugar that can adopt high-pressure hydrogenation process hydrolysis can be obtained after the hydrolysis changes into Xylitol.The wood sugar yield of method of the present invention can be up to one-tenth more than 25%, and 4 tons of corn cobs can produce wood sugar more than 1 ton.Production cost is low, than the production cost decline 2/3 of other production method.The construction investment that method of the present invention can make simultaneously reduces greatly.
(4), specific embodiments
For example the present invention is done more detailed description below:
With the agricultural crop straw is raw material; With raw material pulverizing, add raw material weight 4-6 water doubly, under 125-135 ℃ of temperature boiling 1.5-2.5 hour; With 75-85 ℃ hot wash 3-5 time; Adding raw material weight 2-4 concentration doubly is the sulphuric acid soln of 0.65-0.75%, in the processing that is hydrolyzed of 105-115 ℃ of temperature, reaches 8-10% to xylose concentration.Hydrolysis treatment is that the continuous hydrolysis that carries out in 3-4 the placed in-line hydrolytic decomposition pot is handled, raw material after washing joins elementary hydrolytic decomposition pot earlier and once is being transported to the next stage hydrolytic decomposition pot, hydrolyzed solution is from final stage hydrolytic decomposition pot upwards one-stage hydrolysis jar revolution successively, and the hydrolyzed solution of drawing from elementary hydrolytic decomposition pot enters the filtration operation; Filter; Adopt resin to decolour, resin preferably adopts wide aperture quaternary amine type resin anion(R.A); Adopt ion exchange resin to carry out ion exchange treatment, MT1, MT2 type wood sugar that ion exchange resin preferably selects for use Shenyang Organic Chemical Plant to produce are resin dedicated; Carrying out evaporation concentration under at 0.09Mpa, smaller or equal to 75 ℃ condition handles; Be cooled to 60 ℃, spraying drying obtains xylose product.
With the corn cob is raw material; With raw material pulverizing to particle diameter at 1-3mm, add the water of 4 times of raw material weights, boiling is 2 hours under 130 ℃ of temperature; With 80 ℃ hot washes 4 times; The concentration that adds 3 times of raw material weights is that 0.70% sulphuric acid soln is as hydrolyzed solution, in the processing that is hydrolyzed of 110 ℃ of temperature, reach 8-10% to xylose concentration, hydrolysis treatment is that the continuous hydrolysis that carries out in 3 placed in-line hydrolytic decomposition pots is handled, raw material after washing joins elementary hydrolytic decomposition pot earlier and once is being transported to the next stage hydrolytic decomposition pot, hydrolyzed solution is from final stage hydrolytic decomposition pot upwards one-stage hydrolysis jar revolution successively, and the hydrolyzed solution of drawing from elementary hydrolytic decomposition pot enters the filtration operation; Combine with flame filter press with vacuum suction filter and to filter; Adopt resin to decolour; Adopt ion exchange resin to carry out ion exchange treatment; Carrying out evaporation concentration under at 0.09Mpa, smaller or equal to 75 ℃ condition handles; Be cooled to 60 ℃, spraying drying obtains product.
With the corn cob is raw material; With raw material pulverizing to particle diameter at 1-3mm, add the water of 4 times of raw material weights, boiling is 2 hours under 130 ℃ of temperature; With 80 ℃ hot washes 4 times; The concentration that adds 3 times of raw material weights is that 0.70% sulphuric acid soln is as hydrolyzed solution, in the processing that is hydrolyzed of 110 ℃ of temperature, reach 8-10% to xylose concentration, hydrolysis treatment is that the continuous hydrolysis that carries out in 3 placed in-line hydrolytic decomposition pots is handled, raw material after washing joins elementary hydrolytic decomposition pot earlier and once is being transported to the next stage hydrolytic decomposition pot, hydrolyzed solution is from final stage hydrolytic decomposition pot upwards one-stage hydrolysis jar revolution successively, and the hydrolyzed solution of drawing from elementary hydrolytic decomposition pot enters the filtration operation; To wherein feeding high pressure hydrogen, the temperature of hydrogen is at 70-75 normal atmosphere after hydrolysis; Combine with flame filter press with vacuum suction filter and to filter; Adopt resin to decolour; Adopt ion exchange resin to carry out ion exchange treatment; Carrying out evaporation concentration under at 0.09Mpa, smaller or equal to 75 ℃ condition handles; Be cooled to 60 ℃, spraying drying obtains xylitol products.

Claims (9)

1, a kind of method of extracting wood sugar and Xylitol from agricultural crop straw is characterized in that:
1.1, be raw material with the agricultural crop straw;
1.2, with raw material pulverizing, add raw material weight 4-6 water doubly, under 125-135 ℃ of temperature boiling 1.5-2.5 hour;
1.3, with 75-85 ℃ hot wash 3-5 time;
1.4, to add raw material weight 2-4 concentration doubly be the acid solution of 0.65-0.75%, in the processing that is hydrolyzed of 105-115 ℃ of temperature, reaches 8-10% to xylose concentration;
1.5, filter;
1.6, adopt decolorizing resin to decolour;
1.7, adopt ion exchange resin to carry out ion exchange treatment;
1.8, carry out evaporation concentration under at 0.09Mpa, smaller or equal to 75 ℃ condition and handle;
1.9, be cooled to 60 ℃, spraying drying obtains xylose product.
2, the method for extracting wood sugar and Xylitol from agricultural crop straw according to claim 1 is characterized in that: after hydrolysis to wherein feeding high pressure hydrogen.
3, according to claim 1, the 2 described methods of extracting wood sugar and Xylitol from agricultural crop straw, it is characterized in that: described agricultural crop straw is a corn cob.
4, according to claim 1, the 2 described methods of from agricultural crop straw, extracting wood sugar and Xylitol, it is characterized in that: described hydrolysis treatment is that the continuous hydrolysis that carries out in 3-4 placed in-line hydrolytic decomposition pot is handled, raw material after washing joins elementary hydrolytic decomposition pot earlier and is transported to the next stage hydrolytic decomposition pot more successively, hydrolyzed solution is from final stage hydrolytic decomposition pot upwards one-stage hydrolysis jar revolution successively, and the hydrolyzed solution of drawing from elementary hydrolytic decomposition pot enters the filtration operation.
5, the method for from agricultural crop straw, extracting wood sugar and Xylitol according to claim 3, it is characterized in that: described hydrolysis treatment is that the continuous hydrolysis that carries out in 3-4 placed in-line hydrolytic decomposition pot is handled, raw material after washing joins elementary hydrolytic decomposition pot earlier and is transported to the next stage hydrolytic decomposition pot more successively, hydrolyzed solution is from final stage hydrolytic decomposition pot upwards one-stage hydrolysis jar revolution successively, and the hydrolyzed solution of drawing from elementary hydrolytic decomposition pot enters the filtration operation.
6, according to claim 1, the 2 described methods of extracting wood sugar qualifying Xylitol from agricultural crop straw, it is characterized in that: described filtration is that vacuum suction filter combines with flame filter press.
7, the method for extracting wood sugar and Xylitol from agricultural crop straw according to claim 3, it is characterized in that: described filtration is that vacuum suction filter combines with flame filter press.
8, the method for extracting wood sugar and Xylitol from agricultural crop straw according to claim 4, it is characterized in that: described filtration is that vacuum suction filter combines with flame filter press.
9, the method for extracting wood sugar and Xylitol from agricultural crop straw according to claim 3, it is characterized in that: described filtration is that vacuum suction filter combines with flame filter press.
CNA031108520A 2003-01-10 2003-01-10 Method for extracting xylose and xylitol from straw of crops Pending CN1515578A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CNA031108520A CN1515578A (en) 2003-01-10 2003-01-10 Method for extracting xylose and xylitol from straw of crops

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CNA031108520A CN1515578A (en) 2003-01-10 2003-01-10 Method for extracting xylose and xylitol from straw of crops

Publications (1)

Publication Number Publication Date
CN1515578A true CN1515578A (en) 2004-07-28

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Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102021252A (en) * 2010-12-21 2011-04-20 山东省鲁洲食品集团有限公司 Method and device for continuously hydrolyzing corn bran
CN101130558B (en) * 2007-08-28 2011-09-21 济南圣泉集团股份有限公司 System and method for preparing pentose sugar solution by series continuous hydrolysis
CN102268490A (en) * 2011-06-16 2011-12-07 北京化工大学 Clean technique for co-producing xylose, xylitol and arabinose from agricultural and forestal waste
CN102976895A (en) * 2012-12-12 2013-03-20 郑州金土地能源科技有限公司 Method for producing xylitol through utilizing crop wastes
CN103012065A (en) * 2012-12-27 2013-04-03 中国科学院广州能源研究所 Method for preparing high-concentration polyhydric alcohol by circularly hydrolyzing and hydrogenating biomass
CN103555864A (en) * 2013-10-22 2014-02-05 广西金麦克生物科技有限公司 Preparation method for xylose
CN105123808A (en) * 2015-10-08 2015-12-09 丹阳市中药材科技发展协会 Botanical fungicide for preventing and controlling southern blight of atractylodes and preparation method thereof
CN106831342A (en) * 2017-01-20 2017-06-13 西南交通大学 A kind of method that utilization agricultural crop straw prepares xylitol
CN109207646A (en) * 2018-11-16 2019-01-15 山东福田药业有限公司 A kind of preparation method of xylose
CN109761754A (en) * 2019-01-24 2019-05-17 西安海润新材料有限公司 A kind of discoloration method of Xylitol mother liquor
CN110305990A (en) * 2018-03-20 2019-10-08 郑庆义 A kind of method of xylose and xylose total sugar powder in separation and Extraction straw
US10759727B2 (en) 2016-02-19 2020-09-01 Intercontinental Great Brands Llc Processes to create multiple value streams from biomass sources

Cited By (19)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101130558B (en) * 2007-08-28 2011-09-21 济南圣泉集团股份有限公司 System and method for preparing pentose sugar solution by series continuous hydrolysis
CN102021252A (en) * 2010-12-21 2011-04-20 山东省鲁洲食品集团有限公司 Method and device for continuously hydrolyzing corn bran
CN102021252B (en) * 2010-12-21 2013-02-27 山东省鲁洲食品集团有限公司 Method and device for continuously hydrolyzing corn bran
CN102268490A (en) * 2011-06-16 2011-12-07 北京化工大学 Clean technique for co-producing xylose, xylitol and arabinose from agricultural and forestal waste
CN102976895A (en) * 2012-12-12 2013-03-20 郑州金土地能源科技有限公司 Method for producing xylitol through utilizing crop wastes
CN102976895B (en) * 2012-12-12 2015-09-30 郑州金土地能源科技有限公司 Wastes of crops is utilized to make the method for Xylitol
CN103012065A (en) * 2012-12-27 2013-04-03 中国科学院广州能源研究所 Method for preparing high-concentration polyhydric alcohol by circularly hydrolyzing and hydrogenating biomass
CN103012065B (en) * 2012-12-27 2015-03-18 中国科学院广州能源研究所 Method for preparing high-concentration polyhydric alcohol by circularly hydrolyzing and hydrogenating biomass
CN103555864B (en) * 2013-10-22 2015-07-22 广西金麦克生物科技有限公司 Preparation method for xylose
CN103555864A (en) * 2013-10-22 2014-02-05 广西金麦克生物科技有限公司 Preparation method for xylose
CN105123808A (en) * 2015-10-08 2015-12-09 丹阳市中药材科技发展协会 Botanical fungicide for preventing and controlling southern blight of atractylodes and preparation method thereof
US10759727B2 (en) 2016-02-19 2020-09-01 Intercontinental Great Brands Llc Processes to create multiple value streams from biomass sources
US11840500B2 (en) 2016-02-19 2023-12-12 Intercontinental Great Brands Llc Processes to create multiple value streams from biomass sources
US12139451B2 (en) 2016-02-19 2024-11-12 Intercontinental Great Brands Llc Processes to create multiple value streams from biomass sources
CN106831342A (en) * 2017-01-20 2017-06-13 西南交通大学 A kind of method that utilization agricultural crop straw prepares xylitol
CN106831342B (en) * 2017-01-20 2020-03-10 西南交通大学 Method for preparing xylitol by utilizing crop straws
CN110305990A (en) * 2018-03-20 2019-10-08 郑庆义 A kind of method of xylose and xylose total sugar powder in separation and Extraction straw
CN109207646A (en) * 2018-11-16 2019-01-15 山东福田药业有限公司 A kind of preparation method of xylose
CN109761754A (en) * 2019-01-24 2019-05-17 西安海润新材料有限公司 A kind of discoloration method of Xylitol mother liquor

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