CN102584907B - Maize straw is the method for raw material production wood sugar and pectinose - Google Patents
Maize straw is the method for raw material production wood sugar and pectinose Download PDFInfo
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- CN102584907B CN102584907B CN201210006133.0A CN201210006133A CN102584907B CN 102584907 B CN102584907 B CN 102584907B CN 201210006133 A CN201210006133 A CN 201210006133A CN 102584907 B CN102584907 B CN 102584907B
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Abstract
The present invention relates to a kind of method that maize straw is raw material production wood sugar and pectinose.In reducing sugar in corn stalk hydrolysis, Xylose Content accounts for 65% ~ 75%, and pectinose accounts for 15 ~ 20%, in the process extracting wood sugar, and purity and the crystallization yield of what pectinose was serious affect wood sugar.Method of the present invention comprises the steps: pre-treatment in (1) pot; (2) be hydrolyzed; (3) neutralize; (4) decolour; (5) once exchange; (6) single vaporization; (7) carry out second and third, four secondary ions exchange; (8) double evaporation-cooling; (9) carry out chromatographic separation with chromatographic separation equipment, switching time 5760s, swap time 3360s; (10) dense evaporation eventually, (11) crystallization: massecuite refractive power: 85-86%, cooling rate: 1 DEG C/h, crystallizing cycle: 45-55 h, mixing speed: 1 rev/min, separation temperature: 35-45 DEG C, finally carries out centrifugal oven dry.It is raw material production wood sugar and pectinose that method of the present invention is used for maize straw.
Description
technical field:
the present invention relates to a kind of method that maize straw is raw material production wood sugar and pectinose.
background technology:
maize straw is produced in xylose crystalline massecuite, and Xylose Content accounts for 65% ~ 75%, and pectinose accounts for 15 ~ 20%, in the process extracting wood sugar, and purity and the crystallization yield of what pectinose was serious affect wood sugar.Only has the content reducing pectinose, the cost that maize straw produces wood sugar could be reduced, could realize cornstalk biological matter replaces corn cob to produce wood sugar, significantly can reduce the production cost of wood sugar, Xylitol can be made to enter huge numbers of families, improve the quality of life of ordinary people, at present in corn cob production xylose production, to being separated, just to xylose mother liquid of wood sugar and pectinose, lab scale and pilot scale separation purity on the low side, produce so application is not large.
chromatogram as one mixture analytical method quickly and easily, due to it accurately and fast, conveniently, can be used for oil and chemical industry produce in quality control, obtain widespread use, but apply also few at present as the industrial process for separating of mixture.Chromatogram occurs as a kind of separation means at first in fact, after a while just for analyzing.But preparative scale chromatogram, generally also only has several grams in the past, real large-scale industrial application is also the thing in nearly ten or twenty year.One of reason is that the chromatographic column separating effect that general technology is filled sharply declines with the increase of column diameter; Next is under Finite Concentration, does not have effective chromatographic theory can the amplification design of instruction course.In addition, chromatographic run is intermittent type, is an interruption steady-state process, and unlike can with the chemical engineering unit operation of its competition if rectifying, absorption, extraction etc. are continuous steady-state processs.Large-scale chromatographic process, also there is certain difficulty in operation and equipment all more complicated on chromatogram is amplified.These reasons hamper the tempo of chromatographic technique application in technical scale is separated, and for some time very long in the past, for the large-scale chromatogram slower development of suitability for industrialized production.Nearly ten years due to the joint efforts (the former solves scale effect, and the latter studies chromatographic theory) of chemical engineer and chromatogram expert, chromatogram is made to enter the more ripe applied research stage as a kind of industrial separation purification process.Along with the development of amplifying technique, large-scale chromatogram also can be accomplished as small-sized chromatogram effective.
although preparing chromatograph in industry has great separating power, it neither be omnipotent., interferences very low for target product concentration is a lot, complicated especially system, as the isolation and purification of biological technology products, usually still need to coordinate process or initial gross separation the early stage of carrying out raw material with other conventional isolation techniques, and preparing chromatograph in industry technology is used as the final purification step of finished product.In addition, the isolation technique of preparing chromatograph in industry or a kind of high investment, up to now, is mainly used in isolation and purification high added value and the high product of purity requirement, thus develops particularly rapid in biotechnology and pharmacy industry.Regrettably, large-scale industry preparative chromatography not yet really starts so far in the use of China, still has and waits upon in further R and D.
summary of the invention:
the object of this invention is to provide a kind of method that maize straw is raw material production wood sugar and pectinose, the purity of wood sugar in corn stalk hydrolysis can be brought up to 85% by 70%, make the crystallization of xylose mother liquid second time, make the crystallization yield of wood sugar rise to 70% by 50%.The purity of pectinose rises to 75% by 15% simultaneously, and reach the condition of Crystallization Separation, the yield of pectinose reaches 50%.Both improve the yield of wood sugar, successfully extract high-purity arabinose again.
above-mentioned object is realized by following technical scheme:
maize straw is the method for raw material production wood sugar and pectinose, and the method comprises the steps:
(1) pre-treatment in pot: section maize straw being clipped to 3-4 centimetre, pre-treatment in pot is carried out by the feeding quantity material loading of every pot of 2 tons of maize straws, every pot adds 0.07-0.08%(mass percentage concentration) 17.5 kilograms, sulfuric acid, add water 7.8-8 ton, temperature 110-120 DEG C, pressure 0.05-0.1MPa, 1 hour treatment time, by liquid discharge after pre-treatment;
(2) be hydrolyzed: in pot, pretreated product adds hydrolyzed solution, hydrolyzed solution configuration wash water 6-6.5 ton, 110.5 kilograms, sulfuric acid, hydrolyzed solution sulfuric acid concentration 1.6-1.7%(mass percentage concentration), hydrolysis temperature 110-120 DEG C, pressure 0.15-0.16MPa, heat up 1 hour hydrolysis time 2 hours, carries out washing, pulp water is separated after hydrolysis;
(3) neutralize: isolated liquid after hydrolysis is added the calcium carbonate soln of degree Beaume 14-16 degree, and temperature 80 DEG C, stirs 30 minutes, regulates pH value 2.5-3.0;
(4) decolour, add activated carbon decolorizing in product after the neutralization to solution transmittance 47-55%, refractive index is not less than 6%;
(5) once exchange: carry out ion-exchange with hybrid ionic exchange column, add hydrochloric acid, caustic soda makes resin regeneration, ensure in the process exchange liquid printing opacity>=70% ﹑ refractive power>=5.0% ﹑ inorganic salt 0.05% Yi Xia ﹑ ash content less than 0.1%.
(6) single vaporization: temperature is 80 DEG C-85 DEG C, evaporation concentration to mass percentage concentration is 25%, printing opacity>=20%;
(7) carry out second and third, four secondary ions exchange, add hydrochloric acid, caustic soda makes resin regeneration, ensure printing opacity>=96% exchanging liquid in the process, pH4.3-5.5; Mineral acid less than 0.01.
(8) double evaporation-cooling: evaporation concentration to 60%, control temperature 70-80 DEG C, printing opacity>=60%,
(9) carry out chromatographic separation with chromatographic separation equipment, switching time 5760s, swap time 3360s, be separated after xylose purity be greater than 85%, pectinose purity is greater than 65%, then carries out secondary separation to pectinose and makes its purity be greater than 80%;
(10) eventually dense evaporation: evaporation concentration to 85%-86%, printing opacity>=50%
(11) crystallization: massecuite refractive power: 85-86%, cooling rate: 1 DEG C/h, crystallizing cycle: 45-55 h, mixing speed: 1 rev/min, separation temperature: 35-45 DEG C, finally carries out centrifugal oven dry.
beneficial effect:
1. the present invention can bring up to 85% the purity that maize straw produces wood sugar in the wood sugar massecuite of wood sugar by 70%, makes the crystallization of xylose mother liquid second time, makes the crystallisation recoveries of wood sugar cream rise to 70% by 50%.The purity of pectinose rises to 75% by 15% simultaneously, and reach the condition of Crystallization Separation, the rate of recovery of pectinose reaches 50%.Both improve the yield of wood sugar, successfully extract high-purity arabinose again.
the present invention realizes utilizing maize straw to produce Mu Tang ﹑ pectinose, xylose residue coproduction papermaking.Tradition wood sugar raw materials for production utilize corn cob.The present invention utilizes maize straw to produce wood sugar, not only widen xylose production raw material, and to realize coproduction papermaking is that maize straw is fully used.The present invention can bring up to 85% the purity that maize straw produces wood sugar in the wood sugar massecuite of wood sugar by 70%, makes the crystallization of xylose mother liquid second time, makes the crystallisation recoveries of wood sugar cream rise to 70% by 50%.The purity of pectinose rises to 75% by 15% simultaneously, and reach the condition of Crystallization Separation, the rate of recovery of pectinose reaches 50%.Both improve the yield of wood sugar, successfully extract high-purity arabinose again.
accompanying drawing illustrates:
fig. 1 is process flow sheet of the present invention;
embodiment:
embodiment 1:
maize straw is the method for raw material production wood sugar and pectinose, it is characterized in that: the method comprises the steps:
(1) pre-treatment in pot: section maize straw being clipped to 3-4 centimetre, pre-treatment in pot is carried out by the feeding quantity material loading of every pot of 2 tons of maize straws, every pot adds 0.07-0.08%(mass percentage concentration) 17.5 kilograms, sulfuric acid, add water 7.8-8 ton, temperature 110-120 DEG C, pressure 0.05-0.1MPa, 1 hour treatment time, by liquid discharge after pre-treatment; (2) be hydrolyzed: in pot, pretreated product adds hydrolyzed solution, hydrolyzed solution configuration wash water 6-6.5 ton, 110.5 kilograms, sulfuric acid, hydrolyzed solution sulfuric acid concentration 1.6-1.7%(mass percentage concentration), hydrolysis temperature 110-120 DEG C, pressure 0.15-0.16MPa, heat up 1 hour hydrolysis time 2 hours, carries out washing pulp water and be separated after hydrolysis;
(3) neutralize: isolated liquid after hydrolysis is added the calcium carbonate soln of degree Beaume 14-16 degree, and temperature 80 DEG C, stirs 30 minutes, regulates pH value 2.5-3.0;
(4) decolour, add activated carbon decolorizing in product after the neutralization to solution transmittance 47-55%, refractive index is not less than 6%;
(5) once exchange: carry out ion-exchange with hybrid ionic exchange column, add hydrochloric acid, caustic soda makes resin regeneration, ensure in the process exchange liquid printing opacity>=70% ﹑ refractive power>=5.0% ﹑ inorganic salt 0.05% Yi Xia ﹑ ash content less than 0.1%;
(6) single vaporization: temperature is 80 DEG C-85 DEG C, evaporation concentration to mass percentage concentration is 25%, printing opacity:>=20%;
(7) carry out second and third, four secondary ions exchange, add hydrochloric acid, caustic soda makes resin regeneration, ensure printing opacity>=96% exchanging liquid in the process, pH4.3-5.5; Mineral acid less than 0.01;
(8) double evaporation-cooling: evaporation concentration to 60%, control temperature 70-80 DEG C, printing opacity>=60%;
(9) carry out chromatographic separation with chromatographic separation equipment, switching time 5760s, swap time 3360s, be separated after xylose purity be greater than 85%, pectinose purity is greater than 65%, then carries out secondary separation to pectinose and makes its purity be greater than 80%;
(10) eventually dense evaporation: evaporation concentration to 85%-86%, printing opacity>=50%
(11) crystallization: massecuite refractive power: 85-86%, cooling rate: 1 DEG C/h, crystallizing cycle: 45-55 h, mixing speed: 1 rev/min, separation temperature: 35-45 DEG C, finally carries out centrifugal oven dry.
Claims (1)
1.
maize straw is a method for raw material production wood sugar and pectinose, it is characterized in that: the method comprises the steps:
(1) pre-treatment in pot: section maize straw being clipped to 3-4 centimetre, pre-treatment in pot is carried out by the feeding quantity material loading of every pot of 2 tons of maize straws, every pot adds 17.5 kilograms, the sulfuric acid of 0.07-0.08% by mass percentage concentration, add water 7.8-8 ton, temperature 110-120 DEG C, pressure 0.05-0.1MPa, 1 hour treatment time, by liquid discharge after pre-treatment;
(2) be hydrolyzed: in pot, pretreated product adds hydrolyzed solution, hydrolyzed solution configuration wash water 6-6.5 ton, 110.5 kilograms, sulfuric acid, hydrolyzed solution sulfuric acid is by the 1.6-1.7% of mass percentage concentration, hydrolysis temperature 110-120 DEG C, pressure 0.15-0.16MPa, heat up 1 hour hydrolysis time 2 hours, carries out washing, pulp water is separated after hydrolysis;
(3) neutralize: isolated liquid after hydrolysis is added the calcium carbonate soln of degree Beaume 14-16 degree, and temperature 80 DEG C, stirs 30 minutes, regulates pH value 2.5-3.0;
(4) decolour, add activated carbon decolorizing in product after the neutralization to solution transmittance 47-55%, refractive index is not less than 6%;
(5) once exchange: carry out ion-exchange with hybrid ionic exchange column; Add hydrochloric acid, caustic soda make resin regeneration, ensure in the process to exchange liquid printing opacity>=70% ﹑ refractive power>=5.0% ﹑ inorganic salt 0.05% Yi Xia ﹑ ash content less than 0.1%;
(6) single vaporization: temperature is 80 DEG C-85 DEG C, evaporation concentration to mass percentage concentration is 25%, printing opacity>=20%;
(7) carry out second and third, four secondary ions exchange, add hydrochloric acid, caustic soda makes resin regeneration, ensure printing opacity>=96% exchanging liquid in the process, pH4.3-5.5; Mineral acid less than 0.01;
(8) double evaporation-cooling: evaporation concentration to 60%, control temperature 70-80 DEG C, printing opacity>=60%,
(9) carry out chromatographic separation with chromatographic separation equipment, switching time 5760s, swap time 3360s, be separated after xylose purity be greater than 85%, pectinose purity is greater than 65%, then carries out secondary separation to pectinose and makes its purity be greater than 80%;
(10) eventually dense evaporation: evaporation concentration to 85%-86%, printing opacity>=50%;
(11) crystallization: massecuite refractive power: 85-86%, cooling rate: 1 DEG C/h, crystallizing cycle: 45-55 h, mixing speed: 1 rev/min, separation temperature: 35-45 DEG C, finally carries out centrifugal oven dry.
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| 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 |
| CN106831342B (en) * | 2017-01-20 | 2020-03-10 | 西南交通大学 | Method for preparing xylitol by utilizing crop straws |
| CN112225762A (en) * | 2020-11-09 | 2021-01-15 | 安阳市豫鑫木糖醇科技有限公司 | Process for extracting xylose |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101096376A (en) * | 2006-06-26 | 2008-01-02 | 黄广民 | Method for purifying D-xylose and xylooligosacchrides from coconut hard shell acid hydrolysate |
| CN101665523A (en) * | 2009-09-30 | 2010-03-10 | 济南圣泉集团股份有限公司 | Method for producing L-arabinose and D-xylose |
| CN101792822A (en) * | 2010-03-30 | 2010-08-04 | 天津科技大学 | Method for separating and purifying xylose and arabinose from hemicellulose acid hydrolysis liquid |
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| JP2004261039A (en) * | 2003-02-28 | 2004-09-24 | Unitika Ltd | L-arabinose-containing crystalline powder sugar composition and method for producing the same |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101096376A (en) * | 2006-06-26 | 2008-01-02 | 黄广民 | Method for purifying D-xylose and xylooligosacchrides from coconut hard shell acid hydrolysate |
| CN101665523A (en) * | 2009-09-30 | 2010-03-10 | 济南圣泉集团股份有限公司 | Method for producing L-arabinose and D-xylose |
| CN101792822A (en) * | 2010-03-30 | 2010-08-04 | 天津科技大学 | Method for separating and purifying xylose and arabinose from hemicellulose acid hydrolysis liquid |
Non-Patent Citations (1)
| Title |
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| 结晶木糖的研制;赵先芝;《河南化工》;20011231(第10期);第8-9页 * |
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Inventor after: Feng Jinbao Inventor after: Yang Dongping Inventor before: Wang Shugui Inventor before: Liu Xuezeng Inventor before: Deng Shuqin Inventor before: Liu Xuelu Inventor before: Xiao Jingcheng Inventor before: Feng Jinbao |
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Free format text: CORRECT: INVENTOR; FROM: WANG SHUGUI LIU XUEZENG DENG SHUQIN LIU XUELU XIAO JINGCHENG FENG JINBAO TO: FENG JINBAO YANG DONGPING |
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