CN107893131A - A kind of method of corncob Xylose - Google Patents

A kind of method of corncob Xylose Download PDF

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Publication number
CN107893131A
CN107893131A CN201711135964.7A CN201711135964A CN107893131A CN 107893131 A CN107893131 A CN 107893131A CN 201711135964 A CN201711135964 A CN 201711135964A CN 107893131 A CN107893131 A CN 107893131A
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China
Prior art keywords
corncob
xylose
quality
powder
hydrolyzate
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CN201711135964.7A
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Chinese (zh)
Inventor
江松涛
陈德水
李勉
廖承军
毛宝兴
郑毅
张金建
李山
汪秀秀
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Zhejiang Huakang Pharmaceutical Co Ltd
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Zhejiang Huakang Pharmaceutical Co Ltd
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Priority to CN201711135964.7A priority Critical patent/CN107893131A/en
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    • CCHEMISTRY; METALLURGY
    • C13SUGAR INDUSTRY
    • C13KSACCHARIDES OBTAINED FROM NATURAL SOURCES OR BY HYDROLYSIS OF NATURALLY OCCURRING DISACCHARIDES, OLIGOSACCHARIDES OR POLYSACCHARIDES
    • C13K13/00Sugars not otherwise provided for in this class
    • C13K13/002Xylose

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Biochemistry (AREA)
  • Organic Chemistry (AREA)
  • Saccharide Compounds (AREA)

Abstract

The invention discloses a kind of method of corncob Xylose, it is characterised in that including:(1) corncob is cleaned, dried and crushed and obtain corncob powder;(2) corncob powder is added in hydrolysis reactor, and adds the thermal process water that quality is 3~5 times of corncob powder quality, start to stir, and it is 2~4 to add sulphur acid for adjusting pH value, adds pectase, and temperature is maintained at 45~55 DEG C, 20~60min is incubated, enzymolysis obtains corncob liquid;(3) sulfuric acid is added in the corncob liquid, regulation acidity is 0.6~1.0%, and reaction is hydrolyzed, and wherein hydrolysising reacting temperature is 120~130 DEG C, 30~60min of reaction time, obtains hydrolyzate;(4) hydrolyzate is filtered, obtains the Xylose.The present invention is pre-processed using pectase so that pretreatment fluid does not have to emit, and can directly continue to hydrolyze with acid adding, makes hydrolysis operation easier, more environmentally-friendly;Reduce sewage discharge and water consumption;It is bundle fiber to make hemicellulose degradation, is more beneficial for hydrolyzing.

Description

A kind of method of corncob Xylose
Technical field
The invention belongs to food chemistry technical field, and in particular to a kind of method of corncob Xylose.
Background technology
Xylose is five-carbon ring aldehydo sugar, white crystals or crystalline powder, and sweet, sugariness is the 70% of sucrose.Xylose can improve Human microorganism's environment, promote body immunity.The production of xylose at present is mainly raw material through hydrolyzing, neutralizing, taking off using corncob Color, from hand over, concentration, crystallization, the process finished product xylose such as separation, wherein hydrolysis is the vital step of xylose production, water Solution technique from friendship, crystallization yield to subsequently having profound influence.
Publication No. CN106435047A Chinese patent literature discloses a kind of method of corncob xylose, hydrolyzes work Skill is corncob 3~5mm of granularity, acidity of sulfuric acid 1.5~2.5%, 120~150 DEG C of hydrolysis temperature, 2~4h of hydrolysis time.The method Sulfuric acid dosage is larger, and hydrolysis time is longer.
Publication No. CN105713998A Chinese patent literature discloses a kind of production technology of xylose, its hydrolysis process For corncob 2~3mm of granularity, it is 0.8~1.2% hydrochloric acid to add acidity after high temperature boiling pretreatment, and 2~4h of insulation enters water-filling Solution.The method is using hydrochloric acid as hydrolysis acid, and requirement anti-corruption to equipment is very high, and the reaction time is longer.
In summary, existing corncob hydrolysis process, by the way of low-kappa number, hydrolysis is larger with sour dosage, disappears Substantial amounts of sour waste water is produced while acid consumption, is unfavorable for environmental protection, and the reaction time is longer.Existing corncob hydrolysis process, The yield of xylose is not universal high, and the utilization rate of corncob is relatively low, containing substantial amounts of colloid to follow-up ion exchange in hydrolyzate Very big load is produced, the regeneration frequency of ion-exchange resins is very high.
The content of the invention
In order to solve the above problems, the invention provides a kind of method of corncob Xylose, and not only hydrolysis is few with acid, Reaction time is short, and hydrolyze after xylose yield be improved, the colloid in hydrolyzate is removed, to subsequent filter, from hand over, The processes such as crystallization, separation are all highly beneficial.
The technical scheme is that:A kind of method of corncob Xylose, including:
(1) corncob is cleaned, dried and crushed and obtain corncob powder;
(2) corncob powder is added in hydrolysis reactor, and adds quality as 3~5 times of corncob powder quality Thermal process water, start to stir, and it is 2~4 to add sulphur acid for adjusting pH value, adds pectase, and temperature is maintained at 45~55 DEG C, protects 20~60min of temperature, enzymolysis obtain corncob liquid;
(3) sulfuric acid is added in the corncob liquid, regulation acidity is 0.6~1.0%, reaction is hydrolyzed, its reclaimed water It is 120~130 DEG C to solve reaction temperature, 30~60min of reaction time, obtains hydrolyzate;
(4) hydrolyzate is filtered, obtains the Xylose.
Described corncob in step (1) by selection by winnowing, roller screen, the step such as wash, dry and remove jade in corncob Rice palpus, the impurity such as silt, dry standby and crush the corncob used in next step, preferably, it is described dry after corncob Moisture 8%~10%.
Preferably, the granularity of the corncob powder is 0.1~0.5mm.Corncob is in pulverulence, increases corn Core specific surface area so that corncob and sour contact area are bigger, advantageously in hydrolysis.
Preferably, the thermal process water is steam condensate (SC).
Preferably, the temperature of the steam condensate (SC) is 45~55 DEG C.Steam condensate (SC) of the present invention can use technique Steam condensate (SC) in evaporation process.
Preferably, when being stirred in the step (2), rotating speed is 80~100rpm.Corncob is crushed to powder, realizes Reaction is hydrolyzed under stirring, further increases contact of the corncob with acid, to reducing the reaction time, increases the water of xylose It is all highly beneficial to solve yield.
Preferably, the mass ratio of the corncob powder and thermal process water is 1:4.Both ensure corn under the mass ratio Core powder can have larger mobility, and and can ensures that hydrolyzate has higher refractive power, reduces subsequent evaporation gas consumption.
Preferably, hydrolyzate filters by flame filter press in the step (4), the wood that refractive power is 10~12% is obtained Liquid glucose.Hydrolyzate passes through plate-frame filtering in step (4), obtains refractive power and enters next step bleaching process for 10~12% hydrolyzates, Biomass fuel can be used as by being dried via the filter residue after filtering, and the invention enables hydrolysis residue to be fully used.
Preferably, the quality of the pectase is corncob quality 1~5 ‰.Pectase can be in degrading maize core Pectin, plant cell wall is destroyed, it is bundle fiber to make hemicellulose and cellulose degradation, is more beneficial for the progress of hydrolysis.Glue simultaneously The removal of body material, lifting to subsequent filter speed and from handing over the reduction met all to bring active influence.
Preferably, enzymolysis time is 30min in the step (2).
Preferably, sulfuric acid is the concentrated sulfuric acid that mass fraction is 98% in the step (3), acidity 0.6~1.0%.
Preferably, 123~125 DEG C of hydrolysising reacting temperature in the step (3), reaction time 50min.
Compared with prior art, beneficial effects of the present invention are embodied in:
(1) present invention carries out break process to corncob, and hydrolysis is carried out under stirring, increases corn The contact area of core and acid so that hydrolysis is more abundant, and hydrolysis efficiency is improved, and reaction is reduced with acid amount, during hydrolysis Between shorten, energy consumption reduces, and xylose yield significantly improves.
(2) compared with traditional technique, the present invention is pre-processed using pectase, has advantages below:
A. pretreatment fluid does not have to emit, and can directly continue to hydrolyze with acid adding, makes hydrolysis operation easier, more ring Protect;
B. sewage discharge and water consumption are reduced;
C. it is bundle fiber to make hemicellulose degradation, is more beneficial for hydrolyzing;
D. the removal of colloidal substance can also produce active influence to follow-up decolorization filtering, from friendship, crystallization, centrifuging process.
Embodiment
Embodiment 1
A kind of preparation method of Xylose, comprises the following steps:
(1) corncob is cleaned, dried;
(2) corncob after drying is crushed to the corncob powder that granularity is 0.1~0.5mm;
(3) corncob powder is added in hydrolysis reactor, adds the thermal process that quality is 3 times of corncob powder quality Water, stirring is opened, controls rotating speed 90rpm, adjust pH to 3.0, add 2.5 ‰ pectase of quality corncob powder quality, Temperature 50 C is controlled, is incubated 30min;
(4) continuing to add sulfuric acid, regulation acidity is 1.0%, and reacts 50min under the conditions of 125 DEG C, obtains hydrolyzate, its Middle acid is the concentrated sulfuric acid that mass fraction is 98%, acidity 0.8~1.0%;
(5) hydrolyzate is subjected to plate-frame filtering, collects filtrate, measured hydrolyzate refractive power and determine xylose for 11.5%, HPLC Concentration is 88.72g/L, Xylose Content 80.95%, and xylose yield advantage is that 26.5% (xylose quality/hydrolysis is beautiful in hydrolyzate Rice core quality).
Embodiment 2
A kind of preparation method of Xylose, comprises the following steps:
(1) corncob is cleaned, dried;
(2) corncob after drying is crushed to the corncob powder that granularity is 0.1~0.5mm;
(3) corncob powder is added in hydrolysis reactor, adds the thermal process that quality is 4 times of corncob powder quality Water, stirring is opened, control rotating speed 90rpm, adjust pH to 3.5, add 2 ‰ pectase of quality corncob powder quality, control Temperature 50 C processed, it is incubated 30min;
(4) continuing to add sulfuric acid, regulation acidity is 0.8%, and reacts 45min under the conditions of 123 DEG C, obtains hydrolyzate, its Middle acid is the concentrated sulfuric acid that mass fraction is 98%, acidity 0.8~1.0%;
(5) hydrolyzate is subjected to plate-frame filtering, collects filtrate, it is dense for 9.6%, HPLC measure xyloses to measure hydrolyzate refractive power Spend for 70.86g/L, Xylose Content 81.32%, the xylose yield advantage (xylose quality/hydrolysis of corncob in hydrolyzate that is 28% Quality).
Comparative example 1 (existing process)
A kind of preparation method of Xylose, comprises the following steps:
(1) corncob is cleaned, dried;
(2) corncob is added in hydrolysis reactor, adds the thermal process water that quality is 5 times of corncob powder quality, Acid adding regulation acidity is 0.2%, and 45min is incubated under the conditions of 120 DEG C;
(3) drain sour water, add the thermal process water that quality is 3 times of corncob powder quality, acid adding regulation acidity 2.0%, 120min is reacted under the conditions of 125 DEG C;
(4) hydrolyzate carries out plate-frame filtering, collects filtrate, measures hydrolyzate refractive power and determines xylose concentration for 9.8%, HPLC For 74.58g/L, Xylose Content 78.13%, the xylose yield advantage (xylose quality/hydrolysis of corncob matter in hydrolyzate that is 22% Amount).
Comparative example 2 (does not add pectase)
A kind of preparation method of Xylose, comprises the following steps:
(1) corncob is cleaned, dried;
(2) corncob is crushed to the corncob powder that granularity is 0.1~0.5mm;
(3) corncob powder is added in hydrolysis reactor, adds the thermal process that quality is 3 times of corncob powder quality Water, stirring is opened, control rotating speed 90rpm, acid adding regulation acidity is 1.8%, reacts 120min under the conditions of 120 DEG C, obtains water Solve liquid;
(4) hydrolyzate is subjected to plate-frame filtering, collects filtrate, measured hydrolyzate refractive power and determine xylose for 10.7%, HPLC Concentration is 82.64g/L, Xylose Content 79.48%, and xylose yield advantage is that 26.5% (xylose quality/hydrolysis is beautiful in hydrolyzate Rice core quality).
Comparative example 1 is conventional process conditions, and not add pectase contrast test, embodiment 1 and embodiment 2 are comparative example 2 The process of the present invention, can be seen that from above-mentioned result of implementation:Wood in the xylose hydrolysis fluid obtained under optimum condition of the present invention The yield of sugar is greatly improved, and the present invention can complete water under the conditions of shorter reaction time, relatively low acid concentration Solution reaction.

Claims (10)

  1. A kind of 1. method of corncob Xylose, it is characterised in that including:
    (1) corncob is cleaned, dried and crushed and obtain corncob powder;
    (2) corncob powder is added in hydrolysis reactor, and adds the thermal technology that quality is 3~5 times of corncob powder quality Skill water, start to stir, and it is 2~4 to add sulphur acid for adjusting pH value, adds pectase, and temperature is maintained at 45~55 DEG C, insulation 20 ~60min, enzymolysis obtain corncob liquid;
    (3) sulfuric acid is added in the corncob liquid, regulation acidity is 0.6~1.0%, and reaction is hydrolyzed, wherein hydrolysis is anti- It is 120~130 DEG C to answer temperature, 30~60min of reaction time, obtains hydrolyzate;
    (4) hydrolyzate is filtered, obtains the Xylose.
  2. 2. the method for corncob Xylose as claimed in claim 1, it is characterised in that it is described dry after corncob Moisture 8%~10%.
  3. 3. the method for corncob Xylose as claimed in claim 1, it is characterised in that the granularity of the corncob powder is 0.1~0.5mm.
  4. 4. the method for corncob Xylose as claimed in claim 1, it is characterised in that the thermal process water condenses for steam Water.
  5. 5. the method for corncob Xylose as claimed in claim 4, it is characterised in that the temperature of the steam condensate (SC) is 45~55 DEG C.
  6. 6. the method for corncob Xylose as claimed in claim 1, it is characterised in that when being stirred in the step (2), turn Speed is 80~100rpm.
  7. 7. the method for corncob Xylose as claimed in claim 1, it is characterised in that the corncob powder and thermal process The mass ratio of water is 1:4.
  8. 8. the method for corncob Xylose as claimed in claim 1, it is characterised in that hydrolyzate passes through in the step (4) Flame filter press filtering is crossed, obtains the Xylose that refractive power is 10~12%.
  9. 9. the method for corncob Xylose as claimed in claim 1, it is characterised in that the quality of the pectase is corn Core quality 1~5 ‰.
  10. 10. the method for corncob Xylose as claimed in claim 1, it is characterised in that hydrolysis in the step (3) 123~125 DEG C of temperature, reaction time 50min.
CN201711135964.7A 2017-11-16 2017-11-16 A kind of method of corncob Xylose Pending CN107893131A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109517860A (en) * 2018-12-07 2019-03-26 浙江华康药业股份有限公司 A method of crystal xylose is prepared using xylose mother liquid

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102943131A (en) * 2012-11-30 2013-02-27 安徽丰原发酵技术工程研究有限公司 Xylose preparation method

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102943131A (en) * 2012-11-30 2013-02-27 安徽丰原发酵技术工程研究有限公司 Xylose preparation method

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
荆丽荣: "酶法提取甜玉米芯中低聚木糖的研究", 《哈尔滨商业大学硕士学位论文》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109517860A (en) * 2018-12-07 2019-03-26 浙江华康药业股份有限公司 A method of crystal xylose is prepared using xylose mother liquid

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Application publication date: 20180410

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