CN110499395A - The extracting method of high yield pulp1 hemicellulose xylose - Google Patents

The extracting method of high yield pulp1 hemicellulose xylose Download PDF

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Publication number
CN110499395A
CN110499395A CN201910809161.8A CN201910809161A CN110499395A CN 110499395 A CN110499395 A CN 110499395A CN 201910809161 A CN201910809161 A CN 201910809161A CN 110499395 A CN110499395 A CN 110499395A
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China
Prior art keywords
hemicellulose
xylose
high yield
acidulants
lye
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CN201910809161.8A
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Chinese (zh)
Inventor
冯文军
柴艳民
邓雪燕
刘继霞
贺顺桂
王�琦
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Xinjiang Zhongtai Textile Group Co Ltd
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Xinjiang Zhongtai Textile Group Co Ltd
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Priority to CN201910809161.8A priority Critical patent/CN110499395A/en
Publication of CN110499395A publication Critical patent/CN110499395A/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)
  • Polysaccharides And Polysaccharide Derivatives (AREA)

Abstract

The present invention relates to xylose extractive technique fields in viscose rayon raw material, it is a kind of extracting method of high yield pulp1 hemicellulose xylose, it is carried out as steps described below: pulp and lye are mixed with dipping except after impurity, obtain secondary lye, secondary lye is separated by membrane technology, extracted, dried, and hemicellulose powder is obtained;Sulfuric acid is uniformly mixed with hemicellulose powder, obtains mixed liquor;Mixed liquor is acidified under water bath condition, obtains acidulants;Water is added into acidulants, cooling, suction filtration, obtains high yield pulp1 hemicellulose xylose after acidulants hydrolysis.The present invention in viscose rayon production, carries out technology processing by being mixed with dipping the hemicellulose powder extracted to pulp and lye, extracts wherein high-quality resource hemicellulose xylose, wherein hemicellulose xylose yield can reach 84% for the first time.Present invention reduces the wastes of by-product hemicellulose extra in production process of viscose fiber, improve the value of by-product hemicellulose in viscose rayon production.

Description

The extracting method of high yield pulp1 hemicellulose xylose
Technical field
The present invention relates to xylose extractive technique fields in viscose rayon raw material, are a kind of mentioning for high yield pulp1 hemicellulose xylose Take method.
Background technique
Hemicellulose is a kind of good resource, is the heteromultimer being made of several different types of monosaccharide, these Sugar is pentose and hexose, including xylose, arabinose and galactolipin etc..Hemicellulose xylan Zhan in lignum is total The 50% of amount dissolves in aqueous slkali, the part plant polyose susceptible to hydrolysis far beyond cellulose after chance is sour.It is hydrolyzed in hemicellulose Xylose out can be made into xylitol after processing, can do sweetener, plasticizer, surfactant etc..
Production process of viscose fiber is raw material, raw material main component alpha cellulose, content's index using chemical fiber pulp >=92%, remaining ingredient mainly has ash content, hemicellulose, pentosan etc..In recent years, pass through corncob, bagasse mostly both at home and abroad It is used Deng its hemicellulose is extracted, but extracts hemicellulose in viscose glue industry, production process of viscose fiber steeping liquor The technology industry of xylose waits to develop in plain powder.
Summary of the invention
The present invention provides a kind of extracting method of high yield pulp1 hemicellulose xylose, overcome the above-mentioned prior art no Foot, can provide in production process of viscose fiber, and high yield pulp1 extracts the side of the xylose in hemicellulose powder in sheet steeping lye Method.
The technical scheme is that realized by following measures: a kind of extraction side of high yield pulp1 hemicellulose xylose Method carries out as steps described below: pulp is mixed with dipping with lye and dissolves out impurity, obtains secondary lye, secondary alkali by the first step Liquid is separated by membrane technology, extracted, dried, and hemicellulose powder is obtained;Second step mixes the desired amount of sulfuric acid and hemicellulose powder It closes uniformly, obtains mixed liquor, wherein 1g hemicellulose powder is added in every 4ml sulfuric acid;Third step, by mixed liquor at 30 DEG C to 40 DEG C water bath condition under be acidified 2.0h to 2.5h, obtain acidulants;4th step the desired amount of water is added into acidulants, 120 DEG C to it is cooling after acidulants hydrolysis 60min to 90min under the conditions of 125 DEG C, filter, obtain high yield pulp1 hemicellulose xylose.
Here is the further optimization and/or improvements to invention technology described above scheme:
Above-mentioned sulfuric acid mass percent concentration is 40% to 50%.
Above-mentioned pulp is one of wood pulps, Cotton Pulp, bamboo pulp.
In above-mentioned 4th step, by the water that 80mL to 100mL is added in every 3 grams of acidulants.
The present invention for the first time in viscose rayon production, by pulp and lye be mixed with dipping the hemicellulose powder extracted into The processing of row technology, extracts wherein high-quality resource hemicellulose xylose, wherein hemicellulose xylose yield can reach 84%.This Invention reduces the waste of extra by-product hemicellulose in production process of viscose fiber, improves by-product in viscose rayon production The value of object hemicellulose.
Specific embodiment
The present invention is not limited by the following examples, can determine according to the technique and scheme of the present invention with actual conditions specific Embodiment.It is previously mentioned various chemical reagent and chemical article in the present invention unless otherwise specified, is public in the prior art Know common chemical reagent and chemical article;Percentage in the present invention does not have specified otherwise such as, is mass percent;This hair It is the aqueous solution that solvent is water, for example, hydrochloric acid solution is aqueous hydrochloric acid solution if the solution in bright is without specified otherwise;This Room temperature, room temperature in invention refer generally to 15 DEG C to 25 DEG C of temperature, are commonly defined as 25 DEG C.
The present invention will be further described below with reference to examples:
Embodiment 1: the extracting method of the high yield pulp1 hemicellulose xylose carries out as steps described below: the first step, by pulp and alkali Liquid hybrid infusion dissolves out impurity, obtains secondary lye, and secondary lye is separated by membrane technology, extracted, dried, and obtains hemicellulose Plain powder;The desired amount of sulfuric acid is uniformly mixed with hemicellulose powder, obtains mixed liquor by second step, wherein adds in every 4ml sulfuric acid Enter 1g hemicellulose powder;Mixed liquor is acidified under 30 DEG C to 40 DEG C of water bath condition 2.0h to 2.5h, is acidified by third step Object;The desired amount of water is added into acidulants for 4th step, and acidulants hydrolyze 60min to 90min under the conditions of 120 DEG C to 125 DEG C Cooling afterwards, suction filtration, obtains high yield pulp1 hemicellulose xylose.
The present invention with purified pulp (wood pulps, Cotton Pulp, bamboo pulp) be raw material, during producing viscose rayon, It usually requires to remove the impurity in raw material.Due to purified pulp main component be alpha cellulose, content's index >=92%, Remaining ingredient mainly has ash content, hemicellulose, pentosan etc., is generally dissolved out its impurity using soda-dip pulp, dissolution Impurity is the mixed alkali liquor of hemicellulose and other impurities, and be otherwise known as secondary lye, secondary lye by membrane technology separate, It extracts, drying, obtains hemicellulose powder;Hemicellulose powder is by converting half fiber with the sour process for being further acidified, hydrolyzing Tie up plain xylose.
Embodiment 2: the extracting method of the high yield pulp1 hemicellulose xylose carries out as steps described below: the first step, by pulp It is mixed with dipping with lye and dissolves out impurity, obtain secondary lye, secondary lye is separated by membrane technology, extracted, dried, and obtains half Cellulose powder;The desired amount of sulfuric acid is uniformly mixed with hemicellulose powder, obtains mixed liquor, wherein every 4ml sulfuric acid by second step Middle addition 1g hemicellulose powder;Mixed liquor is acidified under 30 DEG C or 40 DEG C of water bath condition 2.0h or 2.5h, obtained by third step Acidulants;The desired amount of water is added into acidulants for 4th step, under the conditions of 120 DEG C or 125 DEG C acidulants hydrolysis 60min or Cooling after 90min, suction filtration, obtains high yield pulp1 hemicellulose xylose.
Embodiment 3: as the optimization of above-described embodiment, sulfuric acid mass percent concentration is 40% to 50%.
In the present invention, hemicellulose powder hydrolysis xylose efficiency is significant, and the excessively high monosaccharide degradation of sulfuric acid concentration eventually leads to xylose Yield decline.
Embodiment 4: as the optimization of above-described embodiment, pulp is one of wood pulps, Cotton Pulp, bamboo pulp.
Embodiment 5: as the optimization of above-described embodiment, in the 4th step, by 80mL to 100mL is added in every 3 grams of acidulants Water.
Embodiment 6: the extracting method of the high yield pulp1 hemicellulose xylose carries out as steps described below: the first step, by cotton pulp The dregs of rice are mixed with dipping with lye and dissolve out impurity, obtain secondary lye, and secondary lye is separated by membrane technology, extracted, dried, obtained Hemicellulose powder;1.2ml sulfuric acid is uniformly mixed with 0.3g hemicellulose powder, obtains mixed liquor, wherein sulfuric acid matter by second step Measuring percent concentration is 45%;Mixed liquor is acidified 2.5h under 35 DEG C of water bath condition, obtains acidulants by third step;4th 87mL water is added into 3g acidulants for step, and cooling, suction filtration after acidulants hydrolysis 60min, obtains high yield pulp1 under the conditions of 121 DEG C Hemicellulose xylose, high yield pulp1 hemicellulose xylose recovery rate is 84.2% in the present embodiment.
Embodiment 7: the extracting method of the high yield pulp1 hemicellulose xylose carries out as steps described below: the first step, by cotton pulp The dregs of rice are mixed with dipping with lye and dissolve out impurity, obtain secondary lye, and secondary lye is separated by membrane technology, extracted, dried, obtained Hemicellulose powder;1.2ml sulfuric acid is uniformly mixed with 0.3g hemicellulose powder, obtains mixed liquor, wherein sulfuric acid matter by second step Measuring percent concentration is 45%;Mixed liquor is acidified 2h under 35 DEG C of water bath condition, obtains acidulants by third step;4th step, 80mL water is added into 3g acidulants, cooling, suction filtration after acidulants hydrolysis 60min, obtains high yield pulp1 half fiber under the conditions of 121 DEG C Plain xylose is tieed up, high yield pulp1 hemicellulose xylose recovery rate is 84.3% in the present embodiment.
Embodiment 8: the extracting method of the high yield pulp1 hemicellulose xylose carries out as steps described below: the first step, by cotton pulp The dregs of rice are mixed with dipping with lye and dissolve out impurity, obtain secondary lye, and secondary lye is separated by membrane technology, extracted, dried, obtained Hemicellulose powder;1.2ml sulfuric acid is uniformly mixed with 0.3g hemicellulose powder, obtains mixed liquor, wherein sulfuric acid matter by second step Measuring percent concentration is 45%;Mixed liquor is acidified 2.5h under 35 DEG C of water bath condition, obtains acidulants by third step;4th 100mL water is added into 3g acidulants for step, and cooling, suction filtration after acidulants hydrolysis 60min, obtains high yield pulp1 under the conditions of 121 DEG C Hemicellulose xylose, high yield pulp1 hemicellulose xylose recovery rate is 84.1% in the present embodiment.
According to the hemicellulose xylose that embodiment 6,7 and 8 obtains, in high performance liquid chromatograph measurement, available hair Bright hemicellulose xylose recovery rate can reach 84% or more.
In conclusion the present invention for the first time in viscose rayon production, passes through half for being mixed with dipping and extracting to pulp and lye Cellulose powder carries out technology processing, extracts wherein high-quality resource hemicellulose xylose, wherein hemicellulose xylose yield can Reach 84%.Present invention reduces the wastes of by-product hemicellulose extra in production process of viscose fiber, improve viscose rayon The value of by-product hemicellulose in production.
The above technical features constitute embodiments of the present invention, can basis with stronger adaptability and implementation result Actual needs increases and decreases non-essential technical characteristic, to meet the needs of different situations.

Claims (4)

1. a kind of extracting method of high yield pulp1 hemicellulose xylose, it is characterised in that carry out as steps described below: the first step will starch The dregs of rice are mixed with dipping with lye and dissolve out impurity, obtain secondary lye, and secondary lye is separated by membrane technology, extracted, dried, obtained Hemicellulose powder;The desired amount of sulfuric acid is uniformly mixed with hemicellulose powder, obtains mixed liquor, wherein every 4ml sulphur by second step 1g hemicellulose powder is added in acid;Mixed liquor is acidified under 30 DEG C to 40 DEG C of water bath condition 2.0h to 2.5h, obtained by third step To acidulants;The desired amount of water is added into acidulants for 4th step, and acidulants hydrolyze 60min under the conditions of 120 DEG C to 125 DEG C Cooling after to 90min, suction filtration, obtains high yield pulp1 hemicellulose xylose.
2. the extracting method of high yield pulp1 hemicellulose xylose according to claim 1, it is characterised in that sulfuric acid quality percentage Specific concentration is 40% to 50%.
3. the extracting method of high yield pulp1 hemicellulose xylose according to claim 1 or 2, it is characterised in that pulp is wood pulp One of the dregs of rice, Cotton Pulp, bamboo pulp.
4. the extracting method of high yield pulp1 hemicellulose xylose according to claim 1 or 2 or 3, it is characterised in that the 4th step In, by the water that 80mL to 100mL is added in every 3 grams of acidulants.
CN201910809161.8A 2019-08-29 2019-08-29 The extracting method of high yield pulp1 hemicellulose xylose Pending CN110499395A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111996296A (en) * 2020-09-15 2020-11-27 无锡绿色分离应用技术研究所有限公司 Environment-friendly method for extracting xylose from hemicellulose

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US4681935A (en) * 1984-04-02 1987-07-21 Enso-Gutzeit Oy Procedure for recovering soluble carbohydrates contained in wood
US20050203291A1 (en) * 2004-03-11 2005-09-15 Rayonier Products And Financial Services Company Process for manufacturing high purity xylose
CN102643935A (en) * 2012-04-11 2012-08-22 宜宾丝丽雅股份有限公司 Method for preparing xylose by using squeezed waste alkali liquor in viscose fiber production process
CN104017917A (en) * 2014-06-19 2014-09-03 山东福田药业有限公司 Xylose production process
CN104099431A (en) * 2014-08-01 2014-10-15 沈阳新华环境工程有限公司 Method for extracting xylose from viscoce chemical fiber squeezed alkali liquor
CN105969916A (en) * 2016-07-20 2016-09-28 宜宾雅泰生物科技有限公司 Method for preparing xylose by taking squeezed alkali liquid obtained in production of viscose as raw material
CN106191325A (en) * 2016-07-06 2016-12-07 宜宾雅泰生物科技有限公司 The technique that a kind of press lye produced with viscose rayon prepares xylose for raw material
CN106555014A (en) * 2016-12-02 2017-04-05 浙江华康药业股份有限公司 A kind of technique that xylose is prepared as raw material with viscose rayon press lye

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* Cited by examiner, † Cited by third party
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US4681935A (en) * 1984-04-02 1987-07-21 Enso-Gutzeit Oy Procedure for recovering soluble carbohydrates contained in wood
US20050203291A1 (en) * 2004-03-11 2005-09-15 Rayonier Products And Financial Services Company Process for manufacturing high purity xylose
CN102643935A (en) * 2012-04-11 2012-08-22 宜宾丝丽雅股份有限公司 Method for preparing xylose by using squeezed waste alkali liquor in viscose fiber production process
CN104017917A (en) * 2014-06-19 2014-09-03 山东福田药业有限公司 Xylose production process
CN104099431A (en) * 2014-08-01 2014-10-15 沈阳新华环境工程有限公司 Method for extracting xylose from viscoce chemical fiber squeezed alkali liquor
CN106191325A (en) * 2016-07-06 2016-12-07 宜宾雅泰生物科技有限公司 The technique that a kind of press lye produced with viscose rayon prepares xylose for raw material
CN105969916A (en) * 2016-07-20 2016-09-28 宜宾雅泰生物科技有限公司 Method for preparing xylose by taking squeezed alkali liquid obtained in production of viscose as raw material
CN106555014A (en) * 2016-12-02 2017-04-05 浙江华康药业股份有限公司 A kind of technique that xylose is prepared as raw material with viscose rayon press lye

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111996296A (en) * 2020-09-15 2020-11-27 无锡绿色分离应用技术研究所有限公司 Environment-friendly method for extracting xylose from hemicellulose

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Application publication date: 20191126