CN113089137A - Preparation method of efficient extraction solvent for hemicellulose in squeezed waste alkali liquor generated in viscose fiber production - Google Patents

Preparation method of efficient extraction solvent for hemicellulose in squeezed waste alkali liquor generated in viscose fiber production Download PDF

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Publication number
CN113089137A
CN113089137A CN202110377411.2A CN202110377411A CN113089137A CN 113089137 A CN113089137 A CN 113089137A CN 202110377411 A CN202110377411 A CN 202110377411A CN 113089137 A CN113089137 A CN 113089137A
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China
Prior art keywords
solvent
alkali liquor
hemicellulose
waste alkali
viscose fiber
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Pending
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CN202110377411.2A
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Chinese (zh)
Inventor
胡元森
王天贵
卫冉
段定康
朱广有
卫红伟
潘茜
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Henan University of Technology
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Henan University of Technology
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Priority to CN202110377411.2A priority Critical patent/CN113089137A/en
Publication of CN113089137A publication Critical patent/CN113089137A/en
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    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F13/00Recovery of starting material, waste material or solvents during the manufacture of artificial filaments or the like
    • D01F13/02Recovery of starting material, waste material or solvents during the manufacture of artificial filaments or the like of cellulose, cellulose derivatives or proteins
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50Manufacturing or production processes characterised by the final manufactured product
    • Y02P70/62Manufacturing or production processes characterised by the final manufactured product related technologies for production or treatment of textile or flexible materials or products thereof, including footwear

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Polysaccharides And Polysaccharide Derivatives (AREA)

Abstract

The invention relates to a preparation method of a high-efficiency extraction solvent for hemicellulose in squeezed waste alkali liquor generated in viscose fiber production, belonging to the field of chemical engineering application. The waste alkali liquor produced in viscose fiber production has economic value, if separation can be realized, alkali can be recycled, hemicellulose can be used for producing high value-added products such as furfural and the like, and the market potential is huge. The main creators of the invention have invented a production method and a production process for realizing the full recycling of the waste alkali liquor and simultaneously realizing the separation and value-added utilization of hemicellulose, but an organic solvent is needed in the production process, ethanol is generally used in some basic researches, but the dosage is too large, and the solvent and the alkali liquor basically need 3-4: 1, directly affects the economic benefit. The invention is a high-efficiency solvent, and the solvent and alkali liquor basically need 1.5-2: 1, the solvent dosage is greatly reduced, and the economic benefit can be doubled.

Description

Preparation method of efficient extraction solvent for hemicellulose in squeezed waste alkali liquor generated in viscose fiber production
Technical Field
The invention relates to a preparation method of a high-efficiency extraction solvent for hemicellulose in squeezed waste alkali liquor generated in viscose fiber production, belonging to the field of chemical engineering application.
Background
Viscose fiber is an important variety in chemical fiber industry in China, the yield of the viscose fiber in China accounts for about 60% of the total world production, reaches about 400 million tons every year at present, and is continuously increased along with the increase of the demand. In the viscose preparation process, cotton pulp or wood pulp poise is generally soaked by using a sodium hydroxide aqueous solution, and then squeezing and separating are carried out to remove hemicellulose in the pulp poise, so that relatively pure cellulose easy to chemically process is obtained. When the concentration of hemicellulose and cellulose (degradation products) dissolved in the alkali liquor reaches a certain degree, the alkali liquor must be replaced, otherwise the product quality of the viscose fiber will be affected.
The waste alkali liquor generated in the viscose fiber production process has economic value, wherein the NaOH content can reach as high as 240 g/L, and the concentration of hemicellulose and cellulose degradation products (HCD) can reach as high as 35 g/L. If the separation can be realized, the alkali can be recycled, the HCD can be used for producing products with high added values, such as furfural, xylose, xylo-oligosaccharide, medical and expensive food intermediates and the like, and the market potential is huge. Because the hemicellulose is a compound polysaccharide consisting of different monosaccharide groups, the molecular weight is small, the structure is complex, and simultaneously, the NaOH content of the waste alkali liquor is high, and the waste alkali liquor is difficult to recover and treat by adopting a conventional process. At present, the dialysis process and the membrane separation process are mainly adopted in China to purify and recover the waste alkali liquor, but the dialysis process has low alkali liquor recovery efficiency, large water consumption and large floor area and is gradually eliminated. In contrast, the membrane separation method has low cost and good effect and is being popularized and applied. However, the membrane separation method is actually a concentration process of hemicellulose in an aqueous alkali solution, and cannot completely and completely recover and recycle waste alkali liquor, and at least 30-50% of the waste alkali liquor needs to be treated by a traditional method.
The main creators of the invention have invented the production method and the production process for realizing the full recycling of the waste alkali liquor and simultaneously realizing the HCD separation and value-added utilization, and have applied for related patents (the invention patent of 'a waste alkali liquor recycling method' with the application number of 2011510451500.1, and the patent ZL 201520554929.9 'a waste alkali liquor recycling system device'). In the production process, an organic solvent is needed for separating hemicellulose, ethanol is generally used in some basic researches, but the dosage is too large, and the solvent and alkali liquor basically need to be 3-4: 1, directly affects the economic benefit. The invention is a high-efficiency solvent, and the solvent and alkali liquor basically need 1.5-2: 1, the solvent dosage is greatly reduced, and the economic benefit is multiplied.
Disclosure of Invention
The invention relates to a preparation method of a high-efficiency extraction solvent for hemicellulose in squeezed waste alkali liquor generated in viscose fiber production, which is mainly used for preparing the mixing proportion of a plurality of solvents, achieving the production purpose of efficiently extracting the hemicellulose from the waste alkali liquor, greatly reducing the dosage of the solvent and improving the economic benefit by times.
The invention provides a preparation method of a high-efficiency extraction solvent for hemicellulose in squeezed waste alkali liquor generated in viscose fiber production, which comprises the following steps:
1. diluting with 500ml of constant volume in a beaker, adding 300-400 ml of ethanol, adding 30-60 ml of methanol, uniformly mixing, and standing for 20 minutes;
2. adding 20-40 ml of isopropanol into the solvent in the step 1, uniformly mixing, and standing for 20 minutes;
3. adding 20-40 ml of acetone into the solvent in the step 2, uniformly mixing, and standing for 20 minutes;
4. adding 10-20 ml of triethanolamine into the solvent obtained in the step 3, uniformly mixing, and standing for 20 minutes;
5. and (3) adding 20-40 ml of chloroform into the solvent in the step (3), uniformly mixing, and standing for 20 minutes.
The solvent prepared according to the steps is a high-efficiency solvent obtained through a large number of experiments, is specially used for extracting hemicellulose in squeezed waste alkali liquor generated in viscose fiber production, and can be adjusted in a proper proportion in practical application according to specific components of the waste alkali liquor.
Detailed Description
Example 1
Firstly, fixing the volume by a beaker with 500ml, adding 400ml of ethanol, adding 30ml of methanol, uniformly mixing, and standing for 20 minutes; then, adding 20ml of isopropanol, uniformly mixing, and standing for 20 minutes; then adding 20ml of acetone, uniformly mixing, and standing for 20 minutes; then adding 10ml of triethanolamine, mixing uniformly, and standing for 20 minutes; finally, 20ml of chloroform was added, mixed well and allowed to stand for 20 minutes. The obtained high-efficiency solvent and alkali liquor can reach 2: 1, can be used for waste alkali liquor with higher hemicellulose content and higher cellulose decomposition products.
Example 2
Firstly, diluting the mixture to a constant volume of 500ml by using a beaker, adding 350ml of ethanol, adding 50ml of methanol, uniformly mixing, and standing for 20 minutes; then, adding 30ml of isopropanol, uniformly mixing, and standing for 20 minutes; then adding 30ml of acetone, uniformly mixing, and standing for 20 minutes; adding 15ml of triethanolamine, uniformly mixing, and standing for 20 minutes; finally, 25ml of chloroform was added, mixed well and allowed to stand for 20 minutes. The obtained high-efficiency solvent and alkali liquor can reach 1.7: 1, can be used for waste lye with higher hemicellulose content and lower cellulose decomposition products.
Example 3
Firstly, fixing the volume by a beaker with 500ml, adding 300ml of ethanol, adding 60ml of methanol, uniformly mixing, and standing for 20 minutes; then, adding 40ml of isopropanol, uniformly mixing, and standing for 20 minutes; then adding 40ml of acetone, uniformly mixing, and standing for 20 minutes; then adding 20ml of triethanolamine, mixing uniformly, and standing for 20 minutes; finally, 40ml of chloroform was added, mixed well and allowed to stand for 20 minutes. The obtained high-efficiency solvent and alkali liquor can reach 1.5: 1, can be used for waste lye with lower hemicellulose content and lower cellulose decomposition products.

Claims (3)

1. A preparation method of a high-efficiency extraction solvent for hemicellulose in squeezed waste alkali liquor generated in viscose fiber production mainly comprises the following steps:
(1) diluting with 500ml of constant volume in a beaker, adding ethanol and then adding methanol;
(2) adding isopropanol into the solvent in the step (1);
(3) adding acetone into the solvent in the step (2);
(4) adding triethanolamine into the solvent in the step (3);
(5) and (4) adding chloroform into the solvent in the step (4).
2. The mixture of claim 1, wherein the mixture is mixed uniformly in each step and left to stand for 20 minutes.
3. The mixture as described in claim 1, wherein the amount of ethanol added is 300-400 ml, the amount of methanol added is 30-60 ml, the amount of isopropanol added is 20-40 ml, the amount of acetone added is 20-40 ml, the amount of triethanolamine added is 10-20 ml, and the amount of chloroform added is 20-40 ml.
CN202110377411.2A 2021-04-08 2021-04-08 Preparation method of efficient extraction solvent for hemicellulose in squeezed waste alkali liquor generated in viscose fiber production Pending CN113089137A (en)

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CN202110377411.2A CN113089137A (en) 2021-04-08 2021-04-08 Preparation method of efficient extraction solvent for hemicellulose in squeezed waste alkali liquor generated in viscose fiber production

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102585039A (en) * 2012-02-28 2012-07-18 昆明理工大学 Extraction separation method of hemicellulose
CN103333274A (en) * 2013-07-11 2013-10-02 宜宾丝丽雅集团有限公司 Method for extracting and recovering hemicellulose from squeezed waste alkali
CN105297511A (en) * 2015-11-26 2016-02-03 山东福田药业有限公司 Separation method of organic constituent in agricultural waste
CN106283795A (en) * 2016-11-08 2017-01-04 福建农林大学 A kind of method separating hemicellulose and cellulose
CN109320631A (en) * 2018-08-31 2019-02-12 昆明理工大学 A method of extracting hemicellulose
CN109735968A (en) * 2018-12-18 2019-05-10 郑州家善环保科技有限公司 A kind of spent lye recoverying and utilizing method

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102585039A (en) * 2012-02-28 2012-07-18 昆明理工大学 Extraction separation method of hemicellulose
CN103333274A (en) * 2013-07-11 2013-10-02 宜宾丝丽雅集团有限公司 Method for extracting and recovering hemicellulose from squeezed waste alkali
CN105297511A (en) * 2015-11-26 2016-02-03 山东福田药业有限公司 Separation method of organic constituent in agricultural waste
CN106283795A (en) * 2016-11-08 2017-01-04 福建农林大学 A kind of method separating hemicellulose and cellulose
CN109320631A (en) * 2018-08-31 2019-02-12 昆明理工大学 A method of extracting hemicellulose
CN109735968A (en) * 2018-12-18 2019-05-10 郑州家善环保科技有限公司 A kind of spent lye recoverying and utilizing method

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