CN107724074A - A kind of preparation method of water soluble chitosan fiber - Google Patents

A kind of preparation method of water soluble chitosan fiber Download PDF

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Publication number
CN107724074A
CN107724074A CN201710658163.2A CN201710658163A CN107724074A CN 107724074 A CN107724074 A CN 107724074A CN 201710658163 A CN201710658163 A CN 201710658163A CN 107724074 A CN107724074 A CN 107724074A
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CN
China
Prior art keywords
preparation
fiber
chitin fiber
water soluble
concentration
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201710658163.2A
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Chinese (zh)
Inventor
张荷新
蔺洪耀
李叶
陆阳
潘学理
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Qingdao Tong Doctor Marine Biotechnology Co ltd
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Shandong Humanities Co Ltd
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Publication date
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Priority to CN201710658163.2A priority Critical patent/CN107724074A/en
Publication of CN107724074A publication Critical patent/CN107724074A/en
Pending legal-status Critical Current

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    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
    • D06M13/184—Carboxylic acids; Anhydrides, halides or salts thereof
    • D06M13/207—Substituted carboxylic acids, e.g. by hydroxy or keto groups; Anhydrides, halides or salts thereof
    • D06M13/21—Halogenated carboxylic acids; Anhydrides, halides or salts thereof
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/73—Polysaccharides
    • A61K8/736—Chitin; Chitosan; Derivatives thereof
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
    • A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
    • A61L15/22—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing macromolecular materials
    • A61L15/28—Polysaccharides or their derivatives
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L26/00—Chemical aspects of, or use of materials for, wound dressings or bandages in liquid, gel or powder form
    • A61L26/0009—Chemical aspects of, or use of materials for, wound dressings or bandages in liquid, gel or powder form containing macromolecular materials
    • A61L26/0023—Polysaccharides
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
    • C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
    • C08B37/0024—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid beta-D-Glucans; (beta-1,3)-D-Glucans, e.g. paramylon, coriolan, sclerotan, pachyman, callose, scleroglucan, schizophyllan, laminaran, lentinan or curdlan; (beta-1,6)-D-Glucans, e.g. pustulan; (beta-1,4)-D-Glucans; (beta-1,3)(beta-1,4)-D-Glucans, e.g. lichenan; Derivatives thereof
    • C08B37/0027—2-Acetamido-2-deoxy-beta-glucans; Derivatives thereof
    • C08B37/003—Chitin, i.e. 2-acetamido-2-deoxy-(beta-1,4)-D-glucan or N-acetyl-beta-1,4-D-glucosamine; Chitosan, i.e. deacetylated product of chitin or (beta-1,4)-D-glucosamine; Derivatives thereof
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/38—Oxides or hydroxides of elements of Groups 1 or 11 of the Periodic System
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
    • D06M13/144—Alcohols; Metal alcoholates

Abstract

The present invention relates to a kind of using chitin fiber not soluble in water as raw material, sodium chloroacetate is used to prepare the production technology new method of water soluble chitosan fiber for reactant, it is characterised in that：Sodium chloroacetate is used as reaction reagent, reaction system is certain density alkali alcoholic solution.Prepared chitin fiber dissolve in the range of being 6.0 8.0 in pH, and ensure dry fracture strength >=1.15cN/dtex, and substitution value is ＞ 70%, purity >=80%.High biocidal property, flexibility, gas permeability and hygroscopicity can be kept by reaching the chitin fiber of technique requirement, available for the manufacture of fabric and non-woven cloth products, be widely used in medical dressing and cosmetic material technical field.

Description

A kind of preparation method of water soluble chitosan fiber
Technical field
The invention belongs to medical dressing and cosmetic material technical field, discloses a kind of system of water soluble chitosan fiber Preparation Method.
Background technology：
Chitosan be it is a kind of there is excellent biocompatibility, antibacterial ability, hemostatic capability and biodegradable natural High polymer material, there is good fibre forming property.Chitin fiber is using chitosan as primary raw material, is incited somebody to action in appropriate solvent It dissolves, and is configured to certain density colloid spinning solution, then through techniques such as spinneret, solidification forming, stretchings, be prepared into one Determine the high molecular functional material of mechanical strength.
But due to chitosan is dissolved only in acid solution and characteristic not soluble in water, chitin fiber, which is mostly used in, at present knits The manufacture of the product of thing and non-woven fabrics, limit its application in the field such as soluble medical material and cosmetics.Due to High biocidal property, flexibility, gas permeability and the hygroscopicity of pure chitosan fiber are very good, therefore how to prepare low cost, high-performance Water soluble chitosan fiber turn into medicine and cosmetic field technical staff problem urgently to be resolved hurrily.
Chitin fiber is carried out graft reaction by the present invention, can keep the form of fiber after carboxylation processing, and can be Dissolved in the range of wide pH, there is excellent moisture absorbability and moisture retentivity, biocompatibility, broad spectrum antibacterial and biodegradability Etc. specific function, have wide practical use in fields such as medicine, cosmetics and biological health-care products, there is huge economic benefit And social benefit.
The content of the invention
It is an object of the invention to：
The defects of existing for the market demand and prior art, the technical problem to be solved by the invention is to provide one kind Cost is cheap, easy to operate, energy-saving, is widely used, and has the water soluble chitosan fiber of fibre morphology, and the present invention is adopted The technical scheme taken is：A kind of preparation method of water soluble chitosan fiber, including following preparation process：
A certain amount of chitin fiber is weighed to put into reactor, add 10~20 times of chitin fiber weight 5~ The Na0H ethanol solutions of 15% concentration, ethanol solution concentration are 60%~80%, then by 2.0~3.0 times of chitin fiber weight Sodium chloroacetate be added in system, under 50~70 DEG C of heat-retaining conditions react 3.0~6.0h.Reaction terminates rear separation of solid and liquid, Material pH is adjusted to be washed twice to neutrality, then with the ethanol solution of 70~80% concentration in ethanol solution with diluted acid, 90~99% Concentration ethanol is dehydrated once, dries to obtain product.Product does fracture strength >=1.15cN/dtex, pH 6.0-8.0, substitution value ＞ 70%, purity >=80%.
It is excellent that the present invention compared to existing chitosan carboxylation reaction technology has that preparation process is simple, easily controllable, cost is low etc. Point, it is specific as follows：
1st, this invention replaces conventional monoxone to be reacted using sodium chloroacetate, is readily transported, stores, it is nonirritant and Corrosivity, easy to operate, the requirement to consersion unit material is extremely low, significantly improves production environment.
2nd, this invention reaction time is shorter, and the dosage of alkali is less, and the cost of raw material is relatively low, and process is simple, simplifies production Flow corollary equipment, significantly reduce the manufacturing cost of product.
3rd, the product that prepared by this invention is water-soluble preferably, can be completely dissolved in the range of extensive pH, product has Fiber softening form, do fracture strength >=1.15cN/dtex, pH 6.0-8.0, substitution value ＞ 70%, purity >=80%.
In a word, the chitin fiber that prepared by the present invention is a kind of new type water-solubility biomaterial, and its preparation process is simple, work It is non-stimulated to make environment, requirement of the production procedure compared with traditional handicraft simplification, production cost and to equipment is extremely low, has fibre morphology Water soluble chitosan will bring huge potentiality for the development of medical dressing and cosmetic industry.
Brief description of the drawings
Accompanying drawing is water soluble chitosan fiber manufacturing process schematic diagram, refers to Figure of description.
Embodiment
Further illustrated below by specific embodiment to embodiment of the present invention.
Embodiment 1：
200ml 65% ethanol solution is added into the beaker for be provided with electric mixer, 20gNaOH inputs is weighed and burns In cup, opening stirring is uniformly dissolved it, adds 20g chitin fibers, then weighs 50g sodium chloroacetates and add in reaction system, React 4.0h under 60 DEG C of heat-retaining conditions, reaction drains reaction solution after terminating, and material pH is adjusted in ethanol solution with diluted acid to neutrality, Washed twice again with the ethanol solution of 75% concentration, 95% concentration ethanol is dehydrated once, dries to obtain product, detects dry fracture strength 1.15cN/dtex, pH 7.4, substitution value 96.9%, purity 87.0%.
Embodiment 2：
200ml 70% ethanol solution is added into the beaker for be provided with electric mixer, 25gNaOH inputs is weighed and burns In cup, opening stirring is uniformly dissolved it, adds 20g chitin fibers, then weighs 60g sodium chloroacetates and add in reaction system, React 4.5h under 65 DEG C of heat-retaining conditions, reaction drains reaction solution after terminating, and material pH is adjusted in ethanol solution with diluted acid to neutrality, Washed twice again with the ethanol solution of 75% concentration, 95% concentration ethanol is dehydrated once, dries to obtain product, detects dry fracture strength 1.18cN/dtex, pH 7.5, substitution value 85.5%, purity 97.4%.

Claims (3)

  1. A kind of 1. preparation method of water soluble chitosan fiber, it is characterised in that：Preparation method
    Weigh a certain amount of chitin fiber to put into reactor, add the 10~20% of 10~20 times of chitin fiber weight The NaOH ethanol solutions of concentration, ethanol solution concentration is 60%~80%, then the chlorine by 2.0~3.0 times of chitin fiber weight Sodium acetate is added in system, and 3.0~6.0h is reacted under 50~70 DEG C of heat-retaining conditions.Reaction terminates rear separation of solid and liquid, and use is dilute Acid adjusts material pH to be washed twice to neutrality, then with the ethanol solution of 70~80% concentration in ethanol solution, 90~99% concentration Ethanol dehydration once, dries to obtain product.
  2. 2. the preparation method of water soluble chitosan fiber as claimed in claim 1, it is characterised in that：It is anti-to use sodium chloroacetate Reagent is answered, uses certain density alkali alcoholic solution as reaction system.
  3. 3. the preparation method of water soluble chitosan fiber as claimed in claim 1, it is characterised in that：The water-soluble carboxymethyl Dry fracture strength >=1.15cN/dtex of chitin fiber, pH6.0-8.0, substitution value are ＞ 70%, purity >=80%.
CN201710658163.2A 2017-07-31 2017-07-31 A kind of preparation method of water soluble chitosan fiber Pending CN107724074A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201710658163.2A CN107724074A (en) 2017-07-31 2017-07-31 A kind of preparation method of water soluble chitosan fiber

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201710658163.2A CN107724074A (en) 2017-07-31 2017-07-31 A kind of preparation method of water soluble chitosan fiber

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101049513A (en) * 2007-05-13 2007-10-10 刘万顺 Anti hemorrhagic healing traumatic material of chitosan based fiber in water-solubility, preparation method and application
CN101368328A (en) * 2008-08-04 2009-02-18 东华大学 Preparation method for hydroxyethyl group chitosan fiber
CN103120802A (en) * 2012-07-26 2013-05-29 佛山市优特医疗科技有限公司 Soluble hemostatic gauze and preparation methods thereof
US20140316361A1 (en) * 2011-01-11 2014-10-23 Medtrade Products Ltd. Process for the manufacture of a dressing and dressing obtained
CN105153325A (en) * 2015-09-16 2015-12-16 中华全国供销合作总社南京野生植物综合利用研究所 Improved production process of carboxymethyl chitosan

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101049513A (en) * 2007-05-13 2007-10-10 刘万顺 Anti hemorrhagic healing traumatic material of chitosan based fiber in water-solubility, preparation method and application
CN101368328A (en) * 2008-08-04 2009-02-18 东华大学 Preparation method for hydroxyethyl group chitosan fiber
US20140316361A1 (en) * 2011-01-11 2014-10-23 Medtrade Products Ltd. Process for the manufacture of a dressing and dressing obtained
CN103120802A (en) * 2012-07-26 2013-05-29 佛山市优特医疗科技有限公司 Soluble hemostatic gauze and preparation methods thereof
CN105153325A (en) * 2015-09-16 2015-12-16 中华全国供销合作总社南京野生植物综合利用研究所 Improved production process of carboxymethyl chitosan

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
于兹东等: "羧甲基壳聚糖的制备研究", 《广西轻工业》 *

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Effective date of registration: 20190731

Address after: 266000 Qianjiashan Road 359, Huangdao District, Qingdao City, Shandong Province

Applicant after: Qingdao Tong Doctor Marine Biotechnology Co.,Ltd.

Address before: 272100 Guhuai Road West, Mechatronics Road North, Jining City, Shandong Province (Humanities Jiayuan Street Commerce)

Applicant before: SHANDONG RENWEN PROPERTY CO.,LTD.

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Application publication date: 20180223

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