CN103014914A - Method for preparing medical high-efficiency disinfected chitosan fibers by using disinfectant - Google Patents

Method for preparing medical high-efficiency disinfected chitosan fibers by using disinfectant Download PDF

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Publication number
CN103014914A
CN103014914A CN2011102865695A CN201110286569A CN103014914A CN 103014914 A CN103014914 A CN 103014914A CN 2011102865695 A CN2011102865695 A CN 2011102865695A CN 201110286569 A CN201110286569 A CN 201110286569A CN 103014914 A CN103014914 A CN 103014914A
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chitin fiber
preparation
solution
spinning
chitosan
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李永兴
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Abstract

The invention relates to a preparation method of chitosan fibers. The method prepares medical high-efficiency disinfected chitosan fibers by adding a disinfectant during the preparation of a chitosan solution. The method comprises using high-purity chitosan powder, using a 2-4 % acetic acid solution as a solvent, and adding the 0.01-1 % water-soluble disinfectant to prepare a homogeneous and transparent chitosan spinning solution with a concentration of 2 to 20 %; spinning with a spinning machine, extruding filament with a metering pump, sending the extruded filament into a solidification bath for solidifying, stretching, washing with water, washing with alcohol, and drying to obtain the high-temperature-resistance chitosan fibers.

Description

A kind of preparation method who produces Medical efficient sterilizing chitin fiber with disinfectant
Technical field
The invention belongs to biological fiber material preparation technical field, be specifically related to a kind of preparation method of chitin fiber, particularly a kind of about in chitosan solution, adding the preparation method that disinfectant is produced Medical efficient sterilizing chitin fiber
Background technology
Chitin fiber is take shitosan powder or cotton-shaped tablet as main raw material, adopts suitable solvent, prepares suitable spinning solution, through the spray silk, solidify, stretch, wash, the operation such as drying makes.Because fiber itself has good physiological hygiene and antibiotic and sterilizing function, begin in recent years to be applied in high-end functionality textiles development aspect, domestic some university, scientific research institutions and relevant enterprise have been done many research and development and pilot scale successively, obtained many achievements, its technology of preparing is study hotspot and the forward position of current new material technology field.Chinese patent CN94116666.X, CN95119358.9, CN96103888.8, CN01131634.9, CN200810015053.5 etc. are the patents about chitin fiber and preparation method thereof.These inventions all are the preparation methods of chitin fiber, do not relate to medical chitosan fibre.Patent CN101250759A is the preparation method of medical chitosan fibre, it be about need not any additive, the preparation method of production high-purity medical chitin fiber.Be different from foregoing invention, the present invention is a kind of preparation method that broad-spectrum biocide is produced Medical efficient sterilizing chitin fiber that adds.
The used spectrum bactericidal agent polyhexamethylene guanide of the present invention is a kind of environment-friendly type macromolecule polymer disinfection sanitizer of excellence.Has following premium properties: 1, soluble in water; 2, the aqueous solution is nontoxic, colourless, odorless; 3, do not fire, not quick-fried; The ability that 4, extremely strong kill bacteria is arranged, wide spectrum, efficient and have a long-term bacteriostasis; 5, to various materials without erosion; 6, non-corrosiveness; 7, do not contain the harmful substances such as iodine, chlorine, aldehyde; 8, speed of action is fast; 9, stable in properties; Can be described as best bactericide.This product can be evenly and chitin fiber be mixed with the uniform aqueous solution, intermolecular interlinking forms the chelate with coupling compatibilization.Extremely stable with this fiber sterilization ability of making, can make the product of producing keep permanent germ-free condition.
Shitosan is identical with the sterilized principle for germ of polyhexamethylene guanide: the two all is cationic polymer, be easy to absorption and usually be electronegative each bacterioid, virus, by dissolving its lipid, change the permeability of its body film, make the metabolism generation obstacle in its body, suppress its splitting function, make its forfeiture fecundity thereby sterilizing.
Chitin fiber has good hygroscopicity, the active material stripping that sufficient moisture can make polyhexamethylene guanide contain, and rapid kill bacteria reaches antibiotic, anti-insect, mildew-resistant, shrink-proof, the effect that do not harden.
Summary of the invention
For the objective demand of sterilization fibre, the present invention proposes a kind of preparation method of chitin fiber, use the method can produce Medical efficient sterilizing chitin fiber.Implementation step comprises: shitosan preparation of spinning solution, dissolving, filtration, deaeration, measuring pump metering, spray silk, be frozen into silk, stretching, washing, alcohol wash, oil, drying.Implementation is as follows:
The first step, the dissolving of chitosan solution, in the spinning material of chitin fiber, high-purity chitosan powder (or flocculus material) accounts for percentage by weight 2-20%, solvent glacial acetic acid aqueous solution weight is 1-4%, and polyhexamethylene guanide accounts for the 0.5-1% of shitosan, and solubilizer, thinner, defoamer are an amount of, raw material drops in the deionized water successively, start mixer, mixing speed 40-200 rev/min, stirred 1-8 hour.
Second step, middle press filtration, reactor pressure is controlled at below the 1MPa, double-filtration, filter stainless steel 400-800 order.
The 3rd step, the vacuum stirring deaeration, vacuum tank vacuum 95%, mixing speed 40-200 rev/min, a spinning solution high position enters tank, 2-8 hour deaeration time.
The 4th step, metering spray silk, with measuring pump control spray silk speed and initial titre, spray silk liquid immerses coagulating tank.
The 5th step, solidify, spinning solution is coagulating bath in-tank-solidification and preliminary the stretching.
Step after the 6th step reached, the treatment process such as the stretching of the wet spinning that employing is ripe, washing, drying can make Medical efficient sterilizing chitin fiber.
The present invention compared with prior art has the following advantages:
1, compares with common chitin fiber and have stronger sterilization effect.
2, compare with the cotton fiber of processing with polyhexamethylene guanide, the sterilization effect has higher stability, persistence, because the latter soaks and gets in last operation of fibre finish, only form the polymer foil of an antiseptic at fiber surface, wash easily for a long time and come off unsuitable long term storage.
3, compare with the cotton fiber of processing with polyhexamethylene guanide, have better skin compatibility, because chitin fiber has the excellent effect of Promote cell's growth, Cucumber Extract.
Embodiment
Embodiment 1
Get the 30KG deionized water and add reactor, start and stir, drop into 1KG shitosan powder, the 10g polyhexamethylene guanide drops into an amount of glacial acetic acid, urea, zinc acetate, silicone oil successively, stirs 4 hours at 20 ℃, namely gets the uniform shitosan spinning solution of dissolving; Utilize filter pressure filtration, pressure is controlled at below the 1MPa, filter stainless steel 600 orders.Filtrate enters the vacuum defoamation tank from tank deck, and vacuum tank vacuum 95% stirs 4 hours deaeration time; Slurries after the deaeration are pumped to spinning head with metering, spinning head 4000 holes, coagulating bath is the aqueous solution of NaOH, sodium sulphate and ethanol, and coagulation bath temperature is 20 ℃, the stretching ratio 1.5 of fiber, after the stretching, at normal temperatures, carry out successively deionization washing, alcohol wash, oil, drying, namely make chitin fiber, fibre number 1.8dtex can be used for spinning, nonwoven fabric etc.
Embodiment 2
Get the 300KG deionized water and add reactor, start and stir, drop into successively 30KG shitosan tablet, the 10g polyhexamethylene guanide drops into an amount of glacial acetic acid, urea, zinc acetate, silicone oil successively, stirs 4 hours at 20 ℃, namely gets the uniform shitosan spinning solution of dissolving; Utilize filter pressure filtration, pressure is controlled at below the 1MPa, filter stainless steel 800 orders.Filtrate enters the vacuum defoamation tank from tank deck, and vacuum tank vacuum 95% stirs 6 hours deaeration time; Slurries after the deaeration are pumped to spinning head with metering, spinning head 6000 holes, coagulating bath is the aqueous solution of NaOH and ethanol, and coagulation bath temperature is 20 ℃, the stretching ratio 1.4 of fiber, after the stretching, at normal temperatures, carry out successively deionization washing, alcohol wash, oil, drying, namely make chitin fiber, fibre number 2.2dtex can be used for spinning, nonwoven fabric etc.

Claims (7)

1. the preparation method of a chitin fiber, add high-purity chitosan powder (or flocculus material) under the normal temperature and account for percentage by weight 2-20%, solvent glacial acetic acid aqueous solution weight is 1-4%, antiseptic sterilization agent accounts for the 0.01-1% of shitosan, solubilizer, thinner, defoamer is an amount of, raw material drops in the deionized water successively, start mixer, mixing speed 40-200 rev/min, stirred 1-4 hour, with static pressure with twice of solution press filtration, send into vacuum tank and stir deaeration 2-4 hour, obtain the shitosan spinning solution that concentration is about the homogeneous phase transparent of 2-20%, adopt the spinning machine spinning, the silk that measuring pump is extruded enters coagulating tank, and coagulation bath is the aqueous solution of NaOH and ethanol, and the content of NaOH is 4-6%, the content of ethanol is 4-50%, by stretching, washing, alcohol wash, oil, drying obtains Medical efficient sterilizing chitin fiber.
2. the preparation method of chitin fiber according to claim 1 is characterized in that, the molecular weight of described chitosan powder (or flocculus material) is greater than 800,000, and viscosity is at 20 ℃ of time>500mpa.s of normal pressure, deacetylation>85%, and purity is greater than 99%.
3. the preparation method of chitin fiber according to claim 1, it is characterized in that, when dissolving chitosan powder (or flocculus material), add a certain proportion of antiseptic sterilization agent, antiseptic sterilization agent not only refers to be polyhexamethylene guanide, also comprise water-soluble, as to be insoluble to alkali, ethanol organic chemistry antiseptic sterilization agent, ratio is the 0.1-1% of shitosan.
4. the preparation method of chitin fiber according to claim 1 is characterized in that, when filtering chitosan solution, is pressurized to 0.3-0.5Mpa with air compressor machine, makes solution with pressure by filter, filter 400-800 order.
5. the preparation method of chitin fiber according to claim 1 is characterized in that, the chitosan solution after the filtration enters the vacuum defoamation of negative pressure storage tank, tank internal pressure<76mmHG.
6. the preparation method of chitin fiber according to claim 1, it is characterized in that, adopt the spinning machine spinning, the silk that measuring pump is extruded enters coagulating tank, coagulation bath is take NaOH as basic neutralizer, add a certain proportion of sodium sulphate, ethanol etc., course of reaction and the fibroblast molecularly oriented of the diffusion in coagulating tank of regulation and control spinning solution, neutralization, plasticising.
7. the preparation method of chitin fiber according to claim 1 is characterized in that, by stretching, washing, alcohol wash, oil, drying obtains Medical efficient sterilizing chitin fiber.
CN2011102865695A 2011-09-26 2011-09-26 Method for preparing medical high-efficiency disinfected chitosan fibers by using disinfectant Pending CN103014914A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103835025A (en) * 2014-03-07 2014-06-04 青岛大学 Preparation method of permanently-antibacterial poly guanidine alginate fibers
CN104368029A (en) * 2013-08-13 2015-02-25 河北佳民医药科技有限公司 Preparation method of membrane for promoting epidermal cell wet and scar-free growth
CN105770941A (en) * 2014-12-18 2016-07-20 浙江澳兴生物科技有限公司 Sterilization method of chitosan and chitosan derivatives

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JPH0892820A (en) * 1994-09-20 1996-04-09 Omikenshi Co Ltd Production of chitin fiber and chitin film
JPH09241928A (en) * 1996-03-01 1997-09-16 Omikenshi Co Ltd Production of chitin chitosan fiber and structure
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Publication number Priority date Publication date Assignee Title
JPH0892820A (en) * 1994-09-20 1996-04-09 Omikenshi Co Ltd Production of chitin fiber and chitin film
JPH09241928A (en) * 1996-03-01 1997-09-16 Omikenshi Co Ltd Production of chitin chitosan fiber and structure
CN1704510A (en) * 2004-06-02 2005-12-07 秦益民 A silver containing chitosan fiber having antimicrobial function and preparation method
CN102177016A (en) * 2008-08-28 2011-09-07 泰科保健集团有限合伙公司 Anti-microbial fibers and related articles and methods
CN101665985A (en) * 2009-09-07 2010-03-10 江南大学 Preparation method of tea polyphenols/chitosan nanofiber membrane
CN102031590A (en) * 2011-01-12 2011-04-27 武汉理工大学 Novel method for preparing sodium alginate/hydroxypropyl chitosan antibacterial blended fiber

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104368029A (en) * 2013-08-13 2015-02-25 河北佳民医药科技有限公司 Preparation method of membrane for promoting epidermal cell wet and scar-free growth
CN103835025A (en) * 2014-03-07 2014-06-04 青岛大学 Preparation method of permanently-antibacterial poly guanidine alginate fibers
CN103835025B (en) * 2014-03-07 2015-12-09 青岛大学 A kind of preparation method of permanent antibacterial poly-guanidine alginate fibre
CN105770941A (en) * 2014-12-18 2016-07-20 浙江澳兴生物科技有限公司 Sterilization method of chitosan and chitosan derivatives
CN105770941B (en) * 2014-12-18 2018-04-20 浙江澳兴生物科技有限公司 The sterilizing methods of chitosan and chitosan derivatives

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