CN1266922A - Antibacterial viscose fibre and its making method - Google Patents
Antibacterial viscose fibre and its making method Download PDFInfo
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- CN1266922A CN1266922A CN 00100636 CN00100636A CN1266922A CN 1266922 A CN1266922 A CN 1266922A CN 00100636 CN00100636 CN 00100636 CN 00100636 A CN00100636 A CN 00100636A CN 1266922 A CN1266922 A CN 1266922A
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- shitosan
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Abstract
An antibacterial viscose fibre is prepared through preparing low-molecular chitosan by radiation degradation, synthesizing N-formyl chitosan, carboxymethyl chitosan, o-hydroxy ethyl chitosan, N-alkylated chitosan and its quaternary ammonium compound, ultrasonic pulverizing to obtain aqueous dispersed chitosan with granularity less than 5 microns, adding the mixture of said aqueous dispersed chitosan and chitosan derivative to spinning liquid of viscose fibre and preparing fibres. Its advantages are high suppression action on bacteria, durable antibacterial power, and better water absorption and humidity preservation.
Description
The invention belongs to antibacterial viscose fiber and manufacture method thereof
The antibacterial deodourizing of textiles is processed with back arrangement and two kinds of methods of spinning modification.Kind according to antiseptic is different with processing method, can make dissolution type and non-dissolution type antibiotic fabric with finishing method.Industrialized main antibacterial finishing agent has inorganic system and organic system two classes.Inorganic antiseptic mainly contains the porous material of inorganic ion exchangers such as antibacterial zeolite, apatite, calcium phosphate and so on, and metalloid and the ionic compound and the complex compound of mercury, silver, copper, lead.Organic antibacterial agent is mainly quaternary ammonium salts, antibiotic sulfa drugs, fatty acid, phenols, guanidine class, silicone based and halogenated aryl hydrocarbon class.Carry out chemical treatment with above antiseptic at fabric or fiber surface and can obtain the anti-bacterial anti-foul function fiber.But the antibacterial range of this class anti-bacterial fibre is limited, antibiotic rate low (only having 70～80%), and washability poor (Cao Huichun, " development of anti-bacterial fibre ", synthetic fiber, 1999, NO.3, P17); Metallic compound belongs to heavy metal compound mostly, have certain toxicity (Xu Chao, " antibiotic fabric general introduction ", printing and dyeing, 1995, NO.6, P29); The antibiotic sulfa drugs easily cause the drug resistance bacterium (Xu Chao, " antibiotic fabric general introduction ", printing and dyeing, 1995, NO.6, P29); The fragrant ethers of part, aromatic halogenate antiseptic on garment material the forbidding (Zou Chengshu, " the efficient durable antibiotic finish of fabric ", printing and dyeing, 1997, NO.1, P30); Organosilicon-quaternary amine by the development of U.S.'s DOW CORNING (DOW CORNING) company is at present domestic and international most popular a kind of antiseptic, but in use, must control external condition well, otherwise, can make its antibacterial ability forfeiture (Lu Zonglu, " textiles hygienic finishing " because can not remain valid concentration, printing and dyeing, 1995, NO.3, P33); Japanese kokai publication hei 4-289211,6-308109,10-37018 communique reported particle diameter sneaked into manufacture method in the viscose at 10um shitosan fine particles, add a small amount of shitosan can make have broad spectrum antibacterial, the deodorant function fiber (Japanese kokai publication hei 4-289211,6-308109,10-37018) of high-hygroscopicity, safety.But after the powder additive enters spinning solution, can improve spinning fluid viscosity greatly, increase the requirement that the spinning difficulty is checked technology; And the additive of so big particle diameter can make the physical property of fiber decline to a great extent.
The objective of the invention is natural polymer chitosan and derivative thereof and viscose blend preparation are had the natural composite fibre of function such as antibiotic, that height is preserved moisture, overcome the shortcoming that prior art exists.
The present invention has prepared the shitosan of molecular weight 600,000～20,000 with co-60 radiation source 8～48 hours radiation degradations of amount of radiation irradiation with 0.5kGy/ hour under atmospheric environment.The shitosan that degraded obtains is compared with the tegument glycan that extracts from organism, basic no change on structure and properties.Shitosan is joined in the acetate of 0.5M, be stirred to whole dissolvings, remove by filter impurity, in filtrate, drip the NaOH solution of 0.7M, shitosan regeneration is separated out, and until pH value of solution=12, gained shitosan turbid liquid is handled with CPS-2 ultrasonic wave pulverizer, obtain the crystallite shitosan aqueous dispersion of average grain diameter below 5 microns, be concentrated to 2%-10% (w%) back and use.With N-formylated shitosan, N, it is 10% aqueous slkali that O-cm-chitosan, O-cm-chitosan, N-cm-chitosan, N-carboxylic butyl shitosan are mixed with concentration by equal mixed; With the 6-O-hydroxyethyl chitosan, N, N, N-trimethyl chitin, N-butyl-N, N-dimethyl shitosan, N-dodecyl-N, N-dimethyl shitosan, N-butyl shitosan, N, one or more in N-dibutyl shitosan, N-octyl group shitosan, the N-dodecyl shitosan are mixed with 10% aqueous slkali by equal mixed; With the iodine quaternary ammonium salt of N-alkylated chitosan, the chlorine quaternary ammonium salt of N-alkylated chitosan and its quaternary phosphonium hydroxides ammonium derivative are mixed with 10% aqueous slkali by equal mixed.Above-mentioned 3 class chitosan derivatives mixed liquors can use separately, also can use by equal mixed.Add shitosan aqueous dispersion and above-mentioned solution below the particle diameter 5um of preparation to viscose spinning solution (notes: the viscose in sulfonation process or the maturation process) in 10%～90% ratio after mixed, after the high speed dispersion by the manufacture method of common viscose fibre industry production through acid bath moulding → washing → desulfurization → washing → bleaching → washing → pickling → wash → oil → drying and other steps, make natural antibacterial shitosan and derivative modified viscose thereof.Antibiotic odourproof fiber of the present invention is compared with viscose, in outward appearance with there is not any gap in shape, and is improving fiber dyeing and finishing and chemically treated ability.Addition in viscose is 0.3～2.0% of a viscose glue weight to the grain of the present invention's preparation through shitosan aqueous dispersion below 5 microns and chitosan derivatives.Addition is less than these, and then the fiber antibacterial ability is not enough, and adding too much then, fibre strength reduces and should not use.(the excusing from death disintegrating process of shitosan aqueous dispersion is claimed, and shitosan and derivative blended to be used as antiseptic claimed is antibiotic sticking than the protection of fiber spinning solution composition requirement)
The shitosan and the derivative modified viscose thereof of the present invention's preparation are the composites of natural material cellulose and shitosan and derivative thereof, especially shitosan, it is qualified that its excitant, acute toxicity, subacute toxicity, chronic toxicity and anaphylaxis prove by experiment, thereby can use suitable fiber safely as the most comfortable in the ecology.The present invention adopts the ultrasonic wave pulverizer to prepare the littler chitosan particle of particle diameter, and the employing of this crystallite shitosan aqueous dispersion can obviously not improve spinning fluid viscosity, thereby the moulding process of fiber is unaffected.This composite can biodegradation in last earth and pond, and discarded back is free from environmental pollution, is a kind of green product.Fiber of the present invention is compared with now market-oriented antibiotic odourproof fiber, and also having antibacterial effect lastingly, does not influence advantages such as feel, humectant.Fiber of the present invention is applied to have the following advantages on the gertrude with the BLENDED FABRIC of cotton: 1) low irritant, 2) humectant, 3) flexibility, 4) assorted bacterium inhibition of proliferation effect, 5) biodegradable.These advantages can prove that this blending fabric can be used as underskirt and coat, comprise long and short underwear for baby, the upper and lower underskirt that children wear, the women wears wears with the man, T-shirt and sweatshirt, diversified garment market such as nightwear; With the blending fabric of polymer such as polyester can be used for getting into bed dress apparatus, bunk and bedding; And it can also be used to do nonwoven fabric, as medical treatment and health department fabric, or soldier, field man's clothing.
Embodiment:
The preparation of antibiotic property shitosan and derivative modified viscose thereof: the radiation degradation of shitosan: the shitosan of getting 500 gram-molecular weights 1,080,000, degree of deacetylation 85% is contained in the wide-mouth bottle, provides Co by Tianjin Inst. of Technical Physics
60Radiation source under 0.5kGy/ hour dosage of radiation, shone 32 hours, obtained the shitosan oligomer of molecular weight 5.14 ten thousand, degree of deacetylation 87%.The preparation of crystallite shitosan aqueous dispersion: get the acetate stirring and dissolving of above-mentioned shitosan 500 grams with 200mL0.5M, filter the chitosan solution clear liquid, slowly drip the NaOH solution of 0.7M, shitosan regeneration is separated out, gained shitosan turbid liquid was handled 1 hour with CPS-2 ultrasonic wave pulverizer, get the following flocculence shitosan aqueous dispersion of particle diameter 5um, being concentrated to concentration is that 10% (w/w) back is stand-by.N, O-Preparation of Carboxymethylchitosan: take by weighing shitosan 300 grams, add 3 liters of isopropyl alcohols, stir, be warming up to 80 ℃.Add 18M sodium hydroxide solution 500ml, react and after 1 hour system temperature is adjusted to 70 ℃, once add 220 monoxones that restrain, reacted 1 hour.Be cooled to room temperature, add the 250ml deionized water, be adjusted to neutrality, filter with glacial acetic acid.With the methanol aqueous solution washing twice of 70: 30 (V/V), filter.Wash with absolute methanol at last, suction filtration, dry down at 60 ℃.O-Preparation of Carboxymethylchitosan: take by weighing shitosan 300 grams, add 3 liter 42% sodium hydroxide solution, add 350 gram monoxones, reacted 24 hours down at 20 ℃.With hydrochloric acid the pH value is adjusted to 1, suction filtration.With 0.1M salt acid elution 2-3 time, suction filtration.60 ℃ of oven dry down.The preparation of chitosan iodine quaternary ammonium salt: shitosan 100 grams, add 3 liters of N-Methyl pyrrolidone, with nitrogen replacement, stir, add sodium hydroxide solution, 1280 gram iodomethane and the 130 gram sodium iodides of 46ml 6M, reaction is 20 hours in 36 ℃ water-bath, after reaction finishes, continue to stir, to reactant Dropwise 5 00ml ethanol, sediment washs, filters with ethanol.Filtrate is dissolved in 6 premium on currency, filters, and filtrate is put into dialysis bag, dialysis 6 days, the outer liquid of dialysis is changed every day, after the dialysis 80 ℃ of following vacuumizes.The preparation of chitosan quaternary ammonium hydrochloride: get 300 gram chitosan iodine quaternary ammonium salts and be dissolved in 50 liters of deionized waters, add 30 and lift away from sub-exchange resin [amberlite TRA-400 (U type)], at room temperature mix and placed 24 hours.The filter ions exchanger resin, with 5 washings of 15 liters of deionization moisture, mother liquor mixes with cleaning solution, 80 ℃ of following vacuumizes.The preparation of chitosan quaternary ammonium hydroxide: get 300 gram chitosan iodine quaternary ammonium salts and be dissolved in 30 premium on currency, at room temperature mix and add 30 liters of 0.1M sodium hydrate aqueous solutions, put into the dialysis bag dialysis 6 days.After the dialysis 80 ℃ of following vacuumizes.
Get above-mentioned N, O-cm-chitosan and O-cm-chitosan are dissolved in the 5M NaOH aqueous solution after by 1: 1 mixed; Getting above-mentioned chitosan quaternary ammonium derivative is dissolved in the 5M NaOH aqueous solution after by equal mixed; This two alkali lye is hybridly prepared into mixed liquor by weight 20/80.Get this mixed liquor and last preparation crystallite shitosan aqueous dispersion is mixed with antiseptic with 50/50 (w/w) mixed, to add in the viscose spinning solution of sulfonation process with the percent by weight of addition 0,0.5,1.0,1.5,2.0 with antiseptic, (the every premium on currency solution of spinning coagulation bath contains sodium sulfate 275～285 restrains after φ 0.06mm * 40 spinning heads are at spinning coagulation bath for high-speed stirred, fully mixing, deaeration, zinc sulfate 14～15 grams, sulfuric acid 100～110 grams) middle moulding.Fiber after the orientation is through washing → desulfurization (desulfurization bath---Na
2SO
311～14 grams per liters) → washing → bleaching (bleaching bath---NaClO 1 grams per liter) → washing → pickling (pickling bath---HCl 1～2 grams per liter) → wash → oil → drying makes finished fiber.
Claims (2)
1. antibiotic property chitosan derivatives modified viscose fiber and manufacture method thereof, it is characterized in that preparing shitosan with co-60 radiation source radiation degradation, shitosan is joined in the acetate of 0.5M, be stirred to whole dissolvings, remove by filter impurity, in filtrate, drip the NaOH solution of 0.7M, shitosan regeneration is separated out, until pH value of solution=12, gained shitosan turbid liquid is handled with CPS-2 ultrasonic wave pulverizer, obtain the crystallite shitosan aqueous dispersion of average grain diameter below 5 microns, be concentrated to 2%-10% (w%) back and use; With N-formylated shitosan, N, it is 10% aqueous slkali that O-cm-chitosan, O-cm-chitosan, N-cm-chitosan, N-carboxylic butyl shitosan are mixed with concentration by equal mixed; With the 6-O-hydroxyethyl chitosan, N, N, N-trimethyl chitin, N-butyl-N, N-dimethyl shitosan, N-dodecyl-N, N-dimethyl shitosan, N-butyl shitosan, N, one or more in N-dibutyl shitosan, N-octyl group shitosan, the N-dodecyl shitosan are mixed with 10% aqueous slkali by equal mixed; With the iodine quaternary ammonium salt of N-alkylated chitosan, the chlorine quaternary ammonium salt of N alkylated chitosan and its quaternary phosphonium hydroxides ammonium derivative are mixed with 10% aqueous slkali by equal mixed; Above-mentioned 3 class chitosan derivatives mixed liquors can use separately, also can use by equal mixed, add shitosan aqueous dispersion and above-mentioned solution below the particle diameter 5um of preparation to viscose spinning solution (notes: the viscose in sulfonation process or the maturation process) in 10%～90% ratio after mixed, manufacture method by common viscose fibre industry production after the high speed dispersion makes natural antibacterial shitosan and derivative modified viscose thereof, and wherein the addition in viscose is 0.3～2.0% of a viscose glue weight to the grain of invention preparation through shitosan aqueous dispersion below 5 microns and chitosan derivatives.
2. antibiotic property chitosan derivatives modified viscose fiber and manufacture method thereof is characterized in that shitosan is to have prepared the shitosan of molecular weight 600,000～20,000 with co-60 radiation source 8～48 hours radiation degradations of amount of radiation irradiation with 0.5kGy/ hour under atmospheric environment.
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| CN 00100636 CN1266922A (en) | 2000-01-25 | 2000-01-25 | Antibacterial viscose fibre and its making method |
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| CN 00100636 CN1266922A (en) | 2000-01-25 | 2000-01-25 | Antibacterial viscose fibre and its making method |
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Cited By (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1102968C (en) * | 2000-06-23 | 2003-03-12 | 上海士林纺织有限公司 | Modified viscose fibre containing super fine micro granular chitosan and its producing technology |
| CN1103387C (en) * | 2000-03-23 | 2003-03-19 | 上海士林纺织有限公司 | Preparation and product of mixed material of modified chitin-chitosan and viscose fiber spinning dope |
| WO2004009881A1 (en) * | 2002-07-23 | 2004-01-29 | Xiangtan Zenith Fine Chemicals, Co.,Ltd | Modified viscose fibre and its preparing process |
| CN1300178C (en) * | 2004-12-10 | 2007-02-14 | 中国海洋大学 | Chloro-N-trimethyl chitin hyamine |
| CN1303281C (en) * | 2002-12-19 | 2007-03-07 | 全球生技股份有限公司 | Yarn antibacterial treating method |
| CN1325520C (en) * | 2003-12-22 | 2007-07-11 | 盐城工学院 | Preparation of double type amphoteric chitosan derivative |
| US7244700B2 (en) | 2000-10-06 | 2007-07-17 | Reckitt Benckiser (Uk) Limited | Cleaning compositions containing chitosan salt |
| CN1327079C (en) * | 2003-06-30 | 2007-07-18 | 陈良 | Processing method for down with antibacterid, antivirus, mould proof, off odour eliminating and health care functions and use |
| CN1328305C (en) * | 2004-12-13 | 2007-07-25 | 中国科学院上海应用物理研究所 | Chitose superfine powder and production thereof |
| CN100341900C (en) * | 2005-11-16 | 2007-10-10 | 中国药科大学 | Quaterisation chitosan derivatives, preparation method and medicinal preparation containing the derivatives |
| CN100359009C (en) * | 2004-11-01 | 2008-01-02 | 北京航空航天大学 | Preparation of chitosan imbedded microbe sphere and method for biological treatment of sewage using same |
| CN101153081B (en) * | 2006-09-26 | 2011-04-06 | 香港理工大学 | Method of producing chitosan nano grain |
| CN102517668A (en) * | 2011-11-15 | 2012-06-27 | 青岛大学 | Functional luffa regenerated fiber and preparation method thereof |
| CN103643332A (en) * | 2013-12-04 | 2014-03-19 | 阜宁澳洋科技有限责任公司 | Functional composite fiber and preparation method thereof |
| CN103668520A (en) * | 2013-12-04 | 2014-03-26 | 阜宁澳洋科技有限责任公司 | Antibacterial regenerated cellulose fiber and preparation method thereof |
| CN104975504A (en) * | 2015-07-08 | 2015-10-14 | 陕西科技大学 | Method for preparing shoe antibacterial synthesis leather substrate and liner through O-carboxymethyl chitosan grafted nylon 66 fabric |
| CN106757459A (en) * | 2016-11-17 | 2017-05-31 | 胡稳成 | A kind of antibacterial mite-resistant cellulose viscose and preparation method containing sophora alopecuroides extract |
| CN107955997A (en) * | 2017-12-08 | 2018-04-24 | 江苏金太阳纺织科技股份有限公司 | A kind of preparation method of chitosan-allantoin regenerated celulose fibre |
| CN108175136A (en) * | 2018-03-15 | 2018-06-19 | 宁波必博母婴科技有限公司 | A kind of infant-wear of replaceable garment piece |
-
2000
- 2000-01-25 CN CN 00100636 patent/CN1266922A/en active Pending
Cited By (22)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1103387C (en) * | 2000-03-23 | 2003-03-19 | 上海士林纺织有限公司 | Preparation and product of mixed material of modified chitin-chitosan and viscose fiber spinning dope |
| CN1102968C (en) * | 2000-06-23 | 2003-03-12 | 上海士林纺织有限公司 | Modified viscose fibre containing super fine micro granular chitosan and its producing technology |
| US7244700B2 (en) | 2000-10-06 | 2007-07-17 | Reckitt Benckiser (Uk) Limited | Cleaning compositions containing chitosan salt |
| WO2004009881A1 (en) * | 2002-07-23 | 2004-01-29 | Xiangtan Zenith Fine Chemicals, Co.,Ltd | Modified viscose fibre and its preparing process |
| CN1303281C (en) * | 2002-12-19 | 2007-03-07 | 全球生技股份有限公司 | Yarn antibacterial treating method |
| CN1327079C (en) * | 2003-06-30 | 2007-07-18 | 陈良 | Processing method for down with antibacterid, antivirus, mould proof, off odour eliminating and health care functions and use |
| CN1325520C (en) * | 2003-12-22 | 2007-07-11 | 盐城工学院 | Preparation of double type amphoteric chitosan derivative |
| CN100359009C (en) * | 2004-11-01 | 2008-01-02 | 北京航空航天大学 | Preparation of chitosan imbedded microbe sphere and method for biological treatment of sewage using same |
| CN1300178C (en) * | 2004-12-10 | 2007-02-14 | 中国海洋大学 | Chloro-N-trimethyl chitin hyamine |
| CN1328305C (en) * | 2004-12-13 | 2007-07-25 | 中国科学院上海应用物理研究所 | Chitose superfine powder and production thereof |
| CN100341900C (en) * | 2005-11-16 | 2007-10-10 | 中国药科大学 | Quaterisation chitosan derivatives, preparation method and medicinal preparation containing the derivatives |
| CN101153081B (en) * | 2006-09-26 | 2011-04-06 | 香港理工大学 | Method of producing chitosan nano grain |
| CN102517668A (en) * | 2011-11-15 | 2012-06-27 | 青岛大学 | Functional luffa regenerated fiber and preparation method thereof |
| CN102517668B (en) * | 2011-11-15 | 2014-04-09 | 青岛大学 | Functional luffa regenerated fiber and preparation method thereof |
| CN103668520A (en) * | 2013-12-04 | 2014-03-26 | 阜宁澳洋科技有限责任公司 | Antibacterial regenerated cellulose fiber and preparation method thereof |
| CN103643332A (en) * | 2013-12-04 | 2014-03-19 | 阜宁澳洋科技有限责任公司 | Functional composite fiber and preparation method thereof |
| CN103643332B (en) * | 2013-12-04 | 2015-10-07 | 阜宁澳洋科技有限责任公司 | A kind of functional composite fiber and preparation method thereof |
| CN103668520B (en) * | 2013-12-04 | 2016-05-25 | 阜宁澳洋科技有限责任公司 | A kind of antibacterial regenerated celulose fibre and preparation method thereof |
| CN104975504A (en) * | 2015-07-08 | 2015-10-14 | 陕西科技大学 | Method for preparing shoe antibacterial synthesis leather substrate and liner through O-carboxymethyl chitosan grafted nylon 66 fabric |
| CN106757459A (en) * | 2016-11-17 | 2017-05-31 | 胡稳成 | A kind of antibacterial mite-resistant cellulose viscose and preparation method containing sophora alopecuroides extract |
| CN107955997A (en) * | 2017-12-08 | 2018-04-24 | 江苏金太阳纺织科技股份有限公司 | A kind of preparation method of chitosan-allantoin regenerated celulose fibre |
| CN108175136A (en) * | 2018-03-15 | 2018-06-19 | 宁波必博母婴科技有限公司 | A kind of infant-wear of replaceable garment piece |
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