CN1102968C - Modified viscose fibre containing super fine micro granular chitosan and its producing technology - Google Patents
Modified viscose fibre containing super fine micro granular chitosan and its producing technology Download PDFInfo
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- CN1102968C CN1102968C CN00116708A CN00116708A CN1102968C CN 1102968 C CN1102968 C CN 1102968C CN 00116708 A CN00116708 A CN 00116708A CN 00116708 A CN00116708 A CN 00116708A CN 1102968 C CN1102968 C CN 1102968C
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Abstract
The present invention provides a modified viscose fiber containing chitosan ultrafine particles and a preparation technology thereof, and relates to modification of an artificial fiber and a polymer. The modified viscose fiber is prepared by that viscose silk raw liquor is added with 0.5 to 5 wt% of chitosan microparticle with the particle diameter smaller than 10 mum to be uniformly mixed; the fiber is formed by a conventional wet wire spraying technology. As the chitosan microparticles are added in the viscose silk raw liquor, the textiles manufactured by the modified fiber have good hygroscopicity, and good biocompatibility, antibacterial and deodorization performance, biodegradability, etc. are increased. A blending technology is used. Compared with the relevant antibacterial after-treating technology, the production cost of textiles is greatly saved.
Description
Viscose is as the common chemical fibre, though it is good to have a sucting wet air permeability, wears comparatively comfortable characteristics, can not satisfy people this type of textiles is asked in many-sided inspections such as antibiotic property, biocompatibilities; Though chitosan material has biocompatibility, antibacterial and deodouring and is easy to various features such as degradability, but the manufacturing technology that pure chitosan fiber is only arranged at present, or shitosan used as fabric finishing agent. and make particulate and viscose spinning dope co-blended spinning to invest its good dyeability, biocompatibility, antibacterial and deodouring and to be easy to manifold research and products such as degradability about shitosan, but not seeing as yet has report.
The objective of the invention is to provide a kind of modified viscose fiber and manufacturing technique thereof that contains super fine micro granular chitosan.
The present invention is achieved in that the modified viscose fiber of chitosan-containing ultrafine dust, is made up of less than the super fine micro granular chitosan of 10 μ m viscose spinning dope, particle diameter, and wherein the weight of chitosan-containing is 2.0-3.0%.
A kind of manufacturing technique that contains the modified viscose fiber of first glycan ultrafine dust is;
(1) preparation of super fine micro granular chitosan: the shitosan material dissolution is made the shitosan acid solution in the acetum of 0.1-0.5%, then it is splashed into the suspension that forms chitosan particle in the NaOH aqueous solution of 5-8%, it is that the 10000-15000rpm homogenizer grinds that this suspension is injected rotating speed, under 160-190 ℃, it is carried out spray drying and cyclone classified with the spray-dired method of routine again, thereby obtain the super fine micro granular chitosan of particle diameter below 10 μ m.
(2) preparation of the modified viscose fiber of chitosan-containing ultrafine dust: will by the super fine micro granular chitosan of (1) gained by weight percentage composition be that the ratio of 2.0-3.0% is with after viscose spinning dope mixes mutually, adopt conventional viscose wet spinning technology to become silk, promptly get the modified fibre of required chitosan-containing ultrafine dust.
The present invention is owing to added chitosan particle in viscose silk stoste, the textiles that fiber after the modification is made has increased fine qualities such as biocompatibility, antibacterial and deodouring, biological degradability again except that original good hygroscopicity, adopt blending technology, compare with relevant antibiotic postfinishing process, saved the production cost of fabric greatly.Thereby the production cost of fabric is descended greatly.
Following examples will be described further technical characterictic of the present invention:
Embodiment 1: with 500 gram deacetylations be 82%, mean molecule quantity is that 42000 shitosan adds in the 7750 gram aqueous solution that contain 250 gram acetate, obtains the aqueous acetic acid of shitosan after the stirring and dissolving.This solution splashed into shitosan is solidified again separate out in 5% the NaOH aqueous solution and be fine particle.
To neutral, adding water formation shitosan content again is the suspension of 2-2.5% (weight) with above-mentioned chitosan particle water flushing.The employing rotating speed is that the homogenizer of 15000rpm carries out high speed dispersion three times to it, and each time is 5min, filters to remove big chitosan particle through 120 eye mesh screens then.Filtrate is carried out spray drying, and concrete process conditions are: mist flow is that 16ml/min, compressed air pressure are 3.0Kg/m
2, drying air temperature is 175 ℃, it directly is ultra-fine chitosan particle below the 5 μ m that the chitosan particle of drying is carried out can obtaining after cyclone classified 300 gram particles.
The ultra-fine chitosan particle that makes is scattered in once more forms dispersion liquid in the water, accounting for the cellulose percentage composition in shitosan respectively is the spinning solution (fiber content: 9%) that 0.3,0.5,2.0,3.0% ratio adds ultra-fine chitosan particle dispersion liquid viscose, mix, adopt conventional wet spinning process to make the viscose of chitosan-containing particulate.The performance of the fiber of gained is as follows:
Table 1
The intensity of blended fiber is not that sneaking into of ultra-fine chitosan particle below the 5 μ m descends because of particle diameter as can be seen from Table 1.
| Test piece number (Test pc No.) | Shitosan content (%) in the fiber | Fiber number (d) | Dry strength (g/d) | Wet strength (g/d) | Flexural strength (g/d) | Extension at break (%) |
| 1 | 0 | 3.19 | 2.50 | 1.68 | 1.51 | 55.2 |
| 2 | 0.3 | 3.02 | 2.51 | 1.67 | 1.52 | 60.5 |
| 3 | 0.5 | 3.21 | 2.51 | 1.68 | 1.49 | 62.7 |
| 4 | 2.0 | 2.98 | 2.49 | 1.65 | 1.46 | 70.4 |
| 5 | 3.0 | 3.10 | 2.50 | 1.68 | 1.49 | 75.8 |
Embodiment 2: with 500 gram deacetylations be 90%, mean molecule quantity is that 52000 shitosan adds in the 7500 gram aqueous solution that contain 350 gram acetate, obtains the aqueous acetic acid of shitosan after the stirring and dissolving.This solution splashed into shitosan is solidified again separate out in 5% the NaOH aqueous solution and be fine particle.
To neutral, adding water formation shitosan content again is the suspension of 2-2.5% (weight) with above-mentioned shitosan fine particles water flushing.The employing rotating speed is that the homogenizer of 15000rpm carries out high speed dispersion three times to it, and each time is 5min, filters to remove big chitosan particle through 100 eye mesh screens then.Filtrate is carried out spray drying, and concrete process conditions are: mist flow is that 17ml/min, compressed air pressure are 3.0Kg/m
2, drying air temperature is 185 ℃, it directly is ultra-fine chitosan particle below the 10 μ m that the chitosan particle of drying is carried out can obtaining after cyclone classified 360 gram particles.
The ultra-fine chitosan particle that makes is scattered in once more forms dispersion liquid in the water, accounting for the cellulose percentage composition in shitosan respectively is the spinning solution (fiber content: 9%) that 0.3,0.5,2.0,3.0% ratio adds ultra-fine chitosan particle dispersion liquid viscose, mix, adopt conventional wet spinning process to make chitosan particle and cellulosic blended fiber.The performance of the fiber of gained is as follows:
Table 2
The intensity of blended fiber is that sneaking into of ultra-fine chitosan particle below the 10 μ m descends because of particle diameter as can be seen from Table 2, but does not influence the practical application of fiber.
| Test piece number (Test pc No.) | Shitosan content (%) in the fiber | Fiber number (d) | Dry strength (g/d) | Wet strength (g/d) | Flexural strength (g/d) | Split elongation (%) |
| 6 | 0 | 1.22 | 4.56 | 3.77 | 2.06 | 56.4 |
| 7 | 0.3 | 1.19 | 4.57 | 3.67 | 2.25 | 59.4 |
| 8 | 0.5 | 1.21 | 4.52 | 3.69 | 2.26 | 62.0 |
| 9 | 2.0 | 1.20 | 4.48 | 3.52 | 2.11 | 71.5 |
| 10 | 3.0 | 1.27 | 4.37 | 3.52 | 2.05 | 76.3 |
Test case 1:
1～No. 10 sample that obtains among the embodiment 1,2 is not washed and wash antibacterial tests respectively, and the result is as follows:
Table 3
| Sample number | Shitosan content (%) in the fiber | Do not wash sample antibiotic property testing result | Wash the antibiotic property testing result after 5 times |
| 1 | 0 | - | - |
| 2 | 0.3 | Negative | Negative |
| 3 | 0.5 | Positive | Positive |
| 4 | 2.0 | Positive | Positive |
| 5 | 3.0 | Positive | Positive |
| 6 | 0 | - | - |
| 7 | 0.3 | Negative | Negative |
| 8 | 0.5 | Positive | Positive |
| 9 | 2.0 | Positive | Positive |
| 10 | 3.0 | Positive | Positive |
As can be seen from Table 3, have only when the heavily branch content of ultra-fine chitosan particle in the blend regenerated fiber greater than 0.3% the time, the blend regenerated fiber just has antibiotic property.
Test case 2:
1～No. 10 sample that obtains among the embodiment 1,2 is carried out degradation test respectively, and the result is as follows:
Table 4
| Sample number | Shitosan does not wash degradability content (%) testing result (%) testing result (%) after the sample degradation washing 5 times in the fiber |
| To NH 3To H 2S to NH 3To H 2The degradability degradability degradability degradability of S | |
| 1 2 3 4 5 6 7 8 9 10 | 0 0 0 10.0 0 0.3 47.2 30.3 49.7 26.8 0.5 59.5 47.2 71.0 48.7 2.0 72.0 54.2 68.2 54.2 3.0 71.0 63.8 79.0 61.7 0 0 0 10.0 16.7 0.3 51.5 45.8 56.0 32.3 0.5 54.0 68.3 67.0 66.5 2.0 68.1 72.5 78.0 68.8 3.0 68.5 79.2 79.6 70.3 |
As can be seen from Table 4, the weight percentage of ultra-fine chitosan particle is greater than having good degradability in 0.3% the blend regenerated fiber.
Claims (2)
1, the modified viscose fiber of chitosan-containing ultrafine dust is characterized in that, is made up of less than the super fine micro granular chitosan of 10 μ m viscose spinning dope, particle diameter, and wherein the weight percentage of chitosan-containing is 2.0-3.0%.
2, a kind of manufacturing technique of modified viscose fiber of chitosan-containing ultrafine dust is characterized in that:
(1) preparation of super fine micro granular chitosan: the shitosan material dissolution is made the shitosan acid solution in the acetum of 0.1-0.5%, then it is splashed into the suspension that forms chitosan particle in the NaOH aqueous solution of 5-8%, it is that the 10000-1500rpm homogenizer grinds that this suspension is injected rotating speed, under 160-190 ℃, it is carried out spray drying and cyclone classified with the spray-dired method of routine again, thereby obtain the super fine micro granular chitosan of particle diameter below 10 μ m.
(2) preparation of the modified viscose fiber of chitosan-containing ultrafine dust: will be by the super fine micro granular chitosan of (1) gained in the ratio of 2.0-3.0% weight percentage with after viscose spinning dope mixes mutually, adopt conventional viscose wet spinning technology to be shaped, promptly get the modified viscose fiber of required chitosan-containing ultrafine dust.
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| CN00116708A CN1102968C (en) | 2000-06-23 | 2000-06-23 | Modified viscose fibre containing super fine micro granular chitosan and its producing technology |
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| CN00116708A CN1102968C (en) | 2000-06-23 | 2000-06-23 | Modified viscose fibre containing super fine micro granular chitosan and its producing technology |
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| CN1280215A CN1280215A (en) | 2001-01-17 |
| CN1102968C true CN1102968C (en) | 2003-03-12 |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102839439B (en) * | 2012-09-20 | 2014-05-07 | 青岛嘉胜隆贸易有限公司 | Viscose fiber for eliminating bad smell of perspiration and preparation method thereof |
| CN103757917B (en) * | 2014-01-26 | 2016-02-17 | 江汉大学 | The preparation method of the electroactive chitosan-based composite of a kind of tool |
| CN106732454B (en) * | 2016-12-12 | 2019-04-16 | 齐鲁工业大学 | A kind of poplar slab dissolving pulp modifying agent and the method for preparing deodorant |
| CN107142540A (en) * | 2016-12-23 | 2017-09-08 | 句容市申兔工艺针织厂 | A kind of preparation technology of anti-bacterial fibre |
| CN106884323A (en) * | 2017-02-26 | 2017-06-23 | 浙江峰赫纺织有限公司 | A kind of preparation method of chitosan anti-bacteria viscose rayon |
| CN108166157B (en) * | 2017-12-25 | 2020-07-10 | 合肥洁诺无纺布制品有限公司 | Moisture-absorbing and bacteriostatic spunlace non-woven fabric beauty mask base cloth and preparation method thereof |
| CN109056092A (en) * | 2018-07-23 | 2018-12-21 | 澳洋集团有限公司 | A kind of preparation method of antimicrobial form short rayon fiber |
| CN113832741A (en) * | 2021-09-28 | 2021-12-24 | 许成志 | Nano powder modified non-woven fabric and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1233296A (en) * | 1996-09-17 | 1999-10-27 | 三菱丽阳株式会社 | Chitosan-containing acrylic fibers and process for preparing the same |
| CN1261111A (en) * | 2000-01-14 | 2000-07-26 | 东华大学 | Antibacterial fibres containing chitin and its derivatives, and preparing process thereof |
| CN1266922A (en) * | 2000-01-25 | 2000-09-20 | 天津大学 | Antibacterial viscose fibre and its making method |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1233296A (en) * | 1996-09-17 | 1999-10-27 | 三菱丽阳株式会社 | Chitosan-containing acrylic fibers and process for preparing the same |
| CN1261111A (en) * | 2000-01-14 | 2000-07-26 | 东华大学 | Antibacterial fibres containing chitin and its derivatives, and preparing process thereof |
| CN1266922A (en) * | 2000-01-25 | 2000-09-20 | 天津大学 | Antibacterial viscose fibre and its making method |
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Owner name: SHANGHAI SHIHLIN FIBER MATERIALS CO., LTD. Free format text: FORMER OWNER: SHILIN SPINNING CO., LTD., SHANGHAI Effective date: 20040203 |
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Effective date of registration: 20040203 Address after: 201100 Shanghai City No. 6269 humin road Yinxiao building room 1105 Patentee after: Shanghai Shilin Fiber Material Co., Ltd. Address before: 201100 Shanghai City No. 6269 humin road Yinxiao building room 1105 Patentee before: Shilin Spinning Co., Ltd., Shanghai |
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