CN104594025A - Method for preparing novel zinc-oxide-modified ultraviolet-resistant silk - Google Patents
Method for preparing novel zinc-oxide-modified ultraviolet-resistant silk Download PDFInfo
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Abstract
The invention discloses a method for preparing novel zinc-oxide-modified ultraviolet-resistant silk. According to the method, a zinc oxide film layer covers the surface of the silk by adopting an in situ synthesis method. The method specifically comprises the following steps: degumming the silk and performing surface activation; respectively dipping the silk in a zinc precursor solution and a reaction solvent; and finally, adding the silk into a heated and humidified steam, standing, taking out the silk, washing, and drying, thereby obtaining the zinc-oxide-modified ultraviolet-resistant silk. The preparation method is simple, convenient, high in efficiency and low in cost, solves the problem that zinc oxide is difficult to disperse and is suitable for large-scale production. The zinc oxide film layer covers the surface of the silk modified by the method, and the silk has high ultraviolet resistance, and improved mechanical property.
Description
Technical field:
The invention belongs to silk product technical field, particularly a kind of preparation method of uvioresistant silk of novel oxidized zinc modification.
Background technology:
Silk is thread azelon, containing 18 seed amino acids, these amino acid can produce photochemical reaction with ultraviolet, but very strong photochemical reaction can make the peptide bond of silk protein molecular backbone rupture, cause the mechanical strength of silk to decline and yellowing, affect the usability of silk, although therefore silk itself has certain protective action to ultraviolet, but the protective action of itself is very faint, need to carry out anti-ultraviolet finishing.
The uvioresistant material of conventional textiles mainly divides organic uv absorbers and inorganic UV screener, and organic uv absorbers becomes the mode of light and heat to discharge ultraviolet power conversion, and inorganic UV screener is by ultraviolet reflection or scattering.Organic uv absorbers is mainly salicylate system, benzophenone series, benzotriazole system and triazine system etc., the photostability of such material is poor, service life is short, can make fabric variable color, irritant etc. to skin, inorganic UV screener is mainly the particulate such as zinc oxide, titanium dioxide, good to the full wave shielding of UVB, and good light stability, arrange in colourless, on fabric color without impact, and environmentally friendly etc.
The anti-ultraviolet finishing of silk generally adopts organic uv absorbers, but along with expanding economy, to the raising that environment and quality of the life require, inorganic UV screener more and more receives publicity, and is wherein that the developing direction of the high-performance ultraviolet light screener supported is particularly wide with nanometer technology.
Chinese patent CN 101187164B (publication date 2008.07.23) discloses a kind of anti-creasing anti-bacterial anti-violet composite function silk fabric, is to be padded in by silk fabric in multifunction finishing agent that nano titanic oxide sol and Fibroin Hydrolysis liquid is mixed with to obtain.The disclosed functionalized nano shitosan of Chinese patent CN102677465B (publication date 2012.11.14) and nano-titanium dioxide modified tussah silk textiles, tussah silk woven fabric or nonwoven fabric are immersed in shitosan and titania solution, obtains the tussah silk textiles of modification.Chinese patent CN 103572585A (publication date 2014.02.12) discloses a kind of titania modified silk, is take titanate esters as reactant and benzinum for solvent generates fine and close titanium dioxide at silk surface in situ.Current nano titanium oxide is comparatively extensive as the application of anti ultraviolet agent on silk fabric, but the application of nano zine oxide is less.
Summary of the invention:
The object of this invention is to provide a kind of preparation method of uvioresistant silk of novel oxidized zinc modification, after the surface active by silk, impregnated in precursor solution and the reaction solution of zinc respectively, form zinc hydroxide film through reaction in-situ on silk surface, obtain the silk of modified zinc oxide finally by high temperature steam treatment.This preparation method is easy, and cost is low, is applicable to being applied in large-scale production, and the silk of preparation possesses higher ultraviolet-resistent property and mechanical performance.
Object of the present invention is achieved through the following technical solutions:
A preparation method for the uvioresistant silk of novel oxidized zinc modification, it is characterized in that, the method comprises the following steps:
(1) after silk being removed impurity, to come unstuck 60min with the sodium bicarbonate solution of 0.05g/L, spend deionized water clean, 40 DEG C of dryings obtain the silk come unstuck;
(2) after the surface activation process of the silk come unstuck step (1) obtained, 35-50s in the precursor solution of zinc is impregnated in bath raio 1:40, be soaked in reaction dissolvent with bath raio 1:30 again, at 60-70 DEG C, react 5-10min, take out the silk obtaining zinc hydroxide and cover;
(3) steam that the silk that zinc hydroxide step (2) obtained covers is placed in warming and humidifying leaves standstill, and takes out washing and dries, obtain the silk of modified zinc oxide.
Preferred as technique scheme, the silk described in step (1) is mulberry silk, tussah silk or regenerated fibroin fiber.
Preferred as technique scheme, the surface activation process described in step (1) is Cement Composite Treated by Plasma or soaks strong oxidizer.
Preferred as technique scheme, described oxidant is liquor potassic permanganate.
Preferred as technique scheme, the zinc nitrate hexahydrate aqueous solution of the precursor solution of the zinc described in step (2) to be mass fraction be 20-30%.
Preferred as technique scheme, the ammoniacal liquor of to be mass fraction the be 40-50% of the reaction dissolvent described in step (2).
Preferred as technique scheme, the steam of the warming and humidifying described in step (3) is the mixed vapour of ammoniacal liquor and water, and the volume ratio of ammoniacal liquor and water is 2:1, and the temperature of steam is 125-130 DEG C, and humidity is 20%.
Preferred as technique scheme, the time left standstill described in step (3) is 15-20min.
Preferred as technique scheme, the number of times of the washing described in step (3) is 2-3 time.
Preferred as technique scheme, the temperature of the oven dry described in step (3) is 30 DEG C.
Compared with prior art, the present invention has the following advantages:
(1) the present invention adopts silk surface active in conjunction with the Surface Creation one deck zinc-oxide film of in-situ synthesis at silk, and avoid the problem of zinc oxide difficulty dispersion, preparation method is easy, and cost is low, is applicable to large-scale production.
(2) preparation method that the present invention adopts adopts simple dipping gimmick, but adopt of short duration dipping repeatedly in conjunction with the means of moist steam, in the atmosphere of wet-hot steam, the synthesis of accelerating oxidation zinc, the generation nano granular of zinc oxide that the method energy is slowly gentle, to the surface almost not damaged of silk.
(3) silk of this method modification uniformly covers the thick zinc-oxide film of one deck 200nm, except giving silk good uvioresistant performance, going back bacteriostasis antibiosis deodorizing, and improving the mechanical performance of silk.
Detailed description of the invention:
In order to deepen the understanding of the present invention, below in conjunction with embodiment, the invention will be further described, and this embodiment only for explaining the present invention, does not form limiting the scope of the present invention.
Embodiment 1:
(1) after mulberry silk being removed impurity, to come unstuck 60min with the sodium bicarbonate solution of 0.05g/L, spend deionized water clean, 40 DEG C of dryings obtain the silk come unstuck.
(2) by the silk that comes unstuck after plasma treated surface activation, 50s in the zinc nitrate hexahydrate aqueous solution of 20% is impregnated in bath raio 1:40, be soaked in the ammoniacal liquor of 40% with bath raio 1:30 again, at 60 DEG C, react 10min, take out the silk obtaining zinc hydroxide and cover.
(3) be placed in by the silk that zinc hydroxide covers, volume ratio is in ammoniacal liquor and the water mixed vapour of 2:1, is 20% time in humidity, 125 DEG C of standing 20min, and taking-up washing 2 times, 30 DEG C of oven dry obtain the silk of modified zinc oxide.
Embodiment 2:
(1) after tussah silk being removed impurity, to come unstuck 60min with the sodium bicarbonate solution of 0.05g/L, spend deionized water clean, 40 DEG C of dryings obtain the silk come unstuck.
(2) after the Silk Soaking liquor potassic permanganate treatment surface of coming unstuck being activated, 50s in the zinc nitrate hexahydrate aqueous solution of 20% is impregnated in bath raio 1:40, be soaked in the ammoniacal liquor of 40% with bath raio 1:30 again, at 70 DEG C, react 5min, take out the silk obtaining zinc hydroxide and cover.
(3) silk that zinc hydroxide covers being placed in the ammoniacal liquor and water mixed vapour that volume ratio is 2:1, is 20% time in humidity, 130 DEG C of standing 15min, and take out washing 3 times, 30 DEG C of oven dry obtain the silk of modified zinc oxide.
Embodiment 3:
(1) after regenerated fibroin fiber being removed impurity, to come unstuck 60min with the sodium bicarbonate solution of 0.05g/L, spend deionized water clean, 40 DEG C of dryings obtain the silk come unstuck.
(2) by the silk that comes unstuck after plasma treated surface activation, 40s in the zinc nitrate hexahydrate aqueous solution of 25% is impregnated in bath raio 1:40, be soaked in the ammoniacal liquor of 45% with bath raio 1:30 again, at 65 DEG C, react 7min, take out the silk obtaining zinc hydroxide and cover.
(3) be placed in by the silk that zinc hydroxide covers, volume ratio is in ammoniacal liquor and the water mixed vapour of 2:1, is 20% time in humidity, 127 DEG C of standing 17min, and taking-up washing 3 times, 30 DEG C of oven dry obtain the silk of modified zinc oxide.
Embodiment 4:
(1) after mulberry silk being removed impurity, to come unstuck 60min with the sodium bicarbonate solution of 0.05g/L, spend deionized water clean, 40 DEG C of dryings obtain the silk come unstuck.
(2) after the Silk Soaking liquor potassic permanganate treatment surface of coming unstuck being activated, 48s in the zinc nitrate hexahydrate aqueous solution of 29% is impregnated in bath raio 1:40, be soaked in the ammoniacal liquor of 42% with bath raio 1:30 again, at 67 DEG C, react 10min, take out the silk obtaining zinc hydroxide and cover.
(3) be placed in by the silk that zinc hydroxide covers, volume ratio is in ammoniacal liquor and the water mixed vapour of 2:1, is 20% time in humidity, 126 DEG C of standing 16min, and taking-up washing 3 times, 30 DEG C of oven dry obtain the silk of modified zinc oxide.
Embodiment 5:
(1) after regenerated fibroin fiber being removed impurity, to come unstuck 60min with the sodium bicarbonate solution of 0.05g/L, spend deionized water clean, 40 DEG C of dryings obtain the silk come unstuck.
(2) by the silk that comes unstuck after plasma treated surface activation, 50s in the zinc nitrate hexahydrate aqueous solution of 30% is impregnated in bath raio 1:40, be soaked in the ammoniacal liquor of 50% with bath raio 1:30 again, at 70 DEG C, react 10min, take out the silk obtaining zinc hydroxide and cover.
(3) be placed in by the silk that zinc hydroxide covers, volume ratio is in ammoniacal liquor and the water mixed vapour of 2:1, is 20% time in humidity, 130 DEG C of standing 20min, and taking-up washing 3 times, 30 DEG C of oven dry obtain the silk of modified zinc oxide.
Embodiment 6:
(1) after tussah silk being removed impurity, to come unstuck 60min with the sodium bicarbonate solution of 0.05g/L, spend deionized water clean, 40 DEG C of dryings obtain the silk come unstuck.
(2) after the Silk Soaking liquor potassic permanganate treatment surface of coming unstuck being activated, 35s in the zinc nitrate hexahydrate aqueous solution of 20% is impregnated in bath raio 1:40, be soaked in the ammoniacal liquor of 40-50% with bath raio 1:30 again, at 60 DEG C, react 5min, take out the silk obtaining zinc hydroxide and cover.
(3) be placed in by the silk that zinc hydroxide covers, volume ratio is in ammoniacal liquor and the water mixed vapour of 2:1, is 20% time in humidity, 125 DEG C of standing 15min, and taking-up washing 3 times, 30 DEG C of oven dry obtain the silk of modified zinc oxide.
The uvioresistant silk fabric of the modified zinc oxide prepared by embodiment 1-6 is compared with untreated silk fabric, and the grammes per square metre of silk fabric, ultraviolet-resistent property, antibiotic property and mechanical properties results are as shown in the table:
From above-mentioned data, the anti-ultraviolet property of the uvioresistant silk fabric of modified zinc oxide prepared by this method is excellent, and the antibiotic property of fabric and mechanical strength have lifting.
Claims (10)
1. a preparation method for the uvioresistant silk of novel oxidized zinc modification, it is characterized in that, the method comprises the following steps:
(1) after silk being removed impurity, to come unstuck 60min with the sodium bicarbonate solution of 0.05g/L, spend deionized water clean, 40 DEG C of dryings obtain the silk come unstuck;
(2) after the surface activation process of the silk come unstuck step (1) obtained, 35-50s in the precursor solution of zinc is impregnated in bath raio 1:40, be soaked in reaction dissolvent with bath raio 1:30 again, at 60-70 DEG C, react 5-10min, take out the silk obtaining zinc hydroxide and cover;
(3) steam that the silk that zinc hydroxide step (2) obtained covers is placed in warming and humidifying leaves standstill, and takes out washing and dries, obtain the silk of modified zinc oxide.
2. the preparation method of the uvioresistant silk of a kind of novel oxidized zinc modification as claimed in claim 1, is characterized in that, the silk described in step (1) is mulberry silk, tussah silk or regenerated fibroin fiber.
3. the preparation method of the uvioresistant silk of a kind of novel oxidized zinc modification as claimed in claim 1, is characterized in that, the surface activation process described in step (1) is Cement Composite Treated by Plasma or soaks strong oxidizer.
4. the preparation method of the uvioresistant silk of a kind of novel oxidized zinc modification as claimed in claim 3, is characterized in that, described strong oxidizer is liquor potassic permanganate.
5. the preparation method of the uvioresistant silk of a kind of novel oxidized zinc modification as claimed in claim 1, is characterized in that, the zinc nitrate hexahydrate aqueous solution of the precursor solution of the zinc described in step (2) to be mass fraction be 20-30%.
6. the preparation method of the uvioresistant silk of a kind of novel oxidized zinc modification as claimed in claim 1, is characterized in that, the ammoniacal liquor of to be mass fraction the be 40-50% of the reaction dissolvent described in step (2).
7. the preparation method of the uvioresistant silk of a kind of novel oxidized zinc modification as claimed in claim 1, it is characterized in that, the steam of the warming and humidifying described in step (3) is the mixed vapour of ammoniacal liquor and water, the volume ratio of ammoniacal liquor and water is 2:1, the temperature of steam is 125-130 DEG C, and humidity is 20%.
8. the preparation method of the uvioresistant silk of a kind of novel oxidized zinc modification as claimed in claim 1, is characterized in that, the time left standstill described in step (3) is 15-20min.
9. the preparation method of the uvioresistant silk of a kind of novel oxidized zinc modification as claimed in claim 1, is characterized in that, the number of times of the washing described in step (3) is 2-3 time.
10. the preparation method of the uvioresistant silk of a kind of novel oxidized zinc modification as claimed in claim 1, is characterized in that, the temperature of the oven dry described in step (3) is 30 DEG C.
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105686159A (en) * | 2016-03-14 | 2016-06-22 | 浙江大学 | Method for preparing novel mask chip by utilizing fibroin plate cocoons |
| CN105803805A (en) * | 2016-04-21 | 2016-07-27 | 安徽皖翎羽绒制品有限公司 | Treatment method of anti-bacterial and anti-UV (Ultraviolet) down feather |
| CN106149352A (en) * | 2016-08-09 | 2016-11-23 | 东华大学 | A kind of preparation method of nano zinc oxide modified bafta |
| CN106835673A (en) * | 2017-03-27 | 2017-06-13 | 广西科技大学 | A kind of UV resistance zinc oxide silk composite fiber and preparation method thereof |
| CN107287877A (en) * | 2017-06-28 | 2017-10-24 | 合肥市聚丰制丝有限责任公司 | It is a kind of to improve the method for silk performance |
| CN107313244A (en) * | 2017-07-16 | 2017-11-03 | 长沙善道新材料科技有限公司 | The technique that a kind of use silk prepares uvioresistant antibiotic fabric |
| CN107419519A (en) * | 2017-07-16 | 2017-12-01 | 长沙善道新材料科技有限公司 | A kind of preparation method of the affine uvioresistant anti bacteria natural silk fiber of zinc oxide |
| CN107630351A (en) * | 2017-09-29 | 2018-01-26 | 安徽省创安体育用品有限公司 | A kind of preparation method of Anti-static cap cloth |
| CN109680480A (en) * | 2018-11-28 | 2019-04-26 | 湖州品创孵化器有限公司 | A kind of preparation method of health uvioresistant silk fabric |
| CN109695150A (en) * | 2018-11-28 | 2019-04-30 | 湖州品创孵化器有限公司 | A kind of preparation method of pro-skin type uvioresistant silk fabric |
| CN111136968A (en) * | 2019-08-27 | 2020-05-12 | 深圳市大毛牛新材料科技有限公司 | Waterproof anti ultraviolet textile fabric |
| CN113832729A (en) * | 2021-09-15 | 2021-12-24 | 苏州同构科技有限公司 | Washable ultraviolet absorbent and preparation method thereof |
| CN114673006A (en) * | 2022-03-08 | 2022-06-28 | 浙江理工大学 | ZnO-silk fibroin-based antibacterial medical textile coating material |
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| CN105686159B (en) * | 2016-03-14 | 2018-02-02 | 浙江大学 | A kind of method that gauze mask chip is prepared using fibroin plate cocoon |
| CN105686159A (en) * | 2016-03-14 | 2016-06-22 | 浙江大学 | Method for preparing novel mask chip by utilizing fibroin plate cocoons |
| CN105803805A (en) * | 2016-04-21 | 2016-07-27 | 安徽皖翎羽绒制品有限公司 | Treatment method of anti-bacterial and anti-UV (Ultraviolet) down feather |
| CN106149352A (en) * | 2016-08-09 | 2016-11-23 | 东华大学 | A kind of preparation method of nano zinc oxide modified bafta |
| CN106835673A (en) * | 2017-03-27 | 2017-06-13 | 广西科技大学 | A kind of UV resistance zinc oxide silk composite fiber and preparation method thereof |
| CN107287877A (en) * | 2017-06-28 | 2017-10-24 | 合肥市聚丰制丝有限责任公司 | It is a kind of to improve the method for silk performance |
| CN107419519A (en) * | 2017-07-16 | 2017-12-01 | 长沙善道新材料科技有限公司 | A kind of preparation method of the affine uvioresistant anti bacteria natural silk fiber of zinc oxide |
| CN107313244A (en) * | 2017-07-16 | 2017-11-03 | 长沙善道新材料科技有限公司 | The technique that a kind of use silk prepares uvioresistant antibiotic fabric |
| CN107630351A (en) * | 2017-09-29 | 2018-01-26 | 安徽省创安体育用品有限公司 | A kind of preparation method of Anti-static cap cloth |
| CN109680480A (en) * | 2018-11-28 | 2019-04-26 | 湖州品创孵化器有限公司 | A kind of preparation method of health uvioresistant silk fabric |
| CN109695150A (en) * | 2018-11-28 | 2019-04-30 | 湖州品创孵化器有限公司 | A kind of preparation method of pro-skin type uvioresistant silk fabric |
| CN111136968A (en) * | 2019-08-27 | 2020-05-12 | 深圳市大毛牛新材料科技有限公司 | Waterproof anti ultraviolet textile fabric |
| CN111136968B (en) * | 2019-08-27 | 2022-05-27 | 江苏大毛牛新材料有限公司 | Waterproof anti ultraviolet textile fabric |
| CN113832729A (en) * | 2021-09-15 | 2021-12-24 | 苏州同构科技有限公司 | Washable ultraviolet absorbent and preparation method thereof |
| CN114673006A (en) * | 2022-03-08 | 2022-06-28 | 浙江理工大学 | ZnO-silk fibroin-based antibacterial medical textile coating material |
| CN114673006B (en) * | 2022-03-08 | 2023-09-29 | 浙江理工大学 | Antibacterial medical textile coating material based on ZnO-silk fibroin |
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