CN104479155A - Preparation method of chitosan/titanium dioxide sol antibacterialpackaging film - Google Patents
Preparation method of chitosan/titanium dioxide sol antibacterialpackaging film Download PDFInfo
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- CN104479155A CN104479155A CN201410817699.0A CN201410817699A CN104479155A CN 104479155 A CN104479155 A CN 104479155A CN 201410817699 A CN201410817699 A CN 201410817699A CN 104479155 A CN104479155 A CN 104479155A
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Abstract
The invention relates to a method for preparing anenvironment-friendlyhigh polymer material antibacterialpackaging film by mixing chitosan and titanium dioxide sol, and belongs to the technical field of preparation of a novel high polymer material taking renewablebiomass as a raw material. Tetrabutyltitanate, glacial acetic acid and a silane coupling agent (KH570) are slowly dropped in absolute ethyl alcohol respectively and stirred to prepare a precursor, deionized water and hydrochloric acid are sufficiently stirred and dropped in the absolute ethyl alcohol, a dropping liquid is prepared and then dropped in the precursor at a certain speed, modified titanium dioxide sol is obtained, added to a chitosan-acetic acid solution containing glycerin and uniformly stirred, and the chitosan/titanium dioxide sol antibacterialpackaging film is obtained after defoaming and film scraping. According to the preparation method, the titanium dioxide sol reaction temperature is low, the equipment investment is small, and uniform doping of the titanium dioxide sol and a chitosan solution in the molecular level can be realized in shorter time; and the compatibility of the titanium dioxide sol treated by the silanecoupling agentand chitosan is good.
Description
Technical field
The present invention relates to a kind of environmentally friendly macromolecular material chitosan and mix the method manufacturing anti-bacterial packaging film with TiO 2 sol, belong to reproducible biomass for novel high polymer material technical field prepared by raw material.
Background technology
The packaging film surface nutrient that packaged dairy product, fruits and vegetables, meat etc. are rich in nutrition article enriches, the conditions such as general storage temperature, humidity are also relatively applicable to microbial growth, packaging film surface becomes easily infected by microorganism, and microorganism is just easy to move on article, and article are rotted.If use anti-biotic material to prepare packaging film, just can suppress microbial growth, prophylaxis of microbial in the procreation of package material surface, thus prevents the rotten of article further, improves the packaging protecting ability of film.
Current antimicrobial packaging film mostly is nondegradable plastics, although these anti-bacterial packaging films can meet antibacterial demand, produces white garbage, contaminate environment after a large amount of packing film is discarded.In addition, in long-term storage, plastic film and food close contact, have certain influence to food safety.As used biomass-based antibacterial film to replace packaged by plastic film food, above-mentioned pollution problem can be solved.
In the face of the environmental problem such as increasingly serious energy dilemma and " white pollution ", chitosan relies on its good Biodegradable, is considered to one of desirable biological material.Rely on unique restraining and sterilizing bacteria effect, superior film-forming properties and biocompatibility, chitosan has great development prospect in food product pack and fresh-keeping aspect.But the structure and characteristics of chitosan self determines when chitosan film material is applied in food product pack and preserving fruit and vegetable utilizing exists problems, as poor in physical and mechanical properties, production cost is high.Chitosan can by with other organic or inorganic material blending and modifyings, improve its physical and mechanical properties, reduce production cost simultaneously.
Wen Yan, Han Jianbing etc. utilize nano-TiO
2broad spectrum antibacterial, photocatalytic activity prepare chitosan/nano-TiO
2composite antibacterial material, but this research adopts nano-TiO
2powder and chitosan solution are directly blended prepares matrix material, because nanoparticle is easily reunited, causes and is separated.Pang Hongtao etc. adopt hydrothermal method to prepare nano-TiO
2the matrix material of/chitosan, but must carry out at high temperature under high pressure during the method reaction, therefore conversion unit requirement is high, technical difficulty large, security is also poor.
Summary of the invention
The object of the invention is to propose a kind of chitosan/titanium dioxide colloidal sol antimicrobial packaging membrane preparation method, adopt modified TiO 2 sol to mix with chitosan acetic acid solution, be prepared environmentally friendly chitosan/titanium dioxide colloidal sol anti-bacterial packaging film.
A kind of chitosan/titanium dioxide colloidal sol antimicrobial packaging membrane preparation method that the present invention proposes, comprises the following steps:
(1) respectively by tetrabutyl titanate, Glacial acetic acid and silane coupling agent (KH570) slowly instillation 2/3 part of dehydrated alcohol, make after fully stirring and formerly drive liquid;
(2) respectively deionized water and hydrochloric acid in instillation 1/3 part of dehydrated alcohol, are made dropping liquid under fully stirring;
(3) by above-mentioned dropping liquid dripping/obtained 60 DEG C of the speed of the 2s instillation the first step are former to be driven in liquid, stir 1h and obtain modified titanium dioxide sol after leaving standstill 20min;
(4) a certain amount of chitosan is added in the acetic acid solution of 1% (volume ratio), at 60 DEG C, stir 1.5h, add after 0.2% glycerine continues to stir 1.5h and obtain chitosan solution;
(5) by adding the obtained modified titanium dioxide sol of the 3rd step in above-mentioned chitosan solution, stirring 2h, often stirring the ultrasonic 15min of 40min;
(6) above-mentioned mixed solution is loaded deaeration in defoamer;
(7) by the mixed solution knifing machine film forming on a glass after above-mentioned deaeration, chitosan/titanium dioxide colloidal sol anti-bacterial packaging film after drying, is obtained.
A kind of chitosan/titanium dioxide colloidal sol antimicrobial packaging membrane preparation method that the present invention proposes, advantage has: sol-gel method prepares that TiO 2 sol temperature of reaction is low, facility investment is little, and can realize the Uniform Doped on molecular level in the short period of time with chitosan solution; TiO 2 sol after silane coupling agent process and chitosan consistency good, obtained anti-bacterial packaging film surface finish is good, do not occur demixing phenomenon, chitosan/titanium dioxide colloidal sol anti-bacterial packaging film is all greater than 99% to intestinal bacteria and streptococcus aureus antibiotic rate after testing, extends 2 times by the tomato fresh-keeping phase of its packaging.
Embodiment
A kind of chitosan/titanium dioxide colloidal sol antimicrobial packaging membrane preparation method that the present invention proposes, comprises the following steps:
(1) respectively by tetrabutyl titanate, Glacial acetic acid and silane coupling agent (KH570) slowly instillation 2/3 part of dehydrated alcohol, make after fully stirring and formerly drive liquid;
(2) respectively deionized water and hydrochloric acid in instillation 1/3 part of dehydrated alcohol, are made dropping liquid under fully stirring;
(3) by above-mentioned dropping liquid dripping/obtained 60 DEG C of the speed of the 2s instillation the first step are former to be driven in liquid, stir 1h and obtain modified titanium dioxide sol after leaving standstill 20min;
(4) a certain amount of chitosan is added in the acetic acid solution of 1% (volume ratio), at 60 DEG C, stir 1.5h, add after 0.2% glycerine continues to stir 1.5h and obtain chitosan solution;
(5) by adding the obtained modified titanium dioxide sol of the 3rd step in above-mentioned chitosan solution, stirring 2h, often stirring the ultrasonic 15min of 40min;
(6) above-mentioned mixed solution is loaded deaeration in defoamer;
(7) by the mixed solution knifing machine film forming on a glass after above-mentioned deaeration, chitosan/titanium dioxide colloidal sol anti-bacterial packaging film after drying, is obtained.
A kind of chitosan/titanium dioxide colloidal sol antimicrobial packaging membrane preparation method that the present invention proposes, respectively by tetrabutyl titanate, Glacial acetic acid and silane coupling agent (KH570) slowly instill in 2/3 part of dehydrated alcohol, make after abundant stirring and formerly drive liquid, again deionized water and hydrochloric acid are instilled in 1/3 part of dehydrated alcohol under fully stirring, make dropping liquid, afterwards by it dripping/speed of 2s instills 60 DEG C and formerly drives in liquid, stir 1h and obtain modified titanium dioxide sol after standing 20min, modified TiO 2 sol is added in the chitosan acetic acid solution containing 0.2% glycerine and stir, carry out deaeration afterwards, knifing obtains chitosan/titanium dioxide colloidal sol anti-bacterial packaging film.
In one embodiment of the present of invention, first respectively by 1mol tetrabutyl titanate, 1.5mol Glacial acetic acid and silane coupling agent (KH570) slowly instillation 12mol dehydrated alcohol, make after fully stirring and formerly drive liquid; Respectively 2mol deionized water and 0.26mol hydrochloric acid are instilled in 6mol dehydrated alcohol under fully stirring again, make dropping liquid; Afterwards by above-mentioned dropping liquid dripping/obtained 60 DEG C of the speed of the 2s instillation the first step are former to be driven in liquid, stir 1h and obtain modified titanium dioxide sol after leaving standstill 20min; Separately get 3g chitosan to add in the 100ml acetic acid solution of 1% (volume ratio), at 60 DEG C, stir 1.5h, then obtain chitosan solution after adding 0.2ml glycerine continuation stirring 1.5h; Afterwards the modified titanium dioxide sol of 0.09g is added in chitosan solution, stir 2h, often stir the ultrasonic 15min of 40min; Above-mentioned mixed solution is loaded deaeration 30min in defoamer, pours knifing machine into afterwards, on a glass film forming, finally put into 40 DEG C of loft drier, after 24h, obtain the chitosan/titanium dioxide colloidal sol anti-bacterial packaging film of certain specification.
These are only preferred embodiment of the present invention, but scope of the invention process is not limited.
Claims (1)
1. a chitosan/titanium dioxide colloidal sol antimicrobial packaging membrane preparation method, comprises the following steps:
(1) respectively by tetrabutyl titanate, Glacial acetic acid and silane coupling agent (KH570) slowly instillation 2/3 part of dehydrated alcohol, make after fully stirring and formerly drive liquid;
(2) respectively deionized water and hydrochloric acid in instillation 1/3 part of dehydrated alcohol, are made dropping liquid under fully stirring;
(3) by above-mentioned dropping liquid dripping/obtained 60 DEG C of the speed of the 2s instillation the first step are former to be driven in liquid, stir 1h and obtain modified titanium dioxide sol after leaving standstill 20min;
(4) a certain amount of chitosan is added in the acetic acid solution of 1% (volume ratio), at 60 DEG C, stir 1.5h, add after 0.2% glycerine continues to stir 1.5h and obtain chitosan solution;
(5) by adding the obtained modified titanium dioxide sol of the 3rd step in above-mentioned chitosan solution, stirring 2h, often stirring the ultrasonic 15min of 40min;
(6) above-mentioned mixed solution is loaded deaeration in defoamer;
(7) by the mixed solution knifing machine film forming on a glass after above-mentioned deaeration, chitosan/titanium dioxide colloidal sol anti-bacterial packaging film after drying, is obtained.
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| CN201410817699.0A CN104479155A (en) | 2014-12-26 | 2014-12-26 | Preparation method of chitosan/titanium dioxide sol antibacterialpackaging film |
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| CN201410817699.0A CN104479155A (en) | 2014-12-26 | 2014-12-26 | Preparation method of chitosan/titanium dioxide sol antibacterialpackaging film |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105315477A (en) * | 2015-12-01 | 2016-02-10 | 仇颖超 | Preparation method of boron fiber modified chitosan degradable film |
| CN105385248A (en) * | 2015-10-30 | 2016-03-09 | 三棵树涂料股份有限公司 | Preparation method of chitosan-supported titanium dioxide finish coating |
| CN105901015A (en) * | 2016-05-06 | 2016-08-31 | 陈昌 | Antibacterial metal oxide composite material and preparation method thereof |
| CN107022053A (en) * | 2017-04-20 | 2017-08-08 | 安徽春辉仪表线缆集团有限公司 | A kind of epoxidation cage-type silsesquioxane/titanium dioxide grafted propylene nitrile age resister and preparation method thereof |
| CN108653799A (en) * | 2018-05-05 | 2018-10-16 | 东莞市联洲知识产权运营管理有限公司 | A kind of preparation method of hydrophilic antibiotic silicon rubber medical dressing |
| CN108914388A (en) * | 2018-08-15 | 2018-11-30 | 马鞍山卓凡新材料科技有限公司 | A kind of high-strength composite nonwoven with bacteriostasis |
| CN109422888A (en) * | 2017-08-23 | 2019-03-05 | 张家港市六福新材料科技有限公司 | A kind of preparation method of chitosan-titanium dioxide composite film |
| CN112080941A (en) * | 2020-08-31 | 2020-12-15 | 中国科学院地球环境研究所 | Preparation method of antibacterial and antiviral titanium dioxide/chitosan melt-blown fabric |
| CN112812402A (en) * | 2020-12-31 | 2021-05-18 | 浙江省农业科学院 | Anti-fog and anti-bacterial preservative film for fresh-cut fruits and vegetables and preparation method thereof |
| CN113057177A (en) * | 2021-03-31 | 2021-07-02 | 乐山师范学院 | Preparation method of nano-modified titanium dioxide-chitosan-curcumin antibacterial compound |
| CN113248812A (en) * | 2021-05-06 | 2021-08-13 | 金华市伸华包装材料有限公司 | Polyethylene base material packaging film and preparation method thereof |
| CN114507017A (en) * | 2022-03-16 | 2022-05-17 | 福耀玻璃工业集团股份有限公司 | Coating liquid, glass and super-isolation antibacterial laminated glass |
| CN116463848A (en) * | 2023-03-15 | 2023-07-21 | 南通大学 | Preparation method of super-absorbent antibacterial viscose medical dressing |
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| CN103408776A (en) * | 2013-08-23 | 2013-11-27 | 东北林业大学 | Preparation method of antibacterial and fresh-keeping composite packaging film |
| CN104231334A (en) * | 2014-09-23 | 2014-12-24 | 南京工程学院 | Degradable packaging film with antibacterial effect and preparation method thereof |
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| CN103408776A (en) * | 2013-08-23 | 2013-11-27 | 东北林业大学 | Preparation method of antibacterial and fresh-keeping composite packaging film |
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Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105385248A (en) * | 2015-10-30 | 2016-03-09 | 三棵树涂料股份有限公司 | Preparation method of chitosan-supported titanium dioxide finish coating |
| CN105385248B (en) * | 2015-10-30 | 2017-05-24 | 三棵树涂料股份有限公司 | Preparation method of chitosan-supported titanium dioxide finish coating |
| CN105315477A (en) * | 2015-12-01 | 2016-02-10 | 仇颖超 | Preparation method of boron fiber modified chitosan degradable film |
| CN105901015A (en) * | 2016-05-06 | 2016-08-31 | 陈昌 | Antibacterial metal oxide composite material and preparation method thereof |
| CN105901015B (en) * | 2016-05-06 | 2018-05-11 | 徐海军 | A kind of antibacterial metal oxide composite and preparation method thereof |
| CN107022053A (en) * | 2017-04-20 | 2017-08-08 | 安徽春辉仪表线缆集团有限公司 | A kind of epoxidation cage-type silsesquioxane/titanium dioxide grafted propylene nitrile age resister and preparation method thereof |
| CN109422888A (en) * | 2017-08-23 | 2019-03-05 | 张家港市六福新材料科技有限公司 | A kind of preparation method of chitosan-titanium dioxide composite film |
| CN108653799A (en) * | 2018-05-05 | 2018-10-16 | 东莞市联洲知识产权运营管理有限公司 | A kind of preparation method of hydrophilic antibiotic silicon rubber medical dressing |
| CN108653799B (en) * | 2018-05-05 | 2021-11-19 | 唐山尚创医疗科技有限公司 | Preparation method of hydrophilic antibacterial silicone rubber medical dressing |
| CN108914388A (en) * | 2018-08-15 | 2018-11-30 | 马鞍山卓凡新材料科技有限公司 | A kind of high-strength composite nonwoven with bacteriostasis |
| CN112080941A (en) * | 2020-08-31 | 2020-12-15 | 中国科学院地球环境研究所 | Preparation method of antibacterial and antiviral titanium dioxide/chitosan melt-blown fabric |
| CN112812402A (en) * | 2020-12-31 | 2021-05-18 | 浙江省农业科学院 | Anti-fog and anti-bacterial preservative film for fresh-cut fruits and vegetables and preparation method thereof |
| CN113057177A (en) * | 2021-03-31 | 2021-07-02 | 乐山师范学院 | Preparation method of nano-modified titanium dioxide-chitosan-curcumin antibacterial compound |
| CN113248812A (en) * | 2021-05-06 | 2021-08-13 | 金华市伸华包装材料有限公司 | Polyethylene base material packaging film and preparation method thereof |
| CN114507017A (en) * | 2022-03-16 | 2022-05-17 | 福耀玻璃工业集团股份有限公司 | Coating liquid, glass and super-isolation antibacterial laminated glass |
| CN116463848A (en) * | 2023-03-15 | 2023-07-21 | 南通大学 | Preparation method of super-absorbent antibacterial viscose medical dressing |
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