CN101559917A - Preparation method of nano multifunctional assistant and application thereof - Google Patents
Preparation method of nano multifunctional assistant and application thereof Download PDFInfo
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- CN101559917A CN101559917A CNA2009100279964A CN200910027996A CN101559917A CN 101559917 A CN101559917 A CN 101559917A CN A2009100279964 A CNA2009100279964 A CN A2009100279964A CN 200910027996 A CN200910027996 A CN 200910027996A CN 101559917 A CN101559917 A CN 101559917A
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Abstract
The invention relates to a preparation method of a nano multifunctional assistant and an application thereof. The method comprises the steps of (1) preparing nano-scale titanium dioxide, zinc oxide, magnesium hydroxide and aluminum hydroxide respectively; (2) mixing materials according to a certain proportion, adding deionized water, stirring to prepare slurry with the concentration of 40 percent-60 percent, and carrying out the modification to obtain modified slurry; (3) adding deionized water to dilute to the concentration of 10 percent-20 percent, pouring 2-6kg of nano silver-silicon compound and a dispersant in a kettle and stirring to react; (4) slowly dripping 6-12kg of fluorine-containing resin in the kettle under specific conditions, adding a coupling agent and the dispersant to react, keeping the temperature for 50-250 minutes and finally cooling and discharging. The product produced by the method has a plurality of functions of flame-retardant, anti-bacteria, anti-fungus, anti-water, anti-oil, anti-fouling and the like. The prepared nano multifunctional assistant can be applied in a variety of textiles.
Description
Technical field
The present invention relates to a kind of preparation method and application thereof of nano multifunctional assistant.
Background technology
At present, the nanocrystal compound that occurs on the market substantially all is the sterilization auxiliary agent of simple function, and is extensively applied to compound with materials such as resins, coating, is made into products such as nano-antibacterial resin composite materials or nano composite antibacterial coating.But along with the raising of people's living standard, the material of function singleness: as sterilization material; Anti-fungus material; Waterproof, grease proofing, anti-fouling material can not satisfy the demand in market.In the construction of household or service location, decoration process, the consumer often needs to spend the product that great amount of manpower and material resources remove to select and buy multiple difference in functionality, then goes to realize sterilization, sterilization, mildew-resistant, waterproof, purpose such as grease proofing, antifouling respectively.On the wall fitting of being paid attention to by people day by day, service location particularly, abandon easily aging, damaged and the wallpaper that fades and easily produce escaping gas such as formaldehyde, easy contaminated wall finiss, adopt the pattern stereoeffect good, cost is low, and the wall paper with sterilization, sterilization, mildew-resistant, waterproof, function such as grease proofing, antifouling is the main developing direction in market.
Summary of the invention
The technical problem to be solved in the present invention is: a kind of preparation method of nano multifunctional assistant is provided, based on raw material that produce the domestic market, makes the product of its production have fire-retardant, sterilization, mildew-resistant, waterproof, multiple function such as grease proofing, antifouling.
The present invention realizes that the technical scheme that its purpose adopts is: a kind of preparation method of nano multifunctional assistant is characterized in that being made up of following steps: (1) prepares Nano titanium dioxide, 4.5-5.5kg Nano-class zinc oxide, the nanometric magnesium hydroxide of 14-16kg and the nanoscale aluminium hydroxide of 14-16kg of 14-15kg respectively; The titanium dioxide granule particle diameter is below 10 nanometers;
(2) above-mentioned material is mixed and made into composite nano-powder, adds in the reactor, add deionized water and stirring and make the slurry that concentration is 40%-60%, and utilize modifier that slurry is carried out modification and handle and obtain modified slurry;
(3) taking out modified slurry drops in another reactor, it is 10%-20% that the interpolation deionized water and stirring is diluted to concentration, heat temperature raising is controlled at 45-55 ℃ with reactor temperature, in still, drop into the Nano Silver silicon compound of 2-6kg and the dispersant of 0.2-0.5kg, after fully stirring, heat temperature raising makes temperature in the kettle to 70-90 ℃;
(4) after the intensification, adjust PH=5-8 in the still, slowly drip the fluorine resin of 6-12kg in still, the coupling agent of adding 0.2-1kg and the dispersant of 0.2-1kg react, and keep said temperature 50-250 minute, are cooled to 30-45 ℃ of discharging at last.
In the above-mentioned preparation process, modification in the described step (2) is handled and is specially: after adding deionized water and stirring temperature in the kettle is risen to 50-60 ℃, the surface modification auxiliary agent stirring reaction that adds 0.2-0.5kg is after 20-40 minute, drip polyoxyethylene nonylphenol ether-(the 4-10 series) of 0.2-0.5kg metatitanic acid coupling agent and 0.2-0.5kg successively, be warming up to 70-80 ℃ then, after stirring reaction 30-150 minute, naturally cool to 20-40 ℃ and enter next step.
Above-mentioned surface modification auxiliary agent is emulsifying agent TX series or inorganic phosphate.
Coupling agent in the above-mentioned steps (3) is an aluminate coupling agent.
Above-mentioned Nano Silver silicon compound adopts precipitation method preparation among the present invention, be specially: in concentration is to add nanometer SiO2 in 5% the AgNO3 solution, be heated to boiling about 80 ℃, remove the upper strata by washing, then add dispersant, and the slurries beds of precipitation are heated to 60-90 ℃ of reaction 60-300 minute, oven dry forms.
The mix proportion scheme of above-mentioned material of the present invention, fully in conjunction with the market material source, by above-mentioned special process, existing raw material effective fusion such as Nano titanium dioxide, zinc oxide, magnesium hydroxide, aluminium hydroxide, silver-colored silicon compound and fluorine resin are in the same place, utilize the antibacterial functions of the following titanium dioxide of 10 nanometers itself and the basic principle of photocatalyst, the purpose that reach broad-spectrum sterilization, purifies air; Utilize Nano-class zinc oxide to have the ultraviolet ray of absorption, and can strengthen the function of wearability; Utilize magnesia, aluminium hydroxide as fire retardant and desulfurizing agent, possess environmental protection, Halogen, fire-retardant, press down cigarette, reduce the characteristics of material combustion corrosive gas growing amount; Antibiotic, the antimildew function that utilize silver-colored silicon compound to have can effectively suppress to have danger bacterium, fungi growth breeding, and be applicable to various yarn fabrics; Fluorine resin principal item has polytetrafluoroethylene (PTFE), polytrifluorochloroethylene (PCTFE), ethylene-tetrafluoroethylene copolymer (ETFE), polyvinyl fluoride (PVF), tetrafluoroethylene-perfluoroalkyl vinyl ether copolymer etc., it can be widely used in various fabrics, play waterproof, grease proofing, antifouling effect, feel that simultaneously can abundant fabric.
Another purpose of the present invention is can be applied to various yarn fabrics according to the nano multifunctional assistant that above-mentioned preparation method produces, particularly in the making of wall paper; Top layer in the wall paper and/or inner liner are put into the container that above-mentioned nano multifunctional assistant is housed to be soaked, after handling by oven dry, qualitative etc. then, mode by compound or quilting is made into wall paper, through the wall paper after the above-mentioned processing, not only pollution-free, wear-resisting durable, color, pattern stereoeffect are good, can satisfying personalized design and the demand of large area pattern, and after the disposable arrangement of fabric, realize antibiotic, mildew-resistant, waterproof, multiple function such as grease proofing, antifouling, fire-retardant simultaneously.
The specific embodiment
Below in conjunction with embodiment technical scheme of the present invention is described further.
Embodiment 1: a kind of preparation method of nano multifunctional assistant, be made up of following steps:
(1) prepares Nano titanium dioxide, 5kg Nano-class zinc oxide, the nanometric magnesium hydroxide of 15kg and the nanoscale aluminium hydroxide of 15kg of 15kg respectively; The titanium dioxide granule particle diameter is 2 nanometers.
(2) above-mentioned material is weighed back the mixing in the adding reactor, add the 50kg deionized water and stirring, rotating speed is 600 rev/mins, stir after 10 minutes, temperature in the kettle is risen to 60 ℃, add the surface modification auxiliary agent phosphate of 0.3kg, fully stirring reaction is after half an hour, drip the emulsifier op-10 of 0.3kg metatitanic acid coupling agent and 0.3kg, emulsifier op-10 is the condensation product of alkyl phenol and oxirane; Be warming up to 75 ℃ then, stir isothermal reaction after 2 hours, naturally cool to 40 ℃ and enter next step.
(3) modified slurry that takes out is dropped in another reactor, it is 20% that the interpolation deionized water and stirring is diluted to concentration, heat temperature raising is controlled at 50 ℃ with reactor temperature, in still, drop into the Nano Silver silicon compound of 5kg and the dispersant of 0.3kg, after fully stirring, heat temperature raising makes temperature in the kettle to 80 ℃.
(4) after the intensification, adjust PH=6 in the still by oxalic acid, slowly drip the fluororesin of 8kg in still, add the aluminate coupling agent of 0.5kg and the dispersant of 0.5kg and react, maintenance said temperature 2 hours is cooled to 40 ℃ of dischargings at last.
The silicon compound of Nano Silver described in the present invention adopts present known precipitation method preparation, simply be described as: in AgNO3 solution, add nanometer SiO2, be heated to boiling about 80 ℃, remove the upper strata by washing, then add dispersant, and the slurries beds of precipitation are heated to 60-90 ℃ of reaction 60-300 minute, oven dry forms.
Fluorine resin among the present invention also is a matured product, principal item has polytetrafluoroethylene (PTFE), polytrifluorochloroethylene (PCTFE), ethylene-tetrafluoroethylene copolymer (ETFE), polyvinyl fluoride (PVF), tetrafluoroethylene-perfluoroalkyl vinyl ether copolymer etc., it can be widely used in various fabrics, play waterproof, grease proofing, antifouling effect, feel that simultaneously can abundant fabric.
Embodiment 2: a kind of preparation method of nano multifunctional assistant, be made up of following steps:
(1) prepares Nano titanium dioxide, 5.5kg Nano-class zinc oxide, the nanometric magnesium hydroxide of 14kg and the nanoscale aluminium hydroxide of 16kg of 14kg respectively; The titanium dioxide granule particle diameter is 5 nanometers.
(2) above-mentioned material is weighed back the mixing in the adding reactor, interpolation deionized water and stirring compound concentration is 45% slurry, speed of agitator is 650 rev/mins, stirs after 12 minutes, and temperature in the kettle is risen to 55 ℃, the surface modification auxiliary agent TX-10 that adds 0.4kg, fully stirring reaction dripped the polyoxyethylene nonylphenol ether-6 of 0.4kg metatitanic acid coupling agent and 0.4kg after 40 minutes, was warming up to 80 ℃ then, stir isothermal reaction after 100 minutes, naturally cool to 30 ℃ and enter next step.
(3) modified slurry that takes out is dropped in another reactor, it is 15% that the interpolation deionized water and stirring is diluted to concentration, heat temperature raising is controlled at 55 ℃ with reactor temperature, in still, drop into the Nano Silver silicon compound of 6kg and the aqueous dispersion of 0.4kg, after fully stirring, heat temperature raising makes temperature in the kettle to 90 ℃.
(4) after the intensification, adjust PH=7 in the still by oxalic acid, slowly drip the fluororesin of 11kg in still, add the aluminate coupling agent of 0.8kg and the dispersant of 0.7kg and react, maintenance said temperature 200 minutes is cooled to 30 ℃ of dischargings at last.
Related dispersant all is an aqueous dispersion among the present invention.
The nano multifunctional assistant of the present invention's preparation can be widely used in various fabrics, the particularly application in the wall paper compound by the multilayer cloth.The cloth of handling through this auxiliary agent dipping, spraying etc., under the situation that does not influence original color and pattern, the wear-resisting durability of all right obvious raising, and realize antibiotic, mildew-resistant, waterproof, multiple function such as grease proofing, antifouling, fire-retardant simultaneously.
Low cost of manufacture of the present invention can realize producing in batches for the manufacturing of multi-functional wall paper, so in the construction of the household of being widely used in or service location, decoration, and be applicable to China fully from economy and resource view consideration.
Claims (6)
1, a kind of preparation method of nano multifunctional assistant is characterized in that being made up of following steps: (1) prepares Nano titanium dioxide, 4.5-5.5kg Nano-class zinc oxide, the nanometric magnesium hydroxide of 14-16kg and the nanoscale aluminium hydroxide of 14-16kg of 14-15kg respectively; The titanium dioxide granule particle diameter is below 10 nanometers;
(2) above-mentioned material is mixed and made into composite nano-powder, adds in the reactor, add deionized water and stirring and make the slurry that concentration is 40%-60%, and utilize modifier that slurry is carried out modification and handle and obtain modified slurry;
(3) taking out modified slurry drops in another reactor, it is 10%-20% that the interpolation deionized water and stirring is diluted to concentration, heat temperature raising is controlled at 45-55 ℃ with reactor temperature, in still, drop into the Nano Silver silicon compound of 2-6kg and the dispersant of 0.2-0.5kg, after fully stirring, heat temperature raising makes temperature in the kettle to 70-90 ℃;
(4) after the intensification, adjust PH=5-8 in the still, slowly drip the fluorine resin of 6-12kg in still, the coupling agent of adding 0.2-1kg and the dispersant of 0.2-1kg react, and keep said temperature 50-250 minute, are cooled to 30-45 ℃ of discharging at last.
2, the preparation method of nano multifunctional assistant according to claim 1, it is characterized in that: the modification in the described step (2) is handled and is specially: after adding deionized water and stirring temperature in the kettle is risen to 50-60 ℃, the surface modification auxiliary agent stirring reaction that adds 0.2-0.5kg is after 20-40 minute, drip polyoxyethylene nonylphenol ether-(the 4-10 series) of 0.2-0.5kg metatitanic acid coupling agent and 0.2-0.5kg successively, be warming up to 70-80 ℃ then, after stirring reaction 30-150 minute, naturally cool to 20-40 ℃ and enter next step.
3, the preparation method of nano multifunctional assistant according to claim 2 is characterized in that described surface modification auxiliary agent is emulsifying agent TX series or inorganic phosphate.
4, the preparation method of nano multifunctional assistant according to claim 1 is characterized in that the coupling agent in the described step (3) is an aluminate coupling agent.
5, the nano multifunctional assistant of preparation method's production as claimed in claim 1 is used in various yarn fabrics.
6, the nano multifunctional assistant of preparation method's production as claimed in claim 1 is used in wall paper.
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Cited By (13)
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| CN102197825A (en) * | 2010-03-23 | 2011-09-28 | 上海克瑞森环保科技有限公司 | Nanosilver antibacterial agent and preparation method thereof |
| CN102199873A (en) * | 2010-03-23 | 2011-09-28 | 上海沪正纳米科技有限公司 | Transparent nano-silver antibiotic finishing agent and preparation method thereof |
| CN102747816A (en) * | 2012-07-19 | 2012-10-24 | 王�华 | Multifunctional wall cloth and manufacturing method thereof |
| CN102771921A (en) * | 2011-05-10 | 2012-11-14 | 北京大华天坛服装有限公司 | Nano photocatalytic clothing material and preparation method thereof |
| CN103200825A (en) * | 2010-11-02 | 2013-07-10 | 印度德里技术研究院 | Blue coloured aqueous dispersion of silver nanoparticles a process for preparation and compositions thereof |
| WO2014078976A1 (en) * | 2012-11-26 | 2014-05-30 | Wu Jinlong | Multi-functional nanoparticle washing tablet |
| CN105220462A (en) * | 2015-10-30 | 2016-01-06 | 朱忠良 | A kind of textile nano function finishing agent and its preparation method and application |
| CN105369602A (en) * | 2014-08-28 | 2016-03-02 | 青岛鑫润土苗木专业合作社 | Antibacterial flame-retardant textile producing method |
| CN105860141A (en) * | 2016-04-26 | 2016-08-17 | 深圳市博赛新材有限公司 | Method for carrying out modification treatment on heat conducting powder fillers and heat conducting fillers |
| CN106938897A (en) * | 2017-04-07 | 2017-07-11 | 佛山市蓝瑞欧特信息服务有限公司 | A kind of antibacterial and mouldproof tile grout and preparation method thereof |
| CN107646895A (en) * | 2017-08-09 | 2018-02-02 | 深圳沃海森科技有限公司 | Bacteriostatic agent of air-conditioning air inlet and preparation method thereof |
| CN107956107A (en) * | 2017-12-15 | 2018-04-24 | 江苏新瑞贝科技股份有限公司 | A kind of preparation method of oil-proofing agent |
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| CN1284834C (en) * | 2004-08-13 | 2006-11-15 | 中国广州分析测试中心 | Nano multifunctional coating additive |
| DE102006019137A1 (en) * | 2005-05-17 | 2007-10-31 | Wolfgang Dr.-Ing. Beck | Coating material for in-mold coating (IMC) based on an amino-functional reaction partner for isocyanates and process for the preparation |
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| CN101117454A (en) * | 2006-08-01 | 2008-02-06 | 天津市振东涂料有限公司 | Method for preparing multifunctional inner wall paint |
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| CN102199873A (en) * | 2010-03-23 | 2011-09-28 | 上海沪正纳米科技有限公司 | Transparent nano-silver antibiotic finishing agent and preparation method thereof |
| CN102199873B (en) * | 2010-03-23 | 2012-09-26 | 上海沪正纳米科技有限公司 | Transparent nano-silver antibiotic finishing agent and preparation method thereof |
| CN102197825A (en) * | 2010-03-23 | 2011-09-28 | 上海克瑞森环保科技有限公司 | Nanosilver antibacterial agent and preparation method thereof |
| CN102197825B (en) * | 2010-03-23 | 2013-01-23 | 上海沪正纳米科技有限公司 | Nanosilver antibacterial agent and preparation method thereof |
| CN103200825A (en) * | 2010-11-02 | 2013-07-10 | 印度德里技术研究院 | Blue coloured aqueous dispersion of silver nanoparticles a process for preparation and compositions thereof |
| CN103200825B (en) * | 2010-11-02 | 2015-08-12 | 印度德里技术研究院 | Blue water-based dispersion, its preparation method and the composition thereof of silver nano-grain |
| CN102771921B (en) * | 2011-05-10 | 2015-05-13 | 北京大华天坛服装有限公司 | Nano photocatalytic clothing material and preparation method thereof |
| CN102771921A (en) * | 2011-05-10 | 2012-11-14 | 北京大华天坛服装有限公司 | Nano photocatalytic clothing material and preparation method thereof |
| CN102747816A (en) * | 2012-07-19 | 2012-10-24 | 王�华 | Multifunctional wall cloth and manufacturing method thereof |
| WO2014078976A1 (en) * | 2012-11-26 | 2014-05-30 | Wu Jinlong | Multi-functional nanoparticle washing tablet |
| CN105369602A (en) * | 2014-08-28 | 2016-03-02 | 青岛鑫润土苗木专业合作社 | Antibacterial flame-retardant textile producing method |
| CN105220462A (en) * | 2015-10-30 | 2016-01-06 | 朱忠良 | A kind of textile nano function finishing agent and its preparation method and application |
| CN105860141A (en) * | 2016-04-26 | 2016-08-17 | 深圳市博赛新材有限公司 | Method for carrying out modification treatment on heat conducting powder fillers and heat conducting fillers |
| CN106938897A (en) * | 2017-04-07 | 2017-07-11 | 佛山市蓝瑞欧特信息服务有限公司 | A kind of antibacterial and mouldproof tile grout and preparation method thereof |
| CN107646895A (en) * | 2017-08-09 | 2018-02-02 | 深圳沃海森科技有限公司 | Bacteriostatic agent of air-conditioning air inlet and preparation method thereof |
| CN107956107A (en) * | 2017-12-15 | 2018-04-24 | 江苏新瑞贝科技股份有限公司 | A kind of preparation method of oil-proofing agent |
| CN109439030A (en) * | 2018-10-15 | 2019-03-08 | 滕丽阳 | A kind of pipeline antimicrobial coating and preparation method thereof |
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Effective date of registration: 20200316 Address after: No.158, Taidong Road, Zou District, Zhonglou District, Changzhou City, Jiangsu Province Patentee after: Jiangsu Changtai Nanomaterials Co.,Ltd. Address before: Bu Yitai village in Wujin District of Changzhou city of Jiangsu Province in 213000 Patentee before: Wu Jinlong |
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