CN100547044C - The preparation method of aqueous polyurethane and organosilicon, organofluorine copllymerized water-proof air-moisture-permeable antibacterial coating adhesive - Google Patents
The preparation method of aqueous polyurethane and organosilicon, organofluorine copllymerized water-proof air-moisture-permeable antibacterial coating adhesive Download PDFInfo
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- CN100547044C CN100547044C CNB2006100960374A CN200610096037A CN100547044C CN 100547044 C CN100547044 C CN 100547044C CN B2006100960374 A CNB2006100960374 A CN B2006100960374A CN 200610096037 A CN200610096037 A CN 200610096037A CN 100547044 C CN100547044 C CN 100547044C
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Abstract
The present invention relates to the preparation method of a kind of aqueous polyurethane and organosilicon, organofluorine copllymerized water-proof air-moisture-permeable antibacterial coating adhesive.This method is with vulcabond and diatomic alcohol compounds, alkane silicol, hydroxyl fluorosilicon oil, dimethylol propionic acid reaction, produces end group to be-performed polymer of NCO, uses 1 then, the 4-chain expansion of succinic acid.Regulate the pH value to neutrality with amine at last, add the deionized water high-speed stirring that contains antiseptic-germicide, after adding water and regulating viscosity, promptly obtain water-proof air-moisture-permeable antibacterial adhesive coating.Coat the surface of fabric, water-proof air-moisture-permeable not only, also to common bacterium, mould has very strong germicidal action.
Description
Technical field
The present invention relates to a kind of polyurethane water-proof air-moisture-permeable coating adhesive, be specifically related to the preparation method of a kind of aqueous polyurethane and organosilicon, organofluorine copllymerized water-proof air-moisture-permeable antibacterial coating adhesive.Belong to field of chemical technology.
Background technology
Polyurethane water-proof air-moisture-permeable coating adhesive can be given the coating waterproof in weaving, the widespread use of leather field, saturating wet special efficacy.At present, the coating adhesive of urethane is emitted a large amount of deleterious organic solvents, not environmental protection of the utmost point still based on oiliness urethane when producing and be coated with.And novel water-base polyurethane material is dispersion medium because of using nontoxic water, and the utmost point has market potential.But aqueous coating glue is more vulnerable to the infringement of bacterium.
Summary of the invention
The objective of the invention is to overcome above-mentioned deficiency, a kind of high water-proof air-moisture-permeable performance that not only has is provided, and the preparation method of the anti-aqueous polyurethane that kills effect and organosilicon, organofluorine copllymerized water-proof air-moisture-permeable coating adhesive can be arranged most of bacteriums.
The object of the present invention is achieved like this: the preparation method of a kind of aqueous polyurethane and organosilicon, organofluorine copllymerized water-proof air-moisture-permeable antibacterial coating adhesive, it is characterized in that it is with vulcabond and diatomic alcohol compounds, alkane silicol, hydroxyl fluorosilicon oil, dimethylol propionic acid reaction, produce end group to be-performed polymer of NCO; Use 1 then, the 4-chain expansion of succinic acid; Regulate the pH value to neutrality with amine at last, add the deionized water high-speed stirring that contains antiseptic-germicide, after adding water and regulating viscosity, promptly obtain water-proof air-moisture-permeable antibacterial adhesive coating.
Concrete technology of the present invention is: add diatomic alcohol compounds in reactor, alkane silicol and hydroxyl fluorosilicon oil, 100-120 ℃ vacuumized 1.5～2.5 hours, add dimethylol propionic acid, after the dissolving, cool to 70-80 ℃, add vulcabond and catalyzer dibutyl tin laurate (DBTDL), insulated and stirred 90-100min, be cooled to 60-70 ℃, add 1,4-butyleneglycol, insulated and stirred 40-50min, be cooled to 15-25 ℃, add the amine neutralization, add the deionized water that contains antiseptic-germicide, high-speed stirring, after adding water adjusting viscosity, promptly obtain water-proof air-moisture-permeable antibacterial adhesive coating.
Each material of the present invention is to react according to following proportioning:
-NCO :-OH=3-4: 1, wherein-NCO represents isocyanate group;
The mol ratio of alkane silicol, hydroxyl fluorosilicon oil and diatomic alcohol compounds is: the alkane silicol: the hydroxyl fluorosilicon oil: diatomic alcohol compounds=1: 0.4～0.6: 10～12;
The mol ratio of dimethylol propionic acid and diatomic alcohol compounds is: dimethylol propionic acid: diatomic alcohol compounds=1: 12～15;
1, the mol ratio of 4-butyleneglycol and diatomic alcohol compounds is: 1, and 4-butyleneglycol: diatomic alcohol compounds 1: 12～15.
Diatomic alcohol compounds of the present invention is polyoxyethylene glycol or polypropylene glycol;
Alkane silicol of the present invention is dihydroxy ethyl silane or dihydroxymethyl silane;
Amine of the present invention is quadrol or hexanediamine;
Vulcabond of the present invention is an isophorone diisocyanate (IPDI), 1,6-hexamethylene diisocyanate (HDI), tolylene diisocyanate (TDI) or diphenylmethanediisocyanate (MDI);
Molecular weight polyethylene glycol of the present invention is 800-1200; The polypropylene glycol molecular weight is 800-1200; The number-average molecular weight of water-proof air-moisture-permeable antibacterial adhesive coating is 10000-20000, and viscosity is 800-1000cps;
Antiseptic-germicide of the present invention is inorganic carrying silver antimicrobials, and median size is below the 5 μ m.
The present invention not only has high water-proof air-moisture-permeable performance, and can the anti-effect of killing be arranged to most of bacteriums.The present invention coats the surface of fabric, water-proof air-moisture-permeable not only, and also to common bacterium, mould has very strong germicidal action.
Embodiment
Embodiment 1:
Adding 120g polyoxyethylene glycol in flask (molecular weight: 1000), 8g dihydroxymethyl silane, 4g hydroxyl fluorosilicon oil, 100 ℃ vacuumized 2 hours, added the 8g dimethylol propionic acid, after the dissolving, cool to 72 ℃, add 28gHDI and 6 catalyzer DBTDL, insulated and stirred 90min, be cooled to 63 ℃, add 7.6g1, the 4-butyleneglycol, insulated and stirred 40min is cooled to 25 ℃, adds quadrol 10g, the water 228g that is dispersed with 6g and does not have airborne silver-colored silicon oxide is added fast, high-speed stirring 1 hour, product.Detect anti-microbial property (pressing JIS Z2801:2000 standard) after being coated with, its anti-microbial activity value is greater than 4.0.
Embodiment 2:
Adding 120g polypropylene glycol in flask (molecular weight: 1000), 10g dihydroxy ethyl silane, 5g hydroxyl fluorosilicon oil, 100 ℃ vacuumized 2 hours, added the 7.8g dimethylol propionic acid, after the dissolving, cool to 75 ℃, add 30gIPDI and 6 catalyzer DBTDL, insulated and stirred 90min.Be cooled to 60 ℃, adding 7.5g1, the 4-butyleneglycol, insulated and stirred 40min is cooled to 20 ℃, adds quadrol 9g, does not have the water 230 grams adding fast of airborne silver-colored titanium oxide with being dispersed with 6g, and high-speed stirring 1 hour gets product.Detect anti-microbial property (pressing JIS Z2801:2000 standard) after being coated with, its anti-microbial activity value is greater than 4.0.
Embodiment 3:
Adding 120g polyoxyethylene glycol in flask (molecular weight: 800), 9g dihydroxymethyl silane, 4.5g hydroxyl fluorosilicon oil, 100 ℃ vacuumized 2 hours, added the 9g dimethylol propionic acid, after the dissolving, cool to 72 ℃, add 28gHDI and 6 catalyzer DBTDL, insulated and stirred 90min.Be cooled to 65 ℃, add 8.0g1, the 4-butyleneglycol, insulated and stirred 40min is cooled to 20 ℃, adds hexanediamine 10g, the water 230g that is dispersed with 8g and does not have airborne silver-colored silicon oxide is added fast, high-speed stirring 1 hour, product.Detect anti-microbial property (pressing JIS Z2801:2000 standard) after being coated with, its anti-microbial activity value is greater than 4.7.
Claims (8)
1, the preparation method of a kind of aqueous polyurethane and organosilicon, organofluorine copllymerized water-proof air-moisture-permeable antibacterial coating adhesive, it is characterized in that it is with vulcabond and diatomic alcohol compounds, alkane silicol, hydroxyl fluorosilicon oil, dimethylol propionic acid reaction, produce end group to be-performed polymer of NCO; Use 1 then, the 4-chain expansion of succinic acid; Regulate the pH value to neutrality with amine at last, add the deionized water high-speed stirring that contains antiseptic-germicide, after adding water and regulating viscosity, promptly obtain water-proof air-moisture-permeable antibacterial adhesive coating,
Concrete technology is: add diatomic alcohol compounds, alkane silicol and hydroxyl fluorosilicon oil in reactor, 100-120 ℃ vacuumized 1.5～2.5 hours, add dimethylol propionic acid, after the dissolving, cool to 70-80 ℃, add vulcabond and catalyzer dibutyl tin laurate, insulated and stirred 90-100min, be cooled to 60-70 ℃, add 1,4-butyleneglycol, insulated and stirred 40-50min, be cooled to 15-25 ℃, add the amine neutralization, add the deionized water that contains antiseptic-germicide, high-speed stirring, after adding water adjusting viscosity, promptly obtain water-proof air-moisture-permeable antibacterial adhesive coating.
2, the preparation method of a kind of aqueous polyurethane according to claim 1 and organosilicon, organofluorine copllymerized water-proof air-moisture-permeable antibacterial coating adhesive is characterized in that each material is to react according to following proportioning:
-NCO :-OH=3-4: 1, wherein-NCO represents isocyanate group;
The mol ratio of alkane silicol, hydroxyl fluorosilicon oil and diatomic alcohol compounds is: the alkane silicol: the hydroxyl fluorosilicon oil: diatomic alcohol compounds=1: 0.4～0.6: 10～12;
The mol ratio of dimethylol propionic acid and diatomic alcohol compounds is: dimethylol propionic acid: diatomic alcohol compounds=1: 12～15;
1, the mol ratio of 4-butyleneglycol and polyol compound is: 1, and 4-butyleneglycol: polyol compound 1: 12～15.
3, the preparation method of a kind of aqueous polyurethane according to claim 2 and organosilicon, organofluorine copllymerized water-proof air-moisture-permeable antibacterial coating adhesive is characterized in that described diatomic alcohol compounds is polyoxyethylene glycol or polypropylene glycol.
4, the preparation method of a kind of aqueous polyurethane according to claim 2 and organosilicon, organofluorine copllymerized water-proof air-moisture-permeable antibacterial coating adhesive is characterized in that described alkane silicol is dihydroxy ethyl silane or dihydroxymethyl silane.
5, the preparation method of a kind of aqueous polyurethane according to claim 2 and organosilicon, organofluorine copllymerized water-proof air-moisture-permeable antibacterial coating adhesive is characterized in that described amine is quadrol or hexanediamine.
6, the preparation method of a kind of aqueous polyurethane according to claim 2 and organosilicon, organofluorine copllymerized water-proof air-moisture-permeable antibacterial coating adhesive, it is characterized in that described vulcabond is an isophorone diisocyanate, 1,6-hexamethylene diisocyanate, tolylene diisocyanate or diphenylmethanediisocyanate.
7, the preparation method of a kind of aqueous polyurethane according to claim 3 and organosilicon, organofluorine copllymerized water-proof air-moisture-permeable antibacterial coating adhesive is characterized in that described molecular weight polyethylene glycol is 800-1200; The polypropylene glycol molecular weight is 800-1200; The number-average molecular weight of water-proof air-moisture-permeable antibacterial adhesive coating is 10000-20000, and viscosity is 800-1000cps.
8, the preparation method of a kind of aqueous polyurethane according to claim 2 and organosilicon, organofluorine copllymerized water-proof air-moisture-permeable antibacterial coating adhesive is characterized in that described antiseptic-germicide is inorganic carrying silver antimicrobials, and median size is below the 5 μ m.
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| CNB2006100960374A CN100547044C (en) | 2006-09-14 | 2006-09-14 | The preparation method of aqueous polyurethane and organosilicon, organofluorine copllymerized water-proof air-moisture-permeable antibacterial coating adhesive |
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| CNB2006100960374A CN100547044C (en) | 2006-09-14 | 2006-09-14 | The preparation method of aqueous polyurethane and organosilicon, organofluorine copllymerized water-proof air-moisture-permeable antibacterial coating adhesive |
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| CN100547044C true CN100547044C (en) | 2009-10-07 |
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| CN101157822B (en) * | 2007-09-20 | 2010-06-16 | 华明扬 | Method for preparing casing fabric wave-absorption coating glue |
| CN101161747B (en) * | 2007-09-20 | 2010-06-02 | 华明扬 | Preparation method of polycaprolactone siloxane aqueous polyurethane paint for woodenware |
| CN100560673C (en) * | 2007-09-20 | 2009-11-18 | 华明扬 | The preparation method of environment-friendly type wear-resisting weather-proof brightener used for artificial leather |
| CN101186798B (en) * | 2007-11-08 | 2012-03-28 | 江阴市诺科科技有限公司 | Method for preparing water polyurethane siloxane ventilating coating adhesive used for automobiles and shoes |
| CN102505491A (en) * | 2011-11-01 | 2012-06-20 | 吴江市北厍盛源纺织品助剂厂 | Synthesizing method of polyurethane-modified organosilicon antimicrobial auxiliary agent |
| CN102418277A (en) * | 2011-11-01 | 2012-04-18 | 吴江市北厍盛源纺织品助剂厂 | Method for preparing antibacterial polyurethane textile finishing liquid |
| CN103554411B (en) * | 2013-10-19 | 2016-01-06 | 泉州源利鞋材有限公司 | A kind of preparation method of automatic moulding shoe-pad |
| CN103554426B (en) * | 2013-10-29 | 2015-08-26 | 上海汇得化工有限公司 | The burnt discoloration wet polyurethane resin that a kind of hydrolytic resistance is good |
| CN104499295A (en) * | 2014-11-17 | 2015-04-08 | 浙江梦娜袜业股份有限公司 | Water, oil and dirty repellent finishing agent for silk stockings and silk stocking production technology |
| CN105504194B (en) * | 2015-12-28 | 2019-01-01 | 安徽安大华泰新材料有限公司 | A kind of preparation method of hydrophobic thermal polyurethane resin |
| CN106480724B (en) * | 2016-11-16 | 2018-08-24 | 丹东优耐特纺织品有限公司 | The processing method of anti-aging, cold-resistant, antibacterial, high moisture-inhibiting raincoat fabric |
| CN107190350A (en) * | 2017-05-18 | 2017-09-22 | 颍上县鸿达纺织有限公司 | A kind of uvioresistant waterproof spinning of environmental sanitation fabric |
| CN107722218A (en) * | 2017-10-16 | 2018-02-23 | 德清舒华泡沫座椅有限公司 | A kind of organic fluorinated silicone resin modified polyurethane foam |
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| CN1510065A (en) * | 2002-12-25 | 2004-07-07 | 揭阳市天银化工实业有限公司 | Fatty polyurethane aqueous dispersion |
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| CN1510065A (en) * | 2002-12-25 | 2004-07-07 | 揭阳市天银化工实业有限公司 | Fatty polyurethane aqueous dispersion |
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Effective date of registration: 20120119 Address after: 214421 Jiangsu city in Jiangyin Province town of Hua Industrial Zone Patentee after: Jiangyin Ruco Technology Co., Ltd. Address before: 214421 Jiangsu city in Jiangyin Province town of Hua Qin Feng Road No. 53 Patentee before: Hua Mingyang |
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