CN102677469A - Ultramicron three-proofing finishing agent and preparation method thereof - Google Patents
Ultramicron three-proofing finishing agent and preparation method thereof Download PDFInfo
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- CN102677469A CN102677469A CN2012101840676A CN201210184067A CN102677469A CN 102677469 A CN102677469 A CN 102677469A CN 2012101840676 A CN2012101840676 A CN 2012101840676A CN 201210184067 A CN201210184067 A CN 201210184067A CN 102677469 A CN102677469 A CN 102677469A
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Abstract
The invention discloses an ultramicron three-proofing finishing agent and a preparation method thereof. The ultramicron three-proofing finishing agent is prepared in a way that 3 to 35 percent of perfluor hexyl acrylate, 2 to 45 percent of acrylate copolymer, 0.5 to 10 percent of N-methyl acrylamide, 0.1 to 5 percent of surfactant, 0.1 to 5 percent of V-50 initiating agent, 2 to 15 percent of acetic acid, 40 to 70 percent deionized water are selected as raw materials and are combined; and a blend range with better comprehensive performance and lower cost is provided so as to give full play to all the components. Through effective selection and proportional combination of the components, the three-proofing finishing agent provided by the invention is enabled to have the advantages of innocuity, harmlessness, good wash fastness, excellent air permeability, environmental friendliness, simple process, low cost and the like and perfectly meet market demands.
Description
Technical field
The present invention relates to the waterproofing agent technical field, particularly a kind of ultramicron three-proof finishing agent.
Background technology
In the world, no matter technically the water-proof aagent that relevant textiles, clothes are used with by the monopolization of international major company,, from raw material, all receives foreign enterprise control always, carries out the discrimination of technology and product.And China always is weaving, printing and dyeing big country, but in fabric post processing field, special fabric refuse water, oil-refusing finishing agent is technical; Be in backward state, be that patent and technology are the monopolization of external major company, on the other hand all the time on the one hand; China's research and development in this respect drop into relative deficiency, and product sold is the composite at home sale of external product emulsion, wherein fluorine-containing fabric three-proof finishing agent in the market; 2010 annual requirements are about 18000 tons; The per kilogram price does not wait to hundreds of unit from dozens of yuan, and annual increase in demand adds 10%-20% approximately, and market prospects are very wide.
Moreover because all waterproof that has relevant PFOS, a PFOA composition of European Union member countries, refuse oil, soil-releasing finishing agent, in the chemicals of statutory regulations, being higher than 0.005% (5oppm) must not produce and use.European Union member countries make China's textile industry form enormous pressure and raw materials market vacancy after banning use of the relevant chemicals of PFOS and PFDA, APEO.Therefore the task of top priority is to research and develop the new three-proof finishing agent that does not contain PFOS and PFOA, to break technology barriers.
Summary of the invention
The present invention has overcome the deficiency that exists in the above-mentioned prior art, and the three-proof finishing agent of a kind of raw material nontoxic, harmless, waterproof simple, with low cost, grease proofing, decontaminable environmental protection is provided.
Technical scheme of the present invention realizes in the following manner:
A kind of ultramicron three-proof finishing agent, this finishing agent are that the feedstock production by weight components obtains:
As preferably, described surfactant is that the feedstock production by following weight portion obtains: isomerous tridecanol ether 30～40%, OTAC 25～45%, AEO 25～40%.
As preferably, acrylic resin is selected from following monomer by at least two kinds and forms: (methyl) methyl acrylate, (methyl) octadecyl acrylate, (methyl) tetradecyl acrylate; (methyl) butyl acrylate, (methyl) isobutyl acrylate, (methyl) ethyl acrylate; Styrene, butyl acrylate, propyl acrylate; Tetradecyl acrylate, octadecyl acrylate, acrylic acid and their combinations.
As preferably, described acrylic resin is selected from following monomer by at least two kinds and forms: (methyl) methyl acrylate, (methyl) octadecyl acrylate, butyl acrylate and their combination.
As preferably, described acetate is glacial acetic acid.
A kind of preparation method of ultramicron three-proof finishing agent is that the raw material by above-mentioned weight portion prepares through following steps:
(1) under the normal temperature with first monomer, second monomer, the 3rd monomer, surfactant, acetate, deionized water are added to reaction cylinder and stir;
(2) 1/3 said mixture material is poured in the controllable temperature agitated reactor stirred; Heat up and add 1/3 V-50 initator 55 ℃ the time again; Insulation reaction 40～50 minutes is warming up to 75 ℃-85 ℃ then, then remaining 2/3 said mixture material and 2/3 V-50 initator is poured into; Let the abundant catalytic polymerization of initator like this, more help each component generation complete reaction.
(3) nitrogen injection reacted 5～6 hours again in aforesaid reaction vessel; Can obtain uniform particulate mixed material; Can guarantee that under the environment of nitrogen purification degrees makes reaction more evenly lasting, can see this moment be band blue light milky white liquid in the reactant and also quality even, fine and smooth.Sample detects test through the auspicious group in sky, Shanghai and meets environmental protection standard fully.(query report number: SHAH00295233, inquiry phone: 8009991338).
(4), last cold filtration, packing make the emulsion finished product of even particle.
Adopted the invention has the beneficial effects as follows of technique scheme:
The present invention selects perfluoro hexyl acrylic acid ester, acrylate copolymer, N-Methacrylamide, surfactant, V-50 initator, acetate, deionized water to prepare as material combination; Provide a combination property preferable; Lower-cost formula range plays one's part to the full each component.
As having adopted the perfluoro hexyl acrylic acid ester among the present invention; The perfluoro hexyl acrylic acid ester also is: 2-(perfluoro hexyl) ethyl-methyl acrylic acid ester; It has good chemical inertia and positive surface energy; Can make waterproofing agent that surface energy is reduced to 20 and reach below the sound, very excellent hydrophobic oil repellent ability is arranged; The hydroxyl ligand complex of hydroxy acid base and paper and textiles in the acrylate copolymer strengthens adhesive force; The V-50 initator has good lifting polymerization rate usefulness; Penetrability is strengthened rapid even littleization of finishing agent; With the assembly of surfactant under can make waterproofing agent possess good plate-out ability can; And be prone to be dispersed in fabric face can be rapidly even film forming, the good characteristics of generate film properties are arranged.In addition, the adding of N-Methacrylamide can make film adhesion significantly strengthen.
Effective selection through above each composition and proportioning combination, advantage such as it is nontoxic to make that three-proof finishing agent of the present invention has, and wash durability is good, and gas permeability is good, and environmental protection, technology are simple, with low cost is fit to the demand in market very much.
The specific embodiment
The specific embodiment of the present invention is following:
Wherein, the aforesaid propylene acid resin is made up of the monomer of following weight portion: 40% methyl acrylate and 60% butyl acrylate;
Above-mentioned surfactant is that the feedstock production by following weight portion obtains: isomerous tridecanol ether 35%, OTAC 30%, AEO 35%.
The preparation method: under (1) normal temperature with above-mentioned perfluoro hexyl acrylic acid ester, acrylate copolymer, N-Methacrylamide, surfactant, glacial acetic acid, deionized water are added to reaction cylinder and stir;
(2) the said mixture material of above-mentioned 1/3 weight is poured in the controllable temperature agitated reactor stirred; The V-50 initator that adds 1/3 weight when being warming up to 55 ℃ again; Insulation reaction 40 minutes is warming up to 75 ℃ then, then remaining 2/3 said mixture material and 2/3 V-50 initator is poured into.
(3) nitrogen injection reacted 5 hours again in aforesaid reaction vessel, can obtain uniform particulate mixed material.
(4), last cold filtration, packing make the emulsion finished product of even particle.
Wherein, the aforesaid propylene acid resin is made up of the monomer of following weight portion: 55% methyl acrylate and 45% octadecyl methacrylate;
Above-mentioned surfactant is that the feedstock production by following weight portion obtains: isomerous tridecanol ether 30%, OTAC 40%, AEO 30%.
The preparation method: under (1) normal temperature with above-mentioned perfluoro hexyl acrylic acid ester, acrylate copolymer, N-Methacrylamide, surfactant, glacial acetic acid, deionized water are added to reaction cylinder and stir;
(2) the said mixture material of above-mentioned 1/3 weight is poured in the controllable temperature agitated reactor stirred; The V-50 initator that adds 1/3 weight when being warming up to 55 ℃ again; Insulation reaction 45 minutes is warming up to 80 ℃ then, then remaining 2/3 said mixture material and 2/3 V-50 initator is poured into.
(3) nitrogen injection reacted 5 hours again in aforesaid reaction vessel, can obtain uniform particulate mixed material.
Test Example:
The ultramicron three-proof finishing agent consumption 30g/L to 40g/L (being to add 30-40g stoste in every 1000ml water) that the present invention is made is at woven dacron, textile cloth, nylon cloth or wash/cotton blended cloth on.
Application detects with U.S. AATCC2.2 detecting method, refuses the water level and all can reach more than 100 (pad mode 5-10 seconds);
When being that 120 degree or baking temperature are 180 when spending at bake out temperature, as long as under the constant prerequisite of proportioning component of perfluoro hexyl acrylic acid ester, and the various resin kinds in the acrylate copolymer can be organized flexibly and change, and all can make the good finished product of refusing the water level.
In the cone test application; High-grade cone on the automobile (loudspeaker cone); Throw in cone in bath raio and be in 3% the concentration proportioning (every 100ml water is put ultramicron three-proof finishing agent 3g), adopted the impregnation technology dipping 2-5 minute, be placed on 100 ℃ of-130 ℃ of oven for drying then.Effect: cone soaks in water and can not absorb water in 24 hours.
In the test of leather, the water bath raio is (every 100ml water is put ultramicron three-proof finishing agent 4g) in 4% the matched proportion density, adopts impregnation technology equally, then 100 ℃-130 ℃ oven for drying.The result: the water-wash resistance test is carried out 5 times through washing, oven dry repeatedly, and waterproof effect is desirable all the better.
This product seepage velocity is fast, waterproof, and grease proofing effect is good, and low-carbon (LC), ecological ideas environmental protection.
Application performance test result of the present invention is following:
Waterproofing agent consumption and initial waterproof effect (seeing chart)
Woven dacron (golden light suede, thick knitted cloth)
| The ultramicron consumption | 10g/l | 20g/l | 30g/l | 40g/l | 50g/l | 60g/l |
| Refuse the water grade | 70 | 100 | 100 | 100 | 100 | 100 |
Textile cloth (Woven Fabrics)
| The ultramicron consumption | 10g/l | 20g/l | 30g/l |
| Refuse the water grade | 90 | 100 | 100 |
Wash/cotton blended cloth (Woven Fabrics)
| The ultramicron consumption | 10g/l | 20g/l | 30g/l | 40g/l |
| Refuse the water grade | 95 | 100 | 100 | 100 |
Nylon cloth (Woven Fabrics)
| The ultramicron consumption | 10g/l | 20g/l | 30g/l | 40g/l | 60g/l | 80g/l |
| Refuse the water grade | 70 | 90 | 100 | 100 | 100 | 100 |
[0053]Ultramicron all is meant ultramicron three-proof finishing agent of the present invention in the above table;
Other experiment condition
Experimental water: running water
Working solution pH value: 5.5 (waterproofing agent+water)
Pad mode: dried cloth soaked in charging basket 5 ~ 10 seconds
→ let working solution soak into fabric → roll 1 time
Laboratory mangle controlled condition: 0.18MPa, 2.2m/min
Liquid carrying rate: terylene 70%, nylon 60%, wash/cotton 60%, textile 60%
Typing condition: terylene, nylon, wash/cotton blended cloth: 170 ℃ * 1min
Textile cloth: pad → → 170 ℃ * 2min of 120 ℃ of oven dry bakes
WATER REPELLENCY evaluation criterion: U.S. AATCC 22 best 100 minutes, differed from 0 fen most.
Claims (6)
1. ultramicron three-proof finishing agent is characterized in that this finishing agent is that feedstock production by following weight portion obtains:
2. a kind of ultramicron three-proof finishing agent according to claim 1 is characterized in that: described surfactant is that the feedstock production by following weight portion obtains: isomerous tridecanol ether 30～40%, OTAC 25～45%, AEO 25～40%.
3. a kind of ultramicron three-proof finishing agent according to claim 1 is characterized in that: acrylic resin is selected from following monomer by at least two kinds and forms: (methyl) methyl acrylate, (methyl) octadecyl acrylate, (methyl) tetradecyl acrylate; (methyl) butyl acrylate, (methyl) isobutyl acrylate, (methyl) ethyl acrylate; Styrene, butyl acrylate, propyl acrylate; Tetradecyl acrylate, octadecyl acrylate, acrylic acid and their combinations.
4. a kind of ultramicron three-proof finishing agent according to claim 3; It is characterized in that: described acrylic resin is selected from following monomer by at least two kinds and forms: (methyl) methyl acrylate; (methyl) octadecyl acrylate, butyl acrylate and their combination.
5. a kind of ultramicron three-proof finishing agent according to claim 1 is characterized in that: described acetate is glacial acetic acid.
6. the preparation method of a ultramicron three-proof finishing agent is that the raw material by the said weight portion of claim 1 prepares through following steps:
(1) under the normal temperature with first monomer, second monomer, the 3rd monomer, surfactant, acetate, deionized water are added to reaction cylinder and stir;
(2) 1/3 said mixture material is poured in the controllable temperature agitated reactor stirred; Add 1/3 V-50 initator when being warming up to 55 ℃ again; Insulation reaction 40～50 minutes is warming up to 75 ℃-85 ℃ then, then remaining 2/3 said mixture material and 2/3 V-50 initator is poured into;
(3) nitrogen injection reacted 5～6 hours again in aforesaid reaction vessel, can obtain uniform particulate mixed material;
(4), last cold filtration, packing make the emulsion finished product of even particle.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201210184067.6A CN102677469B (en) | 2012-06-01 | 2012-06-01 | Ultramicron three-proofing finishing agent and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201210184067.6A CN102677469B (en) | 2012-06-01 | 2012-06-01 | Ultramicron three-proofing finishing agent and preparation method thereof |
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| CN102677469A true CN102677469A (en) | 2012-09-19 |
| CN102677469B CN102677469B (en) | 2014-06-04 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103435738A (en) * | 2013-04-15 | 2013-12-11 | 湖南多喜爱家纺股份有限公司 | Preparation process of active three-proofing additive for medical fabric |
| CN104233807A (en) * | 2014-09-17 | 2014-12-24 | 王东生 | Low-temperature water-based waterproof agent and production technology thereof |
| CN105887487A (en) * | 2016-05-17 | 2016-08-24 | 江西国桥实业有限公司 | Preparation method of water-repelling and oil-repelling modified acrylate type adhesive |
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| KR20030038366A (en) * | 2001-11-08 | 2003-05-16 | 주식회사 엘지화학 | Acrylate-styrene-acrylonitrile graft copolymer composition and method for preparing thereof |
| CN100999866A (en) * | 2006-01-11 | 2007-07-18 | 丹东恒星精细化工有限公司 | Water-resisting, oil-proof, antifouling agent for fabric and production process thereof |
| CN101161930A (en) * | 2007-09-04 | 2008-04-16 | 山东东岳高分子材料有限公司 | Organic water-proof oil-resist finishing agent for paper and cardboard and preparation thereof |
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2012
- 2012-06-01 CN CN201210184067.6A patent/CN102677469B/en not_active Expired - Fee Related
Patent Citations (3)
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| KR20030038366A (en) * | 2001-11-08 | 2003-05-16 | 주식회사 엘지화학 | Acrylate-styrene-acrylonitrile graft copolymer composition and method for preparing thereof |
| CN100999866A (en) * | 2006-01-11 | 2007-07-18 | 丹东恒星精细化工有限公司 | Water-resisting, oil-proof, antifouling agent for fabric and production process thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103435738A (en) * | 2013-04-15 | 2013-12-11 | 湖南多喜爱家纺股份有限公司 | Preparation process of active three-proofing additive for medical fabric |
| CN103435738B (en) * | 2013-04-15 | 2016-06-15 | 多喜爱家纺股份有限公司 | A kind of preparation technology of Medical face fabric activity three anti-auxiliary agents |
| CN104233807A (en) * | 2014-09-17 | 2014-12-24 | 王东生 | Low-temperature water-based waterproof agent and production technology thereof |
| CN105887487A (en) * | 2016-05-17 | 2016-08-24 | 江西国桥实业有限公司 | Preparation method of water-repelling and oil-repelling modified acrylate type adhesive |
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| CN102677469B (en) | 2014-06-04 |
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Granted publication date: 20140604 Termination date: 20180601 |