CN102603963B - Preparation method of environmentally-friendly polyacrylic ester pigment printing adhesive - Google Patents

Preparation method of environmentally-friendly polyacrylic ester pigment printing adhesive Download PDF

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CN102603963B
CN102603963B CN201210083148.7A CN201210083148A CN102603963B CN 102603963 B CN102603963 B CN 102603963B CN 201210083148 A CN201210083148 A CN 201210083148A CN 102603963 B CN102603963 B CN 102603963B
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emulsification
pigment printing
monomer
preparation
necked flask
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CN102603963A (en
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高党鸽
马建中
张文博
吕斌
陈琛
李学柯
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WEIHAI LIANQIAO NEW MATERIAL SCIENCE & TECHNOLOGY Co.,Ltd.
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Shaanxi University of Science and Technology
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Abstract

The invention relates to a preparation method of an environmentally-friendly polyacrylic ester adhesive, in particular to a preparation method of an environmentally-friendly acrylic resin adhesive for fabric pigment printing. Most commercially-available polyacrylic acid emulsion contains a certain amount of N-hydroxymethyl acrylamide, so that the defect of releasing of formaldehyde in baking and storing processes exists in the prior art. The polyacrylic ester pigment printing adhesive is prepared by performing emulsion polymerization on an acrylic acid monomer and glycidyl methacrylate which serve as raw materials, and is free from formaldehyde release; and after the adhesive is applied to a pigment printing process, the adhesion of a coating on a textile can be enhanced, and net blockage is avoided. After pigment printing, the dry-wet rub fastness of the textile is over grade 2, the fading fastness is over grade 3 after soaping, and the color adhesion is over grade 4.

Description

The preparation method of environment-friendly polypropylene acid esters pigment printing binding agent
Technical field
The present invention relates to a kind of preparation method of environment-friendly polypropylene acid esters tackiness agent, particularly the preparation method of environment-friendly polypropylene acid esters tackiness agent for a kind of textile coating stamp.
Background technology
According to incompletely statistics, whole world pigment printing fabric accounts for 55% left and right of tprinted Fabrics total amount, and in the U.S., pigment printing fabric accounts for 80% of tprinted Fabrics ultimate production, and wash/cotton cloth is nearly all used pigment printing.In recent years, because of technique trend, simplify, reduce the factors such as energy consumption, the ratio of pigment printing is also in rising trend in China, accounts for the level of 20%-25%.Pigment printing be by macromolecular compound as tackiness agent, through certain processing, on fabric, form a kind of transparent coloured film, pigment is anchored to the method on fabric.Polyacrylate emulsion is a widely used class pigment printing binding agent, contains a certain amount of N hydroxymethyl acrylamide in many polyacrylate emulsions, bake with storage process in can discharge formaldehyde.Along with people's environmental consciousness with to the improving constantly of product requirement, many environmental regulations have been promulgated in countries in the world, impel in weaving pigment printing polyacrylate emulsion towards novel, environmental protection and high-performance future development.
The problem that exists formaldehyde to discharge in order to improve polyacrylate(s) printing adhesive, Chinese scholars conducts extensive research, mainly comprise add efficient formaldehyde trapping agent, select other self-cross linking monomers, the method such as functional monomer and change polymerization technique.Adopt the monomer simultaneously with vinyl and epoxy group(ing), can be by vinyl and other acrylic ester monomer copolymerization, epoxy group(ing) can be cross-linked with hydroxyl, carboxyl, amino groups, have good cohesive strength and and fabric between bounding force, thereby after pigment printing, fabric has the performances such as good water-fast, rub resistance.
Summary of the invention
The preparation method who the object of the present invention is to provide a kind of environment-friendly polypropylene acid esters tackiness agent, this tackiness agent is formaldehydeless, and it is applied to pigment printing technique, meets the needs of future development.
For achieving the above object, the preparation method that the present invention adopts is:
The emulsifying agent that sodium lauryl sulphate and nonionogenic tenside are mixed totally 1.55 ~ 3.10g adds in 50.00g distilled water and stirs, wherein nonionogenic tenside can be used alkylphenol polyoxyethylene JFC-1, nonyl polyoxy diene ether TX-10, branched secondary alcohol Soxylat A 25-7 TMN-10, EO/PO multipolymer L-64, sorbitol anhydride oleate Soxylat A 25-7 SP-80, polyoxyethylene carboxylate 99# or trimethylammonium nonyl ethers MS-1, nonionogenic tenside accounts for 10 ~ 70wt% of total emulsifiers consumption, add again methyl methacrylate 24.00-25.60g, glycidyl methacrylate 0.75 ~ 3.00g, use mulser at 1000r/min emulsification 5-10min, add again butyl acrylate 49.60-56.0g, use mulser at 1000r/min emulsification 5-10min, obtain pre-emulsification monomer.0.75g ammonium persulphate is dissolved in to 30.0g water, in the 250mL there-necked flask that agitator, condensing works are housed, add 1/3 pre-emulsification monomer and 1/3 ammonium persulfate solution, under 75-80 ℃ of water bath condition, stir, when in there-necked flask, emulsion blue light is obvious, drip respectively pre-emulsification monomer and the ammonium persulphate of residue 2/3, control time for adding 90-120min, after dripping reaction 20min, be warming up to 75-80 ℃ of insulation reaction 2-3h, naturally cooling, with ammoniacal liquor by emulsion pH regulator to 4.0-4.5, filter discharging.
The present invention is with respect to prior art, and its advantage is as follows:
It is raw material that the present invention adopts acrylic monomer and glycidyl methacrylate, by letex polymerization, makes polyacrylate coating printing adhesive, the formaldehydeless release of this tackiness agent; Be applied in pigment printing technique, can improve the sticking power of coating on fabric, and be difficult for network blocking.After pigment printing, the dry wet rubbing fastness of fabric reaches more than 2 grades, and the fastness of fading after soaping reaches more than 3 grades, and sticky look reaches more than 4 grades.
Embodiment
It is raw material that the present invention adopts acrylic monomer and glycidyl methacrylate, by letex polymerization, makes pigment printing binding agent, the formaldehydeless release of this tackiness agent; Be applied in pigment printing technique, can improve the sticking power of coating on fabric, and be difficult for network blocking.
Embodiment 1, the common 1.94g of emulsifying agent of sodium lauryl sulphate and branched secondary alcohol Soxylat A 25-7 TMN-10 mixing is added in 50.00g distilled water and stirred, wherein branched secondary alcohol Soxylat A 25-7 TMN-10 accounts for the 20wt% of total emulsifiers consumption, add again methyl methacrylate 25.40g, glycidyl methacrylate 1.57g, use mulser at 1000r/min emulsification 6min, add again butyl acrylate 49.60g, use mulser at 1000r/min emulsification 8min, obtain pre-emulsification monomer.0.60g ammonium persulphate is dissolved in to 30.0g water, in the 250mL there-necked flask that agitator, condensing works are housed, add 1/3 pre-emulsification monomer and 1/3 ammonium persulfate solution, under 75 ℃ of water bath condition, stir, when emulsion blue light is obvious in there-necked flask, drip respectively pre-emulsification monomer and the ammonium persulphate of residue 2/3, control time for adding 100min, after dripping reaction 20min, be warming up to 75 ℃ of insulation reaction 2.5h, naturally cooling, with ammoniacal liquor, by emulsion pH regulator to 4.0, filter discharging.
Embodiment 2, the common 3.10g of emulsifying agent of sodium lauryl sulphate and the mixing of pears sugar alcohol acid anhydride oleic acid ester Soxylat A 25-7 is added in 50.00g distilled water and stirred, SP-80 accounts for the 10wt% of total emulsifiers consumption, add again methyl methacrylate 24.80g, glycidyl methacrylate 2.25g, use mulser at 1000r/min emulsification 5min, add again butyl acrylate 55.20g, use mulser at 1000r/min emulsification 10min, obtain pre-emulsification monomer.0.91g ammonium persulphate is dissolved in to 30.0g water, in the 250mL there-necked flask that agitator, condensing works are housed, add 1/3 pre-emulsification monomer and 1/3 ammonium persulfate solution, under 75 ℃ of water bath condition, stir, when emulsion blue light is obvious in there-necked flask, drip respectively pre-emulsification monomer and the ammonium persulphate of residue 2/3, control time for adding 90min, after dripping reaction 20min, be warming up to 75 ℃ of insulation reaction 3h, naturally cooling, with ammoniacal liquor, by emulsion pH regulator to 4.5, filter discharging.
Embodiment 3, the common 2.33g of emulsifying agent of sodium lauryl sulphate and alkylphenol polyoxyethylene JFC-1 mixing is added in 50.00g distilled water and stirred, alkylphenol polyoxyethylene JFC-1 accounts for the 40wt% of total emulsifiers consumption, add again methyl methacrylate 24.00g, glycidyl methacrylate 3.00g, use mulser at 1000r/min emulsification 8min, add again butyl acrylate 49.60g, use mulser at 1000r/min emulsification 8min, obtain pre-emulsification monomer.0.76g ammonium persulphate is dissolved in to 30.0g water, in the 250mL there-necked flask that agitator, condensing works are housed, add 1/3 pre-emulsification monomer and 1/3 ammonium persulfate solution, under 75 ℃ of water bath condition, stir, when emulsion blue light is obvious in there-necked flask, drip respectively pre-emulsification monomer and the ammonium persulphate of residue 2/3, control time for adding 90min, after dripping reaction 30min, be warming up to 75 ℃ of insulation reaction 2h, naturally cooling, with ammoniacal liquor, by emulsion pH regulator to 4.0, filter discharging.
Embodiment 4, the common 1.94g of emulsifying agent of sodium lauryl sulphate and nonyl polyoxy diene ether TX-10 mixing is added in 50.00g distilled water and stirred, nonyl polyoxy diene ether TX-10 accounts for the 20wt% of total emulsifiers consumption, add again methyl methacrylate 25.60g, glycidyl methacrylate 2.25g, use mulser at 1000r/min emulsification 10min, add again butyl acrylate 54.4g, use mulser at 1000r/min emulsification 10min, obtain pre-emulsification monomer.0.75g ammonium persulphate is dissolved in to 30.0g water, in the 250mL there-necked flask that agitator, condensing works are housed, add 1/3 pre-emulsification monomer and 1/3 ammonium persulfate solution, under 75 ℃ of water bath condition, stir, when emulsion blue light is obvious in there-necked flask, drip respectively pre-emulsification monomer and the ammonium persulphate of residue 2/3, control time for adding 100min, after dripping reaction 30min, be warming up to 75 ℃ of insulation reaction 3h, naturally cooling, with ammoniacal liquor, by emulsion pH regulator to 4.5, filter discharging.
Embodiment 5, the emulsifying agent that sodium lauryl sulphate and polyoxyethylene carboxylate 99# are mixed totally 1.55 ~ 3.10g adds in 50.00g distilled water and stirs, polyoxyethylene carboxylate 99# accounts for the 50wt% of total emulsifiers consumption, add again methyl methacrylate 24.00-25.60g, glycidyl methacrylate 3.0g, use mulser at 1000r/min emulsification 10min, add again butyl acrylate 49.60-56.0g, use mulser at 1000r/min emulsification 10min, obtain pre-emulsification monomer.0.91g ammonium persulphate is dissolved in to 30.0g water, in the 250mL there-necked flask that agitator, condensing works are housed, add 1/3 pre-emulsification monomer and 1/3 ammonium persulfate solution, under 75-80 ℃ of water bath condition, stir, when emulsion blue light is obvious in there-necked flask, drip respectively pre-emulsification monomer and the ammonium persulphate of residue 2/3, control time for adding 120min, after dripping reaction 30min, be warming up to 75 ℃ of insulation reaction 3h, naturally cooling, with ammoniacal liquor, by emulsion pH regulator to 4.5, filter discharging.

Claims (4)

1. a preparation method for environment-friendly polypropylene acid esters pigment printing binding agent, its step is as follows:
The emulsifying agent that sodium lauryl sulphate and nonionogenic tenside are mixed totally 1.55 ~ 3.10g adds in 50.00g distilled water and stirs, nonionogenic tenside accounts for 10 ~ 70wt% of total emulsifiers consumption, add again methyl methacrylate 24.00-25.60g, glycidyl methacrylate 0.75 ~ 3.00g, use mulser at 1000r/min emulsification 5-10min, add again butyl acrylate 49.60-56.0g, use mulser at 1000r/min emulsification 5-10min, obtain pre-emulsification monomer; 0.75g ammonium persulphate is dissolved in to 30.0g water, in the 250mL there-necked flask that agitator, condensing works are housed, add 1/3 pre-emulsification monomer and 1/3 ammonium persulfate solution, under 75-80 ℃ of water bath condition, stir, when in there-necked flask, emulsion blue light is obvious, drip respectively pre-emulsification monomer and the ammonium persulphate of residue 2/3, control time for adding 90-120min, after dripping reaction 20min, be warming up to 75-80 ℃ of insulation reaction 2-3h, naturally cooling, with ammoniacal liquor by emulsion pH regulator to 4.0-4.5, filter discharging.
2. the preparation method of environment-friendly polypropylene acid esters pigment printing binding agent according to claim 1, is characterized in that: nonionogenic tenside is alkylphenol polyoxyethylene JFC-1, branched secondary alcohol Soxylat A 25-7 TMN-10.
3. the preparation method of an environment-friendly polypropylene acid esters pigment printing binding agent, it is characterized in that: the common 1.94g of emulsifying agent of sodium lauryl sulphate and branched secondary alcohol Soxylat A 25-7 TMN-10 mixing is added in 50.00g distilled water and stirred, wherein branched secondary alcohol Soxylat A 25-7 TMN-10 accounts for the 20wt% of total emulsifiers consumption, add again methyl methacrylate 25.40g, glycidyl methacrylate 1.57g, use mulser at 1000r/min emulsification 6min, add again butyl acrylate 49.60g, use mulser at 1000r/min emulsification 8min, obtain pre-emulsification monomer, 0.60g ammonium persulphate is dissolved in to 30.0g water, in the 250mL there-necked flask that agitator, condensing works are housed, add 1/3 pre-emulsification monomer and 1/3 ammonium persulfate solution, under 75 ℃ of water bath condition, stir, when emulsion blue light is obvious in there-necked flask, drip respectively pre-emulsification monomer and the ammonium persulphate of residue 2/3, control time for adding 100min, after dripping reaction 20min, be warming up to 75 ℃ of insulation reaction 2.5h, naturally cooling, with ammoniacal liquor, by emulsion pH regulator to 4.0, filter discharging.
4. a preparation method for environment-friendly polypropylene acid esters pigment printing binding agent, is characterized in that:
The common 3.10g of emulsifying agent of sodium lauryl sulphate and the mixing of sorbitol anhydride oleate Soxylat A 25-7 is added in 50.00g distilled water and stirred, sorbitol anhydride oleate Soxylat A 25-7 accounts for the 10wt% of total emulsifiers consumption, add again methyl methacrylate 24.80g, glycidyl methacrylate 2.25g, use mulser at 1000r/min emulsification 5min, add again butyl acrylate 55.20g, use mulser at 1000r/min emulsification 10min, obtain pre-emulsification monomer; 0.91g ammonium persulphate is dissolved in to 30.0g water, in the 250mL there-necked flask that agitator, condensing works are housed, add 1/3 pre-emulsification monomer and 1/3 ammonium persulfate solution, under 75 ℃ of water bath condition, stir, when emulsion blue light is obvious in there-necked flask, drip respectively pre-emulsification monomer and the ammonium persulphate of residue 2/3, control time for adding 90min, after dripping reaction 20min, be warming up to 75 ℃ of insulation reaction 3h, naturally cooling, with ammoniacal liquor, by emulsion pH regulator to 4.5, filter discharging.
CN201210083148.7A 2012-03-27 2012-03-27 Preparation method of environmentally-friendly polyacrylic ester pigment printing adhesive Active CN102603963B (en)

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Families Citing this family (9)

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Publication number Priority date Publication date Assignee Title
CN103103820A (en) * 2012-12-19 2013-05-15 上海奇想青晨新材料科技股份有限公司 Polyacrylate binder for pigment printing and preparation method of polyacrylate binder
CN103554346B (en) * 2013-10-14 2015-11-04 陕西科技大学 Graphene oxide modified polyacrylate prepares the method for pigment printing binding agent
CN103526597A (en) * 2013-10-23 2014-01-22 合肥聚合辐化技术有限公司 Flame-retardant printing adhesive and preparation method thereof
CN105603780A (en) * 2016-01-25 2016-05-25 苏州印丝特纺织数码科技有限公司 Method for preparing petroleum ether modified polyacrylate pigment printing adhesive
CN106567262A (en) * 2016-11-03 2017-04-19 东莞市联洲知识产权运营管理有限公司 Formaldehyde-free adhesive for pigment dyeing and preparation method thereof
CN107286287A (en) * 2017-06-07 2017-10-24 常州诺丁精密机械制造有限公司 A kind of preparation method of pigment printing binding agent
CN107513868A (en) * 2017-09-29 2017-12-26 太仓市金锚新材料科技有限公司 Environment-friendly type low-temperature resistant coating stamp adhesive
CN110685155A (en) * 2019-10-11 2020-01-14 西安工程大学 Quick-drying type crosslinked polyacrylic acid textile size and preparation method thereof
CN111087525A (en) * 2019-12-30 2020-05-01 青岛双利材料科技有限公司 Synthesis method of novel printing and dyeing adhesive

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WO2002103555A2 (en) * 2001-06-18 2002-12-27 Pipedream Metasystems, Inc. Computer system with natural language to machine language translator
CN101423735A (en) * 2008-12-05 2009-05-06 武汉科技学院 Method for preparing environment-friendly type organosilicon modified acrylic ester binding agent

Patent Citations (2)

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WO2002103555A2 (en) * 2001-06-18 2002-12-27 Pipedream Metasystems, Inc. Computer system with natural language to machine language translator
CN101423735A (en) * 2008-12-05 2009-05-06 武汉科技学院 Method for preparing environment-friendly type organosilicon modified acrylic ester binding agent

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