CN102504128B - Preparation method for organic silicon-modified printing adhesive - Google Patents
Preparation method for organic silicon-modified printing adhesive Download PDFInfo
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- CN102504128B CN102504128B CN 201110344711 CN201110344711A CN102504128B CN 102504128 B CN102504128 B CN 102504128B CN 201110344711 CN201110344711 CN 201110344711 CN 201110344711 A CN201110344711 A CN 201110344711A CN 102504128 B CN102504128 B CN 102504128B
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Abstract
The invention discloses a preparation method for an organic silicon-modified printing adhesive. The preparation method comprises the following steps of: preparing an organic silicon pre-emulsion: adding 80-140 parts by weight of deionized water, 3-7 parts by weight of a compounding emulsifier, 8-12 parts by weight of an organic silicon monomer and 0.1-0.2 part by weight of a silane coupling agent into a reaction kettle, stirring at the room temperature for 40-70 minutes, heating to 75-90 DEG C, and reacting at the temperature for 110-130 minutes to obtain the organic silicon pre-emulsion; and preparing a printing adhesive: controlling the temperature of the organic silicon pre-emulsion at 75-85 DEG C, dropwise adding an acrylate monomer and an initiator in sequence while stirring at the high speed of 1,000 revolutions per minute within 2 hours, heating to 4-6 DEG C, preserving heat for reacting for 25-35 minutes, cooling, and adjusting the pH to 6-7 with sodium hydroxide to obtain the organic silicon-modified printing adhesive. The preparation method has the advantages of simple process steps, high storage stability, washability, superior softness and contribution to environmental friendliness.
Description
Technical field
The invention belongs to textile auxiliary's preparing technical field, be specifically related to a kind of preparation method of organic-silicon-modified stamp tackiness agent
Background technology
Pigment printing sticks to granules of pigments on the fabric by means of tackiness agent and reaches painted purpose, and therefore, there is not fastidious property in it to various fibers.And pigment printing technology is simple, chromatogram is extensive, colorant match is easy, do not need washing after the fixation, so it has water saving, energy-conservation characteristics, in global PRINTED FABRIC or title fabric, the share that pigment printing occupies increases year by year.Tackiness agent is the chief component of paint-printing colour size, and its quality directly influences end product quality.At present, it mainly is esters of acrylic acid such as Chinese patent (CN101948555A, CN102190989A, CN101942772A) that pigment printing sticks with glue agent, and itself and adhering fabric power are strong, have good film forming properties, transparent, the pliable and tough and high resilience of the film of formation.
But existing technology has 2 deficiencies: at first, when the acrylate consumption more for a long time, Boardy Feeling; Secondly, when printing dark product, wet fastness to rubbing is poor
Summary of the invention
Task of the present invention is to provide a kind of preparation method of organic-silicon-modified stamp tackiness agent, this method preparation technology is simple to use harsh equipment with need not, and can guarantee that the organic-silicon-modified stamp tackiness agent that obtains has good preservation stability, washing fastness, makes fabric show excellent flexibility and is conducive to avoid undermining environment.
Task of the present invention is finished like this, and a kind of preparation method of organic-silicon-modified stamp tackiness agent may further comprise the steps:
A) preparation organosilicon pre-emulsion:
Earlier deionized water 80-140 weight part, compound emulsifying agent 3-7 weight part, organosilane monomer 8-12 weight part and silane coupling agent 0.1-0.2 weight part are added in the reactor, at room temperature stir 40-70min, temperature is risen to 75-90 ℃, under this temperature, react 110-130min, make the organosilicon pre-emulsion;
B) preparation stamp tackiness agent:
With 75-85 ℃ of organosilicon pre-emulsion control temperature, under stirring fast, 1000r/min is added dropwise to acrylate monomer 30-40 weight part, initiator 0.2-0.4 weight part successively, dropwise in the 2h, intensification 4-6 ℃, insulation reaction 25-35min, cooling transfers to 6-7 with sodium hydroxide 0.1-1 weight part with pH, obtains organic-silicon-modified stamp tackiness agent.
In a specific embodiment of the present invention, described acrylate monomer is at least a in methyl acrylate, Jia Jibingxisuanyizhi, the butyl acrylate.
In another specific embodiment of the present invention, described compound emulsifying agent is at least two kinds in sorbester p17, tween 80, aliphatic acid polyethenoxy ether (AEO9), ten disulfobenzene sulfonic acid, the ten disulfobenzene sodium sulfonates.
In another specific embodiment of the present invention, described organosilane monomer is at least two kinds in octamethylcyclotetrasiloxane, decamethylcyclopentaandoxane, polydimethylsiloxane, the polymethyl hydrogen siloxane.
In another specific embodiment of the present invention, described initiator is a kind of in Potassium Persulphate, the ammonium persulphate.
Also have in the specific embodiment of the present invention, described silane coupling agent is at least a in а-methacryloxypropyl trimethoxy silane, vinyltriethoxysilane, the vinyltrimethoxy silane.
Technical scheme processing step provided by the invention is terse and in preparation process equipment is not had harsh requirement, because the stamp adhesive products that obtains is emulsion, therefore has good preservation stability; Because silane coupling agent is to the full correctability of vinylformic acid list, therefore the PRINTED FABRIC that obtains not only has good washing fastness, and has excellent flexibility; Since in the preparation not with an organic solvent, thereby environmental friendliness.
Embodiment
Embodiment 1:
A) preparation organosilicon pre-emulsion:
Earlier deionized water 140 weight parts, compound emulsifying agent aliphatic acid polyethenoxy ether (AEO9) 4 weight parts, ten disulfobenzene sulfonic acid, 3 weight parts, organosilane monomer octamethylcyclotetrasiloxane 7 weight parts, polymethyl hydrogen siloxane 5 weight parts and silane coupling agent а-methacryloxypropyl trimethoxy silane 0.2 weight part are added in the reactor, at room temperature stir 40min, temperature is risen to 85 ℃, under this temperature, react 120min, make the organosilicon pre-emulsion
B) preparation stamp tackiness agent:
With 80 ℃ of above-mentioned organosilicon pre-emulsion control temperature, under stirring fast, 1000r/min is added dropwise to acrylate monomer methyl acrylate 8 weight parts, butyl acrylate 32 weight parts, initiator potassium persulfate 0.4 weight part successively, drip in the 130min, heat up 5 ℃, insulation reaction 30min, cooling transfers to 6-7 with sodium hydroxide 0.8 weight part with pH, namely gets organic-silicon-modified stamp tackiness agent of the present invention.
Embodiment 2:
A) preparation organosilicon pre-emulsion:
Earlier deionized water 120 weight parts, compound emulsifying agent aliphatic acid polyethenoxy ether (AEO9) 3 weight parts, ten disulfobenzene sodium sulfonates, 2 weight parts, organosilane monomer octamethylcyclotetrasiloxane 8 weight parts, polydimethylsiloxane 2 weight parts and silane coupling agent vinyl Trimethoxy silane 0.2 weight part are added in the reactor, at room temperature stir 70min, temperature is risen to 80 ℃, reaction 110 min make the organosilicon pre-emulsion under this temperature;
B) preparation stamp tackiness agent:
With 80 ℃ of above-mentioned organosilicon pre-emulsion control temperature, under stirring fast, 1000r/min is added dropwise to acrylate monomer Jia Jibingxisuanyizhi 15 weight parts, butyl acrylate 23 weight parts, initiator potassium persulfate 0.4 weight part successively, drip in 130 min.Heat up 6 ℃, insulation reaction 25 min, cooling transfers to 6-7 with sodium hydroxide 0.7 weight part with pH, namely gets organic-silicon-modified stamp tackiness agent of the present invention.
Embodiment 3:
A) preparation organosilicon pre-emulsion:
Earlier deionized water 80 weight parts, compound emulsifying agent sorbester p17 1 weight part, tween 80 2 weight parts, ten disulfobenzene sulfonic acid, 1 weight part, organosilane monomer decamethylcyclopentaandoxane 6 weight parts, polydimethylsiloxane 2 weight parts and silane coupling agent vinyl triethoxyl silane 0.1 weight part are added in the reactor, at room temperature stir 60 min, temperature is risen to 75 ℃, reaction 130 min make the organosilicon pre-emulsion under this temperature;
B) preparation stamp tackiness agent:
With 80 ℃ of above-mentioned organosilicon pre-emulsion control temperature, under stirring fast, 1000r/min is added dropwise to acrylate monomer methyl acrylate 14 weight parts, Jia Jibingxisuanyizhi 16 weight parts, initiator ammonium persulfate 0.2 weight part successively, drip in 130 min.Heat up 4.5 ℃, insulation reaction 32 min, cooling transfers to 6-7 with sodium hydroxide 0.3 weight part with pH, namely gets organic-silicon-modified stamp tackiness agent of the present invention.
Embodiment 4:
A) preparation organosilicon pre-emulsion:
Earlier deionized water 100 weight parts, compound emulsifying agent sorbester p17 2 weight parts, tween 80 2 weight parts, ten disulfobenzene sodium sulfonates, 2 weight parts, organosilane monomer octamethylcyclotetrasiloxane 8 weight parts, polydimethylsiloxane 1 weight part and silane coupling agent а-methacryloxypropyl trimethoxy silane 0.1 weight part are added in the reactor, at room temperature stir 50 min, temperature is risen to 90 ℃, reaction 115 min make the organosilicon pre-emulsion under this temperature;
B) preparation stamp tackiness agent:
With 80 ℃ of above-mentioned organosilicon pre-emulsion control temperature, under stirring fast, 1000r/min is added dropwise to acrylate monomer Jia Jibingxisuanyizhi 7 weight parts, butyl acrylate 28 weight parts, initiator ammonium persulfate 0.3 weight part successively, drip in 130 min.Heat up 4 ℃, insulation reaction 35 min, cooling transfers to 6-7 with sodium hydroxide 0.4 weight part with pH, namely gets organic-silicon-modified stamp tackiness agent of the present invention.
Embodiment 5:
A) preparation organosilicon pre-emulsion:
Earlier deionized water 90 weight parts, compound emulsifying agent aliphatic acid polyethenoxy ether (AEO9) 2 weight parts, ten disulfobenzene sulfonic acid, 1 weight part, organosilane monomer octamethylcyclotetrasiloxane 9 weight parts, polymethyl hydrogen siloxane 2 weight parts and silane coupling agent а-methacryloxypropyl trimethoxy silane 0.1 weight part are added in the reactor, at room temperature stir 45 min, temperature is risen to 82 ℃, reaction 125 min make the organosilicon pre-emulsion under this temperature;
B) preparation stamp tackiness agent:
With 80 ℃ of above-mentioned organosilicon pre-emulsion control temperature, under 1000r/min stirs fast, be added dropwise to acrylate monomer methyl acrylate 9 weight parts, Jia Jibingxisuanyizhi 6 weight parts, butyl acrylate 18 weight parts, initiator potassium persulfate 0.3 weight part successively, drip in 130 min.Heat up 5.5 ℃, insulation reaction 33 min, cooling transfers to 6-7 with sodium hydroxide 0.2 weight part with pH, namely gets organic-silicon-modified stamp tackiness agent of the present invention.
The application of the resulting organic-silicon-modified stamp tackiness agent of above-described embodiment in printing technology: press printing paste prescription (to the mill base weight fraction, down together): coating orchid, 5%; Tackiness agent, 20%; Thickening material, 4%; Water, 71%; Convert to 100% and make the stamp rubber cement, press printing technology: stamp → oven dry (100 ℃, 3 min) → bake (140～150 ℃, 3 min) → aftertreatment → test
Claims (1)
1.
A kind of preparation method of organic-silicon-modified stamp tackiness agent is characterized in that may further comprise the steps:
A) preparation organosilicon pre-emulsion:
Earlier deionized water 80-140 weight part, compound emulsifying agent 3-7 weight part, organosilane monomer 8-12 weight part and silane coupling agent 0.1-0.2 weight part are added in the reactor, at room temperature stir 40-70min, temperature is risen to 75-90 ℃, under this temperature, react 110-130min, make the organosilicon pre-emulsion;
B) preparation stamp tackiness agent:
With 75-85 ℃ of organosilicon pre-emulsion control temperature, under stirring fast, 1000r/min is added dropwise to acrylate monomer 30-40 weight part successively, initiator 0.2-0.4 weight part, dropwise in the 2h, intensification 4-6 ℃, insulation reaction 25-35min, cooling, with sodium hydroxide 0.1-1 weight part pH is transferred to 6-7, obtain organic-silicon-modified stamp tackiness agent, described acrylate monomer is methyl acrylate, at least a in the butyl acrylate, described compound emulsifying agent is sorbester p17, tween 80, in the aliphatic acid polyethenoxy ether at least two kinds, described organosilane monomer is octamethylcyclotetrasiloxane, decamethylcyclopentaandoxane, polydimethylsiloxane, in the polymethyl hydrogen siloxane at least two kinds, described initiator is Potassium Persulphate, a kind of in the ammonium persulphate, described silane coupling agent is а-methacryloxypropyl trimethoxy silane, vinyltriethoxysilane, at least a in the vinyltrimethoxy silane
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| CN 201110344711 CN102504128B (en) | 2011-11-04 | 2011-11-04 | Preparation method for organic silicon-modified printing adhesive |
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| CN102504128B true CN102504128B (en) | 2013-08-28 |
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| CN103924458B (en) * | 2014-03-26 | 2015-12-02 | 东至绿洲环保化工有限公司 | Silicone acrylic emulsion printing adhesive |
| CN107447551B (en) * | 2017-08-16 | 2019-08-13 | 辽宁恒星精细化工有限公司 | Cotton towel fabric hydrophilic acrylic ester coating printing adhesive and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101423734A (en) * | 2008-12-05 | 2009-05-06 | 武汉科技学院 | Method for preparing organosilicon modified acrylic ester binding agent |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101423734A (en) * | 2008-12-05 | 2009-05-06 | 武汉科技学院 | Method for preparing organosilicon modified acrylic ester binding agent |
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Effective date of registration: 20160622 Address after: 201417 No. 819, Hua Bei Road, Shanghai, Fengxian District Patentee after: Shanghai enika Technology Development Co. Ltd. Address before: 215515 Jiangsu city of Suzhou province Changshou City ancient town miaoquan Industrial Park Patentee before: Changshu Kailida Honeycomb Package Material Co., Ltd. |