CN102926212B - Water-based coating adhesive with high elasticity used for cotton and linen fabrics and preparation method thereof - Google Patents
Water-based coating adhesive with high elasticity used for cotton and linen fabrics and preparation method thereof Download PDFInfo
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- CN102926212B CN102926212B CN201210426257.4A CN201210426257A CN102926212B CN 102926212 B CN102926212 B CN 102926212B CN 201210426257 A CN201210426257 A CN 201210426257A CN 102926212 B CN102926212 B CN 102926212B
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Abstract
The invention relates to water-based coating adhesive with high elasticity used for cotton and linen fabrics. The water-based coating adhesive is characterized by being prepared from the following raw materials in weight ratio: 150-200 of octamethylcyclotetrasiloxane, 15-40 of dodecylbenzene sulfonic acid, 1-10 of gamma-aminopropyl triethoxy silane, 1-10 of gamma-glycidoxy propyl trimethoxy silane, and 400-600 of deionized water. A preparation method of the water-based coating adhesive comprises the following steps of: conducting polymerization and neutralization by emulsion, adding 150-230 of polyurethane resin finishing agent, using a water-based polyurethane thickener for thickening, adding 15-38 of polymethylhydrosiloxane and 15-38 of dibutyl tin dilaurate emulsion, and evenly stirring. The water-based coating adhesive has the characteristics of high resilience, wrinkle resistance and smoothness, also can be used for improving the softness and washing durability of the cotton and linen fabrics, and is safe in use and good in environmental friendliness.
Description
Technical field
What the present invention relates to is a kind of high-elastic coating adhesive of water-based for cotton, pitted skin material and preparation method thereof.The key component of this coating adhesive is the modified polyorganosiloxanes of high molecular weight, by being mixed itself and polyurethane resin, crosslinking agent and catalyst, can make cotton, pitted skin material after coating there is high resilience, wrinkle resistance, and soft smooth, tearing brute force obviously improves, and has given fabric new feel style, thereby has greatly improved the added value of fabric.
Background technology
About the high-elastic coating adhesive of water-based of cotton, pitted skin material is there are no patent and bibliographical information.Mostly high-elastic coating adhesive is the high-elastic coating adhesive of solvent-type organosilicon in the market, because it has high-elastic, well-pressed, smooth unique hand feeling style, liked by client.But weak point is the afterwards peculiar feel style meeting of the fabric process washing degradation after being coated with, and 70%-90% be solvent toluene in solvent adhesive, after coating, toluene is dried, not only cause the waste of resource, contaminated environment, if misoperation fire or blast, thereby cause the loss of personnel and property.
Summary of the invention
The object of the invention is to provide in order to overcome the deficiency of above-mentioned prior art existence a kind of high-elastic coating adhesive of water-based of function admirable; it is except having the high resilience of solvent adhesive; wrinkle resistance; outside the features such as slipping; can also improve flexibility and the washing resistance of cotton, pitted skin material; with water, replace solvent effectively to reduce cost of material, protection of the environment, guarantees the safety of producing simultaneously.
The present invention is used for the high-elastic coating adhesive of water-based of cotton, pitted skin material, raw material weight ratio:
Octamethylcy-clotetrasiloxane 150～200,
DBSA 15～40,
Gamma-aminopropyl-triethoxy-silane 1～10,
γ-glycidyl ether oxygen propyl trimethoxy silicane 1～10,
Deionized water 400～600, through emulsion polymerisation, neutralization,
Add polyurethane resin finishing agent 150～230,
The thickening of use polyurethane thickener,
The high containing hydrogen silicone oil 15～38 that adds hydrogen content 1.5%～1.6%, the dibutyl tin laurate emulsion 15～38 of mass percent 18%～20% stirs,
The technical indicator of product:
Outward appearance: white thick liquid,
Solid content: (30 ± 2) %,
Viscosity: 2000-3500mpa.s,
PH value: 6 ± 1,
Ionic: the moon.
Due to the shelf-life that membership affects product that adds of containing hydrogen silicone oil and dibutyl tin laurate emulsion, so preferably add again in use.
Not adding the product before containing hydrogen silicone oil and dibutyl tin laurate emulsion and add the technical indicator of the product after hydrogen content silicone oil and dibutyl tin laurate emulsion not change, is mainly to affect the variation of viscosity between 2000-3500mpa.s.Little on solid content impact, substantially in solid content (30 ± 2) % scope.
Described polyurethane resin finishing agent comprises: the polyurethane resin NANO PU of Tuo Na company, the polyurethane resin SLK of German Rudoiph company, the polyurethane resin FS-550 of Liaoning Sunichem Co., Ltd..One or two kinds of mixing are used.
Described aqueous polyurethane thickener comprises: the polyurethane thickener CA-908 of Guangzhou Xuan Ning Chemical Industry Science Co., Ltd, and the polyurethane thickener PUR-50 of the loyal chemical industry in Shanghai, the polyurethane thickener MA-2 of the safe chemical industry of Nantong break, one or two kinds of mixing are used.
The high containing hydrogen silicone oil 15～38 that adds hydrogen content 1.5%～1.6% during use, the dibutyl tin laurate emulsion 15～38 of mass percent 18%～20% stirs.
The present invention for the preparation method of the high-elastic coating adhesive of water-based of cotton, pitted skin material is:
1, by 150～200 grams of octamethylcy-clotetrasiloxanes, 15～40 grams of DBSAs, 1～10 gram of gamma-aminopropyl-triethoxy-silane, 1～10 gram of γ-glycidyl ether oxygen propyl trimethoxy silicane, 400～600 grams of deionized waters stir and this mixed liquor logical going in the high pressure homogenizer of 30～40Mpa are made to emulsion, then join in the reactor of being furnished with condenser and agitating device, under 65～70 ℃ of conditions, react and within 10～12 hours, carry out emulsion polymerisation, then be cooled to 5～20 ℃ and continue reaction 3～5 hours, with mass percent 10% aqueous sodium carbonate, be adjusted to pH=7,
2, under normal temperature, in step 1 products therefrom, add 150～230 grams of polyurethane resin finishing agents, to be then adjusted to viscosity be 2000～3500 mpa.s to use polyurethane thickener.
3, the high containing hydrogen silicone oil 15～38 that adds hydrogen content 1.5%～1.6%, the dibutyl tin laurate emulsion 15～38 of mass percent 18%～20% stirs.
Due to the shelf-life that membership affects product that adds of containing hydrogen silicone oil and dibutyl tin laurate emulsion, so preferably join again in use in the product that step 2 obtains.
Described polyurethane resin finishing agent can be selected: the polyurethane resin NANO PU of Tuo Na company, the polyurethane resin SLK of German Rudoiph company, the polyurethane resin FS-550 of Liaoning Sunichem Co., Ltd..One or two kinds of mixing are used.
Described aqueous polyurethane thickener can be selected: the polyurethane thickener CA-908 of Guangzhou Xuan Ning Chemical Industry Science Co., Ltd, and the polyurethane thickener PUR-50 of the loyal chemical industry in Shanghai, the polyurethane thickener MA-2 of the safe chemical industry of Nantong break, one or two kinds of mixing are used.
Compared with prior art, the high-elastic coating adhesive technical advance of the water-based of cotton of the present invention, pitted skin material is:
1, in the high-elastic coating adhesive of water-based of cotton of the present invention, pitted skin material, first we select emulsion polymerisation process, the silane coupler of the silane coupler containing amino and epoxy radicals is reacted with silicone intermediate simultaneously, make the modified polyorganosiloxanes of high molecular weight.And the high-elastic glue of solvent type organosilicon is the method that adopts bulk polymerization, if introduce the silane coupler of the tri-alkoxy that contains amino or epoxy radicals in synthetic, is easy to cross-linking reaction occurs and makes modified polyorganosiloxanes gel.Because the present invention introduces amino in polysiloxane molecule, can make flexibility, slipping and the tearing brute force of fabric after coating greatly improve, simultaneously the structure of the tri-alkoxy in coupling agent can increase the self-crosslinking of product itself, can effectively improve elasticity and the wrinkle resistance of fabric after coating.
2, the high-elastic coating adhesive of water-based of cotton of the present invention, pitted skin material by composite polyurethane resin finishing agent can further improve the elasticity of coating adhesive on fabric and with the binding strength of fabric.Because selected several waterborne polyurethane resins all have rubber membrane sense, be simultaneously again pyrolysis closed form polyurethane, after heating-NCO group can with cotton, pitted skin material on-further there is cross-linking reaction, can effectively improve the washing resistance of coating fabric in OH.
3, the high-elastic coating adhesive of the water-based of cotton of the present invention, pitted skin material adopts water to replace solvent toluene, and the cost of material of the product effectively reducing has prevented the pollution on the environment due to the volatilization of a large amount of toluene, has avoided the potential safety hazard in coating production.
embodiment 1
1, by 150 grams of octamethylcy-clotetrasiloxanes, 22.5 grams of DBSAs, 1.5 grams of gamma-aminopropyl-triethoxy-silanes, 7.5 grams of γ-glycidyl ether oxygen propyl trimethoxy silicanes, 424 grams of deionized waters stir and this mixed liquor logical going in the high pressure homogenizer of 30Mpa are made to emulsion, then join in the reactor of being furnished with condenser and agitating device, under 65 ℃ of conditions, react and within 12 hours, carry out emulsion polymerisation, then be cooled to 15 ℃ and continue reaction 3 hours, with mass percent 10% aqueous sodium carbonate, be adjusted to pH=7.
2, under normal temperature, in step 1 products therefrom, add 180 grams of polyurethane resin NANO PU, then with polyurethane thickener CA-908, being adjusted to viscosity is 2500 mpa.s.
3,24.5 grams of high containing hydrogen silicone oils that add hydrogen content 1.5-1.6% in above-mentioned products therefrom, 20 grams of the dibutyl tin laurate emulsions of mass percent 18-20%, use stirs.
embodiment 2
1, by 200 grams of octamethylcy-clotetrasiloxanes, 36 grams of DBSAs, 8 grams of gamma-aminopropyl-triethoxy-silanes, 1.6 grams of γ-glycidyl ether oxygen propyl trimethoxy silicanes, 573 grams of deionized waters stir and this mixed liquor logical going in the high pressure homogenizer of 40Mpa are made to emulsion, then join in the reactor of being furnished with condenser and agitating device, under 70 ℃ of conditions, react and within 10 hours, carry out emulsion polymerisation, then be cooled to 10 ℃ and continue reaction 5 hours, with 10% aqueous sodium carbonate, be adjusted to pH=7.
2, under normal temperature, in step 1 products therefrom, add 230 grams of polyurethane resin NANO PU, then with polyurethane thickener MA-2, being adjusted to viscosity is 3000 mpa.s.
3,31.5 grams of high containing hydrogen silicone oils that add hydrogen content 1.5-1.6% in above-mentioned products therefrom, 24.5 grams of the dibutyl tin laurate emulsions of mass percent 18-20%, use stirs.
embodiment 3
1, by 189 grams of octamethylcy-clotetrasiloxanes, 15 grams of DBSAs, 4.7 grams of gamma-aminopropyl-triethoxy-silanes, 5 grams of γ-glycidyl ether oxygen propyl trimethoxy silicanes, 454 grams of deionized waters stir and this mixed liquor logical going in the high pressure homogenizer of 30Mpa are made to emulsion, then join in the reactor of being furnished with condenser and agitating device, under 65 ℃ of conditions, react and within 12 hours, carry out emulsion polymerisation, then be cooled to 5 ℃ and continue reaction 3 hours, with 10% aqueous sodium carbonate, be adjusted to pH=7.
2, under normal temperature, in step 1 products therefrom, add 167 grams of polyurethane resin NANO PU, then with polyurethane thickener PUR-50, being adjusted to viscosity is 3500 mpa.s.
3, in above-mentioned products therefrom, add 25 grams of the high containing hydrogen silicone oils of hydrogen content 1.5-1.6%, 33 grams of the dibutyl tin laurate emulsions of mass percent 18-20%, use stirs.
embodiment 4
1, by 150 grams of octamethylcy-clotetrasiloxanes, 22.5 grams of DBSAs, 2 grams of gamma-aminopropyl-triethoxy-silanes, 7.5 grams of γ-glycidyl ether oxygen propyl trimethoxy silicanes, 424 grams of deionized waters stir and this mixed liquor logical going in the high pressure homogenizer of 30Mpa are made to emulsion, then join in the reactor of being furnished with condenser and agitating device, under 65 ℃ of conditions, react and within 12 hours, carry out emulsion polymerisation, then be cooled to 15 ℃ and continue reaction 3 hours, with 10% aqueous sodium carbonate, be adjusted to pH=7.
2, under normal temperature, in step 1 products therefrom, add 180 grams of polyurethane resin SLK, then with polyurethane thickener CA-908, being adjusted to viscosity is 2500 mpa.s.
3,24.5 grams of high containing hydrogen silicone oils that add hydrogen content 1.5-1.6% in above-mentioned products therefrom, 20 grams of the dibutyl tin laurate emulsions of mass percent 18-20%, use stirs.
embodiment 5
1, by 200 grams of octamethylcy-clotetrasiloxanes, 36 grams of DBSAs, 8 grams of gamma-aminopropyl-triethoxy-silanes, 1.6 grams of γ-glycidyl ether oxygen propyl trimethoxy silicanes, 573 grams of deionized waters stir and this mixed liquor logical going in the high pressure homogenizer of 40Mpa are made to emulsion, then join in the reactor of being furnished with condenser and agitating device, under 70 ℃ of conditions, react and within 10 hours, carry out emulsion polymerisation, then be cooled to 10 ℃ and continue reaction 5 hours, with 10% aqueous sodium carbonate, be adjusted to pH=7.
2, under normal temperature, in step 1 products therefrom, add 230 grams of polyurethane resin SLK, then with polyurethane thickener MA-2, being adjusted to viscosity is 3000 mpa.s.
3,31.5 grams of high containing hydrogen silicone oils that add hydrogen content 1.5-1.6% in above-mentioned products therefrom, 24.5 grams of the dibutyl tin laurate emulsions of mass percent 18-20%, use stirs.
embodiment 6
1, by 189 grams of octamethylcy-clotetrasiloxanes, 15 grams of DBSAs, 4.7 grams of gamma-aminopropyl-triethoxy-silanes, 5 grams of γ-glycidyl ether oxygen propyl trimethoxy silicanes, 454 grams of deionized waters stir and this mixed liquor logical going in the high pressure homogenizer of 30Mpa are made to emulsion, then join in the reactor of being furnished with condenser and agitating device, under 65 ℃ of conditions, react and within 12 hours, carry out emulsion polymerisation, then be cooled to 5 ℃ and continue reaction 3 hours, with 10% aqueous sodium carbonate, be adjusted to pH=7.
2, under normal temperature, in step 1 products therefrom, add 167 grams of polyurethane resin FS-550, then with polyurethane thickener PUR-50, being adjusted to viscosity is 3500 mpa.s.
3,25 grams of high containing hydrogen silicone oils that add hydrogen content 1.5-1.6% in above-mentioned products therefrom, 33 grams of the dibutyl tin laurate emulsions of mass percent 18-20%, use stirs.
Properties of product test:
The pure-cotton fabric and the specification that by embodiment and comparative example, are 40*40,133*72 in specification are to carry out coating on 21S*21S, 52*53 flax fabric simultaneously, and controlling coating weight is 25 grams/m-
2, under 100 ℃ of conditions, dry, 170 ℃ bake 1min.
Test result is as follows:
The evaluation of pliability is as the criterion to the comprehensive evaluation result of feel with 6 people, ++++be best ,+for the poorest.
Creasy recovery angle is pressed GB/T3819-1997 test
Comparative example 1 product used is the high-elastic coating adhesive FS-850U of Liaoning Sunichem Co., Ltd.'s solvent-borne type.
As can be seen from the above table, the flexibility of the fabric after embodiment coating is better than comparative example 1.Although the creasy recovery angle of the fabric after comparative example 1 coating is close with embodiment before washing, to wash after 5 times, its creasy recovery angle obviously reduces.
Claims (5)
1. for the high-elastic coating adhesive of water-based cotton, pitted skin material, it is characterized in that:
Raw material weight ratio,
Octamethylcy-clotetrasiloxane 150～200,
DBSA 15～40,
Gamma-aminopropyl-triethoxy-silane 1～10,
γ-glycidyl ether oxygen propyl trimethoxy silicane 1～10,
Deionized water 400～600, through emulsion polymerisation, neutralization,
Add polyurethane resin finishing agent 150～230,
The thickening of use polyurethane thickener,
The technical indicator of product:
Outward appearance: white thick liquid,
Solid content: (30 ± 2) %,
Viscosity: 2000-3500mpa.s,
PH value: 6 ± 1,
Ionic: the moon.
2. the high-elastic coating adhesive of water-based of cotton according to claim 1, pitted skin material, is characterized in that:
Described polyurethane resin finishing agent is: the polyurethane resin NANO PU of Tuo Na company, the polyurethane resin SLK of German Rudoiph company, the polyurethane resin FS-550 one of Liaoning Sunichem Co., Ltd.;
Described aqueous polyurethane thickener is: the polyurethane thickener CA-908 of Guangzhou Xuan Ning Chemical Industry Science Co., Ltd, and the polyurethane thickener PUR-50 of the loyal chemical industry in Shanghai, the polyurethane thickener MA-2 of the safe chemical industry of Nantong break, one or two kinds of mixing are used.
3. the high-elastic coating adhesive of water-based of cotton according to claim 1, pitted skin material, it is characterized in that: during use, add raw material weight ratio: the high containing hydrogen silicone oil 15～38 of hydrogen content 1.5%～1.6%, the dibutyl tin laurate emulsion 15～38 of mass percent 18%～20% stirs.
4. for the preparation method of the high-elastic coating adhesive of water-based of cotton, pitted skin material, it is characterized in that:
(1), by 150～200 grams of octamethylcy-clotetrasiloxanes, 15～40 grams of DBSAs, 1～10 gram of gamma-aminopropyl-triethoxy-silane, 1～10 gram of γ-glycidyl ether oxygen propyl trimethoxy silicane, 400～600 grams of deionized waters stir and this mixed liquor logical going in the high pressure homogenizer of 30～40Mpa are made to emulsion, then join in the reactor of being furnished with condenser and agitating device, under 65～70 ℃ of conditions, react and within 10～12 hours, carry out emulsion polymerisation, then be cooled to 5～20 ℃ and continue reaction 3～5 hours, with mass percent 10% aqueous sodium carbonate, be adjusted to pH=7,
(2), in step 1 products therefrom, add 150～230 grams of polyurethane resin finishing agents under normal temperature, then use polyurethane thickener to be adjusted to viscosity be 2500～3500 mpa.s;
(3), add the high containing hydrogen silicone oil 15～38 of hydrogen content 1.5%～1.6%, the dibutyl tin laurate emulsion 15～38 of mass percent 18%～20% stirs;
Due to the shelf-life that membership affects product that adds of silicone oil and dibutyl tin laurate emulsion, add in use in the product that step 2 obtains.
5. the preparation method of the high-elastic coating adhesive of water-based of cotton according to claim 4, pitted skin material, is characterized in that:
Described polyurethane resin finishing agent is: the polyurethane resin NANO PU of Tuo Na company, the polyurethane resin SLK of German Rudoiph company, the polyurethane resin FS-550 of Liaoning Sunichem Co., Ltd., one;
Described aqueous polyurethane thickener is: the polyurethane thickener CA-908 of Guangzhou Xuan Ning Chemical Industry Science Co., Ltd, and the polyurethane thickener PUR-50 of the loyal chemical industry in Shanghai, the polyurethane thickener MA-2 of the safe chemical industry of Nantong break, one or two kinds of mixing are used.
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| CN103741326B (en) * | 2013-12-17 | 2015-03-25 | 葛小飞 | Method for preparing wear-proof cotton and linen fabric |
| CN113957724B (en) * | 2021-12-01 | 2024-02-20 | 辽宁恒星精细化工有限公司 | Water-based organic silicon high-elasticity coating adhesive for textiles and preparation method thereof |
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| JPS5094030A (en) * | 1973-11-26 | 1975-07-26 | ||
| JPS6243424A (en) * | 1985-08-20 | 1987-02-25 | Shin Etsu Chem Co Ltd | Production of silsesquioxane emulsion |
| JP3807850B2 (en) * | 1998-07-16 | 2006-08-09 | 信越化学工業株式会社 | Silicone emulsion composition and air bag base fabric surface-treated with the same |
| GB9826394D0 (en) * | 1998-12-02 | 1999-01-27 | Dow Corning Sa | Method of making silicone-in-water emulsions |
| US6214928B1 (en) * | 1999-11-02 | 2001-04-10 | General Electric Company | Aqueous emulsions of amine-functionalized organopolysiloxanes and method |
| WO2004109008A1 (en) * | 2003-06-04 | 2004-12-16 | Dow Corning Corporation | Silicone/polyurethane coated fabrics |
| CN1297591C (en) * | 2005-03-07 | 2007-01-31 | 华明扬 | Process for preparing anion composite modified organosilicon emulsion |
| JP2007051236A (en) * | 2005-08-19 | 2007-03-01 | Shin Etsu Chem Co Ltd | Silicone emulsion composition and method for treating wood |
| CN100537890C (en) * | 2006-01-18 | 2009-09-09 | 丹东恒星精细化工有限公司 | Finishing agent of polysiloxane fiber and production method |
| US20070244249A1 (en) * | 2006-04-06 | 2007-10-18 | General Electric Company | Two-part translucent silicone rubber-forming composition |
| CN101323665B (en) * | 2008-07-21 | 2010-12-29 | 华明扬 | Preparation of organosilicon amphoteric microemulsion |
| CN101671958B (en) * | 2009-10-13 | 2011-10-26 | 辽宁恒星精细化工（集团）有限公司 | Polysiloxane crease resistant finishing agent composition for natural fiber and preparation method thereof |
| CN101747511B (en) * | 2010-01-20 | 2011-08-03 | 华东理工大学 | Polysiloxane containing fluorine and application thereof |
| 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 |
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