CN104449486A - Preparation method and application of high temperature solvent resistant acrylate pressure sensitive adhesive - Google Patents
Preparation method and application of high temperature solvent resistant acrylate pressure sensitive adhesive Download PDFInfo
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- CN104449486A CN104449486A CN201410719116.0A CN201410719116A CN104449486A CN 104449486 A CN104449486 A CN 104449486A CN 201410719116 A CN201410719116 A CN 201410719116A CN 104449486 A CN104449486 A CN 104449486A
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Abstract
The invention relates to a high temperature solvent resistant acrylate pressure sensitive adhesive which comprises the following components in parts by weight: 150-250 parts of 2-ethylhexyl acrylate, 50-100 parts of butyl acrylate, 3-10 parts of acrylic acid, 3-10 parts of hydroxyethyl acrylate, 10-20 parts of vinyl acetate, 15-35 parts of bornyl isoacrylate, 0.5-3 parts of azobisisobutyronitrile, 0.3-2 parts of N-hydroxymethyl acrylamide and 400-600 parts of ethyl acetate. The mechanical property, high temperature resistance and weather resistance of the emulsion type acrylate pressure sensitive adhesive are improved, so that the application range of the emulsion type acrylate pressure sensitive adhesive is widened, and the pressure sensitive adhesive has the characteristics of high viscidity, high temperature resistance, damp-heat aging resistance and low cost.
Description
Technical field
The invention belongs to pressure sensitive adhesive technical field, relate to a kind of preparation method and application thereof of high temperature resistant solvent-type acrylic ester pressure-sensitive adhesive.
Background technology
The adhesive tape mainly Acrylic Pressure Sensitive Adhesive at present involved door for microwave oven body applied, its main purpose is the protection of a body, has the effects such as explosion-proof, anti-microwave radiation.Major requirement is resistance to elevated temperatures.Universality microwave oven door label requires high temperature resistant 180 DEG C usually, and with baking function is high-power etc., high-end microwave oven then requires high temperature resistant 210 DEG C.Therefore, solvent-type acrylic ester pressure-sensitive adhesive developing direction is resistance to elevated temperatures.
Its requirement of high-temperature-resistant microwave oven door subsides solvent-type acrylic ester pressure-sensitive adhesive involved by patent CN 102516892 A is that 90 ° of stripping strengths are greater than 10N/25mm, and high temperature 210 DEG C toasts after 30 minutes without requirements such as warping, fog.And the present invention emphasizes to coat on 100um particular polyesters film, toast 8 minutes at 130-135 DEG C, its dry glue thickness is the pressure sensitive adhesive of 30-35um, its 180 ° of stripping strengths are greater than 900N/m, just glue and be greater than 12# ball (rolling ball method), hold tack is greater than 24 hours, and laminating microwave oven door-plate is greater than 96 hours without layering, bulge phenomenon, 210 DEG C of bakings in high temperature 190 DEG C of bakings and is greater than 2 hours still without layering, bulge phenomenon.Involved by patent CN 10330515154 A be adopt main rubber (being made up of natural rubber and synthetic rubber), supplementary additive, softening agent, solvent and solidifying agent form.And being mainly used on U.S. line paper, its heat resistance is 120 DEG C.Patent 201010521734 mainly by silicone resin modification acrylate to improve its heat resistance, its cost is high.
Summary of the invention
In order to overcome the above-mentioned shortcoming of prior art, the invention provides one there is viscosity high, high temperature resistant, wet and heat ageing resistant, and the preparation method of the high temperature resistant solvent-type acrylic ester pressure-sensitive adhesive of the low feature of cost and application thereof.
The technical solution adopted for the present invention to solve the technical problems is: a kind of high temperature resistant solvent-type acrylic ester pressure-sensitive adhesive, and it is polymerized according to its weight ratio by following component:
Isooctyl acrylate monomer 150-250
Butyl acrylate 50-100
Vinylformic acid 3-10
Hydroxyethyl acrylate 3-10
Vinyl acetate 10-20
Isobomyl acrylate acid esters 15-35
Azo Diisopropyl azodicarboxylate 0.5-3
N hydroxymethyl acrylamide 0.3-2
Ethyl acetate 400-600
The preparation method of above-mentioned high temperature resistant solvent-type acrylic ester pressure-sensitive adhesive, its preparation process is:
The first step: choose the azo Diisopropyl azodicarboxylate that 250-350 ethyl acetate dissolves 0.5-2 wherein according to above-mentioned weight ratio, dissolve at the vinyl acetate adding the Isooctyl acrylate monomer of 150-250,50-100 butyl acrylate, 15-35 isobomyl acrylate acid esters and 10-20 wherein completely, preparation mixed monomer solution A; Again with the Hydroxyethyl acrylate preparation mixed monomer solution B of the N hydroxymethyl acrylamide of 50-150 acetic acid ethyl dissolution 0.3-2, the vinylformic acid of 3-10 and 3-10;
Second step: the mixed monomer solution A obtained in the first step and mixed monomer solution B is mixed, and divides equally 2 parts, portion is mixed monomer solution C, and another part is mixed monomer solution D;
3rd step: choose 50-100 acetic acid ethyl dissolution 0.4-1 azo Diisopropyl azodicarboxylate, is evenly divided into two parts after preparation initiator, is respectively initiator solution E and initiator solution F;
4th step: choose the ethyl acetate of 50-100 to add in reactor and be warming up to 78-80 DEG C, start after maintaining stable backflow at the uniform velocity to drip mixed monomer solution C to ethyl acetate, time for adding is 2-2.5 hour, dropwise rear insulation 2 hours, and keep temperature of reaction kettle to control at 80-82 DEG C;
5th step: at the uniform velocity drip another part of mixed monomer solution D to mixed solution obtained in the 4th step, time for adding is 2-2.5 hour, after dropwising, more at the uniform velocity add initiator solution E to above-mentioned obtained mixed solution, time for adding is 20-30 minute, dropwise rear insulation after 1 hour, again in mixed solution, at the uniform velocity add initiator solution F, time for adding is 20-30 minute, finally, be incubated 2 hours, and temperature of reaction is controlled at 80-82 DEG C;
6th step: blowing after the temperature of reaction of the 5th step being dropped to less than 45 DEG C, obtained high temperature resistant solvent-type acrylic ester pressure-sensitive adhesive.
The solid of the high temperature resistant solvent-type acrylic ester pressure-sensitive adhesive prepared in described 6th step contains for 40-45%, and monomer conversion is higher than 98%, and viscosity is 1000 ± 250cp.
The application of above-mentioned high temperature resistant solvent-type acrylic ester pressure-sensitive adhesive, its applying step is as follows:
100 high temperature resistant solvent-type acrylic ester pressure-sensitive adhesives are chosen according to weight ratio, add the mixture of 0.01-0.1 part TriMethylolPropane(TMP)-three (3-'-aziridino) propionic ester, coat on 100um polyester film, toast 8 minutes at 130-135 DEG C, its dry glue thickness is the pressure sensitive adhesive of 30-35um, its 180 ° of stripping strengths are greater than 900N/m, just glue and be greater than 12# ball (rolling ball method), hold tack is greater than 24 hours, laminating microwave oven door-plate is greater than 96 hours without layering in high temperature 190 DEG C of bakings, bulge phenomenon, 210 DEG C of bakings are greater than 2 hours still without layering, bulge phenomenon, obtained high temperature resistant solvent-type acrylic ester pressure-sensitive adhesive tape.
The invention has the beneficial effects as follows: improve the mechanical property of development of Acrylate Emulsion Pressure-Sensitive Adhesive and high thermal resistance and weathering resistance, thus improve the range of application of development of Acrylate Emulsion Pressure-Sensitive Adhesive, there is viscosity high, high temperature resistant, wet and heat ageing resistant, and the feature that cost is low.
Embodiment
The present invention is further described for embodiment below.
A kind of high temperature resistant solvent-type acrylic ester pressure-sensitive adhesive, it is polymerized according to its weight ratio by following component:
Isooctyl acrylate monomer 150-250
Butyl acrylate 50-100
Vinylformic acid 3-10
Hydroxyethyl acrylate 3-10
Vinyl acetate 10-20
Isobomyl acrylate acid esters 15-35
Azo Diisopropyl azodicarboxylate 0.5-3
N hydroxymethyl acrylamide 0.3-2
Ethyl acetate 400-600
The preparation method of above-mentioned high temperature resistant solvent-type acrylic ester pressure-sensitive adhesive, its preparation process is:
The first step: choose the azo Diisopropyl azodicarboxylate that 250-350 ethyl acetate dissolves 0.5-2 wherein according to above-mentioned weight ratio, dissolve at the vinyl acetate adding the Isooctyl acrylate monomer of 150-250,50-100 butyl acrylate, 15-35 isobomyl acrylate acid esters and 10-20 wherein completely, preparation mixed monomer solution A; Again with the Hydroxyethyl acrylate preparation mixed monomer solution B of the N hydroxymethyl acrylamide of 50-150 acetic acid ethyl dissolution 0.3-2, the vinylformic acid of 3-10 and 3-10;
Second step: the mixed monomer solution A obtained in the first step and mixed monomer solution B is mixed, and divides equally 2 parts, portion is mixed monomer solution C, and another part is mixed monomer solution D;
3rd step: choose 50-100 acetic acid ethyl dissolution 0.4-1 azo Diisopropyl azodicarboxylate, is evenly divided into two parts after preparation initiator, is respectively initiator solution E and initiator solution F;
4th step: choose the ethyl acetate of 50-100 to add in reactor and be warming up to 78-80 DEG C, start after maintaining stable backflow at the uniform velocity to drip mixed monomer solution C to ethyl acetate, time for adding is 2-2.5 hour, dropwise rear insulation 2 hours, and keep temperature of reaction kettle to control at 80-82 DEG C;
5th step: at the uniform velocity drip another part of mixed monomer solution D to mixed solution obtained in the 4th step, time for adding is 2-2.5 hour, after dropwising, more at the uniform velocity add initiator solution E to above-mentioned obtained mixed solution, time for adding is 20-30 minute, dropwise rear insulation after 1 hour, again in mixed solution, at the uniform velocity add initiator solution F, time for adding is 20-30 minute, finally, be incubated 2 hours, and temperature of reaction is controlled at 80-82 DEG C;
6th step: blowing after the temperature of reaction of the 5th step being dropped to less than 45 DEG C, obtained high temperature resistant solvent-type acrylic ester pressure-sensitive adhesive.
The solid of the high temperature resistant solvent-type acrylic ester pressure-sensitive adhesive prepared in described 6th step contains for 40-45%, and monomer conversion is higher than 98%, and viscosity is 1000 ± 250cp.
The application of above-mentioned high temperature resistant solvent-type acrylic ester pressure-sensitive adhesive, its applying step is as follows:
100 high temperature resistant solvent-type acrylic ester pressure-sensitive adhesives are chosen according to weight ratio, add the mixture of 0.01-0.1 part TriMethylolPropane(TMP)-three (3-'-aziridino) propionic ester, coat on 100um polyester film, toast 8 minutes at 130-135 DEG C, its dry glue thickness is the pressure sensitive adhesive of 30-35um, its 180 ° of stripping strengths are greater than 900N/m, just glue and be greater than 12# ball (rolling ball method), hold tack is greater than 24 hours, laminating microwave oven door-plate is greater than 96 hours without layering in high temperature 190 DEG C of bakings, bulge phenomenon, 210 DEG C of bakings are greater than 2 hours still without layering, bulge phenomenon, obtained high temperature resistant solvent-type acrylic ester pressure-sensitive adhesive tape.
Embodiment 1
A kind of type of resistance to high solvent Acrylic Pressure Sensitive Adhesive, it is polymerized according to its weight ratio by following component:
Isooctyl acrylate monomer 200
Butyl acrylate 70
Vinylformic acid 5
Hydroxyethyl acrylate 5
Vinyl acetate 12
Isobomyl acrylate acid esters 25
Azo Diisopropyl azodicarboxylate 1.6
N hydroxymethyl acrylamide 0.5
Ethyl acetate 600
The preparation method of above-mentioned high temperature resistant solvent-type acrylic ester pressure-sensitive adhesive, its preparation process is:
The first step: choose 400 ethyl acetate according to above-mentioned weight ratio, and dissolve 1 azo Diisopropyl azodicarboxylate wherein, dissolve to add completely 200 Isooctyl acrylate monomer, 70 butyl acrylates, 25 isobomyl acrylate acid esters and 12 vinyl acetate, preparation mixed monomer solution A; With N hydroxymethyl acrylamide, the vinylformic acid of 5, the Hydroxyethyl acrylate preparation mixed monomer solution B of 5 of 100 acetic acid ethyl dissolutions 0.5;
Second step: mixed monomer solution A and mixed monomer solution B is mixed, and divides equally 2 parts, portion is mixed monomer solution C, and another part is mixed monomer solution D;
3rd step: with the azo Diisopropyl azodicarboxylate of the acetic acid ethyl dissolution 0.4-1 of 50, is evenly divided into two parts after preparation initiator, is respectively initiator solution E and initiator solution F;
4th step: the ethyl acetate of 50 is added in reactor and is warming up to 78-80 DEG C, start after maintaining stable backflow at the uniform velocity to drip mixed monomer solution C, time for adding is 2-2.5 hour, dropwises rear insulation 2 hours, and keeps temperature of reaction kettle to control at 80-82 DEG C;
5th step: at the uniform velocity drip another part of mixed monomer solution D in the mixed solution that the 4th step is obtained, time for adding is 2-2.5 hour, after dropwising, at the uniform velocity add initiator solution E, time for adding is 20-30 minute, dropwises rear insulation after 1 hour, again at the uniform velocity add initiator solution F, time for adding is 20-30 minute, finally, is incubated 2 hours and controls at 80-82 DEG C by temperature of reaction;
6th step: blowing after temperature of reaction being dropped to less than 45 DEG C, obtained high temperature resistant solvent-type acrylic ester pressure-sensitive adhesive.
Embodiment 2
A kind of type of resistance to high solvent Acrylic Pressure Sensitive Adhesive, it is polymerized according to its weight ratio by following component:
Isooctyl acrylate monomer 150
Butyl acrylate 90
Vinylformic acid 5
Hydroxyethyl acrylate 5
Vinyl acetate 12
Isobomyl acrylate acid esters 18
Azo Diisopropyl azodicarboxylate 1.6
N hydroxymethyl acrylamide 0.7
Ethyl acetate 500
The preparation method of above-mentioned high temperature resistant solvent-type acrylic ester pressure-sensitive adhesive, its preparation process is as follows:
The first step: the azo Diisopropyl azodicarboxylate choosing 300 acetic acid ethyl dissolutions 1 according to above-mentioned weight ratio, dissolve to add completely 150 Isooctyl acrylate monomer, 90 butyl acrylates, 18 isobomyl acrylate acid esters and 12 parts vinyl acetate, preparation mixed monomer solution A; Again with 100 N hydroxymethyl acrylamide, the vinylformic acid of 5, the Hydroxyethyl acrylate preparation mixed monomer solution B of 5 of acetic acid ethyl dissolution 0.7;
Second step: mixed monomer solution A and mixed monomer solution B is mixed, and divides equally 2 parts, portion is mixed monomer solution C, and another part is mixed monomer solution D;
3rd step: with the azo Diisopropyl azodicarboxylate of the acetic acid ethyl dissolution 0.4-1 of 50, is evenly divided into two parts after preparation initiator, is respectively initiator solution E and initiator solution F;
4th step: the ethyl acetate of 50 is added in reactor and is warming up to 78-80 DEG C, start after maintaining stable backflow at the uniform velocity to drip mix monomer C, time for adding is 2-2.5 hour, dropwises rear insulation 2 hours and controls at 80-82 DEG C by temperature of reaction kettle;
5th step: the mixed solution obtained to the 4th step at the uniform velocity drips another part of mixed monomer solution D, time for adding is 2-2.5 hour, after dropwising, open and at the uniform velocity add initiator solution E, time for adding is 20-30 minute, dropwise rear insulation after 1 hour, again at the uniform velocity add initiator solution F, time for adding is 20-30 minute.Finally, be incubated 2 hours and temperature of reaction is controlled at 80-82 DEG C;
6th step: blowing after temperature of reaction being dropped to less than 45 DEG C, obtained high temperature resistant solvent-type acrylic ester pressure-sensitive adhesive.
Embodiment 3
1, the type of a resistance to high solvent Acrylic Pressure Sensitive Adhesive, it is polymerized according to its weight ratio by following component:
Isooctyl acrylate monomer 180
Butyl acrylate 60
Vinylformic acid 5
Hydroxyethyl acrylate 5
Vinyl acetate 12
Isobomyl acrylate acid esters 22
Azo Diisopropyl azodicarboxylate 1.6
N hydroxymethyl acrylamide 0.5
Ethyl acetate 500
The preparation method of above-mentioned high temperature resistant solvent-type acrylic ester pressure-sensitive adhesive, its preparation process is:
The first step: choose 300 ethyl acetate according to above-mentioned weight ratio and to the azo Diisopropyl azodicarboxylate dissolving 1 in it, dissolve to add completely 180 Isooctyl acrylate monomer, 60 butyl acrylates, 22 isobomyl acrylate acid esters and 12 vinyl acetate, preparation mixed monomer solution A; With N hydroxymethyl acrylamide, the vinylformic acid of 5, the Hydroxyethyl acrylate preparation mixed monomer solution B of 5 parts of 100 acetic acid ethyl dissolutions 1;
Second step: mixed monomer solution A and mixed monomer solution B is mixed, and divides equally 2 parts, portion is mixed monomer solution C, and another part is mixed monomer solution D;
3rd step: the azo Diisopropyl azodicarboxylate of the acetic acid ethyl dissolution 0.6 with 50, is evenly divided into two parts after preparation initiator, is respectively initiator solution E and initiator solution F;
4th step: the ethyl acetate of 50 is added in reactor and is warming up to 78-80 DEG C, start after maintaining stable backflow at the uniform velocity to drip mixed monomer solution C, time for adding is 2-2.5 hour, dropwises rear insulation 2 hours and controls at 80-82 DEG C by temperature of reaction kettle;
5th step: the mixed solution prepared in the 4th step at the uniform velocity drips another part of mixed monomer solution D, and time for adding is 2-2.5 hour, after dropwising, at the uniform velocity adds initiator solution E, and time for adding is 20-30 minute.Dropwise rear insulation after 1 hour, again at the uniform velocity add initiator solution F, time for adding is 20-30 minute.Finally, be incubated 2 hours and temperature of reaction is controlled at 80-82 DEG C;
6th step: blowing after temperature of reaction being dropped to less than 45 DEG C, obtained high temperature resistant solvent-type acrylic ester pressure-sensitive adhesive.
The present invention improves the mechanical property of development of Acrylate Emulsion Pressure-Sensitive Adhesive and high thermal resistance and weathering resistance, thus improves the range of application of development of Acrylate Emulsion Pressure-Sensitive Adhesive, has viscosity high, high temperature resistant, wet and heat ageing resistant, and the feature that cost is low.
Claims (4)
1. a high temperature resistant solvent-type acrylic ester pressure-sensitive adhesive, is characterized in that being polymerized according to its weight ratio by following component:
Isooctyl acrylate monomer 150-250
Butyl acrylate 50-100
Vinylformic acid 3-10
Hydroxyethyl acrylate 3-10
Vinyl acetate 10-20
Isobomyl acrylate acid esters 15-35
Azo Diisopropyl azodicarboxylate 0.5-3
N hydroxymethyl acrylamide 0.3-2
Ethyl acetate 400-600.
2. the preparation method of above-mentioned high temperature resistant solvent-type acrylic ester pressure-sensitive adhesive, is characterized in that preparation process is:
The first step: choose the azo Diisopropyl azodicarboxylate that 250-350 ethyl acetate dissolves 0.5-2 wherein according to above-mentioned weight ratio, dissolve at the vinyl acetate adding the Isooctyl acrylate monomer of 150-250,50-100 butyl acrylate, 15-35 isobomyl acrylate acid esters and 10-20 wherein completely, preparation mixed monomer solution A; Again with the Hydroxyethyl acrylate preparation mixed monomer solution B of the N hydroxymethyl acrylamide of 50-150 acetic acid ethyl dissolution 0.3-2, the vinylformic acid of 3-10 and 3-10;
Second step: the mixed monomer solution A obtained in the first step and mixed monomer solution B is mixed, and divides equally 2 parts, portion is mixed monomer solution C, and another part is mixed monomer solution D;
3rd step: choose 50-100 acetic acid ethyl dissolution 0.4-1 azo Diisopropyl azodicarboxylate, is evenly divided into two parts after preparation initiator, is respectively initiator solution E and initiator solution F;
4th step: choose the ethyl acetate of 50-100 to add in reactor and be warming up to 78-80 DEG C, start after maintaining stable backflow at the uniform velocity to drip mixed monomer solution C to ethyl acetate, time for adding is 2-2.5 hour, dropwise rear insulation 2 hours, and keep temperature of reaction kettle to control at 80-82 DEG C;
5th step: at the uniform velocity drip another part of mixed monomer solution D to mixed solution obtained in the 4th step, time for adding is 2-2.5 hour, after dropwising, more at the uniform velocity add initiator solution E to above-mentioned obtained mixed solution, time for adding is 20-30 minute, dropwise rear insulation after 1 hour, again in mixed solution, at the uniform velocity add initiator solution F, time for adding is 20-30 minute, finally, be incubated 2 hours, and temperature of reaction is controlled at 80-82 DEG C;
6th step: blowing after the temperature of reaction of the 5th step being dropped to less than 45 DEG C, obtained high temperature resistant solvent-type acrylic ester pressure-sensitive adhesive.
3. the preparation method of high temperature resistant solvent-type acrylic ester pressure-sensitive adhesive as claimed in claim 2, it is characterized in that the solid containing being 40-45% of the high temperature resistant solvent-type acrylic ester pressure-sensitive adhesive prepared in described 6th step, monomer conversion is higher than 98%, and viscosity is 1000 ± 250cp.
4. the application of above-mentioned high temperature resistant solvent-type acrylic ester pressure-sensitive adhesive, is characterized in that applying step is as follows:
100 high temperature resistant solvent-type acrylic ester pressure-sensitive adhesives are chosen according to weight ratio, add the mixture of 0.01-0.1 part TriMethylolPropane(TMP)-three (3-'-aziridino) propionic ester, coat on 100um polyester film, toast 8 minutes at 130-135 DEG C, its dry glue thickness is the pressure sensitive adhesive of 30-35um, its 180 ° of stripping strengths are greater than 900N/m, just glue and be greater than 12# ball (rolling ball method), hold tack is greater than 24 hours, laminating microwave oven door-plate is greater than 96 hours without layering in high temperature 190 DEG C of bakings, bulge phenomenon, 210 DEG C of bakings are greater than 2 hours still without layering, bulge phenomenon, obtained high temperature resistant solvent-type acrylic ester pressure-sensitive adhesive tape.
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CN112195004A (en) * | 2020-09-01 | 2021-01-08 | 毕斯文 | High-temperature-resistant pressure-sensitive adhesive composition |
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CN114921199A (en) * | 2022-06-07 | 2022-08-19 | 东莞市胜昊新材料科技有限公司 | Solvent type high-stripping-force high-temperature-resistant high-humidity-resistant glue and preparation method thereof |
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