CN104449486B - The preparation method and applications of high temperature resistant solvent-type acrylic ester pressure-sensitive adhesive - Google Patents
The preparation method and applications of high temperature resistant solvent-type acrylic ester pressure-sensitive adhesive Download PDFInfo
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Abstract
The present invention relates to a kind of high temperature resistant solvent-type acrylic ester pressure-sensitive adhesive, its component and weight ratio Isooctyl acrylate monomer 150 250, butyl acrylate 50 100, acrylic acid 3 10,2-(Acryloyloxy)ethanol 3 10, vinylacetate 10 20, isobomyl acrylate acid esters 15 35, azo azodiisobutyronitrile 0.5 3, N n-methylolacrylamide 0.3 2 and ethyl acetate 400 600.Improve the mechanical property of development of Acrylate Emulsion Pressure-Sensitive Adhesive and heat-resisting quantity and weatherability, 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 of low cost.
Description
Technical field
The invention belongs to pressure sensitive adhesive technical field, relate to the preparation of a kind of high temperature resistant solvent-type acrylic ester pressure-sensitive adhesive
Method and application thereof.
Background technology
The adhesive tape applied in the most involved microwave oven door body is mainly Acrylic Pressure Sensitive Adhesive, its main mesh
Be the protection of door body, there is the effects such as explosion-proof, anti-microwave radiation.Major requirement is resistance to elevated temperatures.Universality door for microwave oven
Patch usually requires that high temperature resistant 180 DEG C, then requires high temperature resistant 210 DEG C with high-end microwave ovens such as baking function are high-power.Therefore,
One developing direction of solvent-type acrylic ester pressure-sensitive adhesive is resistance to elevated temperatures.
Involved by patent CN 102516892 A, high-temperature-resistant microwave oven door patch uses solvent-type acrylic ester pressure-sensitive adhesive
It requires is 90 ° of peel strengths more than 10N/25mm, high temperature 210 DEG C toast 30 minutes after without requirements such as warping, fog.And this
Invention is emphasized to coat on 100um particular polyesters thin film, toasts 8 minutes at 130-135 DEG C, and its dry glue thickness is 30-35um
Pressure sensitive adhesive, its 180 ° of peel strengths are more than 900N/m, and just viscous more than 12# ball (rolling ball method), holding power is more than 24 hours, laminating
Microwave oven door-plate toasts high temperature 190 DEG C and was more than 2 hours still without dividing more than 96 hours without layering, bulge phenomenon, 210 DEG C of bakings
Layer, bulge phenomenon.Involved by patent CN 10330515154 A is to use main rubber (by natural rubber and synthetic rubber
Composition), auxiliary additive, plasticizer, solvent and firming agent composition.And be mainly used on U.S. stricture of vagina paper, its heat resistance is 120
℃.Patent 201010521734 is mainly by organic siliconresin modification acrylate to improve its heat resistance, and its cost is high.
Summary of the invention
In order to overcome the disadvantages mentioned above of prior art, it is high that the present invention provides one to have viscosity, high temperature resistant, wet-heat resisting is old
Change, and the preparation method and applications of the high temperature resistant solvent-type acrylic ester pressure-sensitive adhesive of low cost feature.
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
Stick, it is polymerized according to its weight ratio by following component:
Isooctyl acrylate monomer 150-250
Butyl acrylate 50-100
Acrylic acid 3-10
2-(Acryloyloxy)ethanol 3-10
Vinylacetate 10-20
Isobomyl acrylate acid esters 15-35
Azo azodiisobutyronitrile 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: choosing 250-350 ethyl acetate according to above-mentioned weight ratio, to dissolve the azo azo two of 0.5-2 wherein different
Butyronitrile, is being added thereto to the Isooctyl acrylate monomer of 150-250,50-100 butyl acrylate, 15-35 acrylic acid after dissolving completely
Isoborneol acid esters and the vinylacetate of 10-20, prepare mixed monomer solution A;Again with 50-150 acetic acid ethyl dissolution 0.3-2's
The 2-(Acryloyloxy)ethanol preparation mixed monomer solution B of N hydroxymethyl acrylamide, the acrylic acid of 3-10 and 3-10;
Second step: by the mixed monomer solution A prepared in the first step and mixed monomer solution B mix homogeneously, and divide equally 2
Part, 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 azodiisobutyronitrile, uniformly divide after preparation initiator
It is two parts, respectively initiator solution E and initiator solution F;
4th step: choose in the ethyl acetate of 50-100 is added reactor and be warming up to 78-80 DEG C, maintains stable returning
Starting at the uniform velocity to drip to ethyl acetate mixed monomer solution C after stream, time for adding is 2-2.5 hour, is incubated 2 little after dropping
Time, 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, time for adding to the mixed liquor prepared in the 4th step
For 2-2.5 hour, after dropping, more at the uniform velocity adding initiator solution E to above-mentioned prepared mixed liquor, time for adding is 20-
30 minutes, after being incubated 1 hour, again at the uniform velocity adding initiator solution F in mixed liquor after dropping, time for adding is 20-
30 minutes, finally, it is incubated 2 hours, and reaction temperature is controlled at 80-82 DEG C;
6th step: blowing after the reaction temperature of the 5th step drops to less than 45 DEG C, prepares high temperature resistant solvent-type acrylic ester
Pressure-sensitive adhesive.
In described 6th step, the high temperature resistant solvent-type acrylic ester pressure-sensitive adhesive of preparation is solid containing for 40-45%, and monomer turns
Rate 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:
Choose 100 high temperature resistant solvent-type acrylic ester pressure-sensitive adhesives according to weight ratio, add 0.01-0.1 part three hydroxyl first
The mixture of base propane-three (3-'-aziridino) propionic ester, coats on 100um mylar, toasts 8 at 130-135 DEG C
Minute, its dry glue thickness is the pressure sensitive adhesive of 30-35um, and its 180 ° of peel strengths are more than 900N/m, the most viscous more than 12# ball (spin
Method), holding power be more than 24 hours, laminating microwave oven door-plate high temperature 190 DEG C baking more than 96 hours without layering, bulge phenomenon,
210 DEG C of bakings are more than 2 hours still without layering, bulge phenomenon, prepare 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 heat-resisting quantity and weather-proof
Property, 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 cost
Low feature.
Detailed description of the invention
The present invention is further described for example 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
Acrylic acid 3-10
2-(Acryloyloxy)ethanol 3-10
Vinylacetate 10-20
Isobomyl acrylate acid esters 15-35
Azo azodiisobutyronitrile 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: choosing 250-350 ethyl acetate according to above-mentioned weight ratio, to dissolve the azo azo two of 0.5-2 wherein different
Butyronitrile, is being added thereto to the Isooctyl acrylate monomer of 150-250,50-100 butyl acrylate, 15-35 acrylic acid after dissolving completely
Isoborneol acid esters and the vinylacetate of 10-20, prepare mixed monomer solution A;Again with 50-150 acetic acid ethyl dissolution 0.3-2's
The 2-(Acryloyloxy)ethanol preparation mixed monomer solution B of N hydroxymethyl acrylamide, the acrylic acid of 3-10 and 3-10;
Second step: by the mixed monomer solution A prepared in the first step and mixed monomer solution B mix homogeneously, and divide equally 2
Part, 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 azodiisobutyronitrile, uniformly divide after preparation initiator
It is two parts, respectively initiator solution E and initiator solution F;
4th step: choose in the ethyl acetate of 50-100 is added reactor and be warming up to 78-80 DEG C, maintains stable returning
Starting at the uniform velocity to drip to ethyl acetate mixed monomer solution C after stream, time for adding is 2-2.5 hour, is incubated 2 little after dropping
Time, 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, time for adding to the mixed liquor prepared in the 4th step
For 2-2.5 hour, after dropping, more at the uniform velocity adding initiator solution E to above-mentioned prepared mixed liquor, time for adding is 20-
30 minutes, after being incubated 1 hour, again at the uniform velocity adding initiator solution F in mixed liquor after dropping, time for adding is 20-
30 minutes, finally, it is incubated 2 hours, and reaction temperature is controlled at 80-82 DEG C;
6th step: blowing after the reaction temperature of the 5th step drops to less than 45 DEG C, prepares high temperature resistant solvent-type acrylic ester
Pressure-sensitive adhesive.
In described 6th step, the high temperature resistant solvent-type acrylic ester pressure-sensitive adhesive of preparation is solid containing for 40-45%, and monomer turns
Rate 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:
Choose 100 high temperature resistant solvent-type acrylic ester pressure-sensitive adhesives according to weight ratio, add 0.01-0.1 part three hydroxyl first
The mixture of base propane-three (3-'-aziridino) propionic ester, coats on 100um mylar, toasts 8 at 130-135 DEG C
Minute, its dry glue thickness is the pressure sensitive adhesive of 30-35um, and its 180 ° of peel strengths are more than 900N/m, the most viscous more than 12# ball (spin
Method), holding power be more than 24 hours, laminating microwave oven door-plate high temperature 190 DEG C baking more than 96 hours without layering, bulge phenomenon,
210 DEG C of bakings are more than 2 hours still without layering, bulge phenomenon, prepare 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
Acrylic acid 5
2-(Acryloyloxy)ethanol 5
Vinylacetate 12
Isobomyl acrylate acid esters 25
Azo azodiisobutyronitrile 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 azodiisobutyronitrile wherein, molten
Isooctyl acrylate monomer, 70 butyl acrylate, 25 isobomyl acrylate acid esters and the vinyl acetate of 12 of 200 is added after solving completely
Ester, prepares mixed monomer solution A;With the N hydroxymethyl acrylamide of 100 acetic acid ethyl dissolutions 0.5, the acrylic acid of 5, the propylene of 5
Acid hydroxyl ethyl ester preparation mixed monomer solution B;
Second step: by mixed monomer solution A and mixed monomer solution B mix homogeneously, and divide equally 2 parts, a single for mixing
Liquid solution C, another part is mixed monomer solution D;
3rd step: with the azo azodiisobutyronitrile of the acetic acid ethyl dissolution 0.4-1 of 50, be uniformly divided into after preparation initiator
Two parts, respectively initiator solution E and initiator solution F;
4th step: the ethyl acetate by 50 is warming up to 78-80 DEG C in adding reactor, starts after maintaining stable backflow
At the uniform velocity dropping mixed monomer solution C, time for adding is 2-2.5 hour, is incubated 2 hours, and keeps reactor temperature after dropping
Degree controls at 80-82 DEG C;
5th step: at the uniform velocity dripping another part of mixed monomer solution D in the mixed liquor that the 4th step prepares, time for adding is 2-
2.5 hours, after dropping, at the uniform velocity adding initiator solution E, time for adding is 20-30 minute, is incubated 1 little after dropping
Shi Hou, the most at the uniform velocity adds initiator solution F, and time for adding is 20-30 minute, finally, is incubated 2 hours and by reaction temperature control
System is at 80-82 DEG C;
6th step: blowing after reaction temperature drops to less than 45 DEG C, prepares high temperature resistant solvent-type acrylic ester pressure-sensitive and glues
Agent.
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
Acrylic acid 5
2-(Acryloyloxy)ethanol 5
Vinylacetate 12
Isobomyl acrylate acid esters 18
Azo azodiisobutyronitrile 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: choose the azo azodiisobutyronitrile of 300 acetic acid ethyl dissolutions 1 according to above-mentioned weight ratio, dissolves completely
The Isooctyl acrylate monomer of rear addition 150,90 butyl acrylate, 18 isobomyl acrylate acid esters and the vinylacetate of 12 parts, join
Mixed monomer solution A processed;Again with 100 the N hydroxymethyl acrylamide of acetic acid ethyl dissolution 0.7, the acrylic acid of 5, the propylene of 5
Acid hydroxyl ethyl ester preparation mixed monomer solution B;
Second step: by mixed monomer solution A and mixed monomer solution B mix homogeneously, and divide equally 2 parts, a single for mixing
Liquid solution C, another part is mixed monomer solution D;
3rd step: with the azo azodiisobutyronitrile of the acetic acid ethyl dissolution 0.4-1 of 50, be uniformly divided into after preparation initiator
Two parts, respectively initiator solution E and initiator solution F;
4th step: the ethyl acetate by 50 is warming up to 78-80 DEG C in adding reactor, starts after maintaining stable backflow
At the uniform velocity dropping mix monomer C, time for adding is 2-2.5 hour, is incubated 2 hours and is controlled by temperature of reaction kettle after dropping
80-82℃;
5th step: the mixed liquor prepared to the 4th step at the uniform velocity drips another part of mixed monomer solution D, and time for adding is 2-
2.5 hours, after dropping, opening and at the uniform velocity add initiator solution E, time for adding is 20-30 minute, is incubated 1 after dropping
After hour, the most at the uniform velocity adding initiator solution F, time for adding is 20-30 minute.Finally, insulation 2 hours and by reaction temperature
Control at 80-82 DEG C;
6th step: blowing after reaction temperature drops to less than 45 DEG C, prepares high temperature resistant solvent-type acrylic ester pressure-sensitive and glues
Agent.
Embodiment 3
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 180
Butyl acrylate 60
Acrylic acid 5
2-(Acryloyloxy)ethanol 5
Vinylacetate 12
Isobomyl acrylate acid esters 22
Azo azodiisobutyronitrile 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 dissolve the azo azodiisobutyronitrile of 1 in it,
Isooctyl acrylate monomer, 60 butyl acrylate, 22 isobomyl acrylate acid esters and the vinyl acetate of 12 of 180 is added after dissolving completely
Ester, prepares mixed monomer solution A;With the N hydroxymethyl acrylamide of 100 acetic acid ethyl dissolutions 1, the acrylic acid of 5, the propylene of 5 parts
Acid hydroxyl ethyl ester preparation mixed monomer solution B;
Second step: by mixed monomer solution A and mixed monomer solution B mix homogeneously, and divide equally 2 parts, a single for mixing
Liquid solution C, another part is mixed monomer solution D;
3rd step: the azo azodiisobutyronitrile of the acetic acid ethyl dissolution 0.6 with 50, is uniformly divided into two after preparation initiator
Part, respectively initiator solution E and initiator solution F;
4th step: the ethyl acetate by 50 is warming up to 78-80 DEG C in adding reactor, starts after maintaining stable backflow
At the uniform velocity dropping mixed monomer solution C, time for adding is 2-2.5 hour, is incubated 2 hours and by temperature of reaction kettle control after dropping
System is at 80-82 DEG C;
5th step: the mixed liquor of preparation at the uniform velocity drips another part of mixed monomer solution D in the 4th step, and time for adding is 2-
2.5 hours, after dropping, at the uniform velocity adding initiator solution E, time for adding is 20-30 minute.1 it is incubated little after dropping
Shi Hou, the most at the uniform velocity adds initiator solution F, and time for adding is 20-30 minute.Finally, insulation 2 hours and by reaction temperature control
System is at 80-82 DEG C;
6th step: blowing after reaction temperature drops to less than 45 DEG C, prepares high temperature resistant solvent-type acrylic ester pressure-sensitive and glues
Agent.
The present invention improves the mechanical property of development of Acrylate Emulsion Pressure-Sensitive Adhesive and heat-resisting quantity and weatherability, thus improves breast
The range of application of liquid type acrylate pressure-sensitive adhesive, has viscosity high, high temperature resistant, wet and heat ageing resistant, and the feature of low cost.
Claims (4)
1. a high temperature resistant solvent-type acrylic ester pressure-sensitive adhesive, it is characterised in that be polymerized according to its weight ratio by following component
Form:
Isooctyl acrylate monomer 150-250
Butyl acrylate 50-100
Acrylic acid 3-10
2-(Acryloyloxy)ethanol 3-10
Vinylacetate 10-20
Isobomyl acrylate acid esters 15-35
Azodiisobutyronitrile 0.5-3
N hydroxymethyl acrylamide 0.3-2
Ethyl acetate 400-600.
The preparation method of high temperature resistant solvent-type acrylic ester pressure-sensitive adhesive the most as claimed in claim 1, it is characterised in that preparation
Step is:
The first step: choose 250-350 ethyl acetate according to above-mentioned weight ratio and dissolve the azodiisobutyronitrile of 0.5-2 wherein, molten
It is being added thereto to the Isooctyl acrylate monomer of 150-250,50-100 butyl acrylate, 15-35 isobomyl acrylate after solving completely
Acid esters and the vinylacetate of 10-20, prepare mixed monomer solution A;Again by the N-hydroxyl first of 50-150 acetic acid ethyl dissolution 0.3-2
The 2-(Acryloyloxy)ethanol preparation mixed monomer solution B of base acrylamide, the acrylic acid of 3-10 and 3-10;
Second step: by the mixed monomer solution A prepared in the first step and mixed monomer solution B mix homogeneously, and divide equally 2 parts, one
Part 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 azodiisobutyronitrile, be uniformly divided into two parts after preparation initiator,
It is respectively initiator solution E and initiator solution F;
4th step: choose in the ethyl acetate of 50-100 is added reactor and be warming up to 78-80 DEG C, after maintaining stable backflow
Starting at the uniform velocity to drip mixed monomer solution C to ethyl acetate, time for adding is 2-2.5 hour, is incubated 2 hours after dropping,
And keep temperature of reaction kettle to control at 80-82 DEG C;
5th step: at the uniform velocity dripping another part of mixed monomer solution D to the mixed liquor prepared in the 4th step, time for adding is 2-
2.5 hours, after dropping, more at the uniform velocity adding initiator solution E to above-mentioned prepared mixed liquor, time for adding is that 20-30 divides
Clock, after being incubated 1 hour, at the uniform velocity adds initiator solution F after dropping again in mixed liquor, and time for adding is that 20-30 divides
Clock, finally, is incubated 2 hours, and controls reaction temperature at 80-82 DEG C;
6th step: blowing after the reaction temperature of the 5th step drops to less than 45 DEG C, prepares high temperature resistant solvent-type acrylic ester pressure-sensitive
Adhesive.
The preparation method of high temperature resistant solvent-type acrylic ester pressure-sensitive adhesive the most as claimed in claim 2, it is characterised in that described
In 6th step, monomer conversion is higher than 98% containing for 40-45% for the high temperature resistant solvent-type acrylic ester pressure-sensitive adhesive of preparation solid,
Viscosity is 1000 ± 250cp.
The application of high temperature resistant solvent-type acrylic ester pressure-sensitive adhesive the most as claimed in claim 1, it is characterised in that applying step
As follows:
Choose 100 high temperature resistant solvent-type acrylic ester pressure-sensitive adhesives according to weight ratio, add 0.01-0.1 part trihydroxy methyl third
The mixture of alkane-three (3-'-aziridino) propionic ester, coats on 100um mylar, toasts 8 minutes at 130-135 DEG C,
Its dry glue thickness is the pressure sensitive adhesive of 30-35um, and its 180 ° of peel strengths are more than 900N/m, the most viscous more than 12# ball (rolling ball method), holds
Viscous force is more than 24 hours, and laminating microwave oven door-plate is more than 96 hours without layering, bulge phenomenon, 210 DEG C of bakings in high temperature 190 DEG C baking
Bake more than 2 hours still without layering, bulge phenomenon, prepare high temperature resistant solvent-type acrylic ester pressure-sensitive adhesive tape.
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CN111690359B (en) * | 2020-06-11 | 2022-06-24 | 四川铂利明德科技有限公司 | High-temperature-resistant acrylate adhesive and preparation method thereof |
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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CN102533164B (en) * | 2011-12-07 | 2014-07-09 | 新丰杰力电工材料有限公司 | Thermo-sensitive acrylate pressure-sensitive adhesive and adhesive tape and preparation method of adhesive and adhesive tape |
CN102559101B (en) * | 2011-12-07 | 2014-01-01 | 新丰杰力电工材料有限公司 | Thermal-spalling acrylic ester pressure-sensitive adhesive, adhesive tape and preparation method thereof |
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