CN103773286B - A kind of silk screen printing waterproof glue for thin film circuit and preparation method thereof - Google Patents
A kind of silk screen printing waterproof glue for thin film circuit and preparation method thereof Download PDFInfo
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- CN103773286B CN103773286B CN201410021054.6A CN201410021054A CN103773286B CN 103773286 B CN103773286 B CN 103773286B CN 201410021054 A CN201410021054 A CN 201410021054A CN 103773286 B CN103773286 B CN 103773286B
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Abstract
The present invention discloses a kind of silk screen printing waterproof glue for thin film circuit and preparation method thereof.The acrylic resin modified polymkeric substance (1 and 2) of the lower molecular weight that this waterproof glue is obtained by organo-peroxide cracking by the acrylic resin of commercially available different functionality, different functionality; flow agent, the solvent of adding specified proportion again form; corresponding solidifying agent is coordinated to coat PET by silk screen printing during use; PE; the thin film circuit of the materials such as PP, plays the object of waterproof damp proof insulation, protection circuit.Waterproof glue of the present invention is without the need to adding defoamer, have printing performance superior, can the engineering time long, cohesive force strong, high-temp resisting high-humidity resisting, creep resistance, be easy to advantages such as repeatedly fitting, water resistance is good, substantially increase the work-ing life of thin film circuit, there is wide market application foreground.
Description
Technical field
The invention belongs to electric slurry field, be specifically related to a kind of silk screen printing waterproof glue being applied to thin film circuit.
Background technology
Thin film circuit is with PET, PP etc. for base material, by the flexible circuit board that various electric slurry is made by the printing of the technique such as silk screen printing, baking.Thin film circuit has flexible, lightweight, the plurality of advantages such as transmission performance is stable, shock-resistant, cheap, environmental protection, is nowadays widely used in the button position of electric mechanical Automated condtrol, instrument, medical facilities, consumer electronics, computer, communication, metering and household electrical appliance, toy etc. product.
In order to ensure the work reliability of thin film circuit, usually need to use waterproof glue to seal to protect electronic circuit not wherein to be subject to steam, sweat or other Pollutant effects, simultaneously as the protecting glue of electronic circuit to whole thin film circuit.But existing thin film circuit waterproof glue is often in process of production in order to ensure printing performance, need to add a large amount of defoamers, waterproof glue transparency is caused to be deteriorated, meanwhile, defoamer great majority are silicone based, when being printed onto on PET, defoamer can float on colloid surface along with solvent evaporates in bake process, which results in waterproof glue cohesive force to decline, do not reach the requirement of waterproof, affect the work-ing life of thin film circuit.
Summary of the invention
For the above-mentioned defect that existing thin film circuit waterproof glue exists, the applicant is through Improvement, and object is to provide a kind of silk screen printing waterproof glue for thin film circuit.Waterproof glue of the present invention without the need to adding defoamer, have printing performance superior, can the engineering time long, cohesive force strong, high-temp resisting high-humidity resisting, creep resistance, be easy to advantages such as repeatedly fitting, water resistance is good, it component comprising following weight proportion is made:
Modified low molecular weight acrylic resin 1 50 ~ 66 weight part
Modified low molecular weight acrylic resin 2 25 ~ 40 weight part
Solvent 5 ~ 20 weight part
Flow agent 0.1 ~ 0.3 weight part
Described modified low molecular weight acrylic resin 1 and 2 is respectively the commercially available acrylic resin pressure sensitive adhesive with different functionality, obtains respectively by the scission reaction cracking of organo-peroxide.Particularly, described modified low molecular weight acrylic resin 1 is obtained by organo-peroxide cracking modification by commercially available high carboxylic value low hydroxyl value acrylic resin pressure sensitive adhesive 1, and modified low molecular weight acrylic resin 2 is obtained by low carboxylic value acrylic resin 2 modification of commercially available high hydroxyl value.
Preferably, it is made up of the component comprising following weight proportion:
Modified low molecular weight acrylic resin 1 55 ~ 60 weight part
Modified low molecular weight acrylic resin 2 26 ~ 38 weight part
Solvent 5 ~ 10 weight part
Flow agent 0.15 ~ 0.25 weight part
Particularly, described organo-peroxide is selected from tertbutyl peroxide, peroxidized t-butyl perbenzoate, peroxide-3, 5, 5-tri-methyl hexanoic acid tert-pentyl ester, 2, 5-dimethyl-2, 5-pair-(t-butyl peroxy)-3-hexin, 1, 1-pair-(t-butyl peroxy) hexanaphthene, 4, 4-pair-(t-butyl peroxy) n-butyl pentanoate, 1, 1-pair-(t-butyl peroxy)-3, 3, 5-trimethyl-cyclohexane, the monoperphthalic acid tert-butyl ester, 1, 1-pair-(t-amyl peroxy) hexanaphthene, 3, 3-pair-(t-butyl peroxy) ethyl butyrate, 2, 5-dimethyl-2, 5-pair-(t-butyl peroxy) hexane, 3, 3-pair-(t-amyl peroxy) ethyl butyrate, 2, 2-pair-(t-butyl peroxy) propane, 2, 5-dimethyl-2, 5-is two-one or more of (t-butyl peroxy) hexane, be preferably 1, 1-pair-(t-butyl peroxy)-3, 3, 5-trimethyl-cyclohexane.
Particularly, described organo-peroxide be selected from 1,1-two-(t-butyl peroxy)-3,3,5-trimethyl-cyclohexane.
Particularly, described solvent be selected from high boiling ester class, ketones solvent one or more.
During use, the solidifying agent adding 1 ~ 8 weight part (being preferably 3 ~ 6 weight parts) in this waterproof glue stirs, can carry out screen printing operation, described solidifying agent is selected from one or more mixtures in isocyanic ester polymer or its modified product, aminoresin and modified product thereof, aziridine or derivatives thereof, multifunctional glycidyl amine.
Present invention also offers a kind of preparation method of above-mentioned silk screen printing waterproof glue, it comprises the following steps:
(1) described commercially available acrylic resin pressure sensitive adhesive 1 and 2 is added in high boiling solvent ethylene glycol monomethyl ether acetate according to the weight ratio of 3 ~ 5:1 respectively, heated and stirred distillation removing system mid-boiling point is lower than the low boiler cut of 155 DEG C, change condensing reflux, control temperature 150 ~ 160 DEG C, the described organo-peroxide spent glycol monobutyl ether acetate ester accounting for described acrylic resin pressure sensitive adhesive weight 0.6 ~ 1.2% is diluted to 50wt%, slowly drop in above-mentioned system, controlling rate of addition is 1.5 ~ 2 seconds/, dropwise rear cold filtration and namely obtain modified low molecular weight acrylic resin 1 and 2, controlling its viscosity is 4000 ~ 6000mpa.s, viscosity is too small, be unfavorable for the control of printing precision, viscosity is excessive, easily wire drawing phenomenon is produced in printing process, viscosity measurement is: by gained modified low molecular weight acrylic resin 1 and 2 spent glycol monobutyl ether acetate ester adjustment solid content to 50% respectively, adopt BROOKFIELD viscosity determinator, use viscosity during No. 14 rotors mensuration 20 turns.
(2) described solvent, flow agent and step (1) gained modified low molecular weight acrylic resin 1 and 2 are stirred by weight ratio in agitator, obtain silk screen printing waterproof glue finished product.
Step (1) gained modified low molecular weight acrylic resin 1 and 2 solid content all controls 56 ~ 62%.
Step (2) gained silk screen printing waterproof glue finished product solid content controls 48 ~ 52%.
Compared with existing thin film circuit waterproof glue, the present invention possesses following advantage:
The present invention obtains lower molecular weight with the acrylic resin of commercially available different functionality by organo-peroxide cracking, different functionality, the acrylic resin modified polymkeric substance (1 and 2) that printability is strong, it is according to the object that can not only reach froth breaking after the mixing of specified weight proportioning, overcome in existing thin film circuit waterproof glue owing to adding the drawback that caused by defoamer, water resistance declines, be aided with solvent and the flow agent of specific proportioning again, it is superior that gained waterproof glue possesses printing performance, can the engineering time long, cohesive force is strong, high-temp resisting high-humidity resisting, creep resistance, be easy to repeatedly fit, the advantages such as water resistance is good, also avoid the toxicity faced from monomer synthesize high simultaneously, react uppity drawback.Coordinate corresponding solidifying agent during use, extensively coat the thin film circuit of the materials such as PET, PE, PP by silk screen printing, play the object of waterproof damp proof insulation, protection circuit, greatly improve the work-ing life of thin film circuit, there is wide market application foreground.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described.
Involved by following examples, each raw material is the commercially available universal product if no special instructions.
Preparation embodiment
Embodiment 1
Preparation method is as follows for the present embodiment silk screen printing waterproof glue:
(1) by commercially available high carboxylic value low hydroxyl value acrylic resin pressure sensitive adhesive 14kg(trade mark SH-602, Jiangyin Shuan Hua Science and Technology Ltd. product) join in there-necked flask with 1.2kg ethylene glycol monomethyl ether acetate, in heated and stirred distillation removing system, the cut of less than 155 DEG C is about 1.8kg, change condensing reflux, control temperature is at 150 ~ 160 DEG C, by 58g organo-peroxide 1, 1-pair-(t-butyl peroxy)-3, 3, 5-trimethyl-cyclohexane spent glycol monobutyl ether acetate ester is diluted to 50wt%, in the above-mentioned system of slow dropping, controlling rate of addition is 2 seconds/, dropwise rear cold filtration and measure solid content, record solid containing being 56.8%, contain solid for the adjustment of gained modified low molecular weight acrylic resin 1 spent glycol monobutyl ether acetate ester to 50%, adopt BROOKFIELD viscosity determinator, use viscosity during No. 14 rotors mensuration 20 turns, recording viscosity is 5500mpa.s.
(2) by commercially available high hydroxyl value low carboxylic value acrylic resin pressure sensitive adhesive 24kg(trade mark VT1202, Yuyao Wei Te adhesive article company limited product) join in there-necked flask with 0.8kg ethylene glycol monomethyl ether acetate, the cut of heated and stirred distillation removing system mid-boiling point below 155 DEG C is about 1.8kg, change condensing reflux, control temperature is at 155 ~ 160 DEG C, by 38g organo-peroxide 1, 1-pair-(t-butyl peroxy)-3, 3, 5-trimethyl-cyclohexane spent glycol monobutyl ether acetate ester is diluted to 50wt%, slowly drop in above-mentioned system, controlling rate of addition is 1.6 seconds/, dropwise rear cold filtration and measure solid content, record solid containing being 59.3%, contain solid for the adjustment of gained modified low molecular weight acrylic resin 2 spent glycol monobutyl ether acetate ester to 50%, adopt BROOKFIELD viscosity determinator, use viscosity during No. 14 rotors mensuration 20 turns, recording viscosity is 4350mpa.s.
(3) take each component by weight ratio, stir in agitator, obtain silk screen printing waterproof glue finished product (Gu containing be 51.2%), each component and weight proportion as follows:
Above-mentioned waterproof glue finished product added the aminoresin (Jiangsu Miki Group product) of 3 weight parts and fully stir, can screen printing operation be carried out.
Embodiment 2
(1) by commercially available high carboxylic value low hydroxyl value acrylic resin pressure sensitive adhesive 14kg(trade mark SH-602 Jiangyin Shuan Hua Science and Technology Ltd.) join in there-necked flask with 1.2kg ethylene glycol monomethyl ether acetate, in heated and stirred distillation removing system, the cut of less than 155 DEG C is about 1.8kg, change condensing reflux, control temperature is at 150 ~ 160 DEG C, by 58g organo-peroxide 1, 1-pair-(t-butyl peroxy)-3, 3, 5-trimethyl-cyclohexane spent glycol monobutyl ether acetate ester is diluted to 50wt%, in the above-mentioned system of slow dropping, controlling rate of addition is 2 seconds/, dropwise rear cold filtration and measure solid content, record solid containing being 56.8%, contain solid for the adjustment of gained modified low molecular weight acrylic resin 1 spent glycol monobutyl ether acetate ester to 50%, adopt BROOKFIELD viscosity determinator, use viscosity during No. 14 rotors mensuration 20 turns, recording viscosity is 5500mpa.s.
(2) by commercially available high hydroxyl value low carboxylic value acrylic resin pressure sensitive adhesive 24kg(trade mark VT1212, Yuyao Wei Te adhesive article company limited) join in there-necked flask with 1kg ethylene glycol monomethyl ether acetate, the cut of heated and stirred distillation removing system mid-boiling point below 155 DEG C is about 1.8kg, change condensing reflux, control temperature is at 155 ~ 160 DEG C, by 43g organo-peroxide 1, 1-pair-(t-butyl peroxy)-3, 3, 5-trimethyl-cyclohexane spent glycol monobutyl ether acetate ester is diluted to 50wt%, slowly drop in above-mentioned system, controlling rate of addition is 1.6 seconds/, dropwise rear cold filtration and measure solid content, record solid containing being 59.3%, contain solid for the adjustment of gained modified low molecular weight acrylic resin 2 spent glycol monobutyl ether acetate ester to 50%, adopt BROOKFIELD viscosity determinator, use viscosity during No. 14 rotors mensuration 20 turns, recording viscosity is 4825mpa.s.
(3) take each component by weight ratio, stir in agitator, obtain silk screen printing waterproof glue finished product (Gu containing be 50.8%), each component and weight proportion as follows:
Above-mentioned waterproof glue finished product added 1,3-two (N, N-2-glycidyl aminomethyl) cyclohexane (CAS:65992-66-7) of 0.2 weight part and fully stir, can screen printing operation be carried out.
Embodiment 3
(1) by commercially available high carboxylic value low hydroxyl value acrylic resin pressure sensitive adhesive 14kg(trade mark CF-2, Weifang Fuller novel material company limited) join in there-necked flask with 1.2kg ethylene glycol monomethyl ether acetate, in heated and stirred distillation removing system, the cut of less than 155 DEG C is about 1.8kg, change condensing reflux, control temperature is at 150 ~ 160 DEG C, by 62g organo-peroxide 1, 1-pair-(t-butyl peroxy)-3, 3, 5-trimethyl-cyclohexane spent glycol monobutyl ether acetate ester is diluted to 50wt%, in the above-mentioned system of slow dropping, controlling rate of addition is 2 seconds/, dropwise rear cold filtration and measure solid content, record solid containing being 57.4%, contain solid for the adjustment of gained modified low molecular weight acrylic resin 1 spent glycol monobutyl ether acetate ester to 50%, adopt BROOKFIELD viscosity determinator, use viscosity during No. 14 rotors mensuration 20 turns, recording viscosity is 5875mpa.s.
(2) by commercially available high hydroxyl value low carboxylic value acrylic resin pressure sensitive adhesive 24kg(trade mark CF-214, Jinan Kraft happy chemical industry limit company) join in there-necked flask with 1.3kg ethylene glycol monomethyl ether acetate, the cut of heated and stirred distillation removing system mid-boiling point below 155 DEG C is about 1.8kg, change condensing reflux, control temperature is at 155 ~ 160 DEG C, by 52g organo-peroxide 1, 1-pair-(t-butyl peroxy)-3, 3, 5-trimethyl-cyclohexane spent glycol monobutyl ether acetate ester is diluted to 50wt%, slowly drop in above-mentioned system, controlling rate of addition is 1.6 seconds/, dropwise rear cold filtration and measure solid content, record solid containing being 59.3%, contain solid for the adjustment of gained modified low molecular weight acrylic resin 2 spent glycol monobutyl ether acetate ester to 50%, adopt BROOKFIELD viscosity determinator, use viscosity during No. 14 rotors mensuration 20 turns, recording viscosity is 5375mpa.s.
(3) take each component by weight ratio, stir in agitator, obtain silk screen printing waterproof glue finished product (Gu containing be 51%), each component and weight proportion as follows:
Sea light auspicious trade Co., Ltd product on the isocyanic ester MF-K60X(above-mentioned waterproof glue finished product being added 2.5 weight parts) and fully stir, can screen printing operation be carried out.
The application of silk screen printing waterproof glue and performance test
Silk screen printing parameters of construction technology is as shown in table 1.
Table 1
| Silk screen type | 100 ~ 200 order polyester net or Stainless Steel Cloths |
| Print thickness | 15-20μm |
| Thinner | Ethylene glycol monomethyl ether acetate, diethylene glycol ether acetic ester |
| Curing process | Baking oven or IR drying tunnel: >=130 DEG C × 1.5 ~ 3min |
| Clean-out system | Acetone, N-BUTYL ACETATE |
| Solidifying agent | With corresponding solidifying agent mixing and stirring by weight before using |
| Printing element | PET |
| Laminating base material | PET |
Embodiment 1 ~ embodiment 3 silk screen printing waterproof glue the performance test results and standard are see table 2.
Table 2
From table 2 data: silk screen printing waterproof glue prepared by the embodiment of the present invention 1 ~ embodiment 3 has that printing performance is superior, high-temp resisting high-humidity resisting, resistance to creep, be easy to advantages such as repeatedly fitting; simultaneously as the waterproof glue of thin film circuit; there is good adhesiveproperties and water resistance, the effect playing waterproof damp proof insulation, protection circuit in thin film circuit can be widely used in.
The above is only the preferred embodiment of the present invention, the invention is not restricted to above embodiment.Be appreciated that the oher improvements and changes that those skilled in the art directly derive without departing from the spirit and concept in the present invention or associate, all should think and be included within protection scope of the present invention.
Claims (9)
1., for a silk screen printing waterproof glue for thin film circuit, it is characterized in that the component by comprising following weight proportion is made:
Described modified low molecular weight acrylic resin 1 obtain by organo-peroxide cracking modification for commercially available high carboxylic value low hydroxyl value acrylic resin pressure sensitive adhesive 1, and described modified low molecular weight acrylic resin 2 passes through organo-peroxide cracking modification by commercially available high hydroxyl value low carboxylic value acrylic resin 2 and obtains.
2., as claimed in claim 1 for the silk screen printing waterproof glue of thin film circuit, it is characterized in that the component by comprising following weight proportion is made:
3. according to claim 1 for the silk screen printing waterproof glue of thin film circuit, it is characterized in that: described organo-peroxide is selected from tertbutyl peroxide, peroxidized t-butyl perbenzoate, peroxide-3, 5, 5-tri-methyl hexanoic acid tert-pentyl ester, 2, 5-dimethyl-2, 5-pair-(t-butyl peroxy)-3-hexin, 1, 1-pair-(t-butyl peroxy) hexanaphthene, 4, 4-pair-(t-butyl peroxy) n-butyl pentanoate, 1, 1-pair-(t-butyl peroxy)-3, 3, 5-trimethyl-cyclohexane, the monoperphthalic acid tert-butyl ester, 1, 1-pair-(t-amyl peroxy) hexanaphthene, 3, 3-pair-(t-butyl peroxy) ethyl butyrate, 2, 5-dimethyl-2, 5-pair-(t-butyl peroxy) hexane, 3, 3-pair-(t-amyl peroxy) ethyl butyrate, 2, 2-is two-one or more of (t-butyl peroxy) propane.
4., according to claim 3 for the silk screen printing waterproof glue of thin film circuit, it is characterized in that: that described organo-peroxide is selected from 1,1-is two-(t-butyl peroxy)-3,3,5-trimethyl-cyclohexane.
5. according to claim 1 or 2 for the silk screen printing waterproof glue of thin film circuit, it is characterized in that: described solvent be selected from high boiling ester class, ketones solvent one or more.
6. according to claim 1 for the silk screen printing waterproof glue of thin film circuit, it is characterized in that: during use, the solidifying agent adding 1 ~ 8 weight part in this waterproof glue stirs, and can carry out screen printing operation.
7. described in claim 1 for the preparation method of the silk screen printing waterproof glue of thin film circuit, it is characterized in that comprising the following steps:
(1) described commercially available high carboxylic value low hydroxyl value acrylic resin pressure sensitive adhesive 1 and commercially available high hydroxyl value low carboxylic value acrylic resin 2 are added in high boiling solvent ethylene glycol monomethyl ether acetate according to the weight ratio of 3 ~ 5:1 respectively, heated and stirred distillation removing system mid-boiling point is lower than the low boiler cut of 155 DEG C, change condensing reflux, control temperature 150 ~ 160 DEG C, the described organo-peroxide spent glycol monobutyl ether acetate ester accounting for described acrylic resin pressure sensitive adhesive weight 0.6 ~ 1.2% is diluted to 50wt%, slowly drop in above-mentioned system, controlling rate of addition is 1.5 ~ 2 seconds/, dropwise rear cold filtration and namely obtain modified low molecular weight acrylic resin 1 and 2, controlling its viscosity is 4000 ~ 6000mpa.s,
(2) described solvent, flow agent and step (1) gained modified low molecular weight acrylic resin 1 and 2 are stirred by weight ratio in agitator, obtain silk screen printing waterproof glue finished product.
8. according to claim 7 for the preparation method of the silk screen printing waterproof glue of thin film circuit, it is characterized in that: the solid content of step (1) gained modified low molecular weight acrylic resin 1 and 2 all controls 56 ~ 62%.
9. according to claim 7 for the preparation method of the silk screen printing waterproof glue of thin film circuit, it is characterized in that: step (2) gained silk screen printing waterproof glue finished product solid content controls 48 ~ 52%.
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| CN111440571A (en) * | 2019-12-24 | 2020-07-24 | 宁波激智科技股份有限公司 | Laminating adhesive and anti-oxidation silver reflecting film |
| CN111595843B (en) * | 2020-05-20 | 2022-06-03 | 中国科学院新疆理化技术研究所 | Preparation method and application of viscous sampling detection paper for arrayed colorimetric analysis |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101899274A (en) * | 2009-12-16 | 2010-12-01 | 肖方一 | Acrylate waterproof adhesive and preparation method and application thereof |
| CN102977822A (en) * | 2012-11-13 | 2013-03-20 | 苏州喜仁新材料科技有限公司 | Thermosetting waterproof adhesive and preparation method thereof |
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| JPH06340851A (en) * | 1993-06-02 | 1994-12-13 | Sekisui Chem Co Ltd | Pressure-sensitive adhesive tape or sheet having thin metal layer |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101899274A (en) * | 2009-12-16 | 2010-12-01 | 肖方一 | Acrylate waterproof adhesive and preparation method and application thereof |
| CN102977822A (en) * | 2012-11-13 | 2013-03-20 | 苏州喜仁新材料科技有限公司 | Thermosetting waterproof adhesive and preparation method thereof |
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Address after: 215550 No. 12 East Zhou road, Changshou City Economic Development Zone, Suzhou, Jiangsu, China Patentee after: SUZHOU BEITELI POLYMER MATERIALS CO., LTD. Address before: 215550 No. 12 East Zhou road, Changshou City Economic Development Zone, Suzhou, Jiangsu, China Patentee before: Dongguan Betely New Materials Co., Ltd. |