CN112940628A - High-temperature-resistant UV (ultraviolet) viscosity-reducing adhesive capable of improving initial viscosity - Google Patents
High-temperature-resistant UV (ultraviolet) viscosity-reducing adhesive capable of improving initial viscosity Download PDFInfo
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- CN112940628A CN112940628A CN202110392919.XA CN202110392919A CN112940628A CN 112940628 A CN112940628 A CN 112940628A CN 202110392919 A CN202110392919 A CN 202110392919A CN 112940628 A CN112940628 A CN 112940628A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J4/00—Adhesives based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; adhesives, based on monomers of macromolecular compounds of groups C09J183/00 - C09J183/16
- C09J4/06—Organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond in combination with a macromolecular compound other than an unsaturated polymer of groups C09J159/00 - C09J187/00
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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Abstract
The invention provides a high-temperature resistant UV (ultraviolet) viscosity reducing adhesive for improving initial viscosity performance, which comprises the following raw materials of acrylic resin, alkenyl-terminated polydimethylsiloxane, a photoinitiator, a photosensitive monomer and an organic solvent, wherein a hard monomer in an acrylic resin polymerization monomer comprises an unsaturated benzoxazine monomer and styrene, and the structural formula of the alkenyl-terminated polydimethylsiloxane is as follows. The UV visbreaking glue utilizes the special composition and molecular structure of alkenyl-terminated polydimethylsiloxane, on one hand, the influence of a group with large protective polarity on an easily polarized oxazine structure can be isolated, on the other hand, the surface tension is weak, the surface energy is small, the wettability is good, the UV visbreaking glue wetting time containing the alkenyl-terminated polydimethylsiloxane is favorably shortened, the contact time is prolonged, and the initial adhesion of the UV visbreaking glue is further improved. The invention unexpectedly discovers that the alkenyl-terminated polydimethylsiloxane and the acrylic resin have the function of synergistically improving the high-temperature resistance.
Description
Technical Field
The invention belongs to the technical field of adhesives, and particularly relates to a high-temperature-resistant UV (ultraviolet) anti-sticking adhesive with improved initial sticking performance.
Background
The acrylate adhesive is one of the most widely applied adhesives at present, and has the advantages of excellent weather resistance, aging resistance, small irritation to skin and the like. With the rapid development of science and technology, the acrylate adhesive is applied to more occasions and is modified to have more performances, wherein UV viscosity reduction is one of the performances, the acrylate adhesive has the special performance requirements and comprises the semiconductor industry and the optical instrument industry, and particularly in the processing and manufacturing processes of products such as semiconductor chips, transistors, integrated circuits, printed circuit boards, telescopes, optical microscopes and the like, the acrylate adhesive has certain adhesive force and plays roles of fixing, supporting and protecting when being processed and used, the adhesive force is greatly reduced through UV irradiation after the processing is finished, and the acrylate adhesive is easy to peel.
The published prior art, for example patent CN200410022029.6, discloses a UV-curable peelable pressure-sensitive adhesive film and a preparation method thereof, comprising 90-110 parts by weight of an acrylate copolymer solution; 10-15 parts of urethane acrylate; 10-20 parts of a dipentaerythritol pentaacrylate/dipentaerythritol hexaacrylate mixed monomer; 2-4 parts of ethoxybenzoin. The patent CN201910073195.5 discloses a side vinyl type co-acrylate UV visbreaking adhesive and a preparation method thereof, wherein the side vinyl type co-acrylate UV visbreaking adhesive comprises 30-90 parts of main adhesive, 0.3-3 parts of photoinitiator, 1-5 parts of thermal curing agent and 5-40 parts of reactive diluent; the main adhesive comprises 1-10 parts of isocyanate functional monomer and 100 parts of co-polyacrylate adhesive. The acrylate UV adhesive has good adhesion before UV irradiation, the adhesion is greatly reduced after UV irradiation, and the acrylate UV adhesive can be easily peeled off from the surface of an adherend, but the UV adhesive in the prior art has poor high temperature resistance, the inventor of the prior application CN2021103813047 improves the high temperature resistance, unsaturated benzoxazine is used as a hard monomer to participate in the preparation of acrylic resin, and then a photosensitive monomer, a photoinitiator and the like are added to prepare the high temperature resistant UV adhesive, the adhesive has good high temperature resistance, high adhesive strength can be provided during high temperature process operation, the acrylic adhesive can still play the roles of fixing, supporting and protecting during the high temperature process, but the initial adhesion of the high temperature resistant UV adhesive is low. Initial tack refers to the resistance to separation exhibited by the rapid separation of a pressure sensitive adhesive article immediately after contact with an adherend surface with very light pressure. The initial adhesion is poor, which makes handling difficult when the adhesive is attached to an adherend, the air release is poor, foaming occurs, and not only appearance problems are caused, but also the permanent adhesion and the peel strength are adversely affected. The high-temperature resistant UV visbreaking adhesive has a low initial adhesion, and the groups with large polarity on the acrylic resin are presumed to be influenced by the easily polarized oxazine structure and caused by polarity reduction.
In conclusion, further improvement of the UV viscosity reducing adhesive is needed to obtain a UV viscosity reducing adhesive with good high temperature resistance and high initial adhesion.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide the high-temperature resistant UV visbreaking adhesive with improved initial adhesion performance and the preparation method thereof.
In order to achieve the purpose, the invention adopts the following specific technical scheme:
the utility model provides an improve high temperature resistant UV of initial viscous performance and subtract viscose, subtract the viscose includes following raw materials, acrylic resin, alkenyl end-capped polydimethylsiloxane, photoinitiator, photosensitive monomer, organic solvent, hard monomer in the acrylic resin polymerization monomer includes unsaturated benzoxazine monomer and styrene, the structural formula of alkenyl end-capped polydimethylsiloxane is as follows:
wherein R is1、R4The same or different, are independently selected from hydrogen or methyl; r2、R3The same or different, are independently selected from methylene or carbonyl; n is an integer of 1 to 5.
The high-temperature-resistant UV (ultraviolet) visbreaking glue capable of improving initial adhesion performance comprises, by weight, 30-50 parts of acrylic resin, 5-10 parts of alkenyl-terminated polydimethylsiloxane, 0.5-3 parts of photoinitiator, 20-30 parts of photosensitive monomer and 30-50 parts of organic solvent, wherein the weight ratio of unsaturated benzoxazine monomer to styrene is 1-3: 1.
The main chain on the alkenyl-terminated polydimethylsiloxane molecule is mostly composed of-Si-O-chain links, nonpolar groups on the side chain are arranged outwards in an oriented mode and belong to basic geometric molecular configurations, the special composition and molecular structure enable the alkenyl-terminated polydimethylsiloxane molecule to be particularly flexible, intermolecular action is low, on one hand, groups with large polarity can be isolated and protected from being influenced by an easily polarizable oxazine structure, on the other hand, the alkenyl-terminated polydimethylsiloxane molecule is weak in surface tension, small in surface energy and good in wettability, and is beneficial to shortening of wetting time of UV (ultraviolet) viscosity-reducing adhesive containing the alkenyl-terminated polydimethylsiloxane, contact time is prolonged, and initial adhesion is further improved.
The preparation raw material of the alkenyl-terminated polydimethylsiloxane comprises aminopropyl-terminated silicone oil and an unsaturated epoxy monomer, wherein the molar ratio of the aminopropyl-terminated silicone oil to the unsaturated epoxy monomer is 1: 2.05-2.25.
The weight average molecular weight of the aminopropyl terminated silicone oil is 320-620 g/mol.
The unsaturated epoxy monomer is selected from at least one of allyl glycidyl ether, glycidyl methacrylate and glycidyl acrylate.
Specifically, the preparation method of the alkenyl-terminated polydimethylsiloxane comprises the following steps:
adding aminopropyl terminated silicone oil, unsaturated epoxy monomer, solvent and polymerization inhibitor into a reaction kettle, uniformly stirring, heating, keeping constant temperature reaction, cooling to room temperature, carrying out alkali washing, solvent washing and reduced pressure distillation to obtain viscous liquid.
The temperature is increased to 80-120 ℃, the constant-temperature reaction time is 3-5h, the temperature is reduced to room temperature, the alkali is 5-10% sodium hydroxide or potassium hydroxide solution, the number of alkali washing is 3-5, and the number of solvent washing is 1-3;
the solvent is at least one of cyclohexanone, toluene and dimethylformamide;
the polymerization inhibitor is selected from at least one of 2, 6-di-tert-butyl-p-cresol, 4-tert-butyl catechol and hydroquinone.
The acrylic resin is a copolymer obtained by polymerizing a hard monomer, a soft elastomer and a functional monomer according to a mass ratio of 10:4-6: 3. The hard monomer comprises unsaturated benzoxazine and styrene; preferably, the mass ratio of benzoxazine to styrene is 1-3: 1. The structural formula of the unsaturated benzoxazine monomer is as follows:
R5-R7one of them is allyl, methallyloxy or allyloxy, the others are H or C1-C6 alkyl, C1-C6 alkoxy; r8、R9、R10Independently H, C1-C6 alkyl or C1-C6 alkoxy.
The preparation method of the unsaturated benzoxazine monomer comprises the following steps:
1) adding a phenol compound containing alkenyl, a primary amine compound and formaldehyde into a reaction kettle containing an organic solvent in an inert atmosphere, uniformly stirring, heating to a reflux state for reaction, and then carrying out reduced pressure distillation to obtain a solid for later use;
2) dissolving the solid obtained in the step 1) in an organic solvent, washing with an alkali liquor, then washing with deionized water to be neutral, and drying in vacuum to obtain the unsaturated benzoxazine monomer.
The molar ratio of the phenol compound, the primary amine compound and the formaldehyde in the step 1) is 1:1-1.2: 2-2.4; the organic solvent is at least one selected from dioxane, dimethylformamide, chloroform, toluene and xylene; the phenol compound containing alkenyl is selected from at least one of 4-allylphenol, 3-allylphenol, 2- (allyloxy) phenol, 2-allylphenol, o- (2-methallyloxy) phenol and 4-allyloxyphenol; the primary amine compound is selected from at least one of aniline, m-methylaniline, p-methylaniline and o-methylaniline; the reflux reaction time is 1-3 h.
The organic solvent in the step 2) is at least one of diethyl ether and ethanol; the alkali liquor is selected from aqueous solution of potassium hydroxide or sodium hydroxide, the concentration of the alkali liquor is 0.5-1.5mol/L, and the washing times of the alkali liquor are 1-5 times.
The preparation method of the acrylic resin comprises the following steps:
s1, uniformly mixing the soft monomer, the hard monomer, the functional monomer, the solvent and the initiator in an inert atmosphere for later use;
s2, adding the mixture obtained in the step S1 of 1/4-1/3 into a reaction kettle under an inert atmosphere, heating to react under a stirring condition, then dropwise adding the rest mixture obtained in the step S1, and continuing constant-temperature reaction after dropwise adding is finished;
s3 stopping reaction, distilling under reduced pressure to obtain viscous liquid for later use.
The soft monomer in step S1 is not particularly limited, and is generally an alkyl acrylate, the number of carbon atoms in the alkyl group is an integer of 1 to 6, and examples of the soft elastomer include, but are not limited to, at least one of ethyl acrylate, butyl acrylate, and n-butyl methacrylate; the functional monomer includes but is not limited to at least one of acrylic acid, methacrylic acid, maleic acid, N-methylol acrylamide, acrylic acid glycidyl ether, N-methylol methacrylamide monomer; the solvent is at least one selected from chloroform, dimethyl methyl ether, dipropylene glycol methyl ether, ethyl acetate, toluene and butyl acetate; the initiator is not particularly limited to peroxide initiators commonly used in the art, and may be benzoyl peroxide.
And step S2, heating to 60-90 ℃, wherein the reaction time is 0.5-2h, dripping the mixture in the rest step S1 within 3-5h, and then continuing to react for 1-3h at constant temperature.
The photoinitiator is a free radical photoinitiator including but not limited to at least one of benzoin diethyl ether, 1-hydroxycyclohexyl phenyl ketone, 2-hydroxy-2-methyl-1-phenyl acetone, 2,4, 6-trimethylbenzoyl-diphenyl phosphine oxide.
The photosensitive monomer is a compound of a monofunctional monomer and a multifunctional monomer with the functionality of more than or equal to 3, and the compounding ratio is 0.6-1: 1-2.5.
The monofunctional photosensitive monomer is fluoroalkyl (meth) acrylate, and is specifically selected from at least one of trifluoroethyl methacrylate, hexafluorobutyl methacrylate and trifluoroethyl acrylate, the trifunctional photosensitive monomer comprises but is not limited to at least one of pentaerythritol triacrylate, trimethylolpropane triacrylate and triethoxylated trimethylolpropane triacrylate, and the pentafunctional photosensitive monomer comprises but is not limited to dipentaerythritol pentaacrylate.
For example, the photosensitive monomer is a compound of acrylate with the functionality of 1, 3 and 5, and the molar ratio of the three is 0.6-1:2-3: 0.3-0.5.
The organic solvent is at least one selected from chloroform, dimethyl methyl ether, dipropylene glycol methyl ether, ethyl acetate, toluene and butyl acetate.
Compared with the prior art, the invention has the beneficial effects that:
the alkenyl-terminated polydimethylsiloxane in the UV viscid has a flexible main chain and low intermolecular acting force, and by utilizing the special composition and molecular structure, on one hand, groups with large polarity can be isolated and protected from the influence of an easily polarizable oxazine structure, on the other hand, the UV viscid has weak surface tension, small surface energy and good wettability, is beneficial to shortening the wetting time of the UV viscid containing the alkenyl-terminated polydimethylsiloxane, improves the contact time and further improves the initial adhesion of the UV viscid.
Detailed Description
The present invention will be further described with reference to the following examples, but the present invention is not limited to the descriptions in the following. Unless otherwise specified, "parts" in the examples are parts by weight.
Aminopropyl terminated silicone oil was purchased from Shanghai Guijing New Material science and technology, Inc. and had a weight average molecular weight of 322.7.
Preparation method of alkenyl-terminated polydimethylsiloxane
Preparation example 1
Adding 10mol of aminopropyl terminated silicone oil, 22.5mol of allyl glycidyl ether, 40mol of cyclohexanone and 0.1mol of 4-tert-butyl catechol into a reaction kettle, uniformly stirring, heating to 100 ℃, keeping constant temperature for reaction for 4 hours, cooling to room temperature, washing for 3 times by using 5% sodium hydroxide solution, washing for 3 times by using the cyclohexanone, and finally carrying out reduced pressure distillation to obtain viscous liquid.
1649cm on IR spectrum-1A sharp characteristic absorption peak near indicates that allyl groups are still present.
Preparation example 2
The same as in production example 1 was repeated, except that allyl glycidyl ether was used in an amount of 20.5 mol.
1649cm on IR spectrum-1A sharp characteristic absorption peak near indicates that allyl groups are still present.
Preparation of unsaturated benzoxazine monomers
Preparation example 3
1) Adding 1mol of 4-allylphenol, 1.2mol of aniline and 2.2mol of formaldehyde into a reaction kettle containing 5mol of dioxane under the nitrogen atmosphere, uniformly stirring, heating to a reflux state for reaction, and then carrying out reduced pressure distillation to obtain a light yellow solid for later use;
2) dissolving the light yellow solid obtained in the step 1) in diethyl ether, washing for 3 times by using 0.5mol/L sodium hydroxide solution, then washing to be neutral by using deionized water, and drying in vacuum to obtain the unsaturated benzoxazine monomer compound 1.
Preparation of acrylic resin
Preparation example 4
S1, under the atmosphere of nitrogen, uniformly mixing 10 parts of butyl acrylate, 3 parts of the unsaturated benzoxazine monomer prepared in preparation example 3, 1 part of styrene monomer, 3 parts of N-hydroxymethyl acrylamide, 25 parts of toluene and 0.09 part of benzoyl peroxide for later use;
s2, adding 1/4 of the mixture obtained in the step S1 into a reaction kettle under the nitrogen atmosphere, heating to 85 ℃ under the stirring condition, reacting for 1.5h, dripping the rest of the mixture obtained in the step S1 within 3h, and finally continuing to react for 2h at constant temperature;
s3 stopping reaction, distilling under reduced pressure to obtain viscous liquid for later use.
Preparation example 5
The same as in preparation example 4 except that the unsaturated benzoxazine monomer in preparation example 3 was used in an amount of 2 parts and styrene in an amount of 2 parts.
Preparation example 6
The same as in preparation example 4 except that the unsaturated benzoxazine monomer in preparation example 3 was used in an amount of 4.5 parts and the styrene monomer in an amount of 1.5 parts.
Example 1
2.3 parts of benzoin diethyl ether, 5.8 parts of hexafluorobutyl methacrylate, 19.4 parts of trimethylolpropane triacrylate and 4.8 parts of dipentaerythritol pentaacrylate (the weight ratio of the three photosensitive monomers is 0.6:2:0.5) are uniformly mixed with 50 parts of the acrylic resin prepared in preparation example 4, 10 parts of the alkenyl-terminated polydimethylsiloxane prepared in preparation example 1 and 40 parts of chloroform, and the mixture is kept stand for 30min for defoaming, so that the high-temperature resistant UV viscose reducer is obtained.
Example 2
The same as in example 1 except that preparation example 1 prepared alkenyl terminated polydimethylsiloxane in an amount of 5 parts.
Example 3
The same as example 1 except that the acrylic resin prepared in preparation example 4 was used in an amount of 30 parts.
Example 4
The same as in example 1 except that preparation example 1 prepared alkenyl terminated polydimethylsiloxane in an amount of 3 parts.
Example 5
The same as in example 1 except that preparation example 1 prepared alkenyl terminated polydimethylsiloxane in an amount of 20 parts.
Example 6
The same as example 1 except that the acrylic resin used was prepared for preparation example 5.
Example 7
The same as example 1 except that the acrylic resin used was prepared for preparation example 6.
Example 8
The same as in example 1 except that the alkenyl terminated polydimethylsiloxane used was prepared as in preparation example 2.
Example 9
The procedure of example 1 was repeated, except that the photosensitive monomers were 16.4 parts of trifluoroethyl methacrylate and 13.6 parts of dipentaerythritol pentaacrylate, that is, pentaerythritol triacrylate was not added.
Example 10
The procedure was as in example 1 except that the photosensitive monomer was 30 parts of pentaerythritol triacrylate.
Comparative example 1
The same as in example 1 except that alkenyl terminated polydimethylsiloxane was added, the acrylic resin prepared in preparation example 4 was used in an amount of 60 parts.
Application example
The UV visbreaker prepared in the above examples and comparative examples was coated on the surface of a 40 μm corona PET substrate with a coating amount of 30g/cm2Baking at 100 deg.C for 8min to form a uniform coating with thickness of 2 μm, standing at room temperature for 24h, sticking the PET film coated with the viscose reducing agent on a steel plate, placing under a 750W ultraviolet lamp at a distance of 15cm, irradiating for 1min, and taking out for testing.
The high-temperature resistant UV visbreaking adhesive prepared by the application example is subjected to the following performance tests:
initial adhesion: reference is made to GB/T4852-2002, ball ramp stop test method, 30 ℃ tilt angle, stainless steel plate.
And (3) keeping adhesion: refer to GB/T4851-1998, adhesion tester, test temperature 40 ℃, weight 500 g.
Heat resistance and permanent adhesion: refer to GB/T4851-1998, adhesion tester, test temperature 120 ℃, weight 500 g.
180 ° peel strength: refer to GB/T2792-1995, electronic tensile tester, tape width 25mm, and peeling rate 300 mm/min.
TABLE 1
The above table shows that the initial adhesion of the UV reduced adhesive is improved after the alkenyl-terminated polydimethylsiloxane is added into the UV reduced adhesive, and the number of the steel balls of the UV reduced adhesive can reach more than 10 by adjusting the use amounts of the acrylic resin and the alkenyl-terminated polydimethylsiloxane, and the number of the steel balls of the UV reduced adhesive can reach more than 13 in the preferred embodiment.
Claims (10)
1. The utility model provides an improve high temperature resistant UV of initial viscous performance and subtract viscose, subtract the viscose includes following raw materials, acrylic resin, alkenyl end-capped polydimethylsiloxane, photoinitiator, photosensitive monomer, organic solvent, hard monomer in the acrylic resin polymerization monomer includes unsaturated benzoxazine monomer and styrene, the structural formula of alkenyl end-capped polydimethylsiloxane is as follows:
wherein R is1、R4The same or different, are independently selected from hydrogen or methyl; r2、R3The same or different, are independently selected from methylene or carbonyl; n is an integer of 1 to 6.
2. The UV viscose reducing agent according to claim 1, wherein the viscose reducing agent comprises, by weight, 30-50 parts of acrylic resin, 5-10 parts of alkenyl-terminated polydimethylsiloxane, 0.5-3 parts of photoinitiator, 20-30 parts of photosensitive monomer, and 30-50 parts of organic solvent, and the weight ratio of the unsaturated benzoxazine monomer to styrene is 1-3: 1.
3. The UV viscose reducing agent according to claim 1, wherein the raw material of the alkenyl terminated polydimethylsiloxane comprises aminopropyl terminated silicone oil and an unsaturated epoxy monomer, and the molar ratio of the aminopropyl terminated silicone oil to the unsaturated epoxy monomer is 1: 2.05-2.25.
4. The UV viscose reducer according to claim 1, wherein the unsaturated epoxy monomer is at least one selected from allyl glycidyl ether, glycidyl methacrylate, and glycidyl acrylate.
5. The UV viscose reducing agent according to claim 1, wherein the preparation method of the alkenyl terminated polydimethylsiloxane comprises the following steps:
adding aminopropyl terminated silicone oil, unsaturated epoxy monomer, solvent and polymerization inhibitor into a reaction kettle, uniformly stirring, heating, keeping constant temperature reaction, cooling to room temperature, carrying out alkali washing, solvent washing and reduced pressure distillation to obtain viscous liquid.
6. The UV viscose reducer according to claim 1, wherein the weight ratio of the soft monomer to the hard monomer to the functional monomer in the acrylic resin is 10:4-6: 3.
7. The UV detackifying adhesive of claim 1, wherein the unsaturated benzoxazine monomer has the formula:
R5-R7one of them is allyl, methallyloxy or allyloxy, the others are H or C1-C6 alkyl, C1-C6 alkoxy; r8、R9、R10Independently H, C1-C6 alkyl or C1-C6 alkoxy.
8. The UV viscose reducer according to claim 1, wherein the unsaturated benzoxazine monomer is prepared by a method comprising the steps of:
1) adding a phenol compound containing alkenyl, a primary amine compound and formaldehyde into a reaction kettle containing an organic solvent in an inert atmosphere, uniformly stirring, heating to a reflux state for reaction, and then carrying out reduced pressure distillation to obtain a solid for later use;
2) dissolving the solid obtained in the step 1) in an organic solvent, washing with an alkali liquor, then washing with deionized water to be neutral, and drying in vacuum to obtain the unsaturated benzoxazine monomer.
9. The UV viscose reducing agent according to claim 1, wherein the preparation method of the acrylic resin comprises the following steps:
s1, uniformly mixing the soft monomer, the hard monomer, the functional monomer, the solvent and the initiator in an inert atmosphere for later use;
s2, adding the mixture obtained in the step S1 of 1/4-1/3 into a reaction kettle under an inert atmosphere, heating to react under a stirring condition, then dropwise adding the rest mixture obtained in the step S1, and continuing constant-temperature reaction after dropwise adding is finished;
s3 stopping reaction, distilling under reduced pressure to obtain viscous liquid for later use.
10. The UV viscose reducing agent according to claim 1, wherein the photosensitive monomer is a compound of a monofunctional monomer and a multifunctional monomer with functionality of not less than 3, the compound ratio is 0.6-1:1-2.5, and the monofunctional photosensitive monomer is fluoroalkyl (meth) acrylate, and is specifically selected from at least one of trifluoroethyl methacrylate, hexafluorobutyl methacrylate and trifluoroethyl acrylate.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114395088A (en) * | 2022-02-21 | 2022-04-26 | 江西蓝星星火有机硅有限公司 | Organic silicon photodiffusion resin microsphere, preparation and application |
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| JPH1072525A (en) * | 1996-06-25 | 1998-03-17 | Toray Ind Inc | Molded plastics |
| JPH10251356A (en) * | 1997-03-14 | 1998-09-22 | Shin Etsu Chem Co Ltd | Photo-setting organopolysiloxane composition |
| JPH11100550A (en) * | 1997-09-25 | 1999-04-13 | Shin Etsu Chem Co Ltd | Curing of photo-curing organopolysiloxane composition |
| KR20100002845A (en) * | 2008-06-30 | 2010-01-07 | 대구대학교 산학협력단 | Siloxan compound for silicon hydrogel lens |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH1072525A (en) * | 1996-06-25 | 1998-03-17 | Toray Ind Inc | Molded plastics |
| JPH10251356A (en) * | 1997-03-14 | 1998-09-22 | Shin Etsu Chem Co Ltd | Photo-setting organopolysiloxane composition |
| JPH11100550A (en) * | 1997-09-25 | 1999-04-13 | Shin Etsu Chem Co Ltd | Curing of photo-curing organopolysiloxane composition |
| KR20100002845A (en) * | 2008-06-30 | 2010-01-07 | 대구대학교 산학협력단 | Siloxan compound for silicon hydrogel lens |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114395088A (en) * | 2022-02-21 | 2022-04-26 | 江西蓝星星火有机硅有限公司 | Organic silicon photodiffusion resin microsphere, preparation and application |
| CN114395088B (en) * | 2022-02-21 | 2024-02-27 | 江西蓝星星火有机硅有限公司 | Organosilicon light diffusion resin microsphere, preparation and application |
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