CN114032036A - High-temperature-resistant UV (ultraviolet) curing sealant and preparation method thereof - Google Patents

High-temperature-resistant UV (ultraviolet) curing sealant and preparation method thereof Download PDF

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CN114032036A
CN114032036A CN202111342355.5A CN202111342355A CN114032036A CN 114032036 A CN114032036 A CN 114032036A CN 202111342355 A CN202111342355 A CN 202111342355A CN 114032036 A CN114032036 A CN 114032036A
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temperature resistant
high temperature
acrylate
linear
temperature
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CN114032036B (en
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郭晨婷
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Bonotec Electronic Materials Co ltd
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Bonotec Electronic Materials Co ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J4/00Adhesives 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
    • C09J4/06Organic 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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  • Sealing Material Composition (AREA)
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Abstract

The invention relates to a high-temperature-resistant UV curing sealant and a preparation method thereof. The high-temperature resistant UV curing sealant is composed of modified acrylate, hydrocarbon resin, an acrylic acid monomer, a photoinitiator, a reinforcing filler and an auxiliary agent, wherein the modified acrylate is linear acrylate and derivatives thereof, the linear main chain of the linear acrylate and the derivatives thereof is provided with a polybutadiene structure, the hydrocarbon resin is a linear carbon main chain, and the side chain of the hydrocarbon resin contains a benzene ring structure. The high-temperature-resistant UV curing sealant prepared by the invention can be UV cured and can resist high temperature such as reflow soldering temperature and the like.

Description

High-temperature-resistant UV (ultraviolet) curing sealant and preparation method thereof
Technical Field
The invention belongs to the technical field of adhesives, and particularly relates to a high-temperature-resistant UV (ultraviolet) curing sealant and a preparation method thereof.
Background
With the increasing application range of electronic products, the service life of the electronic products is becoming more and more important, water, oxygen, impurities and the like in the outside air greatly damage the service life of the products, and in order to prevent the water, oxygen, impurities and the like from entering the products, sealing treatment is usually required among all devices in the products. The conventional method is to assemble a formed silica gel sealing ring between electronic devices, but the operation flow is complex, and the sealing ring needs to be fixed by professional manpower or equipment, so that the production efficiency is reduced. Sealing glue is also used for replacing a sealing ring, but the electronic product can meet the reflow soldering requirement during assembly, heat can be generated during use, the sealing glue is easy to lose effectiveness after the product is at high temperature, and adverse effects are caused on the electronic product.
The prior patent with the application number of CN201510961809.5 discloses an epoxy modified acrylic resin for sealant, which is prepared from the following raw materials in parts by weight: methyl methacrylate, butyl acrylate, acrylic acid, an initiator, epoxy resin, a solvent and dodecyl mercaptan. The epoxy modified acrylic resin for the sealant of the patent integrates the advantages of epoxy resin and acrylic resin, so that the composite emulsion has excellent heat resistance, anti-adhesion, mechanical property, excellent adhesive force and the like, but the main chain of the epoxy resin contains a large number of benzene rings, the toughness is extremely poor, no rebound resilience exists, a benzene ring rigid structure can be introduced to the main chain of the sealant by direct addition, the integral toughness of the sealant is greatly reduced, and the sealing performance of the sealant is reduced. In order to avoid reducing the toughness of the sealant, the invention selects to graft a benzene ring on a side chain to improve the heat resistance of the whole sealant, and simultaneously introduces a polybutadiene structure with good toughness on a main chain to offset the side effect of toughness reduction caused by a rigid structure of the benzene ring.
Therefore, the UV curing sealant can be formed at one time, the problem of complex operation flow is solved, the production efficiency is improved, and meanwhile, the high temperature resistance of the UV curing sealant can ensure the sealing performance in the subsequent assembly and use processes.
Disclosure of Invention
The invention aims to solve the problems of the defects of the existing sealing technology, provides a high-temperature-resistant UV curing sealant and a preparation method thereof, and can effectively solve the problems of complex operation process and failure of the sealant after high temperature.
The purpose of the invention can be realized by the following scheme:
the invention provides a high-temperature resistant UV curing sealant, which comprises the following components in parts by weight:
Figure BDA0003352574560000011
Figure BDA0003352574560000021
in one embodiment of the present invention, the modified acrylate is a linear acrylate and a derivative thereof, and the linear acrylate and the derivative thereof have a polybutadiene structure in a linear main chain. Compared with a net structure, the linear structure has the advantages that the structural arrangement is more regular, the molecular chain is more flexible, and the toughness is greatly improved. The polybutadiene structure is similar to a rubber structure, belongs to an elastomer structure, can cause multiple crazes and shear yielding when being impacted by external force, disperses actual impact energy borne on each point when the impact mechanical energy is averagely transmitted to each craze, can prevent the crazes from further deteriorating into cracks due to the polybutadiene structure, and can effectively reduce the stress concentration phenomenon due to the fact that molecules slide mutually and generate shear plastic flow. The polybutadiene structure exists on the main chain, so that the impact resistance of the structure can be utilized to improve the toughness of the sealant. The common carbon long chain structure can resist mechanical impact only through molecular sliding during impact, impact energy is difficult to conduct out, and stress concentration is easy to generate, so that after curing, the sealant prepared from the linear acrylate containing the polybutadiene structure can keep the colloid performance thereof at high temperature and maintain the sealing performance compared with other sealants.
As an embodiment of the invention, the modified acrylate is one or more of Sadoma CN9014NS, NISSO-PB TE-2000 and Japanese osaka BAC-45.
As one embodiment of the present invention, the hydrocarbon resin is a linear carbon main chain having a benzene ring structure in a side chain. The main chain is a linear structure, so that the molecular chains can be regularly arranged, and the toughness of the colloid is kept. The benzene ring structure of the side chain can improve the decomposition temperature of the colloid, reduce the damage to the side chain in the high-temperature process and maintain the sealing performance of the sealant.
As an embodiment of the invention, the hydrocarbon resin is one or more of NOVARES TM85AS, NOVARES TM90S and NOVARES TM20 AS.
As an embodiment of the invention, the acrylic monomer is one or more of N, N-dimethylacrylamide, isodecyl acrylate, isobornyl acrylate and tris (2-hydroxyethyl) isocyanurate triacrylate. The acrylic monomer used in the invention can reduce the viscosity of the sealant and is smoother to use.
As an embodiment of the invention, the photoinitiator is one or more of benzil dimethyl ether, 2,4, 6-trimethylbenzoyl diphenyl phosphorus oxide and bis (2,4, 6-trimethylbenzoyl) phenyl phosphorus oxide.
As an embodiment of the invention, the reinforcing filler is fumed silica.
As an embodiment of the invention, the auxiliary agent is one or more of a defoaming agent, a leveling agent and a silane coupling agent.
As an embodiment of the present invention, the antifoaming agent is Efka-2721; the leveling agent is BYK-333; the silane coupling agent is KH-570.
The invention also provides a preparation method of the cured sealant, which comprises the following steps:
mixing acrylic monomers with a photoinitiator, and heating to dissolve completely; then mixing the modified acrylic resin, the hydrocarbon resin, the reinforcing filler and the auxiliary agent and grinding the mixture to obtain the high-temperature resistant UV curing sealant
Compared with the prior art, the invention has the following beneficial effects:
1. the high-temperature-resistant UV curing sealant can resist the high temperature of 260 ℃ reflow soldering temperature and the like.
2. The sealant can be cured by UV, the photoinitiator forms an excited state in a few seconds by absorbing light energy to initiate molecular chain fracture polymerization, the curing molding time is short, the energy consumption is low, the production efficiency is improved, no by-product is generated in the curing process, high temperature is not generated, and the sealed device is prevented from being damaged.
3. The sealant is liquid before curing, can be tightly attached to sealing devices in different shapes when in use, reduces gaps generated on irregular devices by the traditional sealing ring, and improves the sealing performance.
4. The production process is simple, the raw materials are easy to obtain, and the industrial production is convenient.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples, which are set forth to provide a detailed description of the invention and a detailed description of the operation, will help those skilled in the art to further understand the present invention. It should be noted that the scope of the present invention is not limited to the following embodiments, and that several modifications and improvements made on the premise of the idea of the present invention belong to the scope of the present invention.
Examples 1 to 4
The following formulation prepares high temperature resistant UV curing sealant examples 1-4. Mixing acrylic monomers with a photoinitiator, and heating to dissolve completely; and mixing the modified acrylate, the hydrocarbon resin, the reinforcing filler and the auxiliary agent, and uniformly grinding the mixture on a three-roller machine to obtain the high-temperature resistant UV curing sealant.
The modified acrylate used in the examples was one of linear acrylate and its derivative, and the linear backbone had a polybutadiene structure. The carbon main chain of the used hydrocarbon resin is a linear main chain, and the side chain has a benzene ring structure.
Figure BDA0003352574560000031
Figure BDA0003352574560000041
Comparative example 1
This comparative example provides a high temperature resistant UV curable sealant, similar in composition and preparation to example 1, except that: the modified acrylate is sardomama CNUVE 151NS, and the structure of the modified acrylate is nonlinear modified acrylate without a polybutadiene structure.
Comparative example 2
This comparative example provides a high temperature resistant UV cured sealant, similar in composition and preparation to example 2, except that: piccotac 1095-N, the structure of which is non-linear hydrocarbon resin without a benzene ring structure on the side chain.
The high temperature resistant UV curable sealants prepared in examples 1-4 were tested and the results are shown in the following table.
And (3) testing the water immersion tightness: and fixing the device after the sealing glue is cured in a water container for testing, wherein the height of the device from the water surface is 1.5m, the temperature between the device and the water is stabilized at 15-35 ℃, the difference between the device and the water is less than 5 ℃, and standing for 24 h. And placing the potassium permanganate powder film on the other side of the device to observe whether the color change phenomenon occurs.
Figure BDA0003352574560000042
Figure BDA0003352574560000051
The devices are fixed in a water container for sealing test, and the color of the potassium permanganate powder film is not changed after 24 hours, so that the sealing performance is proved to be good; after the reflow soldering test at 260 ℃, the device is cooled to room temperature and then is subjected to sealing test, the color of the potassium permanganate powder film is not changed, and the sealing performance is proved to be good; the device is placed in a constant temperature and humidity box with the temperature of 85 ℃/85 percent RH for 120h, and is cooled to room temperature for sealing test, the color of the potassium permanganate powder film is not changed, and the sealing performance is proved to be good. The sealing performance of the examples 1, 2, 3 and 4 is satisfactory.
Comparative example 1 is solidified on the same device, the device is fixed in a water container for sealing test, the color of the potassium permanganate powder film is not changed after 24 hours, and the sealing performance is proved to be good; after the reflow soldering test at 260 ℃, the device is cooled to room temperature and then is subjected to a sealing test, the color of the potassium permanganate powder film is changed into mauve, and the colloid has fine cracks under a microscope, so that the sealing property is proved to be NG; the device is placed in a constant temperature and humidity box with the temperature of 85 ℃/85 percent RH for 120h, and is cooled to room temperature for sealing test, the color of the potassium permanganate powder film is not changed, and the sealing performance is proved to be good. Comparative example 1 the sealability was not satisfactory.
Comparative example 2 is solidified on the same device, the device is fixed in a water container for sealing test, the color of the potassium permanganate powder film is not changed after 24 hours, and the sealing performance is proved to be good; after the reflow soldering test at 260 ℃, the device is cooled to room temperature and then is subjected to a sealing test, the color of the potassium permanganate powder film is changed into mauve, and the tightness is proved to be NG; the device is placed in a constant temperature and humidity box with the temperature of 85 ℃/85 percent RH for 120h, and is cooled to room temperature for sealing test, the color of the potassium permanganate powder film is not changed, and the sealing performance is proved to be good. Comparative example 2 the sealability was not satisfactory.
The foregoing description of specific embodiments of the present invention has been presented. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes and modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention.

Claims (10)

1. The high-temperature-resistant UV curing sealant is characterized by comprising the following components in parts by weight:
Figure FDA0003352574550000011
2. the high temperature resistant UV curable sealant according to claim 1, wherein the modified acrylate is one of linear acrylate and its derivatives, and the linear backbone of the linear acrylate and its derivatives has polybutadiene structure.
3. The high temperature resistant UV curable sealant according to claim 2, wherein the modified acrylate is one or more of Sadoma CN9014NS, NISSO-PB TE-2000 and Japanese Osaka BAC-45.
4. The high temperature resistant UV curable sealant according to claim 1, wherein the carbon backbone of the hydrocarbon resin is a linear backbone and the side chain has a benzene ring structure.
5. The high temperature resistant UV curable sealant according to claim 4 wherein said hydrocarbon resin is one or more of NOVARES TM85AS, NOVARES TM90S, and NOVARES TM20 AS.
6. The high temperature resistant UV curable sealant according to claim 1, wherein said acrylic monomer is one or more of N, N-dimethylacrylamide, isodecyl acrylate, isobornyl acrylate, tris (2-hydroxyethyl) isocyanurate triacrylate.
7. The high temperature resistant UV curable sealant according to claim 1, wherein the photoinitiator is one or more of benzil dimethyl ether, 2,4, 6-trimethylbenzoyl diphenyl phosphorus oxide and bis (2,4, 6-trimethylbenzoyl) phenyl phosphorus oxide.
8. The high temperature resistant UV curable sealant according to claim 1, wherein said reinforcing filler is fumed silica.
9. The high-temperature resistant UV curing sealant as claimed in claim 1, wherein the auxiliary agent is one or more of a defoaming agent, a leveling agent and a silane coupling agent.
10. A method of preparing the high temperature resistant UV curable sealant according to claim 1, wherein the method comprises the steps of:
mixing acrylic monomers with a photoinitiator, and heating to dissolve completely; and mixing the modified acrylate, the hydrocarbon resin, the reinforcing filler and the auxiliary agent, and grinding to obtain the high-temperature resistant UV curing sealant.
CN202111342355.5A 2021-11-12 2021-11-12 High-temperature-resistant UV curing sealant and preparation method thereof Active CN114032036B (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106065164A (en) * 2016-07-26 2016-11-02 黄宇 A kind of thermosetting encapsulation environment-friendly resin materials
CN106833498A (en) * 2017-02-24 2017-06-13 广州回天新材料有限公司 One kind sealing marine glue and its preparation method and application
CN112724841A (en) * 2020-12-25 2021-04-30 浙江中特化工有限公司 High-transmittance low-shrinkage liquid optical cement

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106065164A (en) * 2016-07-26 2016-11-02 黄宇 A kind of thermosetting encapsulation environment-friendly resin materials
CN106833498A (en) * 2017-02-24 2017-06-13 广州回天新材料有限公司 One kind sealing marine glue and its preparation method and application
CN112724841A (en) * 2020-12-25 2021-04-30 浙江中特化工有限公司 High-transmittance low-shrinkage liquid optical cement

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