CN110982481A - High-toughness organic silicon three-proofing adhesive - Google Patents
High-toughness organic silicon three-proofing adhesive Download PDFInfo
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- CN110982481A CN110982481A CN201911314088.3A CN201911314088A CN110982481A CN 110982481 A CN110982481 A CN 110982481A CN 201911314088 A CN201911314088 A CN 201911314088A CN 110982481 A CN110982481 A CN 110982481A
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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
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
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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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention relates to a high-toughness organic silicon three-proofing adhesive which comprises the following raw materials in parts by weight: 40-60 parts of polydimethylsiloxane containing silicon hydroxyl at two ends, 20-40 parts of organic silicon modified resin, 10-35 parts of silicone oil, 5-20 parts of cross-linking agent and 0.1-0.5 part of catalyst; the silicone three-proofing adhesive prepared by the invention has the advantages that the resin matrix is modified and contains the epoxy group, and the crosslinking density and the bulk strength of the silicone three-proofing adhesive are both higher than those of alkoxy groups of pure silicone resin in the curing process, so that the mechanical property and the toughness property of the silicone three-proofing adhesive are enhanced.
Description
Technical Field
The invention relates to a high-toughness organic silicon three-proofing adhesive, belonging to the technical field of adhesives.
Technical Field
Electronic equipment and electronic components are in the use, are difficult to avoid receiving the influence of chemical environment such as vibrations, humidity, salt fog, mould, high temperature, and circuit board and relevant electronic product probably produce corrosion, short circuit, mildenes and rot the scheduling problem and lead to product electrical apparatus performance impaired even break down, can influence the count accuracy of smart meter, shorten the life of components and parts.
Three proofings are glued mainly and are dampproofing, prevent salt fog and mould proof, can extensively use in circuit board and relevant electronic product, for it provides three proofings protective properties, become one deck transparent protection film after mainly solidifying through glue, under the protection of this kind of film, make circuit board and relevant equipment avoid the corruption of bad environment, ensure that electronic components is in intact state always, can not receive the chemical action such as other dust, moisture, salt fog simultaneously and lead to the short circuit, thereby reach the live time of extension components and parts, guarantee the stability in use of electronic product of components and parts.
The three-proofing adhesive has a very wide application range, and comprises various integrated circuits, automobile electronic series control boards, household appliance control boards, aviation instrument and meter circuit boards, intelligent meter control boards, precision measurement instrument control boards, flexible printed circuit boards, computer control boards, industrial control boards, semiconductor crystal circuit protection boards, battery protection boards, electronic toy control boards, LED control boards, frequency converter circuit boards, agricultural equipment control boards, electric vehicle control boards, outdoor LED display screens, security control boards, motor control boards and the like, and the market is very huge.
The types of three-proofing glue in the market at present are very huge, including organic silicon, polyurethane, acrylic acid, epoxy resin and the like, and different types have different application ranges. The silicone three-proofing adhesive occupies a large share in the market with the advantages of low VOCs, capability of being cured at normal temperature, low shrinkage rate and the like, and the curing mechanism is that Polydimethylsiloxane (PDMS) containing silicon hydroxyl at two ends and a cross-linking agent undergo a condensation reaction under the participation of moisture and a catalyst, and small molecules are released and are cross-linked to form an elastomer with certain elasticity. However, at present, due to the requirements of low viscosity, normal temperature moisture curing, low hardness and the like, the requirement on the three-proofing silicone adhesive is higher, and the normal temperature moisture curing silicone three-proofing adhesive has poor toughness and low strength, and is easy to break or crack under the conditions of impact, pressing and the like, so that the protection effect of the adhesive is influenced, and therefore the application of the silicone three-proofing adhesive is restricted by the difficult problem.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the high-toughness silicone three-proofing adhesive which has the advantages of high toughness and strength, convenience in operation, no heat release in the curing process, excellent aging resistance, energy conservation, environmental friendliness and the like.
The curing mechanism of the organosilicon type three-proofing adhesive is that Polydimethylsiloxane (PDMS) containing silicon hydroxyl at two ends and a cross-linking agent undergo a condensation reaction under the participation of moisture and a catalyst, and micromolecules are released and are simultaneously cross-linked into an elastomer with certain elasticity. The reasons for the poor strength are mainly that in polydimethylsiloxane systems, the molecular weight of the polydimethylsiloxane body is relatively small and the siloxane bonding of the siloxane polymers in the system is not dense. The invention provides a proper organic silicon modified resin which has a large molecular weight, can enhance the crosslinking density of the resin and the toughness of the resin under a neutral condition, and achieves the purpose of increasing the strength of organic silicon three-proofing adhesive.
The technical scheme for solving the technical problems is as follows: the organic silicon three-proofing adhesive comprises the following raw materials in parts by weight: 40-60 parts of polydimethylsiloxane containing silicon hydroxyl at two ends, 20-40 parts of organic silicon modified resin, 10-35 parts of silicone oil, 5-20 parts of cross-linking agent and 0.1-0.5 part of catalyst.
The polydimethylsiloxane containing silicon hydroxyl groups at two ends, wherein the polysiloxane contains at least two hydroxyl components per molecule, has a molecular weight of 500-2000, and has the following specific molecular formula:
the organic silicon modified resin is epoxy modified organic silicon resin, the molecular weight of the organic silicon modified resin is 1000-5000, and the specific molecular formula is as follows:
the cross-linking agent is polysiloxane with trimethoxyl at one end, and the specific molecular formula is as follows:
the crosslinking agent has a molecular formula, wherein R is a functional group, and R is methyl, ethyl, vinyl, phenyl, methylalkoxy or ethylalkoxy.
The silicone oil is methyl silicone oil, the methyl silicone oil is polysiloxane containing at least six methyl groups per molecule, the molecular weight of the methyl silicone oil is controlled to be 100-2000, and the specific molecular formula is as follows:
the catalyst is organic titanium catalyst, including tetraisopropyl titanate, tetrabutyl titanate, organic chelating titanate, such as DuPont Tyzor series, etc.
The preparation method of the organic silicon modified resin comprises the following steps: adding 20g of ethanol, 11g of 10% wt hydrochloric acid and 15g of distilled water into a four-round-bottom reaction bottle provided with a thermometer, a mechanical stirrer, a constant-pressure dropping funnel and a reflux condenser, quickly stirring at 35 ℃, dropwise adding 50g of tetraethoxysilane, continuously reacting for 2 hours after dropwise adding, heating to 60 ℃, dropwise adding 5g of hexamethyldisiloxane, heating to 80 ℃ after dropwise adding, dropwise adding 15g of mixed liquid of tetramethyldiphenyldisiloxane and KH560, wherein the mass ratio of the tetramethyldiphenyldisiloxane to the KH560 is 1: 1, after the dropwise addition, adding 100g of hexamethyldisiloxane as an extracting agent, and continuously refluxing; and after the reaction is finished, standing for layering, washing the organic solution with sodium bicarbonate aqueous solution, then washing with water to be neutral, carrying out reduced pressure distillation on the organic layer on a rotary evaporator to obtain white powdery solid, and drying in a constant-temperature drying oven to obtain a white powdery solid product, namely the organic silicon modified resin.
The silicone three-proofing adhesive prepared by the invention has the advantages that the resin matrix is modified and contains the epoxy group, and the crosslinking density and the bulk strength of the silicone three-proofing adhesive are both higher than those of alkoxy groups of pure silicone resin in the curing process, so that the mechanical property and the toughness property of the silicone three-proofing adhesive are enhanced.
Detailed Description
The principles and features of this invention are described below in conjunction with examples which are set forth to illustrate, but are not to be construed to limit the scope of the invention.
Example 1
40 parts of polydimethylsiloxane (n ═ 5) containing silicon hydroxyl at two ends, 30 parts of organic silicon modified resin, 15 parts of silicone oil (n ═ 3) and 14.78 parts of cross-linking agent (R is methyl) are added, high-purity nitrogen is blown in after vacuum pumping for premixing for 30min, 0.22 part of catalyst tetraisopropyl titanate is added, high-purity nitrogen is blown in after vacuum pumping for premixing for 30min, and the organic silicon three-proofing adhesive is obtained after uniform mixing.
Example 2
Firstly, 35 parts of polydimethylsiloxane (n ═ 5) with silicon hydroxyl groups at two ends, 35 parts of organic silicon modified resin, 15 parts of silicone oil (n ═ 3) and 14.78 parts of cross-linking agent (R is methyl) are added, high-purity nitrogen is blown in after vacuum pumping for premixing for 30min, 0.22 part of catalyst tetraisopropyl titanate is added, high-purity nitrogen is blown in after vacuum pumping for premixing for 30min, and the organic silicon three-proofing adhesive is obtained after uniform mixing.
Comparative example 1
70 parts of polydimethylsiloxane (n ═ 5) with silicon hydroxyl groups at two ends, 15 parts of silicone oil (n ═ 3) and 14.78 parts of cross-linking agent (R is methyl) are added firstly, high-purity nitrogen is blown in after vacuum pumping for premixing for 30min, 0.22 part of catalyst tetraisopropyl titanate is added, high-purity nitrogen is blown in after vacuum pumping for premixing for 30min, and the organic silicon three-proofing adhesive is obtained after uniform mixing.
Comparative example 2
Adding 70 parts of organic silicon modified resin, 15 parts of silicone oil (n is 3) and 14.78 parts of cross-linking agent (R is methyl), vacuumizing, blowing high-purity nitrogen for premixing for 30min, adding 0.22 part of catalyst tetraisopropyl titanate, vacuumizing, blowing high-purity nitrogen for premixing for 30min, and uniformly mixing to obtain the organic silicon three-proofing adhesive.
The silicone solid crystal glues of examples 1, 2 and comparative examples 1, 2 were tested, test one: testing viscosity by adopting AR-G2 equipment and a conical plate rotor at the rotating speed of 10rpm and the temperature of 25 ℃; and (2) testing: the tensile strength is tested by adopting a universal tensile machine and a dumbbell sample plate, the thickness is 1mm, the speed is 10mm/min, and the temperature is 25 ℃; and (3) testing: surface dry time test, which adopts GB/T13477.5-2002 building sealing material test method part 5, namely surface dry time test method;
TABLE 1 Performance index Table
| Performance index ﹨ sample | Example 1 | Example 2 | Comparative example 1 | Comparative example 2 |
| Viscosity (Pa. s) | 3.2 | 2.8 | 1.3 | 4.6 |
| Adhesive Strength (MPa) | 2.1 | 2.0 | 1.1 | 4.5 |
| Open time(s) | 400 | 380 | 260 | 650 |
As can be seen from the table 1, the tensile strength of the three-proofing adhesive can be effectively improved by introducing the organic silicon modified resin, and the adhesive has better toughness.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the scope of the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention are included in the scope of the present invention.
Claims (6)
1. The high-toughness organic silicon three-proofing adhesive is characterized by comprising the following raw materials in parts by weight: 40-60 parts of polydimethylsiloxane containing silicon hydroxyl at two ends, 20-40 parts of organic silicon modified resin, 10-35 parts of silicone oil, 5-20 parts of cross-linking agent and 0.1-0.5 part of catalyst;
the preparation method of the organic silicon resin comprises the following steps: adding 20g of ethanol, 11g of 10% wt hydrochloric acid and 15g of distilled water into a four-round-bottom reaction bottle provided with a thermometer, a mechanical stirrer, a constant-pressure dropping funnel and a reflux condenser, quickly stirring at 35 ℃, dropwise adding 50g of tetraethoxysilane, continuously reacting for 2 hours after dropwise adding, heating to 60 ℃, dropwise adding 5g of hexamethyldisiloxane, heating to 80 ℃ after dropwise adding, dropwise adding 15g of mixed liquid of tetramethyldiphenyldisiloxane and KH560, wherein the mass ratio of the tetramethyldiphenyldisiloxane to the KH560 is 1: 1, after the dropwise addition, adding 100g of hexamethyldisiloxane as an extracting agent, and continuously refluxing; and after the reaction is finished, standing for layering, washing the organic solution with sodium bicarbonate aqueous solution, then washing with water to be neutral, carrying out reduced pressure distillation on the organic layer on a rotary evaporator to obtain white powdery solid, and drying in a constant-temperature drying oven to obtain a white powdery solid product, namely the organic silicon modified resin.
2. The high-toughness silicone three-proofing adhesive according to claim 1, wherein the silicone modified resin has a molecular formula as follows:
3. the high-toughness silicone three-proofing adhesive according to claim 1, wherein the polydimethylsiloxane containing silicon hydroxyl groups at both ends has the following molecular formula:
4. the high-toughness silicone three-proofing adhesive according to claim 1, wherein the crosslinking agent is a polysiloxane containing trimethoxy at one end, and the specific formula is as follows:
r is methyl, ethyl, vinyl, phenyl, methyl alkoxy, ethyl alkoxy.
5. The high-toughness silicone three-proofing adhesive according to claim 1, wherein the silicone oil is methyl silicone oil, and the specific molecular formula is as follows:
6. The high-toughness silicone three-proofing adhesive according to claim 1, wherein the catalyst comprises one of tetraisopropyl titanate, tetrabutyl titanate and organic chelating titanate.
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| CN201911314088.3A CN110982481A (en) | 2019-12-19 | 2019-12-19 | High-toughness organic silicon three-proofing adhesive |
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| CN201911314088.3A CN110982481A (en) | 2019-12-19 | 2019-12-19 | High-toughness organic silicon three-proofing adhesive |
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Citations (5)
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|---|---|---|---|---|
| CN103342816A (en) * | 2013-06-19 | 2013-10-09 | 广州慧谷化学有限公司 | Organic silicone resin, curable organopolysiloxane composition and application |
| CN103666250A (en) * | 2013-12-13 | 2014-03-26 | 烟台德邦科技有限公司 | Organic silicon coating rubber and preparation method thereof |
| CN103965481A (en) * | 2013-02-01 | 2014-08-06 | 常州化学研究所 | Epoxy function group-containing silicone resin preparation method |
| CN106190015A (en) * | 2016-08-22 | 2016-12-07 | 深圳市新亚新材料有限公司 | A kind of no-solvent type organosilicon coating glue and preparation method thereof |
| CN108129845A (en) * | 2017-12-23 | 2018-06-08 | 广东新翔星科技股份有限公司 | A kind of preparation method of additional organosilicon packaging plastic adhesion promoters |
-
2019
- 2019-12-19 CN CN201911314088.3A patent/CN110982481A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103965481A (en) * | 2013-02-01 | 2014-08-06 | 常州化学研究所 | Epoxy function group-containing silicone resin preparation method |
| CN103342816A (en) * | 2013-06-19 | 2013-10-09 | 广州慧谷化学有限公司 | Organic silicone resin, curable organopolysiloxane composition and application |
| CN103666250A (en) * | 2013-12-13 | 2014-03-26 | 烟台德邦科技有限公司 | Organic silicon coating rubber and preparation method thereof |
| CN106190015A (en) * | 2016-08-22 | 2016-12-07 | 深圳市新亚新材料有限公司 | A kind of no-solvent type organosilicon coating glue and preparation method thereof |
| CN108129845A (en) * | 2017-12-23 | 2018-06-08 | 广东新翔星科技股份有限公司 | A kind of preparation method of additional organosilicon packaging plastic adhesion promoters |
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Address after: No.3-3, Kaifeng Road, Yantai Development Zone, Shandong Province 264006 Applicant after: Yantai Debang Technology Co.,Ltd. Address before: No.3-3, Kaifeng Road, Yantai Development Zone, Shandong Province 264006 Applicant before: DARBOND TECHNOLOGY Co.,Ltd. |
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Application publication date: 20200410 |