Two-component fluorosilicone gel as well as preparation method and application thereof
By using a two-component fluorosilicone gel, combining vinyl fluorosilicone oil and hydrofluorosilicone oil, and using fluorosilane coupling agent and specific catalyst, the transparency and adhesion problems caused by insoluble fluorosilicone gels are solved, and high transparency, high elasticity and good solvent resistance are achieved.
Patent Information
- Application Number
- CN202411913547.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-24
- Publication Date
- 2025-05-06
AI Technical Summary
When using conventional silicone oil systems and perfluoro silicone oil systems, existing fluorosilicone gels lead to insoluble problems, affecting transparency and adhesion, and oil slithering is prone to appear on the gel surface.
A two-component fluorosilicone gel, including vinyl fluorosilicone oil and hydrofluorosilicone oil as the main components, and a fluorosilane coupling agent and a specific catalyst are used to prepare the gel through vulcanization reaction.
It achieves high transparency, high elasticity and good adhesion, avoids oil seepage, and does not degummize after reflow soldering at 260°C, and has good solvent resistance.
Smart Images

Figure BDA0005206322350000021 
Figure BDA0005206322350000031 
Figure BDA0005206322350000051
Abstract
Description
Technical Field
[0001] The invention belongs to the field of polymer materials, and in particular relates to a two-component fluorosilicone gel and a preparation method and application thereof. Background Art
[0002] Silicone gel packaging materials are widely used in power semiconductor packaging. They can insulate and protect the circuits and chips inside the device, thereby improving the reliability and performance of the module. Silicone gel is a special silicone rubber that "coexists solid and liquid". It has the characteristics of high elasticity, low stress and extremely small Young's modulus. Therefore, it can provide better vibration reduction protection for electronic components, ensure that components can work stably under large temperature fluctuations and strong vibration conditions, and extend the service life of components. Addition-type silicone gel does not produce by-products during the curing process, is simple to operate, can quickly and deeply cure, and is non-corrosive. Therefore, its application in the field of electronic and electrical packaging protection has great research value.
[0003] Most of the silicone gel materials reported so far have a hardness level of Shore A or Shore 00, while silicone gels used in some specific occasions need to have a lower hardness to ensure low internal stress and flexibility of the material.
[0004] Fluorosilicone gel system is more suitable for some environments that need to contact with chemical reagents such as acids and alkalis, be exposed to chemical gases, and have high requirements for high temperature resistance. Fluorosilicone gel is a highly elastic gel composed of fluorinated hydrocarbons or fluoroethers and siloxanes. It has high temperature resistance and chemical stability and is mainly used in high-temperature sealing materials, electronic component packaging materials and other fields. Patent CN 114634622 A proposes a solvent-resistant fluorosilicone gel, which is a single-component fluorosilicone gel. The components are added to the system and mixed at one time. The vinyl fluorosilicone oil used is a double-terminal vinyl fluorosilicone oil and a side-chain vinyl fluorosilicone oil, and the catalyst is a general platinum catalyst; Patent CN 118388968 A proposes the preparation of a two-component silicone gel and its preparation method. The vinyl fluorosilicone oil is a single component. According to conventional experience, it is generally a double-terminal vinyl fluorosilicone oil or a side-terminal vinyl fluorosilicone oil. The tackifier used is a conventional organic silane coupling agent, which does not contain fluorine elements; the catalyst used is a general platinum catalyst; and a plasticizer is added to the gel. According to the principle of like dissolves like, ordinary silicone oil systems are not miscible with perfluorosilicone oil systems. Therefore, adding conventional silicone thickeners and platinum catalysts to the above-mentioned fluorosilicone gel system will cause turbidity, which will ultimately affect the transparency and adhesion of the fluorosilicone gel, and oil floating will easily appear on the surface of the gel.
[0005] Based on this, it is necessary to provide a new type of fluorosilicone gel with high transparency, high elasticity and resistance to oil and solvent environments. Summary of the invention
[0006] The purpose of the present invention is to provide a two-component fluorosilicone gel and its preparation method and application in order to solve at least one of the above problems. The present invention solves the problem in the prior art that the organic silicone oil system and the perfluorosilicone oil system are not miscible, which affects the transparency and adhesion of the fluorosilicone gel and the gel surface is prone to oil floating. This solution provides a two-component fluorosilicone gel with good elasticity, no oil seepage, high transparency, no degumming, and good solvent resistance. It can be used in the automotive and electronics industries, electronic components, etc. that require oil-resistant and solvent-resistant environments. It can well protect precision instruments and chips from being corroded by fuel, solvents, and high and low temperatures, and extend the service life of the device.
[0007] The purpose of the present invention is achieved through the following technical solutions:
[0008] The first aspect of the present invention discloses a two-component fluorosilicone gel, comprising the following components in percentage by mass:
[0009]
[0010] The fluorosilicone oil A is vinyl fluorosilicone oil or vinyl perfluoropolyether fluorosilicone oil;
[0011] The fluorosilicone oil B is hydrogen-containing fluorosilicone oil or perfluoropolyether-based hydrogen-containing fluorosilicone oil.
[0012] Preferably, it includes one or more of the following:
[0013] i) The vinyl fluorosilicone oil includes double-terminal vinyl fluorosilicone oil and single-terminal vinyl fluorosilicone oil;
[0014] ii) the viscosity of the vinyl fluorosilicone oil is 100 to 50,000 cp, more preferably 1,000 to 10,000 cp;
[0015] iii) the vinyl perfluoropolyether fluorosilicone oil includes single-end vinyl perfluoropolyether fluorosilicone oil and double-end vinyl perfluoropolyether fluorosilicone oil;
[0016] iv) The viscosity of the vinyl perfluoropolyether fluorosilicone oil is 100 to 50,000 cp, more preferably 1,000 to 10,000 cp.
[0017] Preferably, it includes one or more of the following:
[0018] i) The hydrogen-containing fluorosilicone oil comprises a structure shown in Formula I:
[0019]
[0020] Wherein, m+n=8-60; when R1 and R3 are H and R2 is CH3, it is structure a, and the hydrogen content is 0.01-0.20%, more preferably 0.01-0.15%, and further preferably 0.04-0.10%; when R1, R2, and R3 are all H, it is structure b, and the hydrogen content is 0.2-1.0%, more preferably 0.2-0.8%, and further preferably 0.2-0.5%;
[0021] ii) The hydrogen content of the perfluoropolyether-based hydrogen-containing fluorosilicone oil is 0.02 to 1.0%, more preferably 0.02 to 0.8%, and even more preferably 0.02 to 0.5%.
[0022] Preferably, in the hydrogen-containing fluorosilicone oil of structure a and the hydrogen-containing fluorosilicone oil of structure b, the mass ratio of total hydrogen element (H) to vinyl group (Vi) is 0.7-1.2%, more preferably 0.8-1.0%.
[0023] Preferably, the tackifier is a fluorine-containing silane coupling agent.
[0024] More preferably, the structural formula of the fluorinated silane coupling agent is RSiX3, RSi(CH3)X2, wherein R is one of trifluoropropyl, perfluoropolyether, and perfluoroalkane, and X includes any one of methoxy and ethoxy.
[0025] Preferably, the fluorosilicone platinum catalyst is a platinum catalyst coordinated with trifluoropropyl vinylsiloxane, wherein the Pt content is 5000 ppm.
[0026] Preferably, the inhibitor is selected from one or more of the following: 1-ethynyl-1-cyclohexanol, 3-methyl-1-hexynyl-3-ol, 2-methyl-3-butynyl-2-ol, 3,5-dimethyl-1-hexynyl-3-ol.
[0027] The second aspect of the present invention discloses a method for preparing the two-component fluorosilicone gel as described above, comprising the following steps:
[0028] (1) taking part of fluorosilicone oil A and fluorosilicone platinum catalyst according to the formula, mixing them evenly to obtain component A;
[0029] (2) taking the remaining portion of fluorosilicone oil A and fluorosilicone oil B, an inhibitor and a tackifier according to the formula, mixing them evenly to obtain component B;
[0030] (3) Component A and component B are mixed and vulcanized to obtain the two-component fluorosilicone gel.
[0031] Preferably, the mass ratio of component A to component B is 1-5:1, more preferably 1:1.
[0032] More preferably, the formula of this scheme is calculated by mass:
[0033] Component A:
[0034] Fluorosilicone oil A: 100 parts of double-end vinyl fluorosilicone oil, 0-10 parts of single-end vinyl fluorosilicone oil, or 100 parts of divinyl perfluoropolyether fluorosilicone oil, 0-10 parts of single-end vinyl perfluoropolyether fluorosilicone oil;
[0035] Fluorosilicon platinum catalyst 0.01-0.5 parts;
[0036] Component B:
[0037] Fluorosilicone oil A: 50-70 parts of double-end vinyl fluorosilicone oil, 0-10 parts of single-end vinyl fluorosilicone oil, or 50-70 parts of double-end vinyl perfluoropolyether fluorosilicone oil, 0-10 parts of single-end vinyl perfluoropolyether fluorosilicone oil;
[0038] Fluorosilicone oil B: 30-50 parts of hydrogen-containing fluorosilicone oil of structure a, 1-6 parts of hydrogen-containing fluorosilicone oil of structure b, or 20-40 parts of perfluoropolyether-based hydrogen-containing fluorosilicone oil;
[0039] 1.0 to 5.0 parts of tackifier;
[0040] Inhibitor 0.01~0.5 parts.
[0041] Preferably, the vulcanization is room temperature vulcanization or heated vulcanization, preferably heated vulcanization, and the vulcanization conditions are vulcanization at room temperature or at a temperature of 120 to 150° C. for 30 to 60 minutes.
[0042] The third aspect of the present invention discloses an application of any of the above-mentioned two-component fluorosilicone gels in the electrical field.
[0043] Compared with the prior art, the present invention has the following beneficial effects:
[0044] Fluorosilicone gel is prepared using fluorosilicone oil or perfluoropolyether fluorosilicone oil based on the Si-H addition principle. The prepared gel has good transparency, high elasticity and good adhesion to the substrate.
[0045] The fluorosilicone gel prepared in the embodiment of the present invention has good elasticity, no oil leakage, high transparency, no debonding after 260°C reflow soldering, and good solvent resistance. It can be used in other environments requiring oil resistance and solvent resistance, such as electronic components in the automotive and electronics industries, and can well protect precision instruments and chips from being corroded by fuel, solvents, and high and low temperatures, thereby extending the service life of the devices. DETAILED DESCRIPTION
[0046] The present invention is described in detail below with reference to specific embodiments, but this is by no means a limitation of the present invention.
[0047] In the following description, unless otherwise specified, the reagents used are conventional commercially available products, and the methods used are well known in the art.
[0048] In the following description, unless otherwise specified, the number of parts of each material is by mass.
[0049] A transparent two-component fluorosilicone gel, the two-component fluorosilicone gel comprising the following components in parts by weight:
[0050] Component A:
[0051] Fluorosilicone oil A: 100 parts of double-end vinyl fluorosilicone oil, 0-10 parts of single-end vinyl fluorosilicone oil, or 100 parts of divinyl perfluoropolyether fluorosilicone oil, 0-10 parts of single-end vinyl perfluoropolyether fluorosilicone oil;
[0052] Fluorosilicon platinum catalyst 0.01-0.5 parts;
[0053] Component B:
[0054] Fluorosilicone oil A: 50-70 parts of double-end vinyl fluorosilicone oil, 0-10 parts of single-end vinyl fluorosilicone oil, or 50-70 parts of double-end vinyl perfluoropolyether fluorosilicone oil, 0-10 parts of single-end vinyl perfluoropolyether fluorosilicone oil;
[0055] Fluorosilicone oil B: 30-50 parts of hydrogen-containing fluorosilicone oil of structure a, 1-6 parts of hydrogen-containing fluorosilicone oil of structure b, or 20-40 parts of perfluoropolyether-based hydrogen-containing fluorosilicone oil;
[0056] 1.0 to 5.0 parts of tackifier;
[0057] Inhibitor 0.01-0.5 parts;
[0058] The preparation steps are as follows:
[0059] (1) taking vinyl fluorosilicone oil or vinyl perfluoropolyether fluorosilicone oil and fluorosilicone platinum catalyst in parts by weight and mixing them uniformly to obtain component A;
[0060] (2) taking vinyl fluorosilicone oil or vinyl perfluoropolyether fluorosilicone oil, hydrogen-containing fluorosilicone oil or perfluoropolyether-based hydrogen-containing fluorosilicone oil, an inhibitor, and a tackifier according to weight parts, and mixing them uniformly to obtain component B;
[0061] (3) Component A and component B are uniformly mixed according to a mass ratio, and vulcanized at room temperature or under heating to obtain the two-component fluorosilicone gel.
[0062] The mass ratio of component A to component B is 1 to 5:1, preferably 1:1.
[0063] Vinyl fluorosilicone oil includes: double-end vinyl fluorosilicone oil and single-end vinyl fluorosilicone oil. The viscosity of the fluorosilicone oil is 100-50000cp, preferably 1000-10000cp.
[0064] The vinyl perfluoropolyether fluorosilicone oil includes: single-end vinyl perfluoropolyether fluorosilicone oil and double-end vinyl perfluoropolyether fluorosilicone oil, with a viscosity of 100 to 50,000 cp, preferably 1,000 to 10,000 cp;
[0065] The hydrogen fluorine silicone oil comprises a structure shown in Formula I:
[0066]
[0067] Among them, m+n=8~60; when R1 and R3 are H and R2 is CH3, it is structure a, and the hydrogen content is 0.01~0.20%, more preferably 0.01~0.15%, and further preferably 0.04~0.10%; when R1, R2, and R3 are all H, it is structure b, and the hydrogen content is 0.2~1.0%, more preferably 0.2~0.8%, and further preferably 0.2~0.5%.
[0068] The hydrogen content of the perfluoropolyether-based hydrogen-containing fluorosilicone oil is 0.02 to 1.0%, preferably 0.02 to 0.8%, and more preferably 0.02 to 0.5%.
[0069] The total H:Vi ratio of hydrogen-containing fluorosilicone oil to vinyl fluorosilicone oil is 0.7 to 1.2%, preferably 0.8 to 1.0%;
[0070] The tackifier is a fluorinated silane coupling agent; specifically, the structural formula of the fluorinated silane coupling agent is R(CH2)2SiX3, wherein R is one of trifluoropropyl, perfluoropolyether, and perfluoroalkane, and X includes any one of methoxy and ethoxy.
[0071] The fluorosilicone platinum catalyst is a platinum catalyst coordinated by trifluoropropyl vinylsiloxane, and the Pt content is 5000ppm; in the subsequent embodiments, this fluorosilicone platinum catalyst is used.
[0072] The inhibitor is selected from one or more of the following: 1-ethynyl-1-cyclohexanol, 3-methyl-1-hexynyl-3-ol, 2-methyl-3-butynyl-2-ol, 3,5-dimethyl-1-hexynyl-3-ol.
[0073] Example 1
[0074] Component A: 100 parts of 5000cp double-terminal vinyl fluorosilicone oil, 0.04 parts of fluorosilicone platinum catalyst containing 5000ppm of metal Pt.
[0075] The preparation method is as follows: put double-terminal vinyl fluorosilicone oil and fluorosilicone platinum catalyst into a disperser and stir at a speed of 800-1000 r / min for 1 hour;
[0076] Component B: 50 parts of 5000cp double-terminated vinyl fluorosilicone oil, 50 parts of hydrogen-containing fluorosilicone oil of structure a with a hydrogen content of 0.084%, 3 parts of hydrogen-containing fluorosilicone oil of structure b with a hydrogen content of 0.21%, 3 parts of all-heptadecafluorodecyl triethoxysilane viscosity enhancer, and 0.03 parts of inhibitor 1-ethynyl-1-cyclohexanol;
[0077] The preparation method is as follows: put double-terminal vinyl fluorosilicone oil and hydrogen-containing fluorosilicone oil of structure a into a disperser and stir at a speed of 800-1000 r / min for 0.5 h, put into a 100° C. oven and heat for 1 h, then add hydrogen-containing fluorosilicone oil of structure b, a tackifier and an inhibitor, and stir at a speed of 800-1000 r / min for 0.5 h;
[0078] Mix component A and component B in a mass ratio of 1:1 and vulcanize at room temperature or by heating to obtain a two-component fluorosilicone gel.
[0079] Example 2
[0080] Component A: 95 parts of 5000cp dual-end vinyl fluorosilicone oil, 5 parts of 2450cp single-end vinyl fluorosilicone oil, and 0.07 parts of fluorosilicone platinum catalyst containing 5000ppm of metal Pt.
[0081] The preparation method is as follows: put divinyl fluorosilicone oil, single-end vinyl fluorosilicone oil and fluorosilicone platinum catalyst into a disperser and stir at a speed of 800-1000 r / min for 1 hour;
[0082] Component B: 65 parts of 5000cp double-terminal vinyl fluorosilicone oil, 5 parts of 2450cp single-terminal vinyl fluorosilicone oil, 29 parts of hydrogen-containing fluorosilicone oil of structure a with a hydrogen content of 0.084%, 5 parts of hydrogen-containing fluorosilicone oil of structure b with a hydrogen content of 0.21%, 2 parts of perheptadecafluorodecyl triethoxysilane viscosity enhancer, and 0.05 parts of inhibitor 3,5-dimethyl-1-hexynyl-3-ol;
[0083] The preparation method is as follows: double-end vinyl fluorosilicone oil and hydrogen-containing fluorosilicone oil of structure a are put into a disperser and stirred at a speed of 800-1000 r / min for 0.5 h, put into a 100° C. oven and heated for 1 h, then single-end vinyl fluorosilicone oil, hydrogen-containing fluorosilicone oil of structure b, a tackifier and an inhibitor are added, and stirred at a speed of 800-1000 r / min for 0.5 h;
[0084] Mix component A and component B in a mass ratio of 1:1 and vulcanize at room temperature or by heating to obtain a two-component fluorosilicone gel.
[0085] Example 3
[0086] Component A: 20 parts of 2300 cp dual-end vinyl fluorosilicone oil, 70 parts of 5000 cp dual-end vinyl fluorosilicone oil, 10 parts of 2450 cp single-end vinyl fluorosilicone oil, and 0.08 parts of fluorosilicone platinum catalyst containing 5000 ppm of metal Pt.
[0087] The preparation method is as follows: double-ended vinyl fluorosilicone oil, single-ended vinyl fluorosilicone oil and fluorosilicone platinum catalyst are put into a disperser and stirred at a speed of 800-1000 r / min for 1 hour;
[0088] Component B: 50 parts of 5000cp double-terminal vinyl fluorosilicone oil, 10 parts of 2450cp single-terminal vinyl fluorosilicone oil, 31.5 parts of hydrogen-containing fluorosilicone oil of structure a with a hydrogen content of 0.084%, 3 parts of hydrogen-containing fluorosilicone oil of structure b with a hydrogen content of 0.21%, 3 parts of nine-carbon perfluoropolyether siloxane tackifier, and 0.06 parts of inhibitor 3,5-dimethyl-1-hexynyl-3-ol;
[0089] The preparation method is as follows: double-end vinyl fluorosilicone oil and hydrogen-containing fluorosilicone oil of structure a are put into a disperser and stirred at a speed of 800-1000 r / min for 0.5 h, put into a 100° C. oven and heated for 1 h, then single-end vinyl fluorosilicone oil, hydrogen-containing fluorosilicone oil of structure b, a tackifier and an inhibitor are added, and stirred at a speed of 800-1000 r / min for 0.5 h;
[0090] Mix component A and component B in a mass ratio of 1:1 and vulcanize at room temperature or by heating to obtain a two-component fluorosilicone gel.
[0091] Example 4
[0092] Component A: 20 parts of 2300 cp dual-end vinyl fluorosilicone oil, 70 parts of 5000 cp dual-end vinyl fluorosilicone oil, 10 parts of 2450 cp single-end vinyl fluorosilicone oil, and 0.10 parts of fluorosilicone platinum catalyst containing 5000 ppm of metal Pt.
[0093] The preparation method is as follows: double-ended vinyl fluorosilicone oil, single-ended vinyl fluorosilicone oil and fluorosilicone platinum catalyst are put into a disperser and stirred at a speed of 800-1000 r / min for 1 hour;
[0094] Component B: 50 parts of 5000cp double-terminal vinyl fluorosilicone oil, 10 parts of 2450cp single-terminal vinyl fluorosilicone oil, 39.5 parts of hydrogen-containing fluorosilicone oil of structure a with a hydrogen content of 0.04%, 5.0 parts of hydrogen-containing fluorosilicone oil of structure b with a hydrogen content of 0.21%, 4 parts of nine-carbon perfluoropolyether siloxane tackifier, and 0.08 parts of inhibitor 3,5-dimethyl-1-hexynyl-3-ol;
[0095] The preparation method is as follows: double-end vinyl fluorosilicone oil and hydrogen-containing fluorosilicone oil of structure a are put into a disperser and stirred at a speed of 800-1000 r / min for 0.5 h, put into a 100° C. oven and heated for 1 h, then single-end vinyl fluorosilicone oil, hydrogen-containing fluorosilicone oil of structure b, a tackifier and an inhibitor are added, and stirred at a speed of 800-1000 r / min for 0.5 h;
[0096] Mix component A and component B in a mass ratio of 1:1 and vulcanize at room temperature or by heating to obtain a two-component fluorosilicone gel.
[0097] Example 5
[0098] Component A: 84 parts of 7500 cp double-end vinyl perfluoropolyether fluorosilicone oil, 12 parts of 650 cp single-end vinyl perfluoropolyether fluorosilicone oil, and 0.05 parts of fluorosilicone platinum catalyst containing 5000 ppm of metal Pt.
[0099] The preparation method is as follows: double-end vinyl perfluoropolyether fluorosilicone oil, single-end vinyl perfluoropolyether fluorosilicone oil, and fluorosilicone platinum catalyst are put into a disperser and stirred at a speed of 800-1000 r / min for 1 hour;
[0100] Component B: 56 parts of 7500cp double-terminal vinyl perfluoropolyether fluorosilicone oil, 12 parts of 650cp single-terminal vinyl perfluoropolyether fluorosilicone oil, 32 parts of perfluoropolyether-based hydrogen-containing fluorosilicone oil with a hydrogen content of 0.065%, 4 parts of nine-carbon perfluoropolyether siloxane tackifier, and 0.07 parts of inhibitor 1-ethynyl-1-cyclohexanol;
[0101] The preparation method is as follows: double-end vinyl perfluoropolyether fluorosilicone oil and single-end vinyl perfluoropolyether fluorosilicone oil are put into a disperser and stirred at a speed of 800-1000 r / min for 0.5 h, put into a 100° C. oven and heated for 1 h, then single-end vinyl fluorosilicone oil, perfluoropolyether-based hydrogen-containing fluorosilicone oil, tackifier and inhibitor are added, and stirred at a speed of 800-1000 r / min for 0.5 h;
[0102] Mix component A and component B in a mass ratio of 1:1 and vulcanize at room temperature or by heating to obtain a two-component fluorosilicone gel.
[0103] Example 6
[0104] Component A: 70 parts of 5600 cp double-end vinyl perfluoropolyether fluorosilicone oil, 30 parts of 1000 cp single-end vinyl perfluoropolyether fluorosilicone oil, and 0.05 parts of fluorosilicone platinum catalyst containing 5000 ppm of metal Pt.
[0105] The preparation method is as follows: double-end vinyl perfluoropolyether fluorosilicone oil, single-end vinyl perfluoropolyether fluorosilicone oil, and fluorosilicone platinum catalyst are put into a disperser and stirred at a speed of 800-1000 r / min for 1 hour;
[0106] Component B: 48 parts of 5600cp double-terminal vinyl perfluoropolyether fluorosilicone oil, 30 parts of 1000cp single-terminal vinyl perfluoropolyether fluorosilicone oil, 18 parts of perfluoropolyether-based hydrogen-containing fluorosilicone oil with a hydrogen content of 0.1%, 4 parts of nine-carbon perfluoropolyether siloxane tackifier, and 0.07 parts of inhibitor 1-ethynyl-1-cyclohexanol;
[0107] The preparation method is as follows: double-end vinyl perfluoropolyether fluorosilicone oil and single-end vinyl perfluoropolyether fluorosilicone oil are put into a disperser and stirred at a speed of 800-1000 r / min for 0.5 h, put into a 100° C. oven and heated for 1 h, then single-end vinyl fluorosilicone oil, perfluoropolyether-based hydrogen-containing fluorosilicone oil, tackifier and inhibitor are added, and stirred at a speed of 800-1000 r / min for 0.5 h;
[0108] Mix component A and component B in a mass ratio of 1:1 and vulcanize at room temperature or by heating to obtain a two-component fluorosilicone gel.
[0109] Comparative Example 1
[0110] Component A: 20 parts of 2300 cp dual-end vinyl fluorosilicone oil, 80 parts of 5000 cp dual-end vinyl fluorosilicone oil, and 0.10 parts of an organosilicon platinum complex catalyst containing 3000 ppm of metal Pt.
[0111] The preparation method is as follows: put double-terminal vinyl fluorosilicone oil and organosilicon platinum complex catalyst into a disperser and stir at a speed of 800-1000 r / min for 1 hour;
[0112] Component B: 50 parts of 5000cp double-terminated vinyl fluorosilicone oil, 41.5 parts of hydrogen-containing fluorosilicone oil of structure a with a hydrogen content of 0.04%, 5.2 parts of hydrogen-containing fluorosilicone oil of structure b with a hydrogen content of 0.21%, 4 parts of vinyl trimethoxysilane tackifier, and 0.08 parts of inhibitor 3,5-dimethyl-1-hexynyl-3-ol;
[0113] The preparation method is as follows: double-end vinyl fluorosilicone oil and hydrogen-containing fluorosilicone oil of structure a are put into a disperser and stirred at a speed of 800-1000 r / min for 0.5 h, put into a 100° C. oven and heated for 1 h, then single-end vinyl fluorosilicone oil, hydrogen-containing fluorosilicone oil of structure b, a tackifier and an inhibitor are added, and stirred at a speed of 800-1000 r / min for 0.5 h;
[0114] Mix component A and component B in a mass ratio of 1:1 and vulcanize at room temperature or by heating to obtain a two-component fluorosilicone gel.
[0115] Comparative Example 2
[0116] Take the silicone gel on the market: Wacker 927F silicone gel.
[0117] The formulas of Examples 1 to 6 and Comparative Examples 1 and 2 were integrated as shown in Table 1.
[0118] Table 1 Formulas of fluorosilicone gel of Examples 1 to 6 and Comparative Examples 1 and 2 (parts by weight)
[0119]
[0120]
[0121]
[0122] Performance Test:
[0123] 1. Cone penetration: Tested according to GB / T 269-2023, using a full cone, unit 0.1mm;
[0124] 2. Oil permeability: Place the newly cured silicone gel on oil-absorbing paper and bake at 200 and 225℃ for 200h respectively, and observe the wetting condition of the oil-absorbing paper;
[0125] 3. Test of light transmittance
[0126] According to GB / T 2410-2008 Determination of light transmittance and haze of transparent plastics, it is measured by spectrophotometer.
[0127] 4. Determination of mass change rate
[0128] The shear strength is tested in accordance with the provisions of GB / T 1690-2010 Test method for solvent resistance of vulcanized rubber.
[0129] The test results are summarized in Table 2.
[0130] Table 2 Performance test results of fluorosilicone gel of Examples 1 to 6 and Comparative Examples 1 and 2
[0131]
[0132]
[0133] As shown in Table 2, in Comparative Example 1, no single-end vinyl fluorosilicone oil system is added, and a fluorine-free siloxane tackifier and a fluorine-free organosilicon platinum complex are used as catalysts. The transparency of the fluorosilicone gel obtained is significantly low, and there is oil seepage.
[0134] Through performance testing, the fluorosilicone gel prepared in the embodiment of the present invention has good elasticity, no oil leakage, high transparency, no debonding after 260° C. reflow soldering, good solvent resistance, and is generally equivalent to imported products.
[0135] The above description of the embodiments is to facilitate the understanding and use of the invention by those skilled in the art. It is obvious that those skilled in the art can easily make various modifications to these embodiments and apply the general principles described herein to other embodiments without creative work. Therefore, the present invention is not limited to the above embodiments, and improvements and modifications made by those skilled in the art based on the disclosure of the present invention without departing from the scope of the present invention should be within the scope of protection of the present invention.
Claims
1. A two-component fluorosilicone gel, characterized in that: The following components are included in mass percentage: The fluorosilicone oil A is vinyl fluorosilicone oil or vinyl perfluoropolyether fluorosilicone oil; The fluorosilicone oil B is hydrogen-containing fluorosilicone oil or perfluoropolyether-based hydrogen-containing fluorosilicone oil.
2. A two-component fluorosilicone gel according to claim 1, characterized in that: Include one or more of the following: i) The vinyl fluorosilicone oil includes double-terminal vinyl fluorosilicone oil and single-terminal vinyl fluorosilicone oil; ii) the viscosity of the vinyl fluorosilicone oil is 100 to 50,000 cp; iii) the vinyl perfluoropolyether fluorosilicone oil includes single-end vinyl perfluoropolyether fluorosilicone oil and double-end vinyl perfluoropolyether fluorosilicone oil; iv) The viscosity of the vinyl perfluoropolyether fluorosilicone oil is 100 to 50,000 cp.
3. A two-component fluorosilicone gel according to claim 1, characterized in that: Include one or more of the following: i) The hydrogen-containing fluorosilicone oil comprises a structure shown in Formula I: Wherein, m+n=8-60; when R1 and R3 are H and R2 is CH3, it is structure a, and the hydrogen content is 0.01-0.20%; when R1, R2 and R3 are all H, it is structure b, and the hydrogen content is 0.2-1.0%; ii) The hydrogen content of the perfluoropolyether-based hydrogen-containing fluorosilicone oil is 0.02 to 1.0%.
4. A two-component fluorosilicone gel according to claim 3, characterized in that: In the hydrogen-containing fluorosilicone oil of structure a and the hydrogen-containing fluorosilicone oil of structure b, the mass ratio of total hydrogen elements to vinyl groups is 0.7-1.2%.
5. A two-component fluorosilicone gel according to claim 1, characterized in that: The tackifier is a fluorine-containing silane coupling agent.
6. A two-component fluorosilicone gel according to claim 1, characterized in that: The fluorosilicon-platinum catalyst is a complex of fluorosilicon oligomer and platinum.
7. A two-component fluorosilicone gel according to claim 1, characterized in that: The inhibitor is selected from one or more of the following: 1-ethynyl-1-cyclohexanol, 3-methyl-1-hexynyl-3-ol, 2-methyl-3-butynyl-2-ol, and 3,5-dimethyl-1-hexynyl-3-ol.
8. A method for preparing a two-component fluorosilicone gel as claimed in any one of claims 1 to 7, characterized in that: The steps include: (1) taking part of fluorosilicone oil A and fluorosilicone platinum catalyst according to the formula, mixing them evenly to obtain component A; (2) taking the remaining portion of fluorosilicone oil A and fluorosilicone oil B, an inhibitor and a tackifier according to the formula, mixing them evenly to obtain component B; (3) Component A and component B are mixed and vulcanized to obtain the two-component fluorosilicone gel.
9. The method for preparing a two-component fluorosilicone gel according to claim 8, characterized in that: The mass ratio of component A to component B is 1-5:
1.
10. Use of the two-component fluorosilicone gel according to any one of claims 1 to 7 in the electrical field.
Citation Information
Patent Citations
Solvent resistant fluorosilicone gels
CN114634622A
Cited By
Heat-conducting gel as well as application and use method thereof
CN122037585A