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High-temperature resisting bonding sealed silicone resin and preparation method thereof

A technology of bonding and sealing, silicone resin, applied in chemical instruments and methods, non-polymer adhesive additives, adhesives, etc., can solve the problem of adhesive tensile strength and tensile shear strength less than 2MPa, less than 0.6 MPa, performance degradation and other problems, to achieve the effect of improving heat resistance, improving adhesive properties, and improving resin mechanics

Active Publication Date: 2017-11-17
NEW MATERIAL INST OF SHANDONG ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Patent CN106381122A uses phenyl vinyl silicone resin and silicone oil containing fused ring structure to effectively improve the heat resistance of the material, but the tensile strength and tensile shear strength of the prepared adhesive are less than 2MPa at room temperature, and heat treatment at 400°C for 1 hour After that, the performance is seriously reduced, and the tensile shear strength is lower than 0.6MPa, which still has a large gap with the actual needs

Method used

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  • High-temperature resisting bonding sealed silicone resin and preparation method thereof
  • High-temperature resisting bonding sealed silicone resin and preparation method thereof
  • High-temperature resisting bonding sealed silicone resin and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0027] A high-temperature-resistant adhesive and sealing silicone resin is made of the following raw materials in parts by weight:

[0028]

[0029] The Ph / R of the methylphenyl hydroxy silicone oil described therein is 20%, the viscosity (25°C) is 40000mpa·s, and the low volatile content is 0.14wt%.

[0030] The functionalized POSS is eight [(trialkoxysilyl) propyl]-POSS, its preparation reference (Polymer, 2010, 51 (17) p3867-3878.), the specific preparation process is as follows: anhydrous Diethyl ether 500ml, octavinyl POSS 10g (provided by Beijing Huawei Raycus Chemical Co., Ltd., purity 98%) and trimethoxysilane 73.2g were mixed, and 0.2g chloroplatinic acid isopropanol solution (0.1mol / L) was added to catalyze the reflux reaction After 24 hours, the solvent and unreacted raw materials were distilled off under reduced pressure to obtain 124.1 g of the product with a yield of 97.5%.

[0031]The heat-resistant filler is obtained by mixing iron oxide, aluminum oxide, ce...

Embodiment 2

[0035] A high-temperature-resistant adhesive and sealing silicone resin is made of the following raw materials in parts by weight:

[0036]

[0037] Among them, the methylphenyl hydroxy silicone oil Ph / R is 28%, the viscosity (25°C) is 10000mpa s, and the low volatile content is 0.12wt%. The functionalized POSS is octa[(trialkoxysilyl)propyl]-POSS, The preparation process is consistent with the description in Example 1; the heat-resistant filler is obtained by mixing iron oxide, aluminum oxide, cerium oxide, titanium dioxide, and graphite powder in a mass ratio of 1:5:1:0.2:1; the adhesive is KH560 and silanol sealant The terminal methyl phenyl siloxane oligomer is condensed at 120°C for 1 hour; the crosslinking agent is methyltrimethoxysilane; the catalyst is dibutyltin dilaurate. The preparation of methylphenylpolysiloxane-b-phenylsilsesquioxane block copolymer resin is consistent with that described in Example 1;

[0038] The preparation method of the high-temperature-r...

Embodiment 3

[0040] A high-temperature-resistant adhesive and sealing silicone resin is made of the following raw materials in parts by weight:

[0041]

[0042]

[0043] Among them, the Ph / R of methylphenyl hydroxy silicone oil is 20%, the viscosity (25°C) is 6000mpa·s, and the low volatile content is 0.14wt%.

[0044] Described functionalized POSS is octaglycidyl ether oxypropyl POSS, preparation reference (fine and specialty chemicals, 2011,19 (1), p21-23), concrete preparation process is as follows: the 100ml xylene and 60gKH560 Drop the mixed solution into a mixture of 200ml of isopropanol and 13g of 4% tetramethylammonium hydroxide aqueous solution for 1 hour, continue to stir at room temperature for 7 hours to carry out hydrolysis reaction, then condense at 80°C for 1 hour, and adjust the pH of the solution with saturated saline To neutrality, stirred at room temperature for 1 h, distilled off the solvent under reduced pressure, washed with acetone three times, removed the ace...

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Abstract

The invention relates to high-temperature resisting bonding sealed silicone resin and a preparation method thereof. The high-temperature resisting bonding sealed silicone resin is prepared from the following raw materials: methyl phenyl polysiloxane-b-polyphenylsilsesquioxane block copolymer resin, methyl phenyl hydroxy silicone oil, functional POSS (Polyhedral Oligomeric Silsesquioxane), heat-resisting filler, an adhesive, a cross-linking agent and a catalyst. The preparation method comprises the following steps: firstly, mixing the methyl phenyl polysiloxane-b-polyphenylsilsesquioxane block copolymer resin, the methyl phenyl hydroxy silicone oil and the functional POSS, and then carrying out vacuum stirring and dehydrating at the temperature of 100 to 120 DEG C for 1 to 2 hours; secondly, adding the heat-resisting filler and the cross-linking agent for carrying out vacuum stirring for 30 to 60 minutes, then adding the adhesive and the catalyst for carrying out vacuum stirring for 30 to 60 minutes, discharging and sealing to obtain the high-temperature resisting bonding sealed silicone resin. The resin has the advantages of better heat-resisting property and mechanical property, and no need of white carbon black for reinforcing and priming; in addition, the retention rate of shear strength is more than 90 percent after the resin is subjected to 400 DEG C*1 hour high-temperature treatment, and tensile strength, shear strength and peel strength are still more than 80 percent after the resin is subjected to 330 DEG C*24 hour treatment.

Description

technical field [0001] The invention relates to a silicone resin, in particular to a high-temperature-resistant bonding and sealing silicone resin and a preparation method thereof, belonging to the technical field of organic polymer materials. Background technique [0002] Silicone materials have excellent high and low temperature resistance, ultraviolet resistance, and atmospheric aging resistance, and play an important role in sealing and bonding in the fields of aviation, aerospace, electronics and electrical appliances. With the continuous development of science and technology, military and civilian fields have higher and higher requirements for the high temperature resistance of silicone adhesive sealing materials. Military fields such as sealing, shock absorption, heat insulation and thermal protection of rocket engines in power systems such as aircraft, tanks, and warships; civil fields such as automobile and ship engine cylinder head sealing, connection sealing, high...

Claims

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Application Information

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IPC IPC(8): C09J183/10C09J183/06C09J11/04C09J11/06C09K3/10
CPCC08K2003/2213C08K2003/2227C08K2003/2241C08K2003/2265C08L2201/08C08L2205/025C08L2205/03C08L2205/035C09J11/04C09J11/06C09J183/10C09K3/10C09K2003/1078C08L83/06C08K13/02C08K3/22C08K3/04C08K5/5435C08K5/5419
Inventor 牟秋红彭丹王峰张方志李冰赵宁李金辉于一涛张硕
Owner NEW MATERIAL INST OF SHANDONG ACADEMY OF SCI
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