Room temperature curing ultrahigh temperature-resistant adhesive, liquid silicon resin dedicated for the room temperature curing ultrahigh temperature-resistant adhesive and their preparation methods

A liquid silicon and silica gel adhesive technology, applied in the direction of adhesives, non-polymer adhesive additives, adhesive additives, etc., can solve the problems of temperature resistance limited to 350 ℃, poor bonding performance, etc., to improve the degradation temperature, good Temperature resistance, the effect of excellent temperature resistance

Active Publication Date: 2012-08-08
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main problem of this type of adhesive is its poor bonding performance. For this reason, many researchers have made a lot of improvements.
[0004] Chinese patent CN1101055A reported that the use of silicon nitrogen polymer as a curing agent for silicone rubber can significantly improve the temperature resistance and bonding strength of si

Method used

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  • Room temperature curing ultrahigh temperature-resistant adhesive, liquid silicon resin dedicated for the room temperature curing ultrahigh temperature-resistant adhesive and their preparation methods
  • Room temperature curing ultrahigh temperature-resistant adhesive, liquid silicon resin dedicated for the room temperature curing ultrahigh temperature-resistant adhesive and their preparation methods
  • Room temperature curing ultrahigh temperature-resistant adhesive, liquid silicon resin dedicated for the room temperature curing ultrahigh temperature-resistant adhesive and their preparation methods

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] The preparation method of the liquid silicone resin in this example is as follows: In a three-necked flask equipped with a stirrer, a condenser, and a dropping funnel, add 1091 mL of distilled water and 386 mL of toluene, cool to 0 ° C with ice water, and then place the liquid in the dropping funnel Add 52.9 mL of phenyltrichlorosilane, 83.6 mL of diphenyldichlorosilane, 12.4 mL of methylvinyldichlorosilane, 33.8 mL of dimethyldichlorosilane, and 127 mL of toluene, which were added dropwise into the flask, the temperature was raised to 70°C after dropping, and the stirring was continued for 10 hours to end the reaction. Separate the organic phase, wash with distilled water several times until neutral, dry over anhydrous magnesium sulfate, filter, and remove the solvent under reduced pressure to obtain a transparent liquid silicone resin.

[0045] The liquid silicone resin prepared in this embodiment is R in formula I 1 = methyl or phenyl, R 2 = methyl, vinyl or phenyl...

Embodiment 2

[0047]The preparation method of the liquid silicone resin in this example is as follows: In a three-necked flask equipped with a stirrer, a condenser, and a dropping funnel, add 873 mL of distilled water and 309 mL of toluene, cool to 0 ° C with ice water, and then place the liquid in the dropping funnel Add 16.83 mL of hydrotrichlorosilane, 13.25 mL of diphenyldichlorosilane, 9.9 mL of methylvinyldichlorosilane, 43.74 mL of dimethyldichlorosilane, and 102 mL of toluene, which were added dropwise to In the flask, after dropping, the temperature was raised to 40°C, and stirring was continued for 40 hours to end the reaction. Separate the organic phase, wash with distilled water several times until neutral, dry over anhydrous magnesium sulfate, filter, and remove the solvent from the filtrate under reduced pressure to obtain a transparent liquid silicone resin.

[0048] The liquid silicone resin prepared in this embodiment is R in formula I 1 = methyl or phenyl, R 2 = methyl, ...

Embodiment 3

[0050] The preparation method of the liquid silicone resin in this example is as follows: In a three-neck flask equipped with a stirrer, a condenser, and a dropping funnel, add 873 mL of distilled water and 309 mL of toluene, place it in a water bath at 30°C, and add 30.8 mL of distilled water to the dropping funnel. Add mL of methyltrichlorosilane, 51.61mL of diphenyldichlorosilane, 35.80mL of dimethyldichlorosilane and 102mL of toluene dropwise into the flask, after the dropwise temperature rises to 80°C, continue After stirring for 9 hours, the reaction was terminated. Separate the organic phase, wash with distilled water several times until neutral, dry over anhydrous magnesium sulfate, filter, and remove the solvent under reduced pressure to obtain a transparent liquid silicone resin.

[0051] The liquid silicone resin prepared in this embodiment is R in formula I 1 = methyl or phenyl, R 2 = methyl or phenyl, R 3 =methyl, m=4~6, n=2~4 liquid silicone resin. Its number...

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Abstract

The invention discloses a room temperature curing ultrahigh temperature-resistant adhesive, a liquid silicon resin dedicated for the room temperature curing ultrahigh temperature-resistant adhesive and their preparation methods. The preparation method of the liquid silicon resin comprises the following steps of dissolving organic chlorosilanes in one or more organic solvents, dropwisely adding the mixture obtained by the previous step into a mixture of water and one or more organic solvents, stirring at a temperature of 40 to 100 DEG C for 5 to 40 hours, separating out an organic phase, washing the organic phase by distilled water so that a pH value is 7, drying, filtering, and carrying out solvent removal to obtain the liquid silicon resin which is transparent. The liquid silicon resin as an adhesive base, a silicon-nitrogen polymer as a curing agent and a certain amount of a composite filling material are prepared into the room temperature curing ultrahigh temperature-resistant adhesive. After room temperature curing for 3 days, the room temperature curing ultrahigh temperature-resistant adhesive has single-lap joint shearing strength of 5.63Mpa to stainless steel. After aging at a temperature of 1000 DEG C for 20 minutes, the room temperature curing ultrahigh temperature-resistant adhesive retains shearing strength of 2.16Mpa. After room temperature curing, the room temperature curing ultrahigh temperature-resistant adhesive has the maximum shearing strength of 2.41Mpa at a temperature of 800 DEG C.

Description

technical field [0001] The invention relates to a room temperature curing ultra-high temperature resistant adhesive, a special liquid silicone resin and a preparation method thereof. Background technique [0002] With the development of the aerospace industry and the improvement of the flight speed of the aircraft, higher requirements are put forward for the temperature resistance of the adhesive connecting the various parts of the aircraft. However, the existing ordinary epoxy and phenolic resin adhesives have low temperature resistance and are difficult to meet the requirements. Although polymers containing aromatic heterocycles such as polyimide and polybenzimidazole can withstand high temperatures of 500°C for a short time, Usually it needs high temperature and high pressure to cure, the manufacturing process is complicated and the cost is high; while inorganic adhesives such as phosphate and silicate have good temperature resistance, but due to their high brittleness, p...

Claims

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Application Information

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IPC IPC(8): C08G77/04C08G77/12C08G77/20C08G77/06C09J183/04C09J183/05C09J183/07C09J183/06C09J183/08C09J11/04
Inventor 徐彩虹刘伟罗永明
Owner INST OF CHEM CHINESE ACAD OF SCI
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