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Carborane-containing adhesive resin with resistance to high and low temperature and preparation method thereof

A technology of high and low temperature resistance, adhesives, applied in the direction of adhesives, adhesive types, polyurea/polyurethane adhesives, etc., can solve the problems of harsh conditions, high synthesis difficulty, limited funds and experimental conditions, etc. performance, achieve controllability, achieve the effect of bond strength and high and low temperature resistance

Active Publication Date: 2020-08-07
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

As early as the 1960s, my country carried out research on borohydride compounds. However, due to the long synthesis route of carborane and its derivatives, harsh conditions, high synthesis difficulty and high price, it is limited in terms of funding and experimental conditions. Very limited, so carborane polymers have been in a slow state of development

Method used

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  • Carborane-containing adhesive resin with resistance to high and low temperature and preparation method thereof
  • Carborane-containing adhesive resin with resistance to high and low temperature and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 1) Add 1 mol of trimethylolpropane to 20 ml of ethyl acetate and stir to dissolve, remove water under reduced pressure at 20°C for 10 min, and then store under argon atmosphere;

[0024] 2) Preparation of isocyanate-terminated carborane prepolymer (component A): under argon atmosphere, stir 0.32 mol of PAPI and 5 ml of ethyl acetate at 10°C, heat up to 60°C, add in batches after dehydration The trimethylolpropane-butyl acetate and 1,7-dimethylolcarborane-ethyl acetate took 20 minutes; then the temperature was raised to 70°C for 0.5 hours, and the isocyanate content was measured. After completion, it was cooled to room temperature and released material;

[0025] 3) Preparation of hydroxyl-terminated ABA-type silicone-containing polyether polyol (component B): polydimethylsiloxane and methallyl polyether are added to the tetrahydrochloride with N2 at a molar ratio of 1:0.5 In a flask, heat to 10°C. Add 0.5 ppm of chloroplatinic acid with a syringe, observe the temperatu...

Embodiment 2

[0028] 1) Trimethylolpropane dehydration: first add 1 mol trimethylolpropane into 110 ml ethyl acetate and stir to dissolve, remove water under reduced pressure at 50°C for 35 minutes, and then store under argon atmosphere;

[0029] 2) Preparation of isocyanate-terminated carborane prepolymer (component A): under argon atmosphere, stir 0.32mol PAPI and 30ml ethyl acetate at 35°C, heat up to 65°C, add dehydrated Trimethylolpropane-butyl acetate, 1,7-dimethylolcarborane-ethyl acetate, take 70min; then heat up to 85°C for 3 hours, measure isocyanate content, cool to room temperature after completion, and discharge ;

[0030] 3) Preparation of hydroxyl-terminated ABA-type silicone-containing polyether polyol (component B): polydimethylsiloxane and methallyl polyether are added to a tetrahydrochloride with N2 in a molar ratio of 1:1.5 In a flask, heat to 45°C. Add 8 ppm of chloroplatinic acid with a syringe, observe the temperature change, control the temperature not to exceed 10...

Embodiment 3

[0033] 1) Trimethylolpropane dehydration: first add 1 mol trimethylolpropane into 200 ml ethyl acetate and stir to dissolve, remove water under reduced pressure at 80°C for 60 minutes, and then store under argon atmosphere;

[0034]2) Preparation of isocyanate-terminated carborane prepolymer (component A): under argon atmosphere, stir 0.32mol PAPI and 50ml ethyl acetate at 60°C, heat up to 70°C, add dehydrated Trimethylolpropane-butyl acetate and 1,7-dimethylolcarborane-ethyl acetate took 120 minutes; then heated up to 100°C for 4 hours to measure the isocyanate content, cooled to room temperature after completion, and discharged;

[0035] 3) Preparation of hydroxyl-terminated ABA-type silicone-containing polyether polyol (component B): polydimethylsiloxane and methallyl polyether are added to the tetrahydrochloride with N2 at a molar ratio of 1:2.5 In a flask, heat to 80°C. Add 15 ppm of chloroplatinic acid with a syringe, observe the temperature change, control the temperat...

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Abstract

The invention discloses carborane-containing adhesive resin with resistance to high and low temperature and a preparation method thereof. The resin is prepared by reacting a component A and a component B under the catalysis of dibutyltin dilaurate, wherein the component A is prepared by dissolving 1,7-dihydroxymethyl carbon boron in ethyl acetate, adding polyphenyl polymethylene polyisocyanate anddehydrated trimethylolpropane in batches, and carrying out reacting under the protection of argon; and the component B is prepared by reacting silicon-hydrogen-terminated organic silicon resin and methyl allyl polyether under the catalysis of chloroplatinic acid and the protection of argon. According to the invention, the characteristics of the two components of the polyurethane adhesive are utilized, carborane groups are introduced into the component A, siloxane groups are introduced into the component B, and the two groups are easily combined with each other in the form of covalent bonds through the curing reaction of the component A and the component B. The carborane-siloxane type polyurethane adhesive prepared by the invention has very high bonding strength on steel, aluminum, titanium alloy, carbon materials, ceramic materials and composite materials, can be used for bonding missile nose cone-shells, C-C composite materials of heat-resistant parts of hypersonic aircrafts and graphite structural parts, and has a good military application prospect.

Description

technical field [0001] The invention relates to the field of polyurethane adhesives, in particular to a carborane-containing high-low temperature resistant adhesive resin and a preparation method thereof. Background technique [0002] With the development of hypersonic vehicles, high speed, high friction and engine combustion will generate high temperature, for metals (stainless steel, molybdenum, tungsten and titanium alloys), inorganic fiber reinforced composite materials, graphite, carbon materials, ceramic materials (porous and dense ), quartz, glass, asbestos, and mica, etc., have become increasingly prominent problems with high and low temperature resistance bonding. However, the organic adhesives currently used have limited temperature resistance, and have already decomposed at 300-400°C. In order to further meet the needs of high-tech fields such as aviation, aerospace, and weaponry in my country, high-low temperature resistant adhesives have become the development o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09J175/08C08G18/66C08G18/61C08G18/50C08G18/32C08G18/12C08G77/46
CPCC09J175/08C08G18/3206C08G18/3897C08G18/12C08G18/61C08G18/5096C08G77/46C08G18/50
Inventor 周权倪礼忠宋宁许星烨
Owner EAST CHINA UNIV OF SCI & TECH
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