High-temperature-resistant polymer containing m-carborane group and preparation method of high-temperature-resistant polymer

A technology of high-temperature-resistant polymers and dichlorophenyl-m-carborane, which is applied in the field of high-temperature-resistant polymers and ceramic precursors, can solve the problems of difficult synthesis, high toxicity of raw materials, and low yield, and achieve access and use Convenience and safety, low chemical toxicity and stable chemical properties

Active Publication Date: 2021-06-15
NAT UNIV OF DEFENSE TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

This patented inventor describes different methods that make sure they have good heat resistance while also being able to store them overnight without losing their original quality when needed. These techniques include adding certain substances called meta carriers (metal atoms) into the composition during manufacturing processes such as calcination, sintering, etc., create special structures on the surface of these compositions, and then treat them afterwards under specific temperatures until crystalline phases form naturally within seconds. By controllably changing this phase structure, researchers found out how well the resulting compound was effective against various types of radiation damage caused by alpha rays. Overall, this technology provides technical means for producing strong thermally protected organopolymers useful as antioxiatic/radiation coatings and other applications related to atomic energy science technologies including radioactive waste management.

Problems solved by technology

This patented technical solution describes how certain types of molecules called chalcogenides are found naturally occurring within organisms that contain silicon (Si). These molecular structures make up about 70 per cent of all known natural substances - including many important biological functions such as photosynthesis or bone growth processes. They help stabilise these systems at very specific temperatures during their formation. By introducing them inside another type of material like plastics they could be used for various applications where heat protection, mechanical strength, optical transparency, etc., were needed.

Method used

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  • High-temperature-resistant polymer containing m-carborane group and preparation method of high-temperature-resistant polymer

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preparation example Construction

[0026] The present invention also proposes a method for preparing a high-temperature-resistant polymer containing m-carborane groups as described above, comprising the steps of:

[0027] S1: Under anhydrous and oxygen-free conditions, react n-butyllithium and m-carborane in an aprotic solvent to generate carborane lithium salt, then add cuprous salt and the cuprous salt ligand to obtain carborane alkane-copper mixture, and then adding p-chloroiodobenzene or chloriodobenzene to the carborane-copper mixture, heating and reacting to obtain dichlorophenyl-m-carborane monomer; the reaction yield is about 75-90%.

[0028] S2: Under anhydrous and oxygen-free conditions, add the main catalyst, co-catalyst, reducing agent, main catalyst main ligand, main catalyst auxiliary ligand and polar aprotic solvent, heat the reaction, and then add the dichlorophenyl The carborane monomer is refluxed at 55-80°C for 10-24 hours, and finally the reaction is quenched with hydrochloric acid / methanol ...

Embodiment 1

[0059] This embodiment provides a high-temperature-resistant polymer containing m-carborane groups, the high-temperature-resistant polymer is poly[bis(4-chlorophenyl) m-carborane], the chemical structural formula is (1),

[0060]

[0061] Wherein, n is the degree of polymerization, and n takes an integer of 2-300.

[0062] This embodiment also provides a method for preparing a high-temperature-resistant polymer containing m-carborane groups as described above, comprising the following steps:

[0063] The first part, monomer synthesis:

[0064] 1. Add 2.8847g (0.02mol) m-carborane and a stirring magnet into a glass reactor and seal it.

[0065] 2. Repeat the process of evacuating the reaction vessel and filling it with nitrogen three times.

[0066] 3. Add 50 mL of anhydrous ethylene glycol dimethyl ether into the reaction vessel, and m-carborane dissolves after stirring.

[0067] 4. After applying an ice-water bath for several minutes, slowly add 26 mL (0.0416 mol) of 1....

Embodiment 2

[0086] This embodiment provides a high temperature resistant polymer containing m-carborane group, the high temperature resistant polymer is poly[bis(3-chlorophenyl) m-carborane], the chemical structural formula is (2),

[0087]

[0088] Wherein, n is the degree of polymerization, and n takes an integer of 2-300.

[0089] This embodiment also provides a method for preparing a high-temperature-resistant polymer containing m-carborane groups as described above, comprising the following steps:

[0090] The first part, monomer synthesis:

[0091] 1. Add 2.1635g (0.015mol) of m-carborane and a stirring magnet into a glass reactor and seal it.

[0092] 2. Repeat the process of evacuating the reaction vessel and filling it with nitrogen three times.

[0093] 3. Add 60 mL of anhydrous ethylene glycol dimethyl ether into the reaction vessel, and m-carborane dissolves after stirring.

[0094] 4. After applying an ice-water bath for several minutes, slowly add 19.5 mL (0.0312 mol) ...

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Abstract

The invention discloses a high-temperature-resistant polymer containing m-carborane group and a preparation method of the high-temperature-resistant polymer. The high-temperature-resistant polymer is poly[bis(4-chlorphenyl)-m-carborane] or poly[bis(3-chlorphenyl)-m-carborane], the thermal stability is good, the oxidation resistance is good, the ceramic yield is high, and the polymer can be applied to the fields of boron carbide ceramic precursors, anti-oxidation coatings, neutron shielding materials, photoluminescent materials and the like. The preparation method comprises the steps of monomer synthesis, monomer polymerization and the like, m-carborane which is stable in property and low in toxicity is used as a boron source substance to replace unstable and highly toxic decaborane adopted in the prior art, the process is simple and safe, the synthesis difficulty of the polymer is low, and the preparation method is suitable for mass production.

Description

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Claims

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Application Information

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Owner NAT UNIV OF DEFENSE TECH
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