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Environment-friendly VP block copolymer as well as preparation method and application thereof

A block copolymer, an environment-friendly technology, applied in the field of environment-friendly VP block copolymer and its preparation, can solve the problems of affecting thermal conductivity, concern about powder dispersion effect, difficulty in satisfying high powder dispersion performance, etc., to achieve The effects of stable bonding, excellent hydrolysis resistance, and good market prospects

Active Publication Date: 2021-12-24
宇昂科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chinese patent CN 105777137 introduces a method for modifying the surface of AlN powder with rare earth salt sol; CN101508573 introduces a method for surface treatment using oxyacids, such as phosphate, silicic acid, etc.; CN 107954725 introduces a The combined use of a coupling agent and an organic acid for surface coating can effectively improve the hydrolysis resistance of AlN powder at high temperature; although the above methods have improved the hydrolysis resistance of AlN powder to a certain extent, but There are also certain deficiencies
On the one hand, the use of inorganic acid and coupling agent will inevitably introduce impurity elements such as silicon and phosphorus, which will affect the thermal conductivity. On the other hand, the existing modification methods have no effect on the dispersion effect of the modified powder. Any concern, and the good dispersion performance of AlN powder in water-based slurry is the basic basis for the preparation of high-performance ceramics
Therefore, the existing anti-hydrolysis treatment methods are difficult to meet the requirements of powder anti-hydrolysis without introducing impurity elements and having high dispersion performance

Method used

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  • Environment-friendly VP block copolymer as well as preparation method and application thereof
  • Environment-friendly VP block copolymer as well as preparation method and application thereof
  • Environment-friendly VP block copolymer as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] 1, preparation of endoxy PNVP-OH

[0040] NVP 100g, mercaptoethanol 3g, azo diisobutyronitrile 0.5 g, and 300 g of ethanol were sequentially added to the flask, and the preparation of terminal hydroxyl PNVP was performed under nitrogen protection. The reaction temperature was 75 ° C, and the reaction time was 8 hours; after the reaction was completed, the solvent was evaporated under reduced pressure, i.e., the end hydroxyl PNVP-OH.

[0041] 2, preparation of macromolecular chain transfer agent PA

[0042]10 g of 10 g, N, N'-bicyclic diimide, 4-cyano-4- (phenylthiocyl thiomethythiocyano) pentyl, 4-cyano-4- (phenylthiocyl thiomethythiomethyl) 300 g of dichloromethane, sequentially added argon emptying to the flask after 30 min, and the reaction was at room temperature for 24 hours. After the reaction was completed, the treatment was treated with ice-hexane, and then washed 3 times with diethyl ether, vacuum dried to obtain a macromolecular chain transfer agent PA.

[0043] 3...

Embodiment 2

[0048] 1, preparation of endoxy PNVP-OH

[0049] NVP 100g, mercaptoethanol 4g, azo di isodaryrile 1.0 g, isopropyl alcohol 1000 g, sequentially added to the flask, and the preparation of terminal hydroxyl PNVP was performed under nitrogen protection. The reaction temperature was 85 ° C, and the reaction time was 14 hours; after the reaction was completed, the solvent was evaporated under reduced pressure, i.e., the end hydroxy PNVP-OH.

[0050] 2, preparation of macromolecular chain transfer agent PA

[0051] Termine 15g, N, N'-diisopropyl carbonacethalimide 15g, 4-second Metamipyridine 2g, dichloromethane 500g, sequentially added argon emptying to 30 min after 30 min, at room temperature for 36 hours. After the reaction was completed, the treatment was treated with ice-hexane, and then washed 3 times with diethyl ether, vacuum dried to obtain a macromolecular chain transfer agent PA.

[0052] 3. Preparation of VP block copolymers

[0053] PA 10g, styrene 10.9 g, 9.1 g of nitrogen...

Embodiment 3

[0057] 1, preparation of endoxy PNVP-OH

[0058] NVP 100g, mercaptoethanol 5g, 2,2'-azo (2-methyl-N- (2-hydroxyethyl) proppenamide) 1.5 g, positive propyl alcohol 1500g, sequentially added to the flask, under nitrogen protection Preparation of terminal hydroxyl PNVP. The reaction temperature was 95 ° C, the reaction time was 20 hours; after the reaction was completed, the solvent was evaporated under reduced pressure, i.e., the end hydroxyl PNVP-OH.

[0059] 2, preparation of macromolecular chain transfer agent PA

[0060] 10 g, 1-ethyl-(3-dimethylaminopropyl) carbon diimide hydrochloride 20g, 1-ethyl-(3-dimethylaminopropyl) carbon diimide hydrochloride, 1-ethyl-(3-dimethylaminopropyl) carbon diimide hydrochloride - Dimethylpyridine 5g, dichloromethane 800 g, sequentially added argon emptying to the flask after 30 min, reaction at room temperature for 48 hours. After the reaction was completed, the treatment was treated with ice-hexane, and then washed 3 times with diethyl ether, ...

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Abstract

The invention provides an environment-friendly VP block copolymer as well as a preparation method and application thereof, and the preparation method comprises the following steps: adding N-vinyl pyrrolidone, mercaptoethanol, an initiator and a solvent into a flask, and reacting under the protection of nitrogen; after the reaction is completed, evaporating the solvent and residual monomers under reduced pressure to obtain PNVP-OH; reacting PNVP-OH, an RAFT reagent, a carbodiimide derivative, 4-dimethylaminopyridine and dichloromethane at normal temperature under the protection of argon, after the reaction is completed, carrying out ice cyclohexane precipitation treatment, repeatedly washing with diethyl ether, and drying to obtain a macromolecular chain transfer agent PA; reacting PA, styrene, itaconic anhydride, an initiator and a solvent under the protection of nitrogen, carrying out methanol precipitation treatment, repeatedly washing with diethyl ether, and drying to obtain the VP block copolymer. The VP block copolymer disclosed by the invention is used for surface modification of modified AlN powder, and the modified AlN powder has excellent hydrolysis resistance and good water-based dispersity.

Description

Technical field [0001] The present invention belongs to the field of AlN ceramic modification, and more particularly to an environmentally friendly VP block copolymer and a preparation method thereof. Background technique [0002] AlN ceramics have excellent insulation, thermal conductivity, high temperature resistance, corrosion resistance, and the advantages of matching the thermal expansion coefficient of silicon, which can be applied to integrated circuits and high power device packages and heat dissipation materials; prepare refractories, crucible Surface protection, the performance enhancement of structural materials, etc., and high-purity AlN ceramic is transparent, and can also be used as an optical device. The AlN powder is a raw material for preparing AlN ceramic, and its nature has a direct impact on the preparation process of AlN ceramics and ceramics. However, the surface of the AlN powder is extremely lively, and the hydrolysis reaction of the water vapor in the air...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F293/00C04B35/581C04B35/628
CPCC08F293/005C04B35/581C04B35/62802C08F2438/03
Inventor 王宇朱广东陈占
Owner 宇昂科技有限公司