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Method for preparing electronic grade 2,2-bis[(3-amino-4-hydroxy)phenyl]- hexafluoropropane

A technology of hexafluoropropane and hydroxyl, applied in the field of preparing electronic grade 2

Active Publication Date: 2012-10-03
CHANGZHOU SUNLIGHT PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] It is understood that there are almost no industrial manufacturers of electronic grade 2,2-bis[(3-amino-4-hydroxy)phenyl]-hexafluoropropane in China at present.

Method used

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  • Method for preparing electronic grade 2,2-bis[(3-amino-4-hydroxy)phenyl]- hexafluoropropane

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] In the autoclave of 100L band stirrer, drop into 15kg 2,2-bis[(3-nitro-4-hydroxyl) phenyl]-hexafluoropropane, 0.5kg Pd content are the Pd / C catalyst of 5%, 50kg Methanol solvent, steam is passed into the interlayer of the reaction kettle to heat up, the stirring is started, and the catalytic hydrogenation reaction is carried out under the condition of T=75-80°C. After the hydrogenation reaction is completed, heat filter to separate the Pd / C catalyst, the separated Pd / C catalyst can be recycled, and the separated filtrate is pumped into a 100L crystallization kettle, cooled, crystallized, filtered, and the obtained solid is used for 50Kg Ultrapure water / DMF (50:50) was recrystallized three times, filtered, and dried to obtain 10 kg of finished product, with a mass yield of 66.7%, content: ≥99.0%, and the content of sodium, potassium, calcium, iron, copper, and aluminum were all equal. Less than 1ppm, the filtrate can be applied.

Embodiment 2

[0023] Other conditions are identical with embodiment 1, just change methanol solvent into ethanol solvent, 3% Pd / C catalyst. 9.5kg of the product was obtained, the mass yield was 63.3%, the content: ≥99.0%, and the content of sodium, potassium, calcium, iron, copper, and aluminum were all less than 1ppm.

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Abstract

The invention relates to a method for preparing an electronic grade o-amino-phenol type polymer monomer, belonging to the technical field of chemical engineering of materials. 2,2-di[(3-nitryl-4-hydroxyl group)phenyl]-Hexafluoroacetore takes catalytic hydrogenation reaction in alcohols solvent in the presence of a catalyst; after simple treatment, the product of 2,2-di[(3-amino-4-hydroxyl group)phenyl]-Hexafluoroacetore with high content is obtained; the 2,2-di[(3-amino-4-hydroxyl group)phenyl]-Hexafluoroacetore is recrystallized for a plurality of times by ultrapure water / DMF to obtain the product of electronic grade 2,2-di[(3-amino-4-hydroxyl group)phenyl]-Hexafluoroacetore with very low content of metallic ion. The method is characterized by adoption of catalytic hydrogenation process,low production cost, little pollution to environment, good product quality, high yield, strong market competitiveness and easy industrial popularization and application.

Description

Technical field [0001] The invention relates to a method for preparing electronic grade 2,2-bis[(3-amino-4-hydroxyl)phenyl]-hexafluoropropane, which belongs to the technical field of electronic chemical materials. Background technique [0002] 2,2-bis[(3-amino-4-hydroxy)phenyl]-hexafluoropropane is a material chemical intermediate product with excellent performance. High-performance polybenzoxazole and polyimide materials can be prepared from the monomer. Electronic-grade monomers with extremely low metal ion content are used to synthesize polybenzoxazole and polyimide materials, which are used as coatings in high-tech products and fields such as microelectronics, chips, and semiconductors. [0003] It is known that there are almost no industrial manufacturers of electronic grade 2,2-bis[(3-amino-4-hydroxy)phenyl]-hexafluoropropane in China. Contents of the invention [0004] The purpose of the present invention is to provide a kind of preparation electronic grade 2,2-bi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C215/76C07C213/02
Inventor 胡国宜薛建伟闵雪峰周国平
Owner CHANGZHOU SUNLIGHT PHARMA