Preparation method of 2,2-bis(3-amino-4-hydroxylphenyl)hexafluoropropane

Abstract

The invention discloses a preparation method of 2,2-bis(3-amino-4-hydroxylphenyl)hexafluoropropane, belonging to the technical field of electronic chemical materials. The preparation method comprisesthe following steps: adopting 2,2-bis(3-nitro-4-hydroxylphenyl)hexafluoropropane as raw material and hydrazine hydrate dissolved in methanol as reductant to reduce 2,2-bis(3-nitro-4-hydroxylphenyl)hexafluoropropane under the action of catalyst CeO2-SnO and obtain raw 2,2-bis(3-amino-4-hydroxylphenyl)hexafluoropropane, using chelating agent to remove metal ions in the raw product and performing vacuum sublimation and purification to the obtained 2,2-bis(3-amino-4-hydroxylphenyl)hexafluoropropane in which metal ions are removed and finally obtaining the target product. The method has low production cost, high product purity, low contents of metal ions and high yield.

Description

technical field [0001] The invention discloses a preparation method of 2,2-bis(3-amino-4-hydroxyphenyl)hexafluoropropane, which belongs to the technical field of electronic chemical materials. Background technique [0002] 2,2-bis(3-amino-4-hydroxyphenyl)hexafluoropropane (BISAPAF) is a material chemical intermediate product with excellent performance and one of the important raw materials for the synthesis of polyimide. Polyimide is a high temperature resistant polymer with excellent oxidation stability, chemical resistance, radiation resistance, good toughness and flexibility, and is widely used in aviation / aerospace, electronics / electrical , glass, automobile, precision machinery and automatic office machinery and other fields. With the development of high performance, light weight, thinner and finer information electronic products, higher requirements are put forward for the insulation performance of polyimide materials, so it is necessary to use electronic grade 2,2-bi...

AI Technical Summary

Problems solved by technology

[0007] In the above-mentioned patent documents, the raw materials used in the method of Fushi Chemical in Japan are electronic-grade products, and electronic-grade 2,2-bis(3-amino-4-hydroxyphenyl)hexafluoropropane can be obtained, but the yield of this method is lower than 50 %, the reaction conditions are harsh, the cost is too high, and it is not suitable for industrial production

The method of the Shanghai Institute of Chemical Reagents belongs to the laboratory method, and the purity and heavy metal ions can only meet the requirements of industrial grade products, and cannot meet the requirements of electronic grade products

The catalyst used in the method of Changzhou Sunshine Pharmaceutical Raw Materials Co., Ltd. is a palladium-carbon catalyst. After obtaining the crude product, it is recrystallized several times with ultrapure water / DMF to obtain electronic grade products. This method has unstable product quality, high cost and high product yield. Low, the use of palladium carbon and hydrogen in the reduction process has great potential safety hazards. The solvent used is DMF with a toxic high boiling point, which is easy to form crystals with the product and is difficult to separate, which has a great impact on product quality. After multiple recrystallizations, the total yield It is less than 60%, and it is only suitable for laboratory use. In industrial use, it is difficult to completely remove the metal ions wrapped in crystals with ultrapure water, and the quality cannot meet the requirements of electronic grade.

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