Production process for converting deep pickling yellow phosphorus into electronic grade red phosphorus

A production process and electronic-grade technology, applied in the field of elemental phosphorus preparation, can solve the problems of low recovery rate of yellow phosphorus, insufficient stirring, hidden safety hazards, etc., and achieve the effects of improving product purity, increasing yield, and improving recovery rate.

Inactive Publication Date: 2019-06-07
贵州金鼎电子信息新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] The object of the present invention is to provide a kind of production process that is converted into electronic grade red phosphorus by deep pickling yellow phosphorus, solves the poor effect of removing impurities (especially As, S and C) in the industrial grade yellow phosphoric acid washing process in the prior art, yellow phosphorus Low phosphorus recovery rate, insufficient stirring and potential safety hazards

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  • Production process for converting deep pickling yellow phosphorus into electronic grade red phosphorus

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Effect test

Embodiment 1

[0036] The production process of converting deep pickling yellow phosphorus into electronic grade red phosphorus, the specific method is:

[0037] (1) Deep pickling: Dilute the nitric acid with a mass fraction of 68% to a mass fraction of 20%, add it into a glass-lined cast iron kettle filled with industrial yellow phosphorus, and continue to stir mechanically, and circulate hot water in the outer interlayer of the kettle to keep it warm. Fully react nitric acid with impurities including As, S and C in industrial yellow phosphorus, and then wash the reaction product with pure water, the mass ratio of nitric acid and industrial yellow phosphorus is 1:3.

[0038] (2) Chlorination: The yellow phosphorus after deep pickling is transferred to the chlorination kettle, and chlorine gas is introduced to react with the yellow phosphorus to form phosphorus trichloride. The mass ratio of chlorine gas and yellow phosphorus is 1:0.29.

[0039] (3) Rectification: Control the temperature in ...

Embodiment 2

[0043] The production process of converting deep pickling yellow phosphorus into electronic grade red phosphorus, the specific method is:

[0044](1) Deep pickling: dilute nitric acid with a mass fraction of 68% to a mass fraction of 20%, then add it into a glass-lined cast iron kettle filled with industrial yellow phosphorus, and carry out continuous mechanical stirring, and the outer interlayer of the kettle is circulated for heat Water insulation is used to fully react the impurities including As, S and C in nitric acid and industrial yellow phosphorus, and then the reaction product is washed with pure water. The mass ratio of nitric acid and industrial yellow phosphorus is 1:3.

[0045] (2) Chlorination: The yellow phosphorus after deep pickling is transferred to the chlorination kettle, and chlorine gas is introduced to react with the yellow phosphorus to form phosphorus trichloride. The mass ratio of chlorine gas and yellow phosphorus is 1:0.29.

[0046] (3) Rectificatio...

Embodiment 3

[0050] The production process of converting deep pickling yellow phosphorus into electronic grade red phosphorus, the specific method is:

[0051] (1) Deep pickling: dilute nitric acid with a mass fraction of 68% to a mass fraction of 20%, then add it into a glass-lined cast iron kettle filled with industrial yellow phosphorus, and carry out continuous mechanical stirring, and the outer interlayer of the kettle is circulated for heat Water insulation is used to fully react the impurities including As, S and C in nitric acid and industrial yellow phosphorus, and then the reaction product is washed with pure water. The mass ratio of nitric acid and industrial yellow phosphorus is 1:3.

[0052] (2) Chlorination: The yellow phosphorus after deep pickling is transferred to the chlorination kettle, and chlorine gas is introduced to react with the yellow phosphorus to form phosphorus trichloride. The mass ratio of chlorine gas and yellow phosphorus is 1:0.29.

[0053] (3) Rectificati...

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Abstract

The invention discloses a production process for converting a deep pickling yellow phosphorus into an electronic grade red phosphorus. The industrial yellow phosphorus is successively subjected to thesteps containing deep pickling, chlorination, rectification, hydrogen reduction and atmospheric pressure high temperature conversion to obtain the electronic grade red phosphorus with the purity of 99.9999%. According to the above process, the traditional industrial yellow phosphorus pickling process is improved, on the one hand, a traditional relatively mild gas-introduction stirring is replacedby a mechanical deep stirring, and an interlayer outside the kettle is circulated with hot water to keep warm, so that the yellow phosphorus and nitric acid are fully contacted, impurities that cannot be removed by subsequent processes such as S, C, As and the like are removed, additives are not needed in the reaction process, the product purity is improved, the yellow phosphorus recovery rate isgreatly improved, and the yield of the electronic grade red phosphorus is increased; and on the other hand, a traditional quartz reaction kettle is replaced by an inner glass-lined cast iron kettle with an outer interlayer, so that production safety hidden dangers are reduced.

Description

technical field [0001] The invention relates to the preparation of elemental phosphorus, in particular to the preparation of electronic-grade red phosphorus (6N), and further relates to a production process for converting deep pickling yellow phosphorus into electronic-grade red phosphorus. Background technique [0002] Red phosphorus, molecular formula P 4 , molecular weight 123.8, white phosphorus allotrope, reddish-brown amorphous powder or block solid. Relative density 2.34g / cm 3 , melting point 590°C, fire point above 200°C, insoluble in water, carbon disulfide and organic solvents, slightly soluble in absolute ethanol. Electronic grade red phosphorus is one of the main materials for the synthesis of phosphorus compound semiconductors. It can be used to synthesize compound semiconductors such as indium phosphide (LnP) and gallium phosphide (GaP). It can also be used as a solid phosphorus source for IC doping. It is widely used in Integrated circuits, solar cells, cry...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/023C01B25/047
Inventor 袁欣尹朝蓉
Owner 贵州金鼎电子信息新材料有限公司
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