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A kind of method for preparing potassium hydrogen fluoride by recycling waste electrolyte in fluorine gas production process

A waste electrolyte and production process technology, which is applied in the field of fluorine new materials and fluorine gas production, can solve the problems of affecting electrolyte recycling, increasing difficulty, separation cost, and insufficient separation, so as to achieve low manufacturing cost, reduce production cost, and prepare The effect of simple process

Active Publication Date: 2022-05-10
浙江博瑞中硝科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are two main problems in this process. First, the electrolyte is treated by directly adding water or potassium hydroxide solution to dissolve the metal fluoride or metal ion complex salt that was originally insoluble in the electrolyte into the aqueous solution, resulting in a lot of metal ion impurities Easily soluble in water, increasing the difficulty and cost of subsequent purification
Second, the electrolyte is treated by adjusting the pH process, and the dissolution balance is carried out in the direction of forming metal hydroxide as much as possible to realize the separation of metal ions, but the separation is not sufficient, and the content of iron ions in the obtained product cannot reach the fluorine used for electrolysis. Sodium hydride, which affects the recycling of electrolytes after recovery

Method used

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  • A kind of method for preparing potassium hydrogen fluoride by recycling waste electrolyte in fluorine gas production process
  • A kind of method for preparing potassium hydrogen fluoride by recycling waste electrolyte in fluorine gas production process
  • A kind of method for preparing potassium hydrogen fluoride by recycling waste electrolyte in fluorine gas production process

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Effect test

Embodiment 1

[0031] Take 1000 g of spent electrolyte, heat it to 90°C until it melts completely, and then filter it through a 60-mesh screen, transfer the filtrate into a tetrafluoro bottle, add 1 g of a composition of sodium fluoride and lithium fluoride (wherein sodium fluoride is 0.9 g , lithium fluoride 0.1 g), stirred at a constant temperature of 90°C for 5 hours, then kept at 90°C for 20 hours, filtered with a guanidine-containing PVDF composite filter membrane, maintained the filtrate temperature at 80°C, added 900g of high-purity water while stirring, and stirred until completely After miscibility, add 250g KOH, stir for 2 hours, and filter with guanidine-containing PVDF composite membrane. After filtration, the filtrate is maintained at 80°C, and then begins to cool down and crystallize. Control the cooling rate at 2°C / h, slowly cool down to 5°C, and cool down During the process, the stirring speed was maintained at 40 rpm. After the suspension was centrifuged and dehydrated, the c...

Embodiment 2

[0036] Take 1000 g of spent electrolyte, heat it to 90°C until it melts completely, and then filter it through a 100-mesh screen, transfer the filtrate into a tetrafluoro bottle, add 10 g of a composition of sodium fluoride and lithium fluoride (8.5 g of sodium fluoride, Lithium fluoride 1.5 g), stirred at a constant temperature of 90°C for 5 hours, then kept at 90°C for 24 hours, filtered with a 10-micron PVDF PVDF compound filter membrane containing guanidine, and maintained the filtrate temperature at 85°C, while stirring, add 1000g of high-purity water, stir After complete miscibility, add 285g KOH, stir for 1 hour, and filter with 10 micron PVDF PVDF composite filter membrane containing guanidine. After filtration, the filtrate is maintained at 85°C, and then begins to cool down and crystallize. Control the cooling rate to 2.5°C / h, and slowly cool down To 5°C, maintain the stirring speed at 50 rpm during the cooling process, transfer the crude product to the PTFE tray afte...

Embodiment 3

[0041] Take 1000 g of spent electrolyte, heat it to 95°C until it melts completely, then filter it through a 120-mesh screen, transfer the filtrate into a tetrafluoro bottle, add 20 g of a composition of sodium fluoride and lithium fluoride (18 g of sodium fluoride, Lithium fluoride 2 g), stirred at a constant temperature of 90°C for 5 hours, then kept at 90°C for 24 hours, filtered with a 10-micron PVDF PVDF composite filter membrane containing guanidine, and maintained the filtrate temperature at 80°C, while stirring, add 1050g of high-purity water, stir After complete miscibility, add 290 g KOH, stir for 1 hour, and then filter with a 10-micron PVDF PVDF composite filter membrane containing guanidine. After the filtrate is maintained at 80°C, it begins to cool down and crystallize. Control the cooling rate at 3°C / h, slowly Cool down to 5°C, keep the stirring speed at 60 rpm during the cooling process, and then transfer the suspension to a PTFE tray after centrifugal dehydrat...

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Abstract

Potassium hydrogen fluoride (KHF 2 )Methods. The invention relates to a method for preparing a high-purity potassium bifluoride product through the steps of impurity removal, refining, reaction, crystallization, separation, drying and the like. The index of the prepared potassium bifluoride is better than that of the existing commercial products, and it can be recycled in the production of fluorine gas, which improves the utilization rate of fluorine resources, solves the environmental protection problem of the difficulty and high cost of waste solid treatment in the industrial production of fluorine gas, and improves the fluorine gas production efficiency. The competitiveness of gas production equipment; the production process is simple, clean and environmentally friendly, and has good economic and social benefits.

Description

technical field [0001] The invention relates to the technical field of fluorine gas production, in particular to a method for preparing potassium bifluoride from waste electrolyte produced in the fluorine gas production process, and belongs to the field of energy saving and environmental protection and new fluorine materials. Background technique [0002] Fluorine gas is used to produce UF 6 An indispensable raw material, liquid fluorine is an ideal oxidant for rocket liquid fuel, and occupies a very important position in the national defense industry. In recent years, it has been widely used in civilian industries, such as SF 6 , WF 6 Fluorinating agents such as gases, or as fluorinating agents for plastic surface modification, etc. The current industrial preparation of fluorine gas preferably adopts the medium temperature electrolysis method, and the electrolyte used is potassium hydrogen fluoride, potassium hydrogen fluoride (KHF 2 ) and AHF in a certain ratio to obtai...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01D3/02C01D3/14D01D5/00B01D69/12B01D67/00B01D71/34C25B15/08C25B1/245C08G77/388D01F8/08D01F8/10D01F8/16
CPCC01D3/02C01D3/14D01D5/0084D01D5/0038D01D5/003B01D69/125B01D71/34C25B15/08C25B1/245C08G77/388D01F8/08D01F8/10D01F8/16C01P2006/80C01P2006/82
Inventor 明博付铁柱朱玉洁孙立柱陈刚张学良李军
Owner 浙江博瑞中硝科技有限公司
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