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Method for producing high-purity ammonium fluoride by utilizing sodium hydride waste residues

A technology of sodium hydrogen fluoride and ammonium fluoride, applied in the directions of ammonium fluoride, ammonium halide, alkali metal fluoride, etc., to achieve the effects of controllable reaction conditions, low production cost, comprehensive utilization and green production

Active Publication Date: 2017-05-17
ZHEJIANG DAYANG BIOTECH GROUP
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] In order to solve the above-mentioned problems, reduce production costs, increase economic benefits, improve environmental protection and safety, Wang Guoping and other new technology development, the above-mentioned hydrofluoric acid residue (containing hydrogen fluoride, ammonium fluoride, sodium fluoride and other organic impurities) Through evaporation and concentration, high-concentration anhydrous hydrofluoric acid is recovered, but the generated sodium bifluoride waste remains to be further processed

Method used

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  • Method for producing high-purity ammonium fluoride by utilizing sodium hydride waste residues

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Experimental program
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Effect test

Embodiment 1-1

[0039] Embodiment 1-1, a kind of method utilizing sodium bifluoride waste residue to produce high-purity ammonium fluoride, carries out following steps successively:

[0040] 1), put 200 kg of sodium bifluoride solid waste residue into the reactor, add 1000 liters of ammonium fluoride saturated solution, start stirring, and obtain sodium bifluoride slurry I;

[0041] 2), under stirring, slowly pass ammonia gas (obtained from gasification of liquid ammonia) into the sodium bifluoride slurry I obtained in step 1) until the pH is 8.0, then stop passing ammonia gas;

[0042] Control the speed during the process of passing ammonia gas, so as to control the temperature of the material between 70 and 80 °C;

[0043] 3), suction filter the material obtained in the reaction of step 2) while it is hot (78° C.) to obtain 1050 liters of ammonium fluoride solution I and 135 kg of crude sodium fluoride I;

[0044] 4), step 3) obtained 135 kg of crude sodium fluoride Ⅰ with 65 liters of boi...

Embodiment 1-2

[0051] Embodiment 1-2, a kind of method utilizing sodium bifluoride waste residue to produce high-purity ammonium fluoride, carries out following steps successively:

[0052] 1), put 200 kg of sodium bifluoride solid waste residue into the reactor, add 1000 liters of the ammonium fluoride mother liquor described in step 9) of Example 1-1, start stirring, and obtain sodium bifluoride slurry I;

[0053] 2), under stirring, slowly pass ammonia gas (obtained from gasification of liquid ammonia) into the sodium bifluoride slurry I obtained in step 1) until the pH is 8.0, then stop passing ammonia gas;

[0054] Control the speed during the process of passing ammonia gas, so as to control the temperature of the material between 70 and 80 °C;

[0055] 3), suction filter the material obtained in the reaction of step 2) while it is hot (79° C.), to obtain 1050 liters of ammonium fluoride solution I and 134 kg of crude sodium fluoride I;

[0056] 4), 134 kg of crude product sodium fluor...

Embodiment 2

[0063] Embodiment 2, a kind of method utilizing sodium bifluoride waste residue to produce high-purity ammonium fluoride, carries out following steps successively:

[0064] 1), put 200 kg of sodium bifluoride solid waste residue into the reactor, add 800 liters of the ammonium fluoride mother liquor described in step 9) of Example 1-1, start stirring, and obtain sodium bifluoride slurry I;

[0065] 2), under stirring, slowly pass ammonia gas (obtained from gasification of liquid ammonia) into the sodium bifluoride slurry I obtained in step 1) until the pH is 8.5, then stop passing ammonia gas;

[0066] Control the speed during the process of passing ammonia gas, so as to control the temperature of the material between 70 and 80 °C;

[0067] 3), the material obtained in the reaction of step 2) was filtered while hot (80° C.) to obtain 860 liters of ammonium fluoride solution I and 143 kg of crude sodium fluoride I;

[0068] 4), step 3) gained 143 kilograms of crude product sod...

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Abstract

The invention discloses a method for producing high-purity ammonium fluoride by utilizing sodium hydride waste residues. The method is characterized in that sodium hydride waste residues for producing 2-chlorine-6-fluorotoluene or a similar product and ammonia are taken as raw materials for reaction; the high-purity ammonium fluoride is prepared through the steps of neutral reaction, suction filtration for impurity removal, cooling crystallization, solvent leaching, air flow drying and the like, and meanwhile, by-product sodium fluoride is prepared. The method has the characteristics of being high in reaction speed, controllable in reaction conditions, low in production energy consumption, good in ammonium fluoride quality (the purity is more than or equal to 98.0 percent, and silicate is less than 0.01 percent) and high in raw material conversion rate; no ammonium fluoride evaporative crystallization device is required, so that production equipment is simple.

Description

technical field [0001] The invention belongs to the fields of fine chemical industry and environmental protection, and relates to fine inorganic chemical synthesis technology, in particular to a method for producing high-purity ammonium fluoride by using sodium bifluoride waste residue. Background technique [0002] Ammonium fluoride is a widely used fluorine chemical product in the fluorine chemical industry. It is mainly used as a catalyst for glass etching, wood and wine antiseptic disinfection, fiber mordant dyeing, rare metal extraction and organic synthesis. High-purity ammonium fluoride can also Used in electronics industry. There are two traditional production methods of ammonium fluoride: liquid phase method and gas phase method using hydrofluoric acid as raw material. The liquid phase method is obtained by vaporizing liquid ammonia and passing it into 40% hydrofluoric acid to make it react. The gas phase method is obtained by direct reaction of pure ammonia and h...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01C1/16C01D3/02
CPCC01C1/162C01D3/02C01P2006/80
Inventor 王国平李刚徐旭辉汪贤高胡滨周转忠仇旭辉赵东升王丽佳胡萍韩国英马建明
Owner ZHEJIANG DAYANG BIOTECH GROUP
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