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Preparation method of ammonium hydrogen difluoride

A technology of ammonium bifluoride and ammonium bifluoride crystal, applied in the direction of ammonium fluoride, ammonium halide, etc., to achieve the effect of less demanding conditions, easy realization and significant economic benefits

Inactive Publication Date: 2018-06-26
QINGDAO XIANGZHI ELECTRONICS TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

in production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Set the rotating speed of the agitator to be 120r / min, add 500g of ammonium fluoride solution with a mass percentage concentration of 10% to the polytetrafluoroethylene three-necked bottle, and pass into the ammonium fluoride solution 216.22g of hydrofluoric acid with a mass percentage concentration of 15% Solution (the addition of hydrofluoric acid is 120% of theoretical amount), the adding speed of hydrofluoric acid is 30ml / min; hydrofluoric acid; react 60min, then add the ammoniacal solution 43.36g of mass percent concentration 12% (the add-on of ammoniacal liquor is 110% of theoretical amount) in reaction system, the adding speed of ammoniacal liquor is 30ml / min, and reaction temperature controls 30 ℃, react for 40 minutes; concentrate the ammonium bifluoride solution at 60 ℃, use 7% dilute sulfuric acid solution to absorb the ammonia gas released from the reaction, after crystallization, conduct cooling crystallization, solid-liquid separation to obtain ammonium bif...

Embodiment 2

[0015] Set the rotating speed of the agitator to be 240r / min, add 500g of ammonium fluoride solution with a mass percentage concentration of 20% to the polytetrafluoroethylene three-necked bottle, and pass 337.84g of 20% mass percentage concentration of hydrofluoric acid into the ammonium fluoride solution solution (the addition of hydrofluoric acid is 125% of theoretical amount), the addition speed of hydrofluoric acid is 60ml / min; Reaction 69min; Add 94.59g of aqueous ammonia solution (the addition of ammoniacal liquor is 120% of theoretical amount) of mass percent concentration 15% in reaction system in the back, the adding speed of ammoniacal liquor is 50ml / min, and reaction temperature controls 28 ℃, react for 50 minutes; concentrate the ammonium bifluoride solution at 65 ℃, use 11% dilute sulfuric acid solution to absorb the ammonia gas released from the reaction, after crystallization, carry out cooling crystallization, separate solid-liquid to obtain ammonium bifluoride...

Embodiment 3

[0017] Set the rotating speed of the agitator to be 280r / min, add 500g of ammonium fluoride solution with a mass percentage concentration of 30% to the polytetrafluoroethylene three-necked bottle, and pass 351.35g of 30% mass percentage concentration of hydrofluoric acid into the ammonium fluoride solution solution (the addition of hydrofluoric acid is 130% of theoretical amount), the addition speed of hydrofluoric acid is 90ml / min; Reaction 73min; Add 153.721g of ammonia solution 153.721g (the addition of ammoniacal liquor is 130% of theoretical amount) of mass percentage concentration 18% in reaction system, the adding speed of ammoniacal liquor is 60ml / min, and reaction temperature controls 26 ℃, react for 70 minutes; concentrate the ammonium bifluoride solution at 70 ℃, use 15% dilute sulfuric acid solution to absorb the ammonia gas released from the reaction, after crystallization, conduct cooling crystallization, separate solid-liquid to obtain ammonium bifluoride crystal...

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PUM

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Abstract

The invention discloses a preparation method of ammonium hydrogen difluoride. The preparation method comprises the following steps: adding an unsaturated ammonium fluoride solution with a mass concentration of 10-50% into hydrofluoric acid with a mass concentration of 15-50%, and controlling the reaction temperature to be 40-80 DEG C; after a reaction is finished, adding an ammonia water solutionwith a mass concentration of 12-25% into the reaction system to carry out a reaction with excess hydrofluoric acid, controlling the reaction temperature to be 30 DEG C or below, carrying out a reaction for 40-90 minutes, concentrating the obtained ammonium hydrogen difluoride in a three-neck flask, and then carrying out cooling for crystallizing to obtain ammonium hydrogen bifluoride crystals; anddrying the ammonium hydrogen bifluoride crystals to obtain an ammonium hydrogen bifluoride product. The beneficial effect is that compared with the prior art, the preparation method has simple process route, no harsh condition requirements and easy realization. The prepared ammonium hydrogen bifluoride product ha low water content and high purity, and the product does not cake. In the productionprocess of the ammonium hydrogen bifluoride, the energy consumption problem is concerned, and the excessive energy consumption is avoided. According to the preparation method provided by the invention, fluorine resources are efficiently utilized, and the fluorine resources entering the system are finally converted into ammonium hydrogen bifluoride products. The preparation method has remarkable economic benefits and is suitable for promotion in the fluorine chemical enterprises.

Description

technical field [0001] The invention belongs to the preparation of fluoride salts in the field of chemical industry, and in particular relates to a preparation method of ammonium bifluoride. Background technique [0002] For decades, the global fluorine chemical industry has developed steadily. Fluorine chemical products are widely used in military industry, chemical industry, machinery and other fields due to their excellent properties such as chemical resistance, high and low temperature resistance, aging resistance, low friction, and high insulation. The fastest growing, most high-tech and most promising products in the chemical industry. [0003] Ammonium bifluoride is a kind of fluorine chemical product widely used in the fluorine chemical industry. It is widely used in chemical industry, metallurgy, food and other industries. High-purity ammonium bifluoride can also be applied to semiconductor industry and pharmaceutical industry. Ammonium bifluoride is a colorless or...

Claims

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Application Information

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IPC IPC(8): C01C1/16
CPCC01C1/162
Inventor 不公告发明人
Owner QINGDAO XIANGZHI ELECTRONICS TECH CO LTD