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Method for preparing anti-blocking ammonium bifluoride

A technology of ammonium bifluoride and anti-caking, which is applied in the direction of ammonium halide, etc., to achieve the effect of less waste, low cost and less consumption

Active Publication Date: 2014-11-12
DONGZHI TIANFU CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In recent years, we have been committed to the research and development of green chemical technology. Therefore, in the present invention, the sludge dewatering agent system is applied to the research of ammonium bifluoride anti-caking. This technology is a new technology that has not been reported.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] In the plastic reactor, add 1000 grams of hydrofluoric acid (200 grams of hydrofluoric acid, 10 moles) of mass concentration 20%, and cool to 30 ℃ with ice water, begin to pass into 77 grams of ammonia gas slowly in the reactor ( 4.5 moles), use Congo red test paper to track and detect until the test paper is just brown as the reaction end point, then heat up to 50 ° C for 5 hours, then add 0.04 grams of sludge dehydrating agent, continue stirring for 1 hour, after the reaction is over, cool and crystallize, Centrifuge and dry the precipitate at 50°C to obtain 256 grams of anti-caking ammonium bifluoride with a yield of 99%, a purity of ≥97.0%, and a residue on ignition of ≤0.1%. It can be stored at room temperature (25°C) for 15 months without caking.

Embodiment 2

[0017] In the plastic reactor, add 670 grams of hydrofluoric acid (200 grams of hydrofluoric acid, 10 moles) of mass concentration 30%, and cool to 35 ℃ with ice water, begin to pass into 78 grams of ammonia gas slowly in the reactor ( 4.6 moles), use Congo red test paper to track and detect until the test paper is just brown as the reaction end point, then heat up to 55 ° C for 3 hours, then add 0.06 grams of sludge dehydrating agent, continue to stir and react for 1 hour, after the end of the reaction, cooling and crystallization, Centrifuge and dry the precipitate at 50°C to obtain 257 g of anti-caking ammonium bifluoride with a yield of 99.8%, a purity of ≥97.0%, and a residue on ignition of ≤0.1%. It can be stored at room temperature (25°C) for 15 months without caking.

Embodiment 3

[0019] In the plastic reactor, add 500 grams of hydrofluoric acid (200 grams of hydrofluoric acid, 10 moles) of mass concentration 40%, and cool to 35 ℃ with ice water, begin to pass into 82 grams of ammonia gas slowly in the reactor ( 4.8 moles), use Congo red test paper to track and detect until the test paper is just brown as the reaction end point, then heat up to 55 ° C for 3 hours, then add 0.08 grams of sludge dehydrating agent, continue to stir and react for 1 hour, after the end of the reaction, cooling and crystallization, Centrifuge and dry the precipitate at 50°C to obtain 257 g of anti-caking ammonium bifluoride with a yield of 99.8%, a purity of ≥97.0%, and a residue on ignition of ≤0.1%. It can be stored at room temperature (25°C) for 15 months without caking.

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Abstract

The invention discloses a method for preparing anti-blocking ammonium bifluoride. The method comprises the steps that the hydrofluoric acid with the mass concentration ranging from 20 percent to 40 percent is added in a reactor and cooled into the temperature ranging from 30 DEG C to 40 DEG C, ammonia gas is introduced into the solution slowly, after reaction is completely finished, the temperature is increased to the range from 50 DEG C to 55 DEG C, reaction is carried out for 2-5 hours, the sludge dehydrant is added, the reaction is carried out with stirring under heat preservation for one hour, after reaction is finished, the solution is cooled and crystallized, centrifuging is carried out, and sediment is obtained and dried to obtain the anti-blocking ammonium bifluoride. The sludge dehydrant serves as the anti-blocking reagent, the method is easy to operate, postprocessing is convenient, three wastes are reduced in the production process, the product purity is high, the ignition residues are few, the product standing time is long, the usage amount of the dehydrant is small, and the method is an economical, practical and environmentally-friendly technology.

Description

(1) Technical field [0001] The invention relates to a method for preparing ammonium bifluoride, in particular to a method for preparing anti-caking ammonium bifluoride in a sludge dewatering agent system. (2) Background technology [0002] Ammonium bifluoride molecular formula NH 4 HF 2 , molecular weight 57.04, white or colorless transparent orthorhombic crystal, relative density 1.52 (25°C), melting point 125.6°C, boiling point 239.5°C. It is easy to deliquesce and agglomerate in the air, and is easily soluble in water. The aqueous solution is strongly acidic and has the sour taste of hydrogen fluoride; it is slightly soluble in alcohol. It decomposes in hot water and sublimes in high temperature. Ammonium bifluoride is mainly used as glass etchant, preservative, solvent for metal beryllium made of beryllium oxide, chemical reagent, cleaning agent for boiler feed water system and steam generation system, disinfectant for fermentation industry and surface treatment agent...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01C1/16
Inventor 裴文孙莉王海滨杨振平
Owner DONGZHI TIANFU CHEM
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