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A kind of preparation method of anti-caking 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 burning residue, less three wastes and high product purity

Active Publication Date: 2016-02-24
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) with a mass concentration of 20%, and cool it to 30° C. with ice water, and slowly feed 77 grams of ammonia gas into the reactor ( 4.5 moles), use Congo red test paper to track and detect until the test paper just turns brown as the reaction end point, then heat up to 50 ° C and react for 5 hours, then add 0.04 g of sludge dewatering agent, continue to stir and react for 1 hour, after the reaction is completed, cooling and crystallization, Centrifuge, take the precipitate and dry at 50° C. to obtain 256 g of anti-caking ammonium bifluoride, the yield is 99%, the purity is ≥97.0%, and the residue on ignition is ≤0.1%. Room temperature (25 ℃) placed for 15 months without caking.

Embodiment 2

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

Embodiment 3

[0019] In the plastic reactor, add 500 grams of hydrofluoric acid with a mass concentration of 40% (200 grams of hydrofluoric acid, 10 moles), and cool it to 35°C with ice water, and slowly feed 82 grams of ammonia gas into the reactor ( 4.8 moles), use Congo red test paper to track and detect until the test paper just turns brown as the reaction end point, then heat up to 55 ° C and react for 3 hours, then add 0.08 g of sludge dewatering agent, continue to stir and react for 1 hour, after the reaction is completed, cooling and crystallization, Centrifuge, take the precipitate and dry it at 50° C. to obtain 257 g of anti-caking ammonium bifluoride with a yield of 99.8%, a purity of ≥97.0%, and an ignition residue of ≤0.1%. Room temperature (25 ℃) placed 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 is 57.04, white or colorless transparent orthorhombic crystal, relative density 1.52 (25 ℃), melting point 125.6 ℃, boiling point 239.5 ℃. It is easy to deliquesce and agglomerate in the air, and is easily soluble in water. The aqueous solution is strongly acidic and has a sour taste of hydrogen fluoride; it is slightly soluble in alcohol. Decomposes in hot water and sublimates at high temperature. Ammonium bifluoride is mainly used as glass etchant, preservative, solvent for beryllium oxide to metal beryllium, chemical reagent, cleaning agent for boiler feed water system and steam generation system, fermentation industry disinfectant and surface treatment agent for sili...

Claims

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Application Information

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Patent Type & Authority Patents(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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