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Method for preparing high-purity ammonium fluosilicate

A technology of ammonium fluorosilicate and fluorosilicic acid, applied in the direction of halogenated silicon compounds, etc., can solve the problems of difficult filtration, difficult continuous process, large process energy consumption, etc., and achieves safe and reliable operation, easy continuous production, and process energy consumption. low effect

Inactive Publication Date: 2012-10-03
GUIZHOU KAILIN GRP CO LTD
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Problems solved by technology

This process has the following disadvantages: (1) Since the absorption liquid is ammonium fluorosilicate crystallization liquid, when the absorption liquid reaches a certain concentration, it needs to be discharged from the system for the next cooling and crystallization process, and the continuous process is difficult; (2) During the absorption process of fluorine-containing gas, a large amount of silica will inevitably be produced. Due to its difficulty in filtration, it will be doped in a large amount in the ammonium fluorosilicate product, seriously affecting the quality of the ammonium fluorosilicate product; (3) process energy consumption Large, because the temperature of the ammonium fluorosilicate absorption liquid can reach above 80°C when the reaction is saturated, cooling it to below 30°C for crystallization will consume a lot of energy, thereby increasing production costs

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  • Method for preparing high-purity ammonium fluosilicate

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Embodiment

[0018] The 1000t / a anhydrous hydrofluoric acid industrialization demonstration plant of Guizhou Kailin Group Co., Ltd. adopts this method to produce the intermediate ammonium fluorosilicate.

[0019] The raw material ammonium fluorosilicate concentration is 12%, and the ammonia content in the liquid ammonia is greater than 99.9%. It is sent to the reaction tank for neutralization reaction. The reaction temperature is 30°C-100°C, and the reaction time is 2-30min. When the pH of the reaction system reaches 3 to 5 o'clock, the reaction reaches the end point; pump the reaction liquid into the low-temperature flash evaporation concentration system, flash at a vacuum of 80kPa and a temperature of 70°C, remove water, and concentrate to a saturated state to precipitate crystals; after flash evaporation The solution enters the settling tank, and the material containing ammonium fluorosilicate crystals is released from the bottom of the settling tank. After filtering, a high-purity ammon...

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Abstract

The invention discloses a method for preparing high-purity ammonium fluosilicate. The method comprises the following steps of: (1) feeding fluorosilicic acid of which the concentration is not less than 10 percent and liquid ammonia into a reaction tank for neutral reaction, when a pH value of a reaction system reaches 3 to 5, reaction is finished; (2) pumping a reaction liquid into a low-temperature flash evaporation concentration system to perform low-temperature flash evaporation in a vacuum state, removing a large amount of water in a neutral liquid of the ammonium fluosilicate, concentrating to a saturated state, and then precipitating crystal, wherein steam generated during flash evaporation is subjected to despumation and is discharged to atmosphere air; (3) introducing a solution after flash evaporation into a setting tank, and discharging a material containing ammonium fluosilicate crystal from the setting tank; and (4) filtering the discharged material, and thus obtaining a high-purity ammonium fluosilicate product with purity over 90 percent, wherein a filtering liquid is returned to the reaction tank of neutral reaction for recovery. According to the method, the ammonium fluosilicate crystal product with purity over 90 percent can be produced, energy consumption of a process is low, operation is safe and reliable, continuous production is easy to realize, and the method is applicable for comprehensive utilization of a fluorine resource of a large-scale phosphate fertilizer enterprise.

Description

technical field [0001] The invention relates to fluorine-containing compounds, in particular to fluosilicic acid, and in particular to a preparation method of ammonium fluosilicate. Background technique [0002] As we all know, a large amount of fluorine-containing gas will be produced in the process of production and processing in the phosphorus chemical industry, which exists in the form of silicon tetrafluoride and hydrogen fluoride. If these substances are not recycled, they will cause serious environmental pollution and cause waste of fluorine resources. . Studies have shown that although the fluorine content in phosphate rock is low, the total amount is huge, and it is an important fluorine resource. At present, most of the fluorine-containing gas produced when phosphate rock is used as raw material to produce wet-process phosphoric acid fertilizers is absorbed by water to obtain fluosilicic acid. The recycling of this part of fluorosilicic acid is not only beneficia...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/10
Inventor 何润林刘刚石寅袁佳程
Owner GUIZHOU KAILIN GRP CO LTD
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