Synthetic method of calcium fluoride

A synthetic method and calcium fluoride technology, applied in the direction of calcium/strontium/barium fluoride, calcium/strontium/barium halide, etc., can solve the problems of fluorite price rise, normal production, and close physical properties, etc., to achieve good Social and economic benefits, solving effects that are difficult to use efficiently

Active Publication Date: 2012-06-20
KUNMING DAOERSEN TECH
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AI Technical Summary

Problems solved by technology

In recent years, China's fluorine chemical industry has developed rapidly, and the demand for fluorspar continues to increase. At the same time, the country is controlling the mining of fluorspar, and there is a contradiction between limited mining and increasing demand. On the one hand, the price of fluorspar has risen too fast. On the one hand, many fluorine chemical companies lack basic raw materials and cannot produce normally
[0003] The total amount of fluorine resources contained in phosphate rock is much higher than that of fluorite. In the process of phosphate fertilizer production, fluorine in phosphate rock exists in the form of fluosilicic acid. Now most phosphate fertilizer enterprises use fluosilicic acid to produce sodium fluosilicate, fluorine Sodium silicate has few uses, limited market capacity, and is difficult to process into high value-added fluorine chemical products. Therefore, the price of sodium fluosilicate is low and the development space is limited; if calcium fluoride is produced by the reaction of fluosilicate and calcium hydroxide, There will be incomplete reaction. There is a large amount of calcium fluorosilicate in calcium fluoride products. Calcium fluoride, calcium fluorosilicate, and silicon dioxide are all insoluble and have similar physical properties. It is difficult to find an effective method to separate the above three components. kind of substance

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Experimental program
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Embodiment 1

[0026] After injecting 3000g of fluosilicic acid with a concentration of 5% into the pressurized stirring reactor, feed 2550g of ammonia water with a concentration of 5%, and start stirring while adding ammonia water. The stirring speed is 500rpm, and the reaction pressure is controlled to 0.3MPa. The temperature was 140°C, and after 180 minutes of reaction, the reaction materials were filtered and washed to obtain 5472g of ammonium fluoride solution with a concentration of 4.07%. The filter cake was 150g of wet silica with a water content of 60% and 80g of washing water. Add the ammonium fluoride solution into the ultrasonic reactor, turn on the ultrasonic wave with a frequency of 40KHz, start stirring at a stirring speed of 100rpm, add 220g of calcium hydroxide into the ultrasonic reactor at a uniform speed, the feeding time is 60min, and the reaction temperature is 80°C. The reaction time is 120min. After the reaction is completed, the material is poured into the aging tank,...

Embodiment 2

[0028] After injecting 750g of fluorosilicic acid with a concentration of 20% into the pressurized stirring reactor, feed 638g of ammonia water with a concentration of 20%, and start stirring while adding ammonia water. The stirring speed is 500rpm, and the reaction pressure is controlled at 0.2MPa. The temperature was 80°C, and after reacting for 90 minutes, the reaction materials were filtered and washed to obtain 1320 g of ammonium fluoride solution with a concentration of 16.65%. The filter cake was 148 g of wet silica with a water content of 60%, and the amount of washing water was 80 g. Add the ammonium fluoride solution into the reactor, start stirring, and the stirring speed is 100rpm, add 730g of calcium hydroxide emulsion with a concentration of 30% into the reactor at a uniform speed, the feeding time is 40min, the reaction temperature is 60°C, and the reaction time is 60min, after the reaction is completed, the material is lowered from 50°C to 20°C, the cooling rate...

Embodiment 3

[0030] After injecting 375g of fluorosilicic acid with a concentration of 40% into the pressurized stirring reactor, feed 425g of ammonia water with a concentration of 30%, and start stirring while adding ammonia water. The stirring speed is 100rpm, and the reaction is carried out under normal pressure and normal temperature. After reacting for 30 minutes, the reaction materials were filtered and washed to obtain 1095 g of ammonium fluoride solution with a concentration of 20.07%, and the filter cake was 138 g of wet silica with a water content of 58%, and the amount of washing water was 80 g. Add the ammonium fluoride solution into the ultrasonic reactor, turn on the ultrasonic wave, the frequency is 20KHz, start stirring, the stirring speed is 200rpm, and add 1075g of calcium hydroxide emulsion with a concentration of 20% into the ultrasonic reactor at a uniform speed, and the feeding time is 20min. The temperature is 20°C, and the reaction time is 30 minutes. After the react...

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Abstract

The invention relates to a synthetic method of calcium fluoride, hydrofluosilicic acid produced during a phosphate fertilizer production process is adopted as raw materials so as to synthesize calcium fluoride through two steps of reaction, the first step of reaction is that ammonium fluoride and silicon dioxide are produced through the reaction of fluosilicic acid and ammonia gas or ammonia water, the solubility of ammonium fluoride is high, and the separation of ammonium fluoride from silicon dioxide is achieved through the method of filtering and washing; the second step of reaction is that calcium fluoride and ammonia water are produced through the reaction of ammonium fluoride solution and calcium hydroxide, the separation of calcium fluoride from ammonia water is achieved through the filtering way, ammonia gas is obtained by rectifying the ammonia water, and calcium fluoride is produced by taking ammonium fluoride as an intermediate product. Therefore, the invention overcomes defects of insufficient reaction during the process of synthesizing calcium fluoride through the reaction of hydrofluosilicic acid and calcium hydroxide, and mass of calcium fluosilicate contained in calcium fluoride products, further solves the problem of difficulty separation of calcium fluoride from silicon dioxide mixture, and achieves efficient utilization of by-product hydrofluosilicic acid ofphosphate fertilizer.

Description

technical field [0001] The invention relates to the field of inorganic chemical industry, in particular to a method for synthesizing calcium fluoride. Background technique [0002] Fluorspar, also known as fluorspar, its active ingredient is calcium fluoride, the chemical formula is CaF 2 , it is widely used in the chemical industry and metallurgical industry, and has an important impact on national security, national economy and social development. China has used fluorite as a strategic resource reserve to ensure the sustainable development of fluorine resources. At the same time, fluorite is used as a raw material for the production of hydrofluoric acid, and more than half of the world's fluorite is used for the production of hydrofluoric acid, which is the basic raw material for the entire fluorine chemical industry. In recent years, China's fluorine chemical industry has developed rapidly, and the demand for fluorspar continues to increase. At the same time, the countr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F11/22
Inventor 裴文俊肖怡琳颜思洪
Owner KUNMING DAOERSEN TECH
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