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Producing method of calcium fluoride with white carbon black

A production method and technology for silica, applied in the preparation/separation of silica, silica, ammonia, etc., can solve the problems of difficulty in scaling up the batch process, fine silica particles, fine silica particles, etc. The effect of small particle size, large specific surface area and fine particle size

Active Publication Date: 2013-05-01
KUNMING DAOERSEN TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The invention provides a method for producing calcium fluoride and co-producing white carbon black by using fluosilicic acid by-product of phosphate fertilizer as a raw material. For the first time, the continuous reaction of tubular reactor is used in the reaction process, which overcomes the defect that the existing batch process is difficult to scale up. , and overcome the existing continuous tank reactor stirring speed requirements are too high, the generated silicon dioxide particles are relatively fine, easy to block the reactor and other shortcomings; the calcium fluoride produced by the present invention is of good quality and high purity, which can be sold as a product , and can be used as raw material to produce hydrofluoric acid; the white carbon black produced by the present invention has fine particles, high content and large specific surface area

Method used

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  • Producing method of calcium fluoride with white carbon black

Examples

Experimental program
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Effect test

Embodiment 1

[0018] First pass nitrogen into the tubular reactor, and then pass ammonia into the reactor after 60 seconds. Turn on the fluosilicic acid metering pump, feed 8% fluosilicic acid solution, the feeding speed of fluosilicic acid solution is 0.4 m / s, the residence time of fluosilicic acid is 25 seconds, the feed molar ratio of ammonia gas to fluosilicic acid It is 6.6, after the reaction is completed, the slurry enters the aging tank, and the stirring speed of the aging tank is 50rpm. After aging for 10 minutes, the aging slurry is filtered to obtain white carbon black filter cake and ammonium fluoride solution; white carbon black After the filter cake is washed and dried, a white carbon black product is obtained, and the specific surface area of ​​the white carbon black product is 320m 2 / g, the silicon dioxide content is 98%; the ammonium fluoride solution is passed into the tank reactor, the stirring is started, the stirring speed of the reactor is controlled to be 150rpm, and...

Embodiment 2

[0020] First pass nitrogen into the tubular reactor, and after passing nitrogen for 60 seconds, pass ammonia gas into the reactor. Turn on the fluosilicic acid metering pump, feed 32% fluosilicic acid solution, the feed rate of fluosilicic acid is 0.1 m / s, the residence time of fluosilicic acid is 100 seconds, and the molar ratio of ammonia gas to fluosilicic acid feed is 7.2 , after the reaction was completed, the slurry entered the aging tank, and the aging tank rotating speed was 200rpm. After aging for 120 minutes, the aging slurry was filtered to obtain a white carbon black filter cake and ammonium fluoride solution; the white carbon black filter cake was passed through After washing and drying, a white carbon black product is obtained, and the specific surface area of ​​the white carbon black product is 190m 2 / g, the silica content is 95%; the ammonium fluoride solution is passed into the tank reactor, the stirring is started, the stirring speed of the control reactor i...

Embodiment 3

[0022] First pass nitrogen gas into the tubular reactor, after 60 seconds, pass ammonia gas into the reactor, control the gas velocity of ammonia gas to 10m / s, the residence time of ammonia gas is 1 second, and pass ammonia gas for 30s Finally, turn on the fluosilicic acid metering pump and feed 20% fluosilicic acid solution. The feeding speed of fluosilicic acid solution is 0.16m / s, the residence time of fluosilicic acid is 63 seconds, and the feeding mole of ammonia gas and fluosilicic acid Ratio is 7.2, and after the completion of the reaction, the slurry enters the aging tank, and the aging tank rotating speed is 150rpm. After aging for 60 minutes, the aging slurry is filtered to obtain white carbon black filter cake and ammonium fluoride solution; white carbon black After the filter cake is washed and dried, a white carbon black product is obtained, and the specific surface area of ​​the white carbon black product is 200m 2 / g, the silica content is 96%, the ammonium fluo...

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Abstract

The invention discloses a producing method of calcium fluoride with white carbon black. The producing method comprises the steps of allowing fluorosilicic acid (a wet-process phosphoric acid by-product) and ammonia to react continuously in a tubular reactor, ageing and filtering generated slurry to obtain an ammonium fluoride filtrate and a white carbon black filter cake, and washing and drying the white carbon black filter cake to obtain the white carbon black. Produced ammonium fluoride is good in quality and high in purity; the white carbon black is high in content, small in particle size, large in specific surface area and excellent in reinforcement performance, can be used for completely substituting the existing industrial water glass precipitation-process white carbon black; the ammonium fluoride filtrate and calcium hydroxide react to form a crude product of calcium fluoride and ammonia water; the crude product of calcium fluoride is washed and dried to form calcium fluoride; and the ammonia water is distilled into ammonia to serve as a raw material for ammoniation of fluorosilicic acid.

Description

technical field [0001] The invention relates to a production method for calcium fluoride co-production of white carbon black. Background technique [0002] Phosphate rock contains a large amount of fluorine and silicon resources. During the production of wet-process phosphoric acid, fluorine and silicon are combined to form fluorosilicate. Now wet-process phosphoric acid manufacturers simply process fluorosilicate into sodium fluorosilicate, sodium fluorosilicate There are few uses and limited capacity, and due to the large production capacity of wet-process phosphoric acid, it will inevitably lead to a serious excess production capacity of sodium fluorosilicate, and the price is low. Not only will it not bring economic benefits to wet-process phosphoric acid production enterprises, but it will also become a considerable economic burden for phosphoric acid enterprises. Some small enterprises even give up the production of sodium fluorosilicate and discharge fluorosilicic ac...

Claims

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Application Information

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IPC IPC(8): C01F11/28C01B33/12C01C1/02
Inventor 裴文俊
Owner KUNMING DAOERSEN TECH
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