Method for continuously preparing white carbon black and ammonium fluoride by carrying out fluosilicic acid ammoniation

A technology of white carbon black and fluorosilicic acid, which is applied in the field of preparing white carbon black and ammonium fluoride, can solve the problems of limited utilization of fluorine and silicon resources, small scale of a single set of equipment, and low utilization rate of equipment, and achieve shortening Effects of residence time, inhibition of agglomeration and hard agglomeration, and long operating cycle

Active Publication Date: 2014-05-14
YUNNAN YUNTIANHUA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The process of producing white carbon black and ammonium fluoride by ammonification of fluorosilicate is a batch process in China. The batch process has disadvantages such as low equipment utilization rate, automation degree, and small scale of a single set of equipment.
This technology has not been built in large-scale industrialized devices in China
At the same time, the utilization of fluorine and silicon resources in domestic wet-process phosphoric acid enterprises is limited

Method used

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  • Method for continuously preparing white carbon black and ammonium fluoride by carrying out fluosilicic acid ammoniation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] When the temperature is 0°C and the compressed air is 0.2MPa, start stirring, and at the speed of 3000rpm, add 2% fluosilicic acid and 2% ammonia water at the same time, and the feed rates of fluosilicic acid and ammonia water are 80L / hr and 62L / hr respectively , the residence time is 30s, continuous reaction and filtration to obtain white carbon black filter cake and ammonium fluoride solution, the filter cake is washed and dried to obtain white carbon black. The main economic index of white carbon black within 24 hours is that the specific surface area is 320m2 / g; the DBP absorption value is 3.40, and the concentration of ammonium fluoride solution is 1.7%.

Embodiment 2

[0024] When the temperature is 15°C and the compressed air is 0.3MPa, start stirring, and at the speed of 8000rpm, add 15% fluosilicic acid and 15% ammonia water at the same time, and the feed rates of fluosilicic acid and ammonia water are 20L / hr and 16L / hr respectively , the residence time is 2min, continuous reaction and filtration to obtain white carbon black filter cake and ammonium fluoride solution, the filter cake is washed and dried to obtain white carbon black. The main economic index of white carbon black within 24 hours is that the specific surface area is 190m2 / g; the DBP absorption value is 2.80, and the concentration of ammonium fluoride solution is 13.7%.

Embodiment 3

[0026] When the temperature is 30°C and the compressed air is 0.4MPa, start stirring, and at the speed of 1000rpm, add 25% fluosilicic acid and 25% ammonia water at the same time, and the feeding amount of fluosilicic acid and ammonia water are 13.3L / hr and 10.3L respectively / hr, the residence time is 3min, continuously react and filter to obtain white carbon black filter cake and ammonium fluoride solution, and the filter cake is washed and dried to obtain white carbon black. The main economic index of white carbon black within 24 hours is that the specific surface area is 160m2 / g; the DBP absorption value is 2.20, and the concentration of ammonium fluoride solution is 23.9%.

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Abstract

The invention discloses a method for continuously preparing white carbon black and ammonium fluoride by carrying out fluosilicic acid ammoniation, which relates to a chemical production method, in particular to a method for preparing the white carbon black and the ammonium fluoride. The method comprises the following steps: (a) at a temperature between minus 5 and 30 DEG C, starting a stirrer and an air compressor, blowing compressed air into an outlet pipe of a reactor by the air compressor and adding fluosilicic acid and ammonia into the reactor simultaneously; (b) when the fluosilicic acid and the ammonia are added to the position of an overflow pipe in the reactor, opening an emptying valve to continuously feed and discharge materials and controlling a PH value of the reaction, wherein the period of the continuous reaction is 24 hours; (c) in the reaction process, filtering the materials discharged by the step (b) to obtain a white carbon black filter cake and filtrate of ammonium fluoride, and washing and drying the white carbon black filter cake to obtain a white carbon black finished product, wherein the filtrate is ammonium fluoride solution; and (d) after performing a reaction for 24 hours in the reactor, emptying the materials, cleaning the reactor to be used next time and producing the white carbon black finished product by using the materials according to the step (c), wherein the ammoniation yield of the process can reach 99.99 percent. The method of the invention effectively overcomes the defects of the existing intermittent technology and has the advantages of continuous, stable and simple process and long operation period.

Description

technical field [0001] The invention relates to a chemical production method, in particular to a method for preparing white carbon black and ammonium fluoride. Background technique [0002] Fluosilicic acid is a low-value by-product in the production process of wet phosphate fertilizer. It has few uses and will have a serious impact on environmental protection. The development and utilization of fluosilicic acid urgently needs to be solved. Silica and ammonium fluoride are produced by ammoniation of fluorosilicate. As a reinforcing material with superior performance, silica has a broad market and good development prospects in the processing and application of polymer materials; ammonium fluoride It can be used as a raw material to produce anhydrous hydrofluoric acid, and many fluorides can be derived. This route is a more effective way for the comprehensive utilization of fluosilicic acid. [0003] The production of white carbon black and ammonium fluoride by ammonification...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B33/18C01C1/16
Inventor 明大增吴立群梁雪松李志祥杨跃华梅毅杨亚斌钟英杨先王汝春杨云松罗如意
Owner YUNNAN YUNTIANHUA
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