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Method for producing fluorine series compounds and white carbon black

A production method, a technology for silica, applied in chemical instruments and methods, silicon compounds, alkali metal fluorides, etc.

Inactive Publication Date: 2008-09-24
夏克立
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] Due to some problems in the above method, especially economic problems, it is still unable to compete with the traditional production method using fluorite as raw material. So far, all fluorine chemical products except sodium fluorosilicate are still mainly based on fluorite. produced for raw materials

Method used

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  • Method for producing fluorine series compounds and white carbon black
  • Method for producing fluorine series compounds and white carbon black
  • Method for producing fluorine series compounds and white carbon black

Examples

Experimental program
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Effect test

Embodiment 1

[0088] Bring the concentration to ~20% NH 4 The F solution is introduced into the exhaust gas absorption system of the chemical formation chamber with an annual output of 100,000 tons of ordinary calcium for absorption, and the concentration ~ 34% (NH 4 ) 2 SiF 6Solution, add it and liquid ammonia to the ammoniator at the same time and control its pH value at 7.2-7.5, then pass liquid ammonia into the ammoniator and control the final pH value of the ammoniation reaction to be above 8, and the temperature at 50-70 ℃, the obtained slurry is aged for 1 hour and then filtered, washed countercurrently with clean water until the eluate is close to neutral, and the filter cake is dried at 110 ℃ to obtain a specific surface area of ​​110m 2 / g of precipitated silica (silica) product and a concentration of 40.6% NH 4 F in ammonium fluoride solution. Such as ~ 34% (NH 4 ) 2 SiF 6 When the solution is introduced into a container with a stirring blade and cooled to ~ 20°C, ammonium...

Embodiment 2

[0090] Ready 700g 32% NH 4 F solution and 200 g 99% Na 2 SiF 6 . In a reactor equipped with a stirrer, first add ~150 g of 32% NH 4 F solution, then slowly add ~ 43 grams of sodium fluorosilicate at a temperature of 65 ° C, and then add the remaining ammonium fluoride solution and sodium fluorosilicate in proportion and uniformly, the entire feeding time is 1 hour, and then add After finishing, continue to stir and react for half an hour. Control a certain rate to put the reaction slurry into a pre-filled with a small amount of 32% NH 4 In the ammoniator with stirring of the F solution, feed ammonia to keep the pH value of the liquid phase in the ammoniator at pH 7.2 to 7.5. After the reaction slurry is added, continue to pass ammonia to increase the pH value of the liquid phase. High and keep the pH above 8, while controlling the slurry temperature in the range of 50-70°C. Stop stirring after the ammoniation is finished, settle naturally, release the upper suspension, t...

Embodiment 3

[0092] Set the flow rate to 1.46m 3 / hr concentration 410g / lNH 4 ammonium fluoride solution and a flow rate of 3.12m 3 Sodium chloride solution with a concentration of 25.5% NaCl / hr was added to the first reactor, and after ~45 minutes of reaction, it overflowed into the second reactor, and at the same time, 0.94m 3 / hr25.5% NaCl sodium chloride solution, the reaction material overflows into the thickener after staying in the second reactor for 30 minutes, and the thick phase is filtered, washed, and dried to obtain sodium fluoride products, and the dilute phase and filtrate Contains 53.9g / l sodium chloride and 164.4g / l ammonium chloride. It can be separated by thermal separation method. Ammonium chloride is used as a by-product, and sodium chloride is returned to participate in the reaction. It is entrusted to use ARL9800XP+ X-fluorescence spectrometer for analysis. The results are shown in the table:

[0093] Table 1. Sodium Fluoride product quality of the present inventi...

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Abstract

The invention relates to a method utilizing waste gas containing fluoride in fertilizer production or fluorine-containing gas or sodium fluorosilicate in fluorine chemical production as raw materials to product series compounds of fluorine and white carbon black. The ammonium fluoride and / or ammonia are / is introduced into an absorption system to get a (NH4) 2SiF6 solution with the absorbing solution concentration of 25 to 37 percent or the ammonium fluoride and the sodium fluorosilicate react to get a reaction product of sodium fluoride crystallization, fluosilicic acid solution and septenary-fluorine compound NH4F.(NH4)2SiF6 crystallization. The absorption liquid or the reaction product is aminated to get precipitated silica (white carbon black) with the specific surface of 100-180m<2> / g, and the latter can get a sodium fluoride product and an NH4F solution with the concentration of 30 to 45 percent. The solution used as a starting point can nearly prepare all inorganic fluoride chemical products, and ammonium fluoride, sodium fluoride, potassium fluoride, ammonium bifluoride, cryolite, aluminum fluoride, sodium hydrogen diffluoride and hydrofluoric acid production, etc. are main. The method has simplicity, effectiveness and higher economic benefit, and simultaneously, fluorine and silicon in the waste gas containing fluoride of phosphate fertilizer for the pollution of environment can be basically eliminated, and basically no waste water, waste gas and waste residue are discharged.

Description

[0001] This application is intended to be abandoned. The patent No. 01108196.1 applied on April 10, 2001 is "the production method of fluorine compound and silicon dioxide", and the patent No. applied on February 8, 2002 is 02112659.3 "using sodium fluorosilicate as The continuation and development of the production method for preparing fluorine compounds and silicon dioxide from raw materials" and the patent No. 200510040163.3 "Method for Utilizing Fluorine Waste Gas in Phosphate Fertilizer Production" filed on May 24, 2005. technical field [0002] The production method of fluorine series compounds and white carbon black belongs to the technical field of inorganic chemical industry, and specifically involves the use of fluorine-containing waste gas in phosphate fertilizer production or fluorine-containing gas in fluorine chemical production, or sodium fluorosilicate as raw materials to produce fluorine series compounds and have High specific surface area silica (precipitated ...

Claims

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Application Information

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IPC IPC(8): C01B33/12C01B33/20C01C1/16C01D3/02C01F7/50C01F7/04C01F7/54
Inventor 夏克立
Owner 夏克立
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