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Method for preparing potassium fluoride by employing fluosilicic acid with co-production of white carbon black

A technology of potassium fluorosilicate and white carbon black, which is applied in the field of preparation of potassium fluoride and co-production of white carbon black, can solve the problems of affecting product quality, affecting the quality of white carbon black products, and poor control of dosage, so as to avoid product quality , solve the bottleneck of environmental protection, the effect of high utilization rate of raw materials

Active Publication Date: 2015-02-04
DUOFUDUO KUNMING TECH DEV CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These two methods are theoretically feasible, but in actual production, in order to meet the requirements of clean production and resource conservation, the mother liquor produced by the preparation of potassium fluoride needs to be recycled for the preparation of raw material slurry. For example, in the patent CN103101931A, potassium fluoride is filtered The final filtrate is returned to be used for the preparation of potassium fluorosilicate slurry or potassium carbonate solution for recycling, which results in the PO 4 3- and SO 4 2- The accumulated problems in the product affect the quality of the product, and in the process of alkali hydrolysis with potassium hydroxide, the dosage is not easy to control, and a slight excess will cause SiO 2 Dissolution, thus affecting the product quality of silica

Method used

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  • Method for preparing potassium fluoride by employing fluosilicic acid with co-production of white carbon black
  • Method for preparing potassium fluoride by employing fluosilicic acid with co-production of white carbon black
  • Method for preparing potassium fluoride by employing fluosilicic acid with co-production of white carbon black

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Effect test

Embodiment 1

[0046] Utilize fluosilicic acid of the present embodiment to prepare the method for potassium fluoride coproduction white carbon black, as figure 1 shown, including the following steps:

[0047] 1) Take a fluosilicic acid solution (a by-product of the phosphate fertilizer industry) with a mass concentration of 8%, stir under normal temperature and pressure, and add potassium carbonate slurry with a mass concentration of 50% at a uniform speed for reaction. The molar ratio of fluosilicic acid to potassium carbonate The reaction time is 1.0:1.2, the reaction time is 30min, the pH at the end of the reaction is controlled to be 6.5-7.0, the temperature at the end of the reaction is 30°C, and it is filtered after the reaction to obtain a trace amount of SiO 2 Potassium fluorosilicate ointment and mother liquor A; Mother liquor A contains PO with a mass fraction of 0.1% 4 3- , 0.5% SO 4 2- and a small amount of K + ;

[0048] 2) adding excess calcium hydroxide to the mother li...

Embodiment 2

[0056] The method that utilizes fluosilicic acid of the present embodiment to prepare potassium fluoride to co-produce white carbon black comprises the following steps:

[0057] 1) Take a fluosilicic acid solution (a by-product of the phosphate fertilizer industry) with a mass concentration of 18%, stir under normal temperature and pressure, and add a potassium carbonate slurry with a mass concentration of 35% at a uniform speed to react, the molar ratio of fluosilicic acid to potassium carbonate The reaction time is 1.0:1.5, the reaction time is 30min, the pH at the end of the reaction is controlled to be 6.5-7.0, the temperature at the end of the reaction is 58°C, and it is filtered after the reaction to obtain a trace amount of SiO 2 Potassium fluorosilicate ointment and mother liquor A; Mother liquor A contains PO with a mass fraction of 0.1% 4 3- , 0.5% SO 4 2- and a small amount of K + ;

[0058] 2) adding excess calcium oxide to the mother liquor A obtained in step...

Embodiment 3

[0066] The method that utilizes fluosilicic acid of the present embodiment to prepare potassium fluoride to co-produce white carbon black comprises the following steps:

[0067] 1) Take a fluosilicic acid solution (a by-product of the phosphate fertilizer industry) with a mass concentration of 30%, stir under normal temperature and pressure, and add potassium carbonate slurry with a mass concentration of 10% at a uniform speed for reaction. The molar ratio of fluosilicic acid to potassium carbonate The reaction time is 1.0:1.2, the reaction time is 20min, the pH at the end of the reaction is controlled to be 6.5-7.0, the temperature at the end of the reaction is 60°C, after the reaction is completed, filter to obtain a trace amount of SiO 2 potassium fluorosilicate ointment and mother liquor A; mother liquor A contains 1% PO 4 3- , 0.5% SO 4 2- and a small amount of K + ;

[0068] 2) adding excess calcium hydroxide to the mother liquor A obtained in step 1) for reaction a...

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Abstract

The invention discloses a method for preparing potassium fluoride by employing fluosilicic acid with co-production of white carbon black. The method includes following steps: (1) adding potassium carbonate in a fluosilicic acid solution and performing filtration after the reaction to obtain a potassium fluosilicate paste and a mother liquid A; (2) adding calcium oxide or calcium hydroxide to the mother liquid A, performing filtration after the reaction for removing precipitation, and adding potassium carbonate with filtration to obtain a mother liquid B; (3) mixing the potassium fluosilicate paste and the mother liquid B, adding hydrofluoric acid and SiO2 for reaction to obtain a potassium fluosilicate slurry material B; and (4) adding a white carbon black seed crystal to the potassium fluosilicate slurry material B with addition of potassium carbonate for performing an alkaline hydrolysis reaction, performing filtration to obtain a potassium fluoride solution and white carbon black paste and drying the potassium fluoride solution and the white carbon black paste. In the method, by means of the technologies of step-by-step alkaline hydrolysis and impurity removing in the mother liquids, a problem of accumulation of PO4<3-> and SO4<2-> in the raw material fluosilicic acid solution in a product. The potassium fluoride and the white carbon black are high in qualities and are low in production cost. High-quality and cleaning production of fluorine and silicon resources in phosphatic fertilizer industry and hydrofluoric acid industry is achieved.

Description

technical field [0001] The invention belongs to the technical field of fluorine chemical industry, and in particular relates to a method for preparing potassium fluoride and co-producing white carbon black by utilizing fluosilicic acid. Background technique [0002] Potassium fluoride is an important inorganic compound, which is widely used in glass engraving, food antiseptic, electroplating and preparation of potassium hydrogen fluoride; in the field of welding, it is mainly used as a flux for welding of various alloys or metals; in the field of organic compound generation It is used as a fluorinating agent, and can also be used as an absorbent for absorbing hydrogen fluoride and water. It is used in the field of pesticides to produce sodium fluoroacetate and ammonium fluoroacetate insecticides, and in the field of medicine to prepare norfloxacin. The traditional production method of potassium fluoride is to use hydrofluoric acid and potassium hydroxide as raw materials. Du...

Claims

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Application Information

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IPC IPC(8): C01B33/12C01D3/02
Inventor 王慧陈宏伟李霞刘海霞王建萍张良李娇娇常仑耿梦湍张小斌
Owner DUOFUDUO KUNMING TECH DEV CO LTD
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