Method for preparing potassium fluoride and coproducing ultrafine white carbon black from ammonium fluorosilicate byproduct in phosphate fertilizer production

A technology of ammonium fluorosilicate and fine white carbon black, which is applied in the directions of alkali metal fluoride, silicon oxide, silicon dioxide, etc., to achieve the effect of extending the product chain, reducing production costs and reducing preparation costs

Active Publication Date: 2014-03-26
ANHUI LIUGUO CHEM CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The technical process is simple, and the recovery rate of fluorine and silicon resources is high, but it is limited to low-end products of ammonium fluorosilicate

Method used

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  • Method for preparing potassium fluoride and coproducing ultrafine white carbon black from ammonium fluorosilicate byproduct in phosphate fertilizer production
  • Method for preparing potassium fluoride and coproducing ultrafine white carbon black from ammonium fluorosilicate byproduct in phosphate fertilizer production
  • Method for preparing potassium fluoride and coproducing ultrafine white carbon black from ammonium fluorosilicate byproduct in phosphate fertilizer production

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preparation example Construction

[0024] The preparation of ammonium fluorosilicate adopts the method disclosed in Chinese patent ZL201010200763.2: as figure 1 As shown, the ammonium fluorosilicate crystallization mother liquor is used as the washing liquid in the fluorine absorption system of phosphate fertilizer to absorb fluorine-containing tail gas of phosphate fertilizer to obtain a high-concentration fluorine-containing rich liquid, filter solid impurities through a filter press, and send the liquid phase to the jet for neutralization The device is neutralized with ammonia, crystallized by cooling crystallizer and filtered by filter press to obtain ammonium fluorosilicate crystallization mother liquor and ammonium fluorosilicate solid product, and the ammonium fluorosilicate crystallization mother liquor is returned to the phosphate fertilizer fluorine absorption system.

[0025] It is also possible to follow the conventional ammonia addition neutralization method introduced in the background technology o...

Embodiment 1

[0028] The ammonium fluorosilicate and potassium hydroxide are respectively configured so that the concentration of the ammonium fluorosilicate solution is 20% and the concentration of the potassium hydroxide solution is 35%. Add the ammonium fluorosilicate solution into the reactor, and slowly add the potassium hydroxide solution at a speed of no more than 4ml / min at a temperature of 85°C. KOH / n (NH4)2SiF6 The molar ratio is 6.2:1, stirring, after reacting for 1h, when the pH value of the titration end point is 9.0, stop the reaction, and prepare a slurry containing white carbon black precipitation and potassium fluoride solution, and the reaction tail gas is a mixture of ammonia and water vapor , back as a neutralized raw material for the preparation of ammonium fluorosilicate solid. After the reaction slurry is aged for 0.5h, it is sent to a filter press to filter while it is hot. The solid phase is water-containing white carbon black, and the liquid phase is potassium f...

Embodiment 2

[0030] Method is with embodiment 1. Among them, the concentration of ammonium fluorosilicate solution is 20%, the concentration of potassium hydroxide solution is 35%, the reaction temperature is controlled at 90°C, and the titration end point pH value is 8.5.

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Abstract

The invention relates to a method for preparing potassium fluoride and coproducing ultrafine white carbon black from an ammonium fluorosilicate byproduct in phosphate fertilizer production, which comprises the following steps: reacting a 20-40% ammonium fluorosilicate solution and a 30-35% potassium hydroxide solution at 80-85 DEG C, wherein the pH value at the end point of the reaction is 8-10, and the reaction tail gas is used as a neutralizing raw material for preparation of solid ammonium fluorosilicate; aging the reaction slurry, and performing hot filtration; washing the solid phase, and drying to obtain the white carbon black product; and concentrating to crystallize the liquid phase and drying, or concentrating the liquid phase and performing spray drying, thus obtaining the potassium fluoride product. According to the invention, the high-added-value potassium fluoride product is obtained, and the ultrafine white carbon black product is coproduced at the same time; no waste water, waste gas and solid waste are discharged; and the method is simple in process, low in cost, friendly to environment and high in economic benefits.

Description

technical field [0001] The invention relates to a method for utilizing fluorine-containing tail gas in phosphate fertilizer production, in particular to a method for preparing potassium fluoride and co-producing superfine white carbon black with ammonium fluorosilicate, a by-product of phosphate fertilizer. Background technique [0002] Phosphoric acid extraction, phosphoric acid concentration and other processes in the production of phosphate fertilizers will produce a large amount of fluorine-containing tail gas (SiF 4 +HF). The process usually requires a supporting washing device. The existing absorption process mainly uses water to absorb fluorine-containing tail gas to generate fluosilicic acid with a concentration of 8% to 18% by weight for recovery. Large-scale phosphate fertilizer enterprises sell sodium fluorosilicate produced by the reaction of recovered fluorosilicic acid and sodium salt as a product. The low-end product produces a large amount of acidic sewage a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01D3/02C01B33/12
Inventor 周玉新沈浩郭嘉张斌刘祎刘荣廖厚琪朱英俊彭克荣
Owner ANHUI LIUGUO CHEM CO LTD
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