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A method for recovering fluorine in industrial monoammonium phosphate neutralization slurry

An industrial monoammonium phosphate and recovery method technology, which is applied in the field of recovery of fluorine in industrial monoammonium phosphate neutralization slurry, can solve the problem that industrial monoammonium phosphate neutralization slurry cannot be completely consumed, restricts industrial monoammonium phosphate production, and industrial The problems of monoammonium phosphate plant parking and other issues have been solved, and the effects of low cost, improved quality and convenient operation have been achieved.

Active Publication Date: 2020-05-15
HUBEI XIANGYUN GROUP CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] However, there is an increasing demand for 58% and 60% fertilizer grade ammonium phosphate in the market. Adding too much slurry will cause the nutrients of fertilizer ammonium phosphate to fail to meet the standard, resulting in the inability of industrial monoammonium phosphate neutralization slurry to be completely consumed.
A large amount of unconsumable slag often causes the tank to be full, which leads to the shutdown of the industrial monoammonium phosphate plant, thereby restricting the production of industrial monoammonium phosphate. Therefore, it is urgent to develop a new comprehensive utilization technology for neutralizing slag

Method used

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  • A method for recovering fluorine in industrial monoammonium phosphate neutralization slurry
  • A method for recovering fluorine in industrial monoammonium phosphate neutralization slurry
  • A method for recovering fluorine in industrial monoammonium phosphate neutralization slurry

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Experimental program
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Effect test

Embodiment 1

[0031] The solid content of the neutralized slurry was controlled at about 40%, and 98% concentrated sulfuric acid was added to the slurry according to 80% of the solid phase mass of the slurry, and the reaction was stirred at 90 °C for 1 h. Filtration to obtain acidolysis filtrate, P in the acidolysis filtrate 2 O 5 The content is about 15%, the fluorine content is about 2.2%, and the acid hydrolysis rate of phosphorus and fluorine is above 99%.

Embodiment 2

[0033] The acid hydrolysis filtrate obtained by separation in Example 1 was cooled, crystallized and filtered at a temperature of 5°C to 10°C to obtain an acid hydrolysis filtrate for removing impurities. The main component of the precipitated crystal was magnesium ammonium sulfate hexahydrate, and the main content was analyzed. above 99%.

Embodiment 3

[0035] The impurity-removing acid hydrolysis filtrate obtained in Example 2 was added with anhydrous sodium sulfate solid in a molar ratio of 6:1 according to the fluorine content in the filtrate, the reaction temperature was 40°C, and the reaction time was 0.5h, and fluorosilicic acid was obtained after filtration and washing. sodium. The filtered filtrate can be prepared into water-soluble fertilizer, and also used as the raw material of binary fertilizer and ternary fertilizer. The purity of sodium fluorosilicate is 98.7%, and the yield of fluorine is 50%.

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Abstract

The invention relates to a method for recycling fluorine in neutralized slurry of industrial monoammonium phosphate. The method comprises the following steps: a, preparing the neutralized slurry and water into turbid liquid; b, slowly adding sulfuric acid in the turbid liquid and reacting, and then filtering to obtain acid-hydrolyzed filtrate; c, cooling, crystalizing and filtering the acid-hydrolyzed filtrate to obtain impurity-removed acid-hydrolyzed filtrate; and d, adding anhydrous sodium sulfate solid in the impurity-removed acid-hydrolyzed filtrate, reacting and filtering, and washing and drying filter cakes to obtain sodium fluosilicate products, wherein the filtrate is used for production of complex fertilizers. The method is simple to operate and low in treatment cost; and a way for comprehensive utilization of the neutralized slurry is provided for industrial monoammonium phosphate production enterprises.

Description

technical field [0001] The invention relates to the field of chemical production, in particular to a method for recovering fluorine in industrial monoammonium phosphate neutralization slurry. Background technique [0002] The industrial monoammonium phosphate neutralized slurry comes from the filter cake produced during the neutralization and post-filtration process during the production of industrial monoammonium phosphate from wet phosphoric acid. The filter cake is mixed with water to form a slurry, hereinafter referred to as the neutralized slurry. For industrial monoammonium phosphate production enterprises, the amount of neutralized slurry is very large, and every 1 ton of industrial monoammonium phosphate produced produces 2.5-3 tons of slurry. The composition of the neutralized slurry is relatively complex, mainly including NH 4 H 2 PO 4 , (NH 4 ) 2 HPO 4 , MgHPO 4 , FeMg(NH 4 ) 2 (HPO 4 ) 2 ·F 3 , AlMg(NH 4 ) 2 (HPO 4 ) 2 ·F 3 Equal double salt, th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B33/10C01F5/40
CPCC01B33/103C01F5/40C01P2006/80
Inventor 居丽何俊孔小雁梁蕾余莹黄忠丁一刚
Owner HUBEI XIANGYUN GROUP CHEM