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A kind of comprehensive utilization method of phosphoric acid sludge

A technology of sludge and phosphoric acid, applied in the field of secondary resource utilization, can solve the problems of fouling and clogging of the filtration system, low conversion rate of superphosphate, increase in the content of too large particles in the product, etc., and achieves easy operation, simple process flow, and equipment requirements. simple effect

Active Publication Date: 2017-01-18
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In the production system of wet-process phosphoric acid, the existence of sludge increases the production consumption of wet-process phosphoric acid and reduces the output of high-quality wet-process phosphoric acid, etc.
At present, the wet-process phosphoric acid production enterprises mainly return the phosphoric acid sludge and the phosphoric acid contained together to the production system to implement closed cycle operation, but it will lead to difficulties in filtering the phosphoric acid slurry, high viscosity of liquid phosphoric acid, fouling and blockage of the filtration system and other problems; secondly It is used for the production of PMAP, but it will lead to a large increase in the content of too large particles (≥1mm) in the product, uneven color of the product, etc.; or it is used for the production of superphosphate, but it will lead to problems such as low conversion rate of superphosphate

Method used

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  • A kind of comprehensive utilization method of phosphoric acid sludge

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Example 1: The acid residue mixture containing wet-process phosphoric acid was separated by a plate and frame filter press to obtain a phosphoric acid sludge filter cake. The filtrate was used as wet-process phosphoric acid; for the phosphoric acid sludge filter cake, the stirring speed was 400 rpm, Add it to the reactor where water has been added beforehand at room temperature, keep the solid (filter cake) mass volume ratio to 1:2, add 5.0mol / l hydrochloric acid solution, and react for 2 hours at natural temperature. Control The end point of the reaction is PH≤1.0. After the reaction, the leaching solution is obtained by vacuum filtration and separation; adding titanium tetrachloride solution to the leaching solution at a stirring speed of 200 rpm and room temperature to make the Ti in the system 4+ And PO 4 3- The molar ratio is 3:4, react for 4 hours to promote the formation of titanium phosphate precipitation, and then use vacuum filtration to separate the solid mater...

Embodiment 2

[0019] Example 2: The acid residue mixture containing wet-process phosphoric acid was separated by pressure filtration using a plate and frame filter press to obtain a phosphoric acid sludge filter cake. The filtrate was used as wet-process phosphoric acid; for the phosphoric acid sludge filter cake, the stirring speed was 400 rpm, Add it to the reactor where water has been added beforehand at room temperature, keep the solid (filter cake) mass volume ratio to 1:4, add 4.0mol / l hydrochloric acid solution, and react for 4 hours at natural temperature. Control The end point of the reaction is PH≤1.0. After the reaction, the leaching solution is obtained by vacuum filtration and separation; adding titanium tetrachloride solution to the leaching solution at a stirring speed of 500 rpm and room temperature to make the Ti in the system 4+ And PO 4 3- The molar ratio is 3:4, the reaction is 2 hours to promote the formation of titanium phosphate precipitation, and then the solid materia...

Embodiment 3

[0021] Example 3: The acid residue mixture containing wet-process phosphoric acid was separated by a plate and frame filter press to obtain a phosphoric acid sludge filter cake. The filtrate was used as wet-process phosphoric acid; for the phosphoric acid sludge filter cake, the stirring speed was 400 rpm, At room temperature, add it to the reactor where water has been added in advance, keep the solid (filter cake) mass volume ratio 1:3, then add 5.5 mol / l hydrochloric acid solution, and react at natural temperature for 3 hours. Control The end point of the reaction is PH≤1.0. After the reaction, the leaching solution is obtained by vacuum filtration and separation; the titanium tetrachloride solution is added to the leaching solution at a stirring speed of 300 rpm and room temperature to make the Ti in the system 4+ And PO 4 3- The molar ratio is 3:4, react for 3 hours to promote the formation of titanium phosphate precipitation, and then use vacuum filtration to separate the s...

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Abstract

The invention discloses a comprehensive utilization method of phosphoric acid sludge. The comprehensive utilization method comprises the following steps: leaching phosphoric acid sludge by using a phosphoric acid solution, precipitating the lixivium by using a titanium tetrachloride solution, separating, washing and drying, thereby obtaining a titanium phosphate product; adding concentrated sulfuric acid into the filtrate to precipitate calcium so as to obtain high-quality calcium sulfate, and evaporating and concentrating the calcium precipitated filtrate at normal pressure till the content of FeCl3 is greater than 38%, thereby obtaining a ferric chloride solution product. By adopting the comprehensive utilization method disclosed by the invention, valent components in phosphoric acid sludge can be effectively utilized, titanium phosphate, calcium sulfate and ferric trichloride products with high additional values can be prepared, secondary utilization of resources is achieved, and the comprehensive utilization method has the characteristics of simple process, simple equipment requirements, easiness in operation, safety and the like.

Description

Technical field [0001] The invention belongs to the research field of secondary resource utilization in the chemical industry, and specifically relates to the comprehensive utilization of phosphoric acid sludge produced in the production process of wet-process phosphoric acid. Background technique [0002] Phosphoric acid sludge is a mixture of subsequent precipitation salts produced during the process of wet-process phosphoric acid production due to evaporation and concentration, wet-process phosphoric acid aging, clarification, and storage. The main components are oxides of phosphorus, calcium, iron, magnesium, and aluminum. Or phosphate, etc., which contains 35-45% P 2 O 5 , 15~20%Fe 2 O 3 , 8~13%CaO, about 5% SO 4 2- , 3~5%F and 3~5%K 2 O and Na 2 O, etc., is a good secondary resource, which can be used to extract valuable elements such as phosphorus, calcium, and iron to produce chemical products with higher added value. [0003] In the production system of wet-process phospho...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B25/37C01F11/46C01G49/10B09B3/00
Inventor 苏毅张琼李国斌胡亮李沪萍罗康碧
Owner KUNMING UNIV OF SCI & TECH