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Chemical polishing waste phosphoric acid treatment method and fertilizer preparation method

A technology of chemical polishing and treatment methods, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve problems such as poor sales of calcium hydrogen phosphate market, complicated precipitation and separation, and low added value of products, and achieve obvious Economic and environmental benefits, easy reaction conditions, and easy large-scale production

Active Publication Date: 2020-10-23
SHENZHEN SHENTOU ENVIRONMENT TECH CO LTD
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  • Claims
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Problems solved by technology

This method will produce a large amount of phosphorus-containing sludge, increase the cost of landfill, and even cause environmental pollution
[0004] At present, there are some relevant patents and literature reports on the comprehensive utilization of this kind of waste phosphoric acid. For example, patent CN101456547 B uses lime milk as a neutralizing agent, and realizes the purification of heavy metal ions and the production of fertilizer-grade calcium hydrogen phosphate by step-by-step precipitation method. preparation, but the market sales of calcium hydrogen phosphate is not good, and the added value of the product is low
Patent 201610795470.0 proposes a resource recycling method for aluminum polishing waste phosphoric acid solution, which adopts adding fluorine-containing solution and sodium salt to precipitate and remove aluminum in the form of cryolite, and then produces calcium hydrogen phosphate and ordinary calcium by calcium salt three-step precipitation method, sulfuric acid and Phosphoric acid is fully utilized, but the precipitation and separation are complicated and the added value of the product is low
[0005] In view of the fact that such waste liquid contains a large amount of phosphoric acid components, and phosphorus-containing products have high economic value, the inventor has developed a series of recycling processes, which include purifying and removing impurities of such waste acid and preparing products such as urea phosphate, Because this kind of waste acid often contains more impurities, and urea phosphate is easily soluble in water, although the process of preparing urea phosphate products has undergone relevant purification processes and multi-stage recovery, the recovery rate of phosphorus resources has reached about 90%, but there are still A small amount of high-concentration phosphorus and urea-containing mother liquor
At present, there are almost no relevant research reports on the comprehensive utilization of this kind of mother liquor. Generally, comprehensive treatment is used to meet the discharge standards.

Method used

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  • Chemical polishing waste phosphoric acid treatment method and fertilizer preparation method

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preparation example Construction

[0043] The present invention also provides a kind of preparation method of potassium dihydrogen phosphate, comprises the following steps:

[0044] Adding a neutralizing agent to the mother liquor of urea phosphate crystallization prepared from chemically polished waste phosphoric acid, stirring and reacting to generate a precipitate of metal ions, and filtering to obtain a filtrate;

[0045]Adding a precipitating agent to the filtrate to precipitate impurity ions, and filtering again to obtain a purified solution;

[0046] Evaporating the purified solution under reduced pressure, the mass ratio of urea to water in the purified solution after the reduced-pressure evaporation is 0.75 to 1.4, cooling and crystallizing to obtain crystals and mother liquor, filtering and separating the crystals, washing and drying, Potassium dihydrogen phosphate product is obtained.

[0047] The potassium dihydrogen phosphate product obtained in the embodiment of the present invention has a direct...

Embodiment 1

[0056] Get chemical polishing waste phosphoric acid to prepare 500mL of urea phosphate crystallization mother liquor, wherein total phosphorus content is 113g / L, total nitrogen is 99.4g / L, sulfate radical 5.6g / L, aluminum content 4.5g / L, iron (Fe) content 23mg / L L, copper (Cu) content 16mg / L, zinc (Zn) content 28mg / L, lead (Pb) content 0.3mg / L.

[0057] Slowly add potassium hydroxide with a concentration of 30% to the mother liquor of urea phosphate crystallization prepared by chemical polishing waste phosphoric acid, control the pH value at about 4.2, stir for 2.0 hours, and filter to remove the precipitates of metal ions such as aluminum;

[0058] In the filtrate of above-mentioned gained, add appropriate amount of barium hydroxide by sulfate radical metering 100% to remove sulfate radical ion, then add by the precipitant potassium sulfide of heavy metal total molar weight 95%, remove part copper (Cu), lead (Pb), Arsenic (As), zinc (Zn), filtered to obtain purified solution;...

Embodiment 2

[0063] Take chemical polishing waste phosphoric acid to prepare 500mL of urea phosphate crystallization mother liquor, wherein total phosphorus content is 115g / L, total nitrogen is 102.1g / L, sulfate radical 2.7g / L, aluminum content 3.5g / L, Fe content 10mg / L, Cu The content is 18mg / L, the Zn content is 31mg / L, and the Pb content is 0.1mg / L.

[0064] Slowly add potassium carbonate with a concentration of 28% to the mother liquor for preparing urea phosphate crystallization from chemically polished waste phosphoric acid, control the pH value at about 4.6, stir for 0.5h, and filter to remove the precipitates of metal ions such as aluminum.

[0065] Add an appropriate amount of barium chloride to remove sulfate ions in the filtrate of the above-mentioned gained by 95% of the sulfate radical metering, then add the precipitant ammonium sulfide according to the total molar weight of heavy metals 100%, remove part of Cu, Pb, As, Zn, and filter to obtain Purifying fluid.

[0066] The p...

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Abstract

The invention provides a chemical polishing waste phosphoric acid treatment method. The method comprises the following steps: a neutralizer is added to mother liquor of urea phosphate crystals prepared from chemical polishing waste phosphoric acid, a stirring reaction is performed, a precipitate of metal ions is formed and filtered, and a filtrate is obtained; a precipitant is added to the filtrate, foreign ions are precipitated, filtering is performed again, and a purified solution is obtained; the purified solution is subjected to reduced-pressure evaporation until the mass ratio of urea to water is 0.75-1.4, then cooling crystallization, filtering separation, washing and drying are performed, and a monopotassium phosphate product is obtained; mother liquor obtained after cooling crystallization is evaporated and concentrated until phosphorus content of the mother liquor is 3.5%-5.0%, vacuum drying is performed, and nitrogen-phosphorus-potassium compound fertilizer is obtained. Nitrogen and phosphorus resources in the mother liquor of the urea phosphate crystals are recovered mainly in forms of monopotassium phosphate and the nitrogen-phosphorus-potassium compound fertilizer, production process is simple and low in cost, nitrogen-phosphorus resource using rate is high, and the economic value is high.

Description

technical field [0001] The present invention relates to the technical field intersecting environmental protection and phosphorus chemical production, mainly to the technical field of industrial waste liquid, in particular to a treatment method for preparing urea phosphate crystallization mother liquor from chemical polishing waste phosphoric acid, nitrogen-phosphorus-potassium compound fertilizer and phosphoric acid The preparation method of potassium dihydrogen. Background technique [0002] Chemical polishing waste phosphoric acid mainly comes from a large amount of waste liquid produced by polishing metal surfaces in electroplating industry, coating, anodic oxidation and various surface treatment processes. It contains high concentration of phosphoric acid, sulfuric acid, nitric acid, acetic acid and heavy metal ions, etc. Harmful chemical substances, highly corrosive, belonging to the HW34 category of the "National Hazardous Waste List". [0003] The general way to deal...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C05G1/00C01B25/30C07C273/02C07C275/02
CPCC01B25/30C01B25/305C05G1/00C07C273/02C07C275/02
Inventor 唐瑜钟周兆安陈志传徐丽阳慎义勇薛志强
Owner SHENZHEN SHENTOU ENVIRONMENT TECH CO LTD
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