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A method for recovering cryolite from fluorine-containing waste residue in pesticide industry

A cryolite and waste slag technology, applied in the field of cryolite recovery, can solve the problems of difficult treatment and disposal of fluorine-containing waste slag, complex resource utilization process, etc., achieve significant economic and environmental benefits, alleviate random stacking, and facilitate operation

Active Publication Date: 2016-04-20
TONGJI UNIV
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  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Therefore, in view of the difficulties in the treatment and disposal of fluorine-containing waste residues in the pesticide industry at the present stage, and the complicated resource utilization process, the present invention provides a method for recovering cryolite from fluorine-containing waste residues in the pesticide industry, aiming to explore a new path resource-based process

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] The object of treatment is fluorine-containing waste residue from a pesticide production plant. The slag is in the shape of yellow sand, pH=10-12, and the fluorine content in the slag is 39.5wt%. X-ray diffractometer (XRD) detection shows that the fluorine in the fluorine-containing waste slag mainly exists in the form of NaF. Separating and preparing cryolite from this kind of fluorine-containing waste residue specifically includes the following steps:

[0027] (1) Add 2L of water and 50g of fluorine-containing waste residue from the pesticide industry into the reactor, adjust the pH of the mixed solution to 7 with 1mol / L nitric acid, and mechanically stir for 0.5h at 25°C with the speed of the mixer at 400r / min, and then mix the solution Filtrate and filter residue were obtained by filtration.

[0028] (2) Add 100 mL of aluminum sulfate solution to the filtrate obtained in step (1), the F / Al ratio in the mixture is 5, adjust the mixed solution with 1mol / L nitric acid...

Embodiment 2

[0034] The method for reclaiming cryolite from pesticide industry fluorine-containing waste residue adopts the following steps:

[0035] (1) Extraction of fluorine-containing waste residues in the pesticide industry: Mix the fluorine-containing waste residues in the pesticide industry with water, the liquid-solid ratio of water to fluorine-containing waste residues is 25mL / g, and the fluorine-containing waste residues are the production process of fluorine-containing pesticides and their intermediates The fluorine-containing solid waste produced in the fluoride, in which fluorine mainly exists in the form of sodium fluoride, adjust the pH value of the mixed solution to 5 with industrial-grade concentrated sulfuric acid, control the reaction temperature at 25 ° C, and mechanically stir for 5 hours. After the reaction is completed, filter to obtain The filtrate and filter residue were analyzed for components. The results showed that the fluorine concentration in the filtrate was ...

Embodiment 3

[0038] The method for reclaiming cryolite from pesticide industry fluorine-containing waste residue adopts the following steps:

[0039] (1) Extraction of fluorine-containing waste residues in the pesticide industry: Mix the fluorine-containing waste residues in the pesticide industry with water, the liquid-solid ratio of water to fluorine-containing waste residues is 40mL / g, and the fluorine-containing waste residues are the production process of fluorine-containing pesticides and their intermediates The fluorine-containing solid waste produced in the process, in which fluorine mainly exists in the form of sodium fluoride, adjust the pH value of the mixed solution to 6 with the strong acid waste water produced in the acid production process, control the reaction temperature at 60 ° C, mechanically stir for 3 hours, and wait for the reaction to end Finally, the filtrate and filter residue are obtained by filtration, and the filter residue is added to cement to solidify and then...

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Abstract

The invention relates to a method for reclaiming cryolite from fluorine containing pesticide industrial waste residues. The method comprises the following steps: (1) extracting fluorine containing pesticide industrial waste residues: mixing the fluorine containing pesticide industrial waste residues and water, regulating the pH value of the mixed solution by using acid, heating and mechanically stirring; and filtering to obtain filtrate and filtered slag after the reaction is completed; (2) preparing cryolite: adding molten aluminum into the filtrate, regulating the initial pH value of the mixed solution by acid or alkali, heating and mechanically stirring; filtering to obtain filtrate and filtered slag; refluxing and extracting the filtrate, mixing the obtained filtrates and reacting once again; washing and drying the filtered slag to obtain the product cryolite. Compared with the prior art, the method realizes reduction and harmless treatment of fluorine containing waste slag, and reclamation of flurorine resourcess; the treatment process is simple, the operation is convenient, the cost is low and the secondary pollution is hardly caused; and the method has remarkable economic, social and environment benefits.

Description

technical field [0001] The invention belongs to the field of comprehensive utilization of solid waste resources, in particular to a method for recovering cryolite from fluorine-containing waste residues in the pesticide industry. Background technique [0002] The development of fluorine-containing pesticides has become the main body of the creation of new pesticides. Among the thousands of pesticide varieties in the world, fluorine-containing pesticides account for about 15%. Among the 86 newly developed chemical pesticides in the world in the past 10 years, 34 are fluorine-containing compounds. . Fluorine-containing pesticides have become the leading species in the development and application of the pesticide industry now and even in the future. In the synthesis process of fluorine-containing pesticide intermediates, a large amount of fluorine-containing waste residue will be produced. Generally, 0.2 tons of fluorine-containing waste residue will be generated for every to...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01F7/54
Inventor 何品晶李杨章骅邵立明吕凡
Owner TONGJI UNIV