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Method for preparing aluminum polychlorid from byproduct generated in methyl diethyl phosphate production

A technology of diethyl methyl phosphite and polyaluminum chloride, applied in the direction of aluminum chloride, chemical instruments and methods, aluminum halide, etc., to achieve the effects of reducing acid consumption, high basicity, and reducing the formation of aluminum sol

Active Publication Date: 2018-12-21
ZHEJIANG XINAN CHEM INDAL GROUP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The object of the present invention is to provide a kind of method that utilizes the by-product that produces in the production of diethyl methyl phosphite to prepare polyaluminum chloride, solve the recycling problem of the by-product solid slag rich in sodium tetrachloroaluminate, reduce To avoid pollution to the environment, at the same time turn waste into wealth, and achieve the rational use of resources

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  • Method for preparing aluminum polychlorid from byproduct generated in methyl diethyl phosphate production

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Effect test

Embodiment 1

[0052] A kind of method that utilizes methyl diethyl phosphite to produce by-product to prepare polyaluminum chloride comprises the steps:

[0053] (1) Add 200 g of the by-product solid residue into 1000 mL of methanol, analyze at 50 ° C, filter while hot to remove the precipitated sodium chloride, and collect the solution;

[0054] (2) add 40g water in the solution and cool to make aluminum chloride hydrate crystallize and separate out, filter to obtain aluminum chloride hydrate, and filtrate is reused as solvent;

[0055] (3) Dissolve aluminum chloride hydrate in water so that the concentration of aluminum chloride is 60g / L, then add calcium aluminate powder in 5 times for hydrolysis polymerization reaction, control the reaction temperature at 50°C, when the pH value of the solution is 3.7 , aged at 50°C for 4h, and finally dried to obtain polyaluminum chloride.

Embodiment 2

[0057] A kind of method that utilizes methyl diethyl phosphite to produce by-product to prepare polyaluminum chloride comprises the steps:

[0058] (1) Add 200 g of the by-product solid residue into 800 mL of ethanol, analyze at 70° C., filter while hot to remove the precipitated sodium chloride, and collect the solution;

[0059] (2) add 80g water in the solution and cool to make aluminum chloride hydrate crystallize and separate out, filter to obtain aluminum chloride hydrate, and filtrate is reused as solvent;

[0060] (3) Dissolve aluminum chloride hydrate in water so that the concentration of aluminum chloride is 100g / L, then add calcium aluminate powder in 4 times for hydrolysis polymerization reaction, control the reaction temperature at 60°C, when the pH value of the solution is 3.9 , aged at 55°C for 3h, and finally dried to obtain polyaluminum chloride.

Embodiment 3

[0062] A kind of method that utilizes methyl diethyl phosphite to produce by-product to prepare polyaluminum chloride comprises the steps:

[0063] (1) Add 200 g of by-product solid residue into 900 mL of n-butanol, analyze at 100 ° C, filter while hot to remove the precipitated sodium chloride, and collect the solution;

[0064] (2) add 70g water in the solution and cool to make aluminum chloride hydrate crystallize and separate out, filter to obtain aluminum chloride hydrate, and filtrate is reused as solvent;

[0065] (3) Dissolve aluminum chloride hydrate in water so that the concentration of aluminum chloride is 90g / L, then add calcium aluminate powder in 2 times for hydrolysis polymerization reaction, control the reaction temperature at 80°C, when the pH value of the solution is 3.8 , aged at 65°C for 1h, and finally dried to obtain polyaluminum chloride.

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Abstract

The invention provides a method for preparing aluminum polychlorid from byproducts generated in methyl diethyl phosphate production. The method comprises the following steps: (1) dispersing byproductsolid dregs into a solvent, analyzing, and collecting a solution; (2) cooling the solution with water, and separating aluminum chloride hydrate crystal; (3) hydrolyzing and polymerizing the aluminum chloride hydrate crystal, and aging, thereby obtaining the aluminum polychlorid. By adopting the method, solid dregs rich in sodium tetrachloroaluminate are adopted as a raw material, an inorganic polymeric flocculant, namely the aluminum polychlorid, is successfully prepared through steps of simple processes, and not only is the problem of waste disposal solved, but also a high additional value product can be successfully made.

Description

technical field [0001] The invention belongs to the technical field of inorganic chemistry, and relates to a method for preparing polyaluminum chloride by utilizing by-products produced in the production of diethyl methylphosphite. Background technique [0002] Diethyl methylphosphonite (CH 3 P(OEt) 2 ) is an important organic chemical intermediate, which is widely used in the fields of pesticides, medicines and synthetic materials. At present, there are mainly two routes for preparing diethyl methyl phosphite in industry: (1) EP0391329A2 discloses that phosphorus trichloride and triethyl phosphite are used as raw materials to prepare diethyl chlorophosphonite. The process route for obtaining diethyl methylphosphite by reaction is also the main process technology for producing diethyl methylphosphite in my country at present. However, due to its large synthesis difficulty, high production technology requirements, and complicated technological process, etc., There are still ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F7/56C02F1/52
CPCC01F7/56C02F1/5245
Inventor 周曙光秦龙余神銮姜胜宝祝小红王萍付萍
Owner ZHEJIANG XINAN CHEM INDAL GROUP
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