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Treatment method of sodium tetrachloroaluminate solid residues

A technology of sodium tetrachloroaluminate and a treatment method, applied in the field of inorganic chemistry, can solve problems such as high cost, complicated process, difficult separation, etc., and achieve the effects of simple operation, simple process flow and cost reduction

Active Publication Date: 2020-09-22
ZHEJIANG XINAN CHEM INDAL GROUP
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The method not only does not separate aluminum and sodium before the high-temperature reaction, but a large amount of phosphoric acid or phosphate needs to be added to the high-temperature reaction, which increases the processing cost, but also belongs to the high-temperature reaction with high energy consumption, and the product obtained by the high-temperature reaction is Mixture of sodium phosphate and aluminum tripolyphosphate, difficult to separate
[0007] In summary, the treatment methods disclosed in the prior art all have disadvantages such as complex process, high cost, and risk of cross-contamination. Therefore, it is urgent to develop an effective treatment method for sodium tetrachloroaluminate solid slag method to achieve the purpose of cost reduction, efficient and thorough resource utilization of sodium tetrachloroaluminate solid slag

Method used

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  • Treatment method of sodium tetrachloroaluminate solid residues
  • Treatment method of sodium tetrachloroaluminate solid residues

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Effect test

Embodiment 1

[0052] This embodiment provides a method for treating sodium tetrachloroaluminate solid slag. The sodium tetrachloroaluminate solid slag is derived from preparing methyl chloride, phosphorus trichloride, aluminum powder and aluminum trichloride as main raw materials. In the production process of base phosphine dichloride, the content of sodium tetrachloroaluminate in the solid slag is 95%, and the treatment method comprises the following steps:

[0053] (1) 100g of solid slag with a sodium tetrachloroaluminate content of 95% is added to 400g of water for dissociation, dissociated for 1h at 80°C, and then 70g of hydrogen chloride gas is introduced, that is, the mass ratio of solid slag and hydrogen chloride is 1: 0.7, there is aluminum chloride hexahydrate to separate out, then through a solid-liquid separation to obtain aluminum chloride hexahydrate solid and a filtrate;

[0054] Among them, 121.5g of aluminum chloride hexahydrate solid was obtained by one solid-liquid separat...

Embodiment 2

[0057] The present embodiment provides a method for treating the solid slag of sodium tetrachloroaluminate, and the solid slag of sodium tetrachloroaluminate is the same as that in Embodiment 1, and the treatment method includes the following steps:

[0058] (1) 100g of solid slag with a sodium tetrachloroaluminate content of 95% is added to 400g of water for dissociation, dissociated at 80 ° C for 1h, and then 100g of hydrogen chloride gas is introduced, that is, the mass ratio of solid slag and hydrogen chloride is 1: 1.0, there is aluminum chloride hexahydrate to separate out, then through a solid-liquid separation to obtain aluminum chloride hexahydrate solid and a filtrate;

[0059] Among them, 127.6g of aluminum chloride hexahydrate solid was obtained by one solid-liquid separation, which was dried by vacuum drying at 60 °C for 8 hours to obtain 116.0g of aluminum chloride hexahydrate product;

[0060] (2) the primary filtrate obtained in step (1) is concentrated and cry...

Embodiment 3

[0062] The present embodiment provides a method for treating the solid slag of sodium tetrachloroaluminate, and the solid slag of sodium tetrachloroaluminate is the same as that in Embodiment 1, and the treatment method includes the following steps:

[0063] (1) 100g of solid slag with a sodium tetrachloroaluminate content of 95% is added to 400g of water for dissociation, dissociated at 80 ° C for 1h, and then 150g of hydrogen chloride gas is introduced, that is, the mass ratio of solid slag and hydrogen chloride is 1: 1.5, there is aluminum chloride hexahydrate to separate out, then through a solid-liquid separation to obtain aluminum chloride hexahydrate solid and a filtrate;

[0064] Among them, 131.1g of aluminum chloride hexahydrate solid was obtained by one solid-liquid separation, which was dried by vacuum drying at 60 ° C for 8 hours to obtain 117.6g of aluminum chloride hexahydrate product;

[0065] (2) the primary filtrate obtained by step (1) is concentrated and cr...

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Abstract

The invention relates to a treatment method of sodium tetrachloroaluminate solid residues. The treatment method comprises the following steps: (1) mixing sodium tetrachloroaluminate solid residues with water for dissociation, then adding a separating agent to separate out aluminum chloride hexahydrate, or directly mixing the sodium tetrachloroaluminate solid residues with the separating agent fordissociation, separating out aluminum chloride hexahydrate, and then carrying out primary solid-liquid separation to obtain an aluminum chloride hexahydrate solid and primary filtrate; and (2) carrying out concentration crystallization and secondary solid-liquid separation on the primary filtrate to obtain a sodium chloride solid and a secondary filtrate. According to the treatment method, an organic solvent does not need to be introduced, cross contamination does not exist, and the cost can be reduced; the aluminum chloride and the sodium chloride which are obtained by dissociating the sodiumtetrachloroaluminate solid residues are fully recycled, so that the high resource utilization of the sodium tetrachloroaluminate solid residues is realized, the obtained secondary filtrate can be returned to a solid residue dissociation stage to provide a separating agent, the concept of circular economy is embodied, and the method has the advantages of simple process flow, simplicity and convenience in operation and the like.

Description

technical field [0001] The invention relates to the technical field of inorganic chemistry, in particular to a method for treating sodium tetrachloroaluminate solid slag. Background technique [0002] Methylphosphine dichloride is an important organic chemical intermediate, which is widely used in pesticides, medicines, synthetic materials and other fields. At present, the domestic synthetic processes for preparing methyl phosphine dichloride mainly include ternary complex method and alkyl aluminum method. However, no matter what kind of synthesis process, after separating the product methyl phosphine dichloride, a large amount of solid waste will be generated, the main component of which is sodium tetrachloroaluminate, and also contains a small amount of impurities such as organic phosphine. Since sodium tetrachloroaluminate is easily soluble in water, solid waste is often dissolved in water and discharged directly, which will not only cause great pollution to the environm...

Claims

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Application Information

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IPC IPC(8): C01F7/56C01D3/14C01F7/62C07F9/52
CPCC01F7/56C01F7/62C01D3/14C07F9/52C01P2006/80
Inventor 周曙光秦龙余神銮祝小红王萍姜胜宝付萍闫涛涛陆建明董飞
Owner ZHEJIANG XINAN CHEM INDAL GROUP
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