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Method for reducing content of iron ions in orthophosphorous acid

A technology of iron ions and phosphorous acid, applied in the chemical field, can solve the problems of difficult treatment of regenerated liquid, high production cost, large environmental pollution, etc., and achieve the effects of simple operation, scientific principle and low cost.

Inactive Publication Date: 2014-08-20
JIANGSU DAMING TECH
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The ion exchange method has the problem of regeneration of the ion exchange resin. It is difficult to deal with the regeneration solution with strong acid to regenerate the resin, which causes great environmental pollution. The solvent extraction method generally uses n-butanol as the extraction agent. Although the solvent can be recycled, it requires phosphorous acid solution The concentration is between 15% and 30%, and the amount of solvent used is very large. In one cycle, the yield of phosphorous acid is very low, and the production cost is relatively high.

Method used

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  • Method for reducing content of iron ions in orthophosphorous acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] 1000kg of phosphorous acid mother liquor with an iron ion content of 200ppm is dropped into the reactor, and the stirring is started. In the jacket of the reactor, icy brine is introduced to control the material temperature in the kettle to be 20° C., 2 kg of activated carbon is added, and then sodium formamate solution is slowly added dropwise ( 40% mass percent concentration) 3kg, the control reaction temperature is 20~22 ℃, dropwise completes heat preservation reaction for 30 minutes, then pressure filtration, the filtrate is transferred to the concentrated kettle and distilled under reduced pressure to 120 ℃ under the vacuum degree of -0.095MPa, Then transfer to the crystallization kettle for cooling and crystallization, and finally transfer to the centrifugal kettle to obtain 815kg of phosphorous acid finished product. The detected phosphorous acid content is 99.24%, and the iron ion content is 16ppm.

Embodiment 2

[0024] 1000kg of phosphorous acid mother liquor with an iron ion content of 800ppm is dropped into the reactor, and the stirring is started. In the jacket of the reactor, icy brine is introduced to control the temperature of the material in the kettle to be 10° C., 2 kg of activated carbon is added, and then sodium formamate solution is slowly added dropwise ( 40% mass percentage concentration) 8kg, the control reaction temperature is 10~12 ℃, dropwise completes heat preservation reaction for 30 minutes, then pressure filtration, the filtrate is transferred to the concentration kettle and distilled under reduced pressure to 120 ℃ under -0.095MPa vacuum degree, Then transfer to the crystallization kettle for cooling and crystallization, and finally transfer to the centrifugal kettle to obtain 800kg of phosphorous acid finished product. The detected phosphorous acid content is 98.58%, and the iron ion content is 42ppm.

Embodiment 3

[0026] 500kg of phosphorous acid mother liquor with an iron ion content of 300ppm is dropped into the reactor, and the stirring is started. In the jacket of the reactor, icy brine is introduced to control the temperature of the material in the kettle to be 5° C., 2 kg of activated carbon is added, and then sodium formamate solution is slowly added dropwise ( 40% mass percentage concentration) 7kg, control the reaction temperature to be 5~7 ℃, dropwise complete the insulation reaction for 30 minutes, then press filter, transfer the filtrate to the concentration kettle and distill under reduced pressure to 120 ℃ under the vacuum degree of -0.095MPa, Then transfer to the crystallization kettle for cooling and crystallization, and finally transfer to the centrifugal kettle to obtain 435kg of phosphorous acid finished product. The detected phosphorous acid content is 99.10%, and the iron ion content is 21ppm.

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Abstract

The invention discloses a method for reducing the content of iron ions in orthophosphorous acid. An iron-containing orthophosphorous acid mother liquor reacts with a sodium dimethyldithiocarbamate solution to reduce the content of iron ions in order to obtain highly pure orthophosphorous acid. The method has the advantages of scientific principle, safe and environmentally friendly process, simple operation, high purity of the obtained orthophosphorous acid, and low cost of reaction raw materials.

Description

technical field [0001] The invention belongs to the field of chemical industry, and in particular relates to a method for reducing the content of iron ions in phosphorous acid. Background technique [0002] Phosphorous acid is a dibasic acid with reducing properties. It is used as a raw material for the manufacture of phosphite, pesticide intermediates, and organic phosphorus water treatment agents. It is also used as a plastic stabilizer or antioxidant. At present, the production methods of phosphorous acid mainly include phosphorus trichloride hydrolysis method and dimethyl phosphite residue hydrolysis method. Iron ions will inevitably be brought into the production process or raw materials, and the level of iron ion content will directly affect downstream products. The quality even limits the application in downstream products. Therefore, it is of great practical significance to study the reduction of iron ion content in phosphorous acid and improve product quality. [...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/163
Inventor 潘小明嵇颖耀仇国才
Owner JIANGSU DAMING TECH
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