Method for oxidizing yellow phosphorus to remove arsenic

A yellow phosphorus and arsenic removal technology, applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc. Issues such as unsatisfactory production efficiency and safety

Inactive Publication Date: 2020-08-14
贵州新天鑫化工有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For example, Chinese patent 200710065980.3 discloses one or more of hydrogen peroxide, nitric acid and hypochlorous acid as the base oxidant, bromine, bromic acid, bromate, bromide or their mixture as oxidation enhancer, and yellow phosphorus Put them together into a stirring reactor and react at 50-90°C for 1.5-3 hours to remove arsenic. Although the phosphorus yield can reach 99% when the arsenic removal rate is 76.7%, the phosphorus yield is less than 93% when the arsenic removal rate is 98.6%. , can not achieve high arsenic removal rate and high phosphorus yield at the same time, and the reaction time is long
Chinese patent 201310743962.1 discloses that nitric acid solution is used as the basic oxidant, potassium iodide solution is used as the oxidation catalyst, and sodium hypochlorite solution is used as the oxidation enhancer, and the basic oxidant, yellow phosphorus, oxidation catalyst, and oxidation enhancer are sequentially put into the stirred reactor at a certain time interval. agent, the feeding time is more than 2 hours, and the reaction time is 3 hours. After the reaction, the arsenic yellow phosphorus is obtained by washing

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  • Method for oxidizing yellow phosphorus to remove arsenic

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Preparation of oxidant solution: 10wt% H 2 o 2 , 0.1wt% phosphoric acid and 89.9wt% water were uniformly mixed to obtain an oxidizing agent solution;

[0038] Prepare oxidation catalyst solution: mix 1wt% KI and 99wt% water evenly to obtain oxidant catalyst solution;

[0039] The oxidant solution and the oxidation catalyst solution were pre-mixed continuously for 1 s at a flow ratio of 8:1 using a micro-mixer to obtain a mixed fluid; Mix in the element, redox reaction in the micro-packed bed at 70°C for 5 minutes, place the obtained reaction system in a phase separator for phase separation, and obtain the aqueous phase and the crude yellow phosphorus (lower phase), and the crude yellow phosphorus Wash with 3wt% hydrogen peroxide to obtain dearsenic yellow phosphorus; supplement H in the obtained water phase 2 o 2 , phosphoric acid and KI to its initial concentration, to obtain the aqueous phase circulation liquid, and recycle;

[0040] The arsenic content in the aq...

Embodiment 2

[0042] Preparation of oxidant solution: 30wt% H 2 o 2 , 0.1wt% phosphoric acid and 69.9wt% water were uniformly mixed to obtain an oxidizing agent solution;

[0043] Prepare oxidation catalyst solution: mix 2wt% KI and 98wt% water evenly to obtain oxidant catalyst solution;

[0044] The oxidant solution and the oxidation catalyst solution were premixed continuously for 0.1s at a flow ratio of 4:1 by a micro-mixer to obtain a mixed fluid; Mix in a micro-dispersion element, redox reaction in a micro-packed bed at 90°C for 1 min, place the resulting reaction system in a phase separator for phase separation, and obtain an aqueous phase and crude yellow phosphorus (lower phase). The crude phosphorus product is washed with 6wt% hydrogen peroxide to obtain dearsenic yellow phosphorus; the obtained aqueous phase is supplemented with H 2 o 2 , phosphoric acid and KI to its initial concentration, to obtain the aqueous phase circulation liquid, and recycle;

[0045] The arsenic cont...

Embodiment 3

[0047] Preparation of oxidant solution: 30wt% H 2 o 2 , 0.03wt% phosphoric acid and 69.97wt% water were uniformly mixed to obtain an oxidizing agent solution;

[0048] Prepare oxidation catalyst solution: mix 0.5wt% KI and 99.5wt% water uniformly to obtain oxidant catalyst solution;

[0049] The oxidant solution and the oxidation catalyst solution were premixed continuously for 0.5s at a flow ratio of 5:1 by a micro-mixer to obtain a mixed fluid; Mix in the dispersing element, redox reaction in the micro-packed bed at 60°C for 1 min, put the obtained reaction system in a phase separator for phase separation, and obtain the aqueous phase and the crude yellow phosphorus (lower phase), and the yellow phosphorus The crude product is filtered with a 3 μm sand core funnel to obtain the dersensic yellow phosphorus; the obtained aqueous phase is supplemented with H 2 o 2 , phosphoric acid and KI to its initial concentration, to obtain the aqueous phase circulation liquid, and recy...

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Abstract

The invention provides a method for oxidizing yellow phosphorus to remove arsenic, and belongs to the technical field of chemical engineering. The method for oxidizing yellow phosphorus to remove arsenic comprises the following steps of: premixing an oxidant solution and an oxidation catalyst solution by using a mixer, introducing the obtained mixed fluid into a micro-dispersion element to be mixed with a yellow phosphorus raw material, carrying out an oxidation-reduction reaction in a micro-packed bed, and carrying out phase splitting to obtain arsenic-removed yellow phosphorus, wherein the oxidation catalyst solution comprises a potassium iodide solution or a hydrogen iodide solution. Through efficient mixing of the oxidant solution and the oxidation catalyst solution, effective formation of I2 can be ensured, and meanwhile, I2 is prevented from being separated out of the solution; the yellow phosphorus raw material and the mixed fluid keep a huge liquid-liquid phase interface in themicro-dispersion element and the micro-packed bed, shuttling of I2 between a yellow phosphorus phase and a water phase is effectively enhanced, the arsenic removal reaction speed is increased, the high arsenic removal rate and the high phosphorus yield can be achieved at the same time, operation is easy, consumed time is short, and the method is suitable for large-scale production.

Description

technical field [0001] The invention relates to the technical field of chemical industry, in particular to a method for oxidatively removing arsenic from yellow phosphorus. Background technique [0002] Yellow phosphorus is an important basic raw material for the production of fine phosphorus chemical products. Industrial yellow phosphorus contains various impurities such as organic matter, arsenic, sulfur, iron, etc., and its content directly affects the application range of yellow phosphorus. Among them, arsenic and phosphorus belong to the same main group, and their properties are very close. It is easy to enter the product in the production of yellow phosphorus. The content of arsenic in industrial yellow phosphorus can be as high as 300-400ppm. It is difficult to remove and has a great impact on the quality of yellow phosphorus. Moreover, arsenic is a highly toxic element, and its detection amount is subject to very strict restrictions in applications such as food, med...

Claims

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Application Information

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IPC IPC(8): C01B25/047
CPCC01B25/047
Inventor 吕阳成甘立炜王美波
Owner 贵州新天鑫化工有限公司
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