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A kind of stripping equipment and method of supporting molybdenum tfa organic phase

An extraction equipment and organic phase technology, applied in the field of stripping, can solve the problems of emulsification interface, signal lag, easy damage of acid-base balance, etc., achieve the effect of stable reaction state, stable control interface, and saving transition acid consumption

Active Publication Date: 2021-04-13
BEIJING RESEARCH INSTITUTE OF CHEMICAL ENGINEERING AND METALLURGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] 2) The multi-stage countercurrent process is likely to cause emulsification or generate interface dirt
[0008] 3) Cut-off phenomenon often occurs, and the acid-base balance of all levels of operation is easily damaged
[0009] The stripping of molybdenum-containing organic phase is actually an acid-base neutralization reaction, which is the continuous neutralization process of ammonia water in the first stage of the mixing clarifier and acid in the organic phase. The flow ratio of the two is QA / QO≈0.1, and the flow rate of the water phase is Low, when the interface fluctuates, the water phase between the stages is prone to cut-off, the concentration of molybdenum in the first-stage stripping liquid increases, and the acidity increases, and the ammonium molybdate will precipitate and emulsify, making the extraction operation difficult
[0010] 4) The end point of the reaction is not easy to control
Due to the small flow ratio and the large retention fraction of the aqueous phase, when the flow rate of the final stripping agent is adjusted according to the pH of the first stripping liquid, the signal lags seriously, making it difficult to control the end point of the stripping

Method used

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  • A kind of stripping equipment and method of supporting molybdenum tfa organic phase
  • A kind of stripping equipment and method of supporting molybdenum tfa organic phase
  • A kind of stripping equipment and method of supporting molybdenum tfa organic phase

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Effect test

example 1

[0074] The side length of the mixing chamber is 400mm, the side ratio of the mixing chamber and the clarification chamber is 1:3, 4-stage (n1=4) back extraction, 2-stage (n2=2) countercurrent washing. Molybdenum-containing tri-fatty amine (7.5% TFA+15% TBP) kerosene solution, molybdenum concentration 10.0g / L, organic phase flow rate is 10L / min, is added from the mixing chamber in the first stage of stripping, lotion flow rate is 1L / min, from the washing The final mixing chamber joins. Add ammonia from the pre-mixing chamber, adjust the amount of ammonia added to control pH1=10; adjust the reflux adjustment device to control the contact ratio in the mixing chamber; adjust the interface control device to control the stability of the interface; adjust the speed of the stirring paddle to control the appropriate stirring intensity . The reaction temperature was 25°C. The stripping solution with a molybdenum concentration of 100g / L can be obtained; the molybdenum concentration of ...

example 2

[0076] The side length of the mixing chamber is 500mm, the side ratio of the mixing chamber and the clarification chamber is 1:2, 4-stage (n1=3) back extraction, 3-stage (n2=3) countercurrent washing. Molybdenum-containing tri-fatty amine (7.5% TFA+15% TBP) kerosene solution, molybdenum concentration 10.0g / L, organic phase flow rate is 20L / min, add from the mixing chamber in the first stage of stripping, lotion flow rate is 1L / min, from the washing The final mixing chamber joins. The concentrated ammonia water is added from the pre-mixing chamber, the flow rate of the concentrated ammonia water is approximately 1L / min, and the amount of concentrated ammonia water added is fine-tuned to control pH1=10.5; the reflux adjustment device is adjusted to control the contact ratio in the mixing chamber; the interface control device is adjusted to control the stability of the interface; Adjust the speed of the stirring paddle to control the proper stirring intensity. The reaction tempe...

example 3

[0078]The side length of the mixing chamber is 400mm, the side ratio of the mixing chamber and the clarification chamber is 1:3, 4-stage (n1=4) back extraction, 4-stage (n2=4) countercurrent washing. Molybdenum-containing tri-fatty amine (7.5% TFA+15% TBP) kerosene solution, molybdenum concentration 10.0g / L, organic phase flow rate is 13L / min, is added from the mixing chamber in the first stage of stripping, lotion flow rate is 1L / min, from the washing The final mixing chamber joins. Add ammonia gas from the pre-mixing chamber, adjust the amount of ammonia added to control pH1=10.8; adjust the reflux adjustment device, control the contact ratio in the mixing chamber; adjust the interface control device, control the stability of the interface; adjust the speed of the stirring paddle, and control the appropriate stirring intensity . The reaction temperature was 25°C. The stripping solution with a molybdenum concentration of 130g / L can be obtained; the molybdenum concentration ...

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Abstract

The present invention relates to a stripping equipment and method for carrying molybdenum TFA organic phase. The equipment includes a stripping section and a washing section; ..., first stage n1 section mixing chamber, section partition plate, mixed phase outlet, stripping clarification chamber, stripping solution outlet, ultra-stable interface control device I, pre-mixing chamber, reflux regulating chamber, reflux regulating device, reflux pipe, Aqueous phase channel I and stirring paddle. The method comprises the following steps: the first step, the loaded organic phase is continuously pumped into the first-stage mixing chamber; the second step, the mixed phase enters the back extraction clarification chamber through the mixed phase outlet, and the back extraction clarification In the third step, the organic phase in the back extraction clarification chamber enters into the primary washing mixing chamber through the organic phase channel I. In the present invention, the concentration of molybdenum in the stripping solution can be increased from 100g / L to ~180g / L; the entrainment of the lean organic phase reduces the loss of the stripping agent from 30% to less than 1%.

Description

technical field [0001] The invention belongs to the field of stripping, and in particular relates to stripping equipment and a method for carrying molybdenum TFA organic phase. Background technique [0002] In the current process of extracting molybdenum by TFA, the process of preparing ammonium molybdate crystals from the molybdenum-containing organic phase uses ammonia as the stripping agent, and the mixed solution of ammonium molybdate and ammonia is obtained through 4 or more stages of countercurrent stripping. and the poor organic phase, after purification and removal of impurities and sulfuric acid neutralization, control the pH ≈ 2, and precipitate ammonium molybdate crystals. After solid-liquid separation, the crystals and mother liquor are obtained. The crystals are ammonium molybdate products. The mother liquor and the lean organic phase are respectively Return to extract for reuse. [0003] The existing molybdenum stripping process equipment has the following pro...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C22B3/02C22B3/32C22B34/34
CPCC22B3/02C22B34/34C22B3/32Y02P10/20
Inventor 周志全张永明支梅峰赵凤岐舒祖骏牛玉清
Owner BEIJING RESEARCH INSTITUTE OF CHEMICAL ENGINEERING AND METALLURGY