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Method for recovering diantimony trioxide from monochlorodifluoromethane reaction residual liquid

A technology of difluorochloromethane and antimony trioxide, which is applied in the field of recovery of antimony trioxide, can solve the problems of difficult mother liquor treatment, high consumption of sodium hydroxide, and unfavorable stable operation of equipment, and achieves low cost and no alkali consumption Liquid, easy-to-control effects

Inactive Publication Date: 2020-03-24
江苏梅兰化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage is that the consumption of hydrochloric acid used in the extraction step and sodium hydroxide used in the neutralization step is very high, and there are unhydrolyzed antimony ions in the large amount of hydrolyzed mother liquor after the antimony oxide solid is separated, which makes it difficult to treat the mother liquor, which is not conducive to the long-term operation of the device. run smoothly

Method used

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Examples

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Embodiment 1

[0009] Embodiment 1, the present invention discloses a method for recovering antimony trioxide from the reaction raffinate of chlorodifluoromethane, which comprises the following steps: step 1, extraction, reacting 300 mL of chlorodifluoromethane with an extractant The waste antimony pentachloride in the raffinate is slowly added to 900mL in the hydrolysis kettle for extraction, and the feeding speed of process water during extraction is 1m 3 / h, the extraction agent is process water during extraction, the weight ratio of difluorochloromethane reaction residue to process water is controlled at 1:3, and stirring is started during the hydrolysis process, and the stirring is turned off after the mixed liquid is cooled to room temperature and left to stand for 0.5 After 1 hour, separate with a separatory funnel, and wash the organic phase with the inorganic phase solution three times to obtain an aqueous solution containing antimony ions, and then use a flow rate of 100 L / min nitro...

Embodiment 2

[0013] Embodiment 2, the present invention discloses a method for recovering antimony trioxide from the reaction raffinate of chlorodifluoromethane, which comprises the following steps: step 1, extraction, reacting 300 mL of chlorodifluoromethane with an extractant The waste antimony pentachloride in the raffinate is slowly added to 1500mL in the hydrolysis kettle for extraction, and the feeding speed of process water during extraction is 2m 3 / h, the extraction agent is process water during extraction, the weight ratio of difluorochloromethane reaction raffinate to process water is controlled at 1:5, and stirring is started during the hydrolysis process, and the stirring is turned off after the mixed liquid is cooled to room temperature and left to stand for 0.5 After 1 hour, separate with a separatory funnel, and wash the organic phase with the inorganic phase solution three times to obtain an aqueous solution containing antimony ions, and then use a flow rate of 100 L / min ni...

Embodiment 3

[0017] Embodiment 3, the present invention discloses a method for recovering antimony trioxide from the reaction raffinate of chlorodifluoromethane, which comprises the following steps: step 1, extraction, reacting 300 mL of chlorodifluoromethane with an extractant The waste antimony pentachloride in the raffinate is slowly added to 1800mL in the hydrolysis kettle for extraction, and the feeding speed of process water during extraction is 0.8m 3 / h, the extraction agent is process water during extraction, the weight ratio of difluorochloromethane reaction residue to process water is controlled at 1:10, and stirring is started during the hydrolysis process, and the stirring is turned off after the mixed liquid is cooled to room temperature and left to stand for 0.5 After 1 hour, separate with a separatory funnel, and wash the organic phase with the inorganic phase solution three times to obtain an aqueous solution containing antimony ions, and then use a flow rate of 100 L / min n...

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Abstract

The invention discloses a method for recovering diantimony trioxide from a monochlorodifluoromethane reaction residual liquid. The method comprises the following steps: 1, extracting: extracting wasteantimony pentachloride in a monochlorodifluoromethane reaction residual liquid in a hydrolysis kettle by using an extracting agent to obtain an antimony ion-containing aqueous solution, carrying outsteam stripping on the antimony ion-containing aqueous solution by using nitrogen with a flow rate of 100 L / min for 6 hours, and absorbing the steam stripping substance by using an alkaline solution;2, reducing: reducing the antimony ion-containing aqueous solution by using a reducing agent to obtain an aqueous solution containing trivalent antimony ions; 3, hydrolyzing: hydrolyzing the aqueous solution containing the trivalent antimony ions by using water to obtain a turbid liquid containing diantimony trioxide solid; and 4, carrying out suction filtration on the hydrolyzed turbid liquid containing the diantimony trioxide solid, and drying to obtain diantimony trioxide with a content of 99.9% and a particle size of more than 400 meshes and a hydrolysis mother liquor.

Description

technical field [0001] The invention relates to a method for recovering antimony trioxide from difluorochloromethane reaction raffinate. Background technique [0002] According to the Montreal Convention, after 2030, F22 needs to be completely phased out except for maintenance and special purposes. However, as the basic raw material for the production of new fluorine-containing materials-tetrafluoroethylene monomer, its demand will still be at a low level in the next few decades. A pretty high level. The process of preparing F22 at home and abroad generally adopts the liquid-phase catalytic fluorination method. The catalyst antimony pentachloride used in this method will be poisoned and invalidated due to the accumulation of impurities in the reaction. , There are also toxic substances such as antimony halides, and the residual liquid is difficult to treat in an environmentally friendly manner, which has become a problem restricting the preparation of catalytic fluorination...

Claims

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Application Information

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IPC IPC(8): C01G30/00
CPCC01G30/001C01G30/005
Inventor 刘子璇王卫国孙政
Owner 江苏梅兰化工有限公司
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