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A kind of preparation method of chlorine absorbing agent, chlorine absorbing agent and application thereof

A chlorine absorbing agent and a technology for chlorine absorbing agent are applied in the preparation of chlorine absorbing agent, chlorine absorbing agent and its application fields, which can solve the problems of high energy consumption of phosgene, incomplete separation, unfavorable chlorine removal and the like, and achieve a large processing capacity , the effect of simple production process

Active Publication Date: 2022-04-19
WANHUA CHEMICAL (NINGBO) CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In the prior art, the activated carbon protection reactor filled with activated carbon is used to detect whether chlorine is contained in phosgene, and carbon monoxide and chlorine are further reacted; the separation of chlorine and phosgene by rectification towers requires high energy consumption and incomplete separation; the increase of CO The molar excess ratio can reduce the chlorine content in phosgene, but it will increase the energy consumption of CO separation, and CO is a non-condensable gas, which will increase the safety risk; the use of water-containing chlorine absorbent will make the phosgene contain water, and the application of phosgene It affects the production of isocyanate; the use of powdered chlorine absorbing agent is not conducive to the removal of chlorine in phosgene in industry, and may cause chlorine absorbing agent to be entrained in phosgene

Method used

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  • A kind of preparation method of chlorine absorbing agent, chlorine absorbing agent and application thereof
  • A kind of preparation method of chlorine absorbing agent, chlorine absorbing agent and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] (1) Prepare a reaction solution with zinc nitrate, 2-methylimidazole, and methanol at a molar ratio of 1:4:300, and stir until clear. Alumina ceramic balls with a diameter of 8mm and an average pore diameter of 100nm were selected and added to a polytetrafluoroethylene-lined reactor as a carrier. The volume ratio of the alumina ceramic balls to the reaction solution was 1:20. Slowly add the reaction solution into the above reactor, and add 0.10%wt ZIF-8 seed crystals into the reactor, then seal the reactor and maintain crystallization at 100°C for 2 hours, cool naturally to room temperature, and take out the alumina in the reactor The ceramic ball carrier was soaked in methanol for 24 hours, then taken out and dried under vacuum at 40°C.

[0058] (2) Place the alumina ceramic ball with the ZIF-8 crystal film on the surface in the ammonia solution of 0.005mol / L copper nitrate with a volume ratio of 1:2 (that is, the volume of the ammonia solution of copper nitrate is tha...

Embodiment 2

[0060] (1) Prepare a reaction solution with zinc chloride, 2-methylimidazole, and DMF at a molar ratio of 1:8:300, and stir until clear. Alumina ceramic balls with a diameter of 4 mm and an average pore diameter of 300 nm were selected and added to a polytetrafluoroethylene-lined reactor as a carrier. The volume ratio of the alumina ceramic balls to the reaction solution was 1:10. Slowly add the reaction solution into the above reactor, and add 0.10%wt ZIF-8 seed crystals into the reactor, then seal the reactor and maintain crystallization at 100°C for 2 hours, cool naturally to room temperature, and take out the alumina in the reactor The ceramic ball carrier was soaked in methanol for 24 hours, then taken out and dried under vacuum at 40°C.

[0061] (2) Place the alumina ceramic ball with the ZIF-8 crystal film on the surface in a 0.015mol / L copper chloride ammonia solution with a volume ratio of 1:4, maintain 30°C and immerse for 4 hours, remove the immersion solution, and ...

Embodiment 3

[0063] (1) Prepare a reaction solution with zinc acetate, 2-methylimidazole, and methanol at a molar ratio of 1:4:200, and stir until clear. Alumina ceramic balls with a diameter of 6mm and an average pore diameter of 100nm were selected and added to a polytetrafluoroethylene-lined reactor as a carrier. The volume ratio of the alumina ceramic balls to the reaction solution was 1:15. Slowly add the reaction solution into the above reactor, and add 0.10%wt ZIF-8 seed crystals into the reactor, then seal the reactor and maintain crystallization at 100°C for 2 hours, cool naturally to room temperature, and take out the alumina in the reactor The ceramic ball carrier was soaked in methanol for 24 hours, then taken out and dried under vacuum at 40°C.

[0064] (2) Place the alumina ceramic ball with the ZIF-8 crystal film on the surface in an ammonia solution of 0.01mol / L basic copper carbonate with a volume ratio of 1:3, maintain 70°C for 1 hour, and remove the immersion solution. ...

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Abstract

The invention relates to a preparation method of a chlorine absorbing agent, comprising: 1) using an alumina ceramic ball as a carrier, reacting an inorganic salt of zinc and 2-methylimidazole in a solvent to form ZIF-8 on the surface of the alumina ceramic ball crystalline film to obtain spherical ZIF-8 / alumina ceramic ball particles; 2) the spherical ZIF-8 / alumina ceramic ball particles obtained in step 1) are impregnated in the inorganic salt ammonia solution of copper, and then separated, washed, Dry and roast to obtain the chlorine absorbing agent of the present invention. Through the method of physical adsorption and chemical adsorption, the raw material phosgene is refined with a chlorine absorbing agent, thereby reducing the chlorine gas in the phosgene to less than 500ppm, and the refined phosgene is used in the production of isocyanate, which can reduce the crude isocyanate product. The color appearance brings a certain improvement effect.

Description

technical field [0001] The invention relates to a preparation method of a chlorine absorbing agent, a chlorine absorbing agent and an application thereof. Background technique [0002] Phosgene is mainly used in the fields of organic synthesis, pesticides, drugs, dyes and intermediates of other chemical products. Phosgene reacts with amines to synthesize isocyanates, such as toluene diisocyanate (TDI), 4,4'-diphenylmethane diisocyanate (MDI), hexamethylene diisocyanate (HDI), isophorone diisocyanate ( IPDI) etc. At present, isocyanates are mainly prepared by the phosgene method. The corresponding amines such as diphenylmethanediamine and polymethylene polyphenylpolyamine are mixed with an inert solvent and then fully mixed with phosgene for phosgenation reaction to obtain A photochemical reaction solution, the photochemical reaction solution is subjected to phosgene removal and solvent removal to obtain crude isocyanate. Chlorine in phosgene will cause the reaction to pro...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/08B01J20/30B01D53/02C01B32/80
CPCB01J20/08B01J20/06C01B32/80B01D53/02B01J2220/4812B01J2220/4806B01D2257/2025B01D2257/2045B01D2256/26B01D2253/1124
Inventor 周宇杰赵东科董超李超群文放张宏科王文博李翀王强强
Owner WANHUA CHEMICAL (NINGBO) CO LTD
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