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Reaction system for halogenating ion exchange resins and halogenation method of ion exchange resins

A technology of ion exchange resin and reaction system, applied in chemical instruments and methods, physical/chemical process catalysts, organic compounds/hydrides/coordination complex catalysts, etc., can solve the problem of high toxicity, high price and easy leakage of halogens, etc. problem, to achieve the effect of reducing the sulfonic acid group shedding rate, improving thermal stability, and simple process

Active Publication Date: 2014-08-06
XIAN ORIGIN CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Among the three approaches, the halogenated monomers required by the first method are difficult to obtain and expensive, and are not suitable for large-scale industrial use. The resistance is large, it is difficult for the halogen to attack the ring, and the halogenation effect is not ideal
However, these elemental halogens are highly toxic, especially chlorine gas, which is not only highly toxic, but also has problems such as easy leakage and inconvenient operation.

Method used

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  • Reaction system for halogenating ion exchange resins and halogenation method of ion exchange resins

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Embodiment 1

[0029] The reaction system for the halogenated ion exchange resin of the present embodiment comprises a catalyst and a halogenating reagent, and the catalyst is FeBr 3 The quality of the catalyst is 1% of the quality of the ion-exchange resin to be halogenated; the halogenation reagent includes solution A and solution B, and the solution A is the hydrobromic acid of 6mol / L, and the solution B is a mass concentration of 25 % sodium bromate aqueous solution; the mol ratio of the bromine element in the solution A and the bromine element in the solution B is 2.4: 1; the quality of the solute in the solution B is 37.5% of the ion exchange resin mass to be halogenated.

[0030] The halogenation method of the present embodiment is:

[0031] Step 1. Swell 100g of styrene-based resin white balls with 150mL of dichloroethane at room temperature for 2 hours, filter and bake at 60°C until the surface is dry to obtain a swelled ion exchange resin;

[0032] Step 2, place the ion exchange r...

Embodiment 2

[0036] The reaction system for the halogenated ion exchange resin of the present embodiment includes a catalyst and a halogenation reagent, and the catalyst is CuCl 2 The quality of the catalyst is 0.1% of the mass of the ion-exchange resin to be halogenated; the halogenation reagent includes solution A and solution B, and the solution A is 2mol / L hydrochloric acid, and the solution B is 30% of the mass concentration Potassium chlorate aqueous solution; the molar ratio of the chlorine element in the solution A to the chlorine element in the solution B is 2.7:1; the mass of the solute in the solution B is 18% of the mass of the ion exchange resin to be halogenated.

[0037] The halogenation method of the present embodiment is:

[0038] Step 1. Swell 100g of styrene-based resin white balls with 200mL of carbon tetrachloride at 50°C for 0.5h, filter and bake at 70°C until the surface is dry to obtain a swelled ion exchange resin;

[0039] Step 2, place the ion exchange resin of ...

Embodiment 3

[0043] The reaction system for the halogenated ion exchange resin of the present embodiment includes a catalyst and a halogenating reagent, and the catalyst is CuBr with a mass ratio of 1:1. 2 and FeBr 3The quality of the catalyst is 5% of the ion-exchange resin quality to be halogenated; The halogenation reagent includes solution A and solution B, and the solution A is the hydrobromic acid of 12mol / L, and the solution B is potassium bromate and high The mixed aqueous solution of sodium bromate, wherein the mass concentration of potassium bromate is 10%, and the mass concentration of sodium perbromate is 20%; The mol ratio of the bromine element in the described solution A and the bromine element in the solution B is 3: 1; The mass of the solute in the solution B is 30% of the mass of the ion exchange resin to be halogenated.

[0044] The halogenation method of the present embodiment is:

[0045] Step 1. Swell 100g of styrene-based resin white balls with 180mL of dichloroeth...

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Abstract

The invention discloses a reaction system for halogenating ion exchange resins. The reaction system comprises a catalyst and a halogenating agent, wherein the catalyst is chloride and / or bromide; the mass of the catalyst accounts for 0.1%-5% of the mass of ion exchange resin to be halogenated; the halogenating agent comprises a solution A and a solution B, the solution A is hydrochloric acid of which the concentration is 0.1mol / L-12mol / L and / or hydrobromic acid of which the concentration is 0.1mol / L-12mol / L, the solute of the solution B is one or more hypochlorite, chlorate, perchlorate, hypobromite, bromate and perbromate. Furthermore, the invention also discloses a halogenation method of ion exchange resins. According to the reaction system for halogenating ion exchange resins disclosed by the invention, low-toxic salts and acids are adopted as halogen sources instead of chlorine and bromine with high toxicity, and all materials in the operation are liquid or solid and thus the potential safety hazard of toxic gas leakage is avoided and the reaction system is safer.

Description

technical field [0001] The invention belongs to the technical field of halogenation of ion exchange resins, and in particular relates to a reaction system and a halogenation method for halogenating ion exchange resins. Background technique [0002] Ion exchange resins, especially strong-acid cation exchange resins, are commonly used catalysts in many organic reactions such as etherification, esterification, and alkylation. However, resin catalysts generally have the disadvantage of poor thermal stability. The sulfonic acid group is easy to fall off, resulting in a reduction in catalytic activity. [0003] In order to improve the thermal stability of the resin, a common method is to bond electron-withdrawing groups, such as halogens and nitro groups, to the aromatic rings of the resin. There are generally three ways to introduce halogen into the resin: [0004] (1) Directly polymerize with halogen-containing monomers to prepare resins, as described in British Patent GB13935...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J7/14B01J31/10
Inventor 张睿齐小峰谢小莉王红梅段超潘蕊娟
Owner XIAN ORIGIN CHEM TECH
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