A kind of synthetic method of chloromethyl polystyrene resin

A technology of chloromethyl polystyrene and polystyrene resin, which is applied in the synthesis field of chloromethyl polystyrene resin, can solve the problems of health hazards for operators, unsuitable for long-term large-scale use, high toxicity, etc., and achieves environmental friendliness. , the effect of less toxicity and less toxic by-products

Inactive Publication Date: 2017-11-10
HUNAN NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the prior art, chloromethyl ether is often used to chloromethylate polystyrene resins. Chloromethyl ether is highly toxic and is likely to cause health hazards to operators, so it is not suitable for long-term large-scale use.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Weigh the specific surface area as 75m 2 / g of polystyrene resin 26.5g; take 100g of methylal and 14g of concentrated hydrochloric acid, mix and heat distillation, and move the 60-105°C fraction to a three-necked reaction flask; place the three-necked reaction flask in an ice bath environment, and control the temperature to low At 15°C, add 38g of paraformaldehyde, 14g of concentrated hydrochloric acid with a mass fraction of ≥36% and 34.5g of concentrated sulfuric acid with a mass fraction of ≥98% into a three-necked reaction flask, stir and mix evenly; weigh the specific surface area of ​​75m 2 / g polystyrene resin 26.5g was added into a three-necked reaction flask, and left to swell for 1h. Within half an hour, anhydrous ferric chloride with a total mass of 8.33 g was added three times, stirred and dissolved completely. Heat to 40°C, drop 100g of chlorosulfonic acid at a rate of one drop every 3 seconds with a dropping funnel, and then keep it at 40°C for 48h to obt...

Embodiment 2

[0023] Weigh the surface area as 250m 2 26.5 g of polystyrene resin per g; take 79.5 g of methylal and 8.0 g of concentrated hydrochloric acid, mix and heat to distill, and move the fraction at 60-105°C to a three-necked reaction flask. Place the three-necked reaction bottle in an ice bath environment, control the temperature below 15°C, add 16.0g of paraformaldehyde, 8.0g of concentrated hydrochloric acid with a mass fraction of ≥36% and 16.0g of concentrated sulfuric acid with a mass fraction of ≥98% into the three-necked reaction bottle, stir to combine. The specific surface area to be weighed is 250m 2 26.5 g of polystyrene resin per g was added to the reaction flask, and left to swell for 1.5 h. Then within 10 minutes, anhydrous zinc chloride with a total mass of 5.3 g was added in three times on average, and stirred to dissolve completely. Then it was heated to 30°C, and 80.0 g of sulfone dichloride was added dropwise at a rate of one drop every 2 seconds with a dropp...

Embodiment 3

[0025] Weigh the specific surface area as 350m 2 / g of polystyrene resin 26.5g; take 132.5g of methylal and 35.0g of concentrated hydrochloric acid, mix and heat to distill, and move the fraction at 60-105°C to a three-necked reaction flask. Place the three-necked reaction bottle in an ice bath environment, control the temperature below 15°C, then add 66.0g of paraformaldehyde, 35.0g of concentrated hydrochloric acid with a mass fraction of ≥36% and 50.0g of concentrated sulfuric acid with a mass fraction of ≥98% into the three-necked reaction bottle In the reaction bottle, stir to mix well. The specific surface area to be weighed is 350m 2 / g polystyrene resin 26.5g was added into a three-necked reaction flask, and left to swell for 1.5h. Within 10 minutes, add anhydrous aluminum chloride with a total mass of 5.8 g three times, and stir to dissolve completely. Then it was heated to 35°C, and 125.5g of sulfone dichloride was added dropwise at a rate of one drop every 3 seco...

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Abstract

A synthesis method of chloromethyl polystyrene resin comprises the following steps of mixing methylal and concentrated hydrochloric acid, heating for distillation, receiving 60-105 DEG C fraction, adding trioxymethylene or paraformaldehyde in the received 60-105 DEG C fraction, adding concentrated hydrochloric acid and concentrated sulfuric acid, uniformly stirring and mixing, adding polystyrene resin, standing for swelling for 45-90min, adding a catalyst after the swelling, dropwise adding chlorosulfonic acid or sulfone dichloride, holding 30-60 DEG C for reaction for 12-96h, and obtaining the chloromethyl polystyrene resin. The method has the simple steps, the synthesized chloromethyl polystyrene resin is stable in structure, and a chlorine content of the resin can reach above 17%. Compared with the traditional chloromethylation method, a reaction raw material is low in toxicity, fewer toxic byproducts are generated in a reaction process, injuries to production and experiment personnel are reduced, and the method is friendlier to an environment at the same time.

Description

technical field [0001] The invention relates to a synthesis method of chloromethyl polystyrene resin. Background technique [0002] Chloromethylated polystyrene resin is the precursor or intermediate of many functional polymer microspheres, that is, it can be used as the parent polymer to react with macromolecules to obtain polymer compounds with various functions. For example, using chloromethylated polystyrene resin as a raw material, ion exchange resins, chelating resins, and adsorption resins with special functional groups can be synthesized, which is of great significance in the chemical field. Not only can ion exchange resins, chelating resins and macroporous adsorption resins be prepared through further cross-linking reactions; at the same time, catalyst supports can be synthesized for use in organic synthesis and combinatorial chemical systems; they can also be used for immobilization of biological functional polymers, Separation and purification. However, in the p...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F12/08C08F8/24
Inventor 黄小贝钟广明宋青霞黄雅丹曹伟钟世华徐满才
Owner HUNAN NORMAL UNIVERSITY
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