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Preparation method of chloromethyl styrene resin

A technology of chloromethyl styrene and polystyrene resin, which is applied in the field of preparation of chloromethyl styrene resin, can solve the problems of high production cost, and achieve the effect of low production cost and reduced production cost

Inactive Publication Date: 2014-04-09
SHANGHAI INST OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The purpose of the present invention is in order to solve above-mentioned long-chain alkyl chloromethyl ether method, the production cost is higher in the reaction preparation chloromethyl styrene resin process of the long-chain chloromethyl ether that is made with butanediol and styrene resin The problem is to provide a method of making long-chain chloromethyl ether by using non-cyclic long-chain diols, and then chloromethylating polystyrene resin to prepare chloromethyl styrene resin.

Method used

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  • Preparation method of chloromethyl styrene resin

Examples

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Embodiment 1

[0034] A preparation method of chloromethyl styrene resin, specifically comprising the following steps:

[0035] (1) Add 20g of paraformaldehyde, 190g of solvent 1 and 30g of dihydric alcohol into the reaction vessel in sequence, react for 12 hours in the presence of dry hydrogen chloride gas, and then carry out vacuum distillation under the condition that the pressure is lower than 5 mmHg Purify to obtain 31g of long-chain chloromethyl ethers containing two chloromethyl groups, with a yield of 57%;

[0036] The solvent 1 is ethylene dichloride;

[0037] Described dihydric alcohol is 1,6-hexanediol;

[0038] (2), take 15g of long-chain chloromethyl ether obtained in step (1), add 20g of dry macroporous polystyrene resin balls, 35g of solvent 2, and 2.4g of catalyst, and carry out chloromethylation reaction at room temperature under stirring conditions 14h, the catalyst was added in three times, that is, 0.8g was added every 4.5h. After the reaction, the reaction solution was...

Embodiment 2

[0048] A preparation method of chloromethyl styrene resin, specifically comprising the following steps:

[0049] (1) Add 20g of paraformaldehyde, 200g of solvent 1 and 27g of diol into the reaction vessel in sequence, react for 6 hours in the presence of dry hydrogen chloride gas, and then carry out vacuum distillation under the condition that the pressure is lower than 5 mmHg Purify, obtain 27g long-chain chloromethyl ether, productive rate 51%;

[0050] The solvent 1 is dichloromethane;

[0051] Described dihydric alcohol is 1,6-hexanediol;

[0052] (2) Take 10g of long-chain chloromethyl ether prepared in step (1), add 5g of dry gel polystyrene resin balls, 54g of solvent 2, and 1.8g of catalyst, and stir at room temperature for chloromethylation reaction for 12h After the reaction, the reaction solution is filtered with a sand core funnel to remove the solvent (including solvent 1 and solvent 2), glycol and unreacted long-chain chloromethyl ether to obtain resin balls;

...

Embodiment 3

[0061] A preparation method of chloromethyl styrene resin, specifically comprising the following steps:

[0062] (1) Add 20g of paraformaldehyde, 300g of solvent 1, 30g of dihydric alcohol and 110g of p-toluenesulfonyl chloride into the reaction vessel in sequence, stir and react for 24 hours, and then carry out vacuum distillation and purification under the condition that the pressure is controlled below 5 mmHg , obtain 24g long-chain chloromethyl ether, productive rate 47%;

[0063] The solvent 1 is ethylene dichloride;

[0064] The dihydric alcohol is 1,8-octanediol;

[0065] (2) Take 15g of the long-chain chloromethyl ether prepared in step (1), add 10g of dry macroporous polystyrene resin balls, 40ml of solvent 2, and 2.4g of catalyst, and carry out the chloromethylation reaction under ultrasonic conditions at room temperature for 8 hours , the catalyst was added in three times, adding 0.8g every 2h. After the reaction, the reaction solution was filtered with a sand cor...

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Abstract

The invention discloses a preparation method of chloromethyl styrene resin. The preparation method is as follows: first reacting a long chain diol with trioxymethylene in the presence of dry hydrogen chloride, thionyl chloride or benzene sulfonyl chloride for preparing long chain chloromethyl ether; performing chloromethylation reaction of the obtained long chain chloromethyl ether and styrene resin in conditions of aluminum chloride, stannous chloride, concentrated sulfuric acid or titanium tetrachloride catalysis, filtering an obtained reaction liquid to obtain resin balls, and washing with a mixed solution to remove a surface catalyst to obtain the chloromethyl polystyrene resin. The preparation method of the chloromethyl styrene resin has the advantages of environmental protection and no pollution, at the same time, the used long chain diol also can be recycled, so that the preparation method has the characteristic of low production cost.

Description

[0001] technical field [0002] The present invention relates to a kind of preparation method of chloromethyl styrene resin, specifically is to utilize the dibasic long-chain chloromethyl ether prepared by long-chain dihydric alcohol to replace methyl chloromethyl ether, carry out the chloromethyl ether of polystyrene resin and these binary long-chain chloromethyl ethers will not be cyclized during the reaction, and will regenerate long-chain dibasic alcohols during the chloromethyl reaction. technical background [0003] Chloromethyl styrene resin is an important intermediate in the preparation of reactive polymers, and is widely used in the preparation of ion exchange resins, adsorption resins, polymer reagents, catalyst carriers and other fields. It used to be prepared by chloromethylation of methyl chloromethyl ether (referred to as chloromethyl ether) with polystyrene resin. In the 1970s, chloromethyl ether was found to be a strong carcinogenic compound (lung cancer), ...

Claims

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Application Information

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IPC IPC(8): C08F12/08C08F8/24
Inventor 李永胜金谊王永光高志男吕燕雯
Owner SHANGHAI INST OF TECH
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