Preparation method of sulfonic acid type aromatic block cation exchange resin

A cation exchange and sulfonic acid type technology, applied in the direction of cation exchange materials, can solve the problems of ion exchange resins that have not been reported, and achieve the effect of increasing the quantity, increasing the free volume, and improving the adsorption capacity

Active Publication Date: 2019-09-27
XI AN JIAOTONG UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the literature and patents on the preparation of ion exchange resins using aromatic block polymers have not been reported.

Method used

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  • Preparation method of sulfonic acid type aromatic block cation exchange resin
  • Preparation method of sulfonic acid type aromatic block cation exchange resin
  • Preparation method of sulfonic acid type aromatic block cation exchange resin

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preparation example Construction

[0026] A kind of preparation method of sulfonic acid type aromatic block type cation exchange resin of the present invention comprises the following steps:

[0027] a. Dissolve the block polymer in chloroform to obtain a polymer solution with a mass fraction of 0.5 to 20 wt%, place the polymer solution in an ice-water bath (<2°C), and then add the mass fraction to the polymer solution 1~25% chloromethylation reagent trimethylchlorosilane or 1,4-dichloromethoxybutane and 0.25~6.25% catalyst anhydrous tin tetrachloride, react in the above ice-water bath for 10~60min After that, move to normal temperature to react for 6-10 hours, then move to normal temperature to react. After the reaction, drop the reaction mixture into the precipitant propanol, isobutanol or acetone to obtain a precipitate; filter the precipitate with a suction filter funnel, Wash the obtained precipitate with 200-400 mL of propanol, and then dry the washed precipitate in an oven at 25-80°C for 12-24 hours to o...

Embodiment 1

[0033] The block polymer used is polystyrene-ethylene / butylene-styrene (SEBS), where R is a combination of one molecule of ethylene and one molecule of 1-butene monomer, m=400, n 1 =n 2 =n=30, n'=6.

[0034] (1) Chloromethylation reaction: 10.0g SEBS was dissolved in 250mL chloroform to obtain a polymer solution with a mass fraction of 2.6wt%, and the polymer solution was sequentially added in an ice-water bath (0°C) with a mass fraction of 9.5 % of trimethylchlorosilane and 3.2% anhydrous tin tetrachloride, reacted for 30 minutes under the above ice-water bath conditions, continued the reaction for 6 hours at room temperature, added a mass fraction of 120% propanol solution to precipitate the polymer, and baked it in an oven at 25°C Dry in medium for 24h to obtain the chloromethylation product SEBS@CH with a chloromethylation rate of 43% 2 Cl, whose structure is shown below:

[0035]

[0036] (2) Grafting polystyrene reaction: 2g chloromethylated block polymer is mixed wi...

Embodiment 2

[0041] Using the raw material SEBS in Example 1, the SEBS-g-PSt polymer solution was prepared according to the chloromethylation reaction and grafted polystyrene reaction in Example 1. Different from Example 1, in the obtained SEBS-g-PSt polymer solution, a mass fraction of 200% styrene was added as a porogen, and then the mixed solution was added dropwise to 400mL propanol solution to precipitate polymer resin The particles were finally dried in an oven at 50° C. for 24 hours to obtain polystyrene-grafted SEBS (SEBS-g-PSt-2) spherical particles after adding porogen. Then carry out sulfonation according to the sulfonation method in Example 1 to obtain the sulfonic acid type cation exchange resin S-SEBS-g-PSt-2 with an ion exchange capacity of 2.18.

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Abstract

The invention discloses a preparation method of a sulfonic acid type aromatic block cation exchange resin. The preparation method comprises following steps: a chloromethylation reagent and a catalyst are added into a block polymer solution, and a precipitating agent is added dropwise so as to obtain a precipitate; after drying, an obtained chloromethylation block polymer and toluene are mixed, styrene, complex triphenyl phosphine, and a catalyst are added successively, stirring dissolving is carried out, nitrogen is introduced under vacuum conditions, heating is carried out, ascorbic acid is added, styrene is added, an obtained product is subjected to precipitation, filtering, washing, and drying so as to obtain a grafted product; concentrated sulfuric acid, acetic anhydride, and 1, 2-dichloroethane are mixed so as to obtain a sulfonating agent solution, reaction is carried out in ice-water bath, the grafted product is added, reaction, filtering, deionized water washing, and drying are carried out so as to obtain the sulfonic acid type aromatic block cation exchange resin. In processing of heavy metal ion containing waste liquid, the advantages are that: many adsorption sites are achieved, adsorption capacity is large, regeneration can be realized, no pollution is caused, solvent resistance is excellent, mechanical strength is high, wear resistance is high, and excellent practical using capacity is achieved.

Description

technical field [0001] The invention belongs to the technical field of ion exchange resins, and in particular relates to a preparation method and application of a sulfonic acid type cation exchange resin. Background technique [0002] Industrial pollution has caused serious excess of heavy metal ions in surface water, which has brought great harm to the environment and human health. The traditional chemical precipitation process used to treat sewage containing heavy metal ions produces a large amount of heavy metal sludge and is not suitable for occasions with low metal ion content. Ion exchange is an efficient, economical, and environmentally friendly treatment method for heavy metals. It can not only effectively remove heavy metal ions, but also realize the recycling of heavy metals through the regeneration of ion exchange materials. The key to the adsorption of heavy metal ions by the ion exchange method lies in the performance of the ion exchange material itself. [00...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F287/00C08F212/08C08F8/36C08F8/24C08J9/28B01J39/20
CPCB01J39/20C08F8/24C08F8/36C08F287/00C08J9/28C08J2351/00C08F212/08
Inventor 李娜曾飞祥王子恒
Owner XI AN JIAOTONG UNIV
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