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Preparation method of secondary cross-linked resin adsorbent and secondary cross-linked resin adsorbent

A technology of secondary cross-linking and resin adsorption, applied in chemical instruments and methods, other chemical processes, alkali metal compounds, etc., can solve the problem that the secondary cross-linking method is not very thorough, the safety hazards are difficult to avoid residues, and the synthesis process is complicated. and other problems, to achieve the effect of good industrial application prospects, improved amphiphilicity, and simple synthesis process steps

Active Publication Date: 2020-12-04
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For the suspension double bond method, the cost of divinylbenzene (DVB) which is one of the raw materials is relatively high, and the residual double bond secondary crosslinking method often cannot be very thorough; Methyl ether belongs to a class of carcinogens, which are highly volatile and highly toxic. There are safety hazards in the preparation process and it is difficult to avoid residues. Moreover, its synthesis process is relatively complicated and there are many by-products, which limit its application.

Method used

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  • Preparation method of secondary cross-linked resin adsorbent and secondary cross-linked resin adsorbent
  • Preparation method of secondary cross-linked resin adsorbent and secondary cross-linked resin adsorbent
  • Preparation method of secondary cross-linked resin adsorbent and secondary cross-linked resin adsorbent

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preparation example Construction

[0028] The preparation method of the secondary cross-linked resin adsorbent of the present invention, the synthesis process is as follows figure 1 As shown, after the monovinylbenzene suspension polymer beads are fully swollen in an organic solvent, under the action of a catalyst, they undergo a ring-opening addition reaction with an epoxide to introduce alcoholic hydroxyl groups or A "phenyl alkyl alcohol-catalyst" intermediate is generated, and the alcohol hydroxyl group or "alkyl alcohol-catalyst" will continue to undergo secondary cross-linking reaction with adjacent benzene rings to obtain a secondary cross-linked resin adsorbent. Wherein, adjacent refers to the adjacent or similar spatial position relationship, such as the front, back, left and right, up and down positions of the alcoholic hydroxyl group in three-dimensional space, as long as there are benzene rings in these positions, the alcoholic hydroxyl group will continue to cross-link with the benzene ring. The fi...

Embodiment 1

[0042] Add the premixed water phase into a 1L four-necked flask, and the composition of the water phase includes: 500 g of deionized water, 1 g of polyvinyl alcohol, and 20 g of sodium chloride. Stirring was started at room temperature, and the stirring speed was 100 rpm, so that the polyvinyl alcohol and sodium chloride were completely dissolved. Turn off the stirring and add the premixed oil phase. The composition of the oil phase includes: styrene 80g, methylstyrene 17g, divinylbenzene 3g, toluene 50g, 3# white oil 50g, azobisisobutyronitrile 0.3, peroxide Dibenzoyl 0.4g. Turn on the stirring to carry out the suspension polymerization reaction, the stirring speed is 120rpm, first raise the temperature to 65°C, react for 5h, then raise the temperature to 80°C and mature for 3h, to obtain the white balls of polymer beads. After the reaction is completed, the white balls of the polymer beads are filtered, washed with water, and washed with ethanol to become the precursor of t...

Embodiment 2

[0046] Add 75g of 1,2-dichloroethane and 10g of white polymer beads into a 500ml three-neck flask respectively, and let stand at room temperature to swell for 4h. After that, under mechanical stirring, add epichlorohydrin and anhydrous ferric chloride according to the ratio of (white ball: epichlorohydrin: anhydrous ferric chloride is 10:3:3 (weight ratio)), and control the stirring speed at room temperature 150rpm, react for 10 hours, then raise the temperature to 80°C and react for 10 hours. After the reaction was completed, when the temperature dropped to room temperature, the mother liquor was filtered out, stirred and washed with 60 g of acetone-hydrochloric acid solution at 130 rpm for 2 hours, then stirred and washed with 20 g of acetone for 3 times each time, and vacuum-dried at 60°C to constant weight to obtain a post-crosslinked resin Adsorbent. Polymer bead white ball raw material is the same as in Example 1, and the BET specific surface area of ​​the secondary cro...

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Abstract

The invention discloses a preparation method of a secondary cross-linked resin adsorbent with a high specific surface area and high strength, which takes monovinylbenzene suspension polymer beads as areaction precursor, and comprises the following steps: after fully swelling the polymer beads in an organic solvent, carrying out ring-opening addition reaction on the polymer beads and epoxide underthe action of a catalyst to obtain the secondary cross-linked resin adsorbent with high specific surface area and high strength, introducing a functional group to a benzene ring of the polymer bead body, and continuously carrying out secondary crosslinking reaction on the functional group and the adjacent benzene ring to obtain the secondary crosslinking resin adsorbent. The invention provides anovel secondary cross-linking method except for traditional secondary cross-linking of chloromethylated beads and secondary cross-linking of residual double bonds. The method has the advantages of accessible raw materials, simple synthesis technique and low cost, is environment-friendly, and is suitable for industrial production.

Description

technical field [0001] The invention relates to the technical field of polymer separation and purification materials, in particular to a preparation method of a secondary crosslinked polystyrene resin adsorbent. Background technique [0002] Porous polymer adsorbent—polystyrene resin adsorbent is more and more widely used in the separation and purification of target molecules in many fields such as biomedicine, natural product extraction, food cosmetics, chromatographic packing, and wastewater treatment. . The continuous expansion of application fields has also put forward higher requirements for resin adsorbents. Resin products with characteristics such as high specific surface area, high strength, high stability, recyclability and low toxicity have a broader application prospect. However, polystyrene resin adsorbents often require a secondary cross-linking reaction to obtain higher specific surface area, strength and stability. For example, the Chinese patent application...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/26B01J20/28B01J20/30
CPCB01J20/267B01J20/28064B01J20/28066B01J20/28083
Inventor 王玉明赵伟国欧洋孙家宽
Owner WANHUA CHEM GRP CO LTD
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