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Preparation method of surface hydroxylated polystyrene resin

A technology of polystyrene resin and hydroxylation, which is applied in the field of surface hydroxylated polystyrene resin and its preparation, can solve the problems of low surface hydroxyl content, low strength of resin microspheres, uneven distribution, etc., and achieve large particle size, Solve the effect of complex and unstable reaction process and high intensity

Active Publication Date: 2021-03-23
FUJIAN AGRI & FORESTRY UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The technical problem to be solved by the present invention is to provide a method for preparing polystyrene resin with hydroxyl groups on the surface, which solves the problems caused by the steric hindrance effect of the existing large-diameter polystyrene resin microspheres in the polymerization process. The content of surface hydroxyl groups is low and the distribution is uneven, the polymerization process of adding auxiliary monomers is complicated, difficult to control, the strength of resin microspheres is low, and the cost is high.

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  • Preparation method of surface hydroxylated polystyrene resin

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[0019] The invention discloses a preparation method of surface hydroxylated polystyrene resin, the method comprising the following steps:

[0020] Step 1. Pretreatment of unmodified polystyrene resin: first, swell polystyrene resin microspheres in dichloromethane for 10-20 hours, and then successively wash with tetrahydrofuran, ultrapure water, absolute ethanol, and absolute methanol Filter three times, and finally vacuum-dry at 20-40°C to constant weight;

[0021] Step 2, hydroxylation modification of polystyrene resin microspheres: take the polystyrene resin obtained in step 1 in a container, add carbon disulfide reagent to swell, then place the container in an ice-water bath, add aluminum bromide and 4 -Chlorophenol; continue to place in the ice-water bath for 20-30 minutes, and then place it in a water-bath shaker at 20-40°C for reaction; after the reaction is completed, wash and filter with tetrahydrofuran, dilute hydrochloric acid, water, and methanol respectively severa...

Embodiment 1

[0026] Example 1: Unmodified polystyrene resin pretreatment: first 0.5g of unmodified polystyrene resin microspheres were swelled in dichloromethane for 10 hours, then successively washed with tetrahydrofuran, ultrapure water, absolute ethanol, anhydrous Water and methanol were washed and filtered three times, and finally vacuum-dried at 20°C to constant weight;

[0027] Hydroxylation modification of polystyrene resin microspheres: Take 0.3 g of polystyrene resin obtained in step 1 in a container, add 100 ml of carbon disulfide reagent for swelling, then place the container in an ice-water bath, and add 0.4 g of aluminum bromide in turn and 2g of 4-chlorophenol; continue to place in an ice-water bath for 30 minutes, and then place it in a water-bath shaker at 20°C for 5 hours; after the reaction, wash and filter with tetrahydrofuran, dilute hydrochloric acid, water, and methanol respectively several times, Finally, it was vacuum dried at 40°C to constant weight. Hydroxylated ...

Embodiment 2

[0028] Example 2: Unmodified polystyrene resin pretreatment: first 0.5g unmodified polystyrene resin microspheres were swelled in dichloromethane for 5 hours, then successively washed with tetrahydrofuran, ultrapure water, absolute ethanol, anhydrous Water and methanol were washed and filtered three times, and finally vacuum-dried at 30°C to constant weight;

[0029] Hydroxylation modification of polystyrene resin microspheres: Take 0.3 g of polystyrene resin obtained in step 1 in a container, add 50 ml of carbon disulfide reagent for swelling, then place the container in an ice-water bath, and add 0.6 g of aluminum bromide in turn and 2g of 4-chlorophenol; continue to place in an ice-water bath for 25 minutes, and then place it in a water-bath shaker at 30°C for 10 hours; after the reaction, wash and filter with tetrahydrofuran, dilute hydrochloric acid, water, and methanol respectively several times, Finally, it was vacuum dried at 40°C to constant weight. Hydroxylated poly...

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Abstract

The invention provides a preparation method of surface hydroxylated polystyrene resin. Used unmodified resin is large-particle-size polystyrene resin, and a monomer for modification is 4-chlorophenol.The preparation method comprises the following steps: firstly, swelling polystyrene resin microspheres by using dichloromethane, then conducting washing and filtering for multiple times by using tetrahydrofuran, ultrapure water, absolute ethyl alcohol and methanol in sequence, and finally conducting drying in vacuum; and then carrying out Friedel-Crafts reaction on the pretreated resin and 4-chlorophenol to obtain hydroxylated polystyrene resin microspheres. The method solves the problems of complex and unstable reaction process, low surface hydroxyl polymerization degree and non-uniform distribution when hydroxyl is grafted on the surface of the traditional polystyrene resin microsphere.

Description

【Technical field】 [0001] The invention relates to a surface hydroxylated polystyrene resin and a preparation method thereof. 【Background technique】 [0002] Polystyrene resin microspheres refer to rigid beads prepared with styrene as a monomer and divinylbenzene as a crosslinking agent, with diameters ranging from tens of nanometers to hundreds of microns. The different sizes determine the different physical properties of the microspheres. Nanoscale polystyrene resin microspheres are usually used as catalyst supports because of their relatively small surface energy. Micron-sized polystyrene resin microspheres have relatively large surface energy, and using them as catalyst supports cannot effectively reduce the reaction activation energy, but using them as adsorbents has a better effect. Compared with pure solid resin microspheres, resin microspheres with porous structure have higher specific surface area and higher adsorption performance. [0003] Unmodified polystyrene ...

Claims

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Application Information

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IPC IPC(8): C08J7/02C08J7/12C08L25/06
CPCC08J7/02C08J7/12C08J2325/06
Inventor 苗庆显张琛孟令超陈礼辉
Owner FUJIAN AGRI & FORESTRY UNIV
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