Preparation method for ion exchange resin beads by stepwise suspension polymerization

An ion exchange resin and suspension polymerization technology, applied in ion exchange, ion exchange treatment devices, chemical instruments and methods, etc., can solve the problems of increased monomer dissolution loss, poor uniformity of white sphere particle size, and increased pollution of mother liquor, etc. Guaranteed yield and particle size uniformity, improved white ball yield and particle size uniformity, and reduced solubility

Active Publication Date: 2020-05-12
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] First, the uniformity of white ball particle size is poor
According to the national standard, the yield of qualified white balls in the range of 0.3-0.8mm particle size can only reach 85-90% (calculated by monomer weight); secondly, for monomers with high polarity or water solubility, such as methyl methacrylate, etc. , or when it is necessary to add polar organic pore-forming solvents such as various alcohols to prepare macroporous white balls, 8-15% of inorganic salts such as table salt must be added to the dispersion medium water, otherwise the dissolution loss of monomers will increase greatly and it will be difficult to form balls , which will not only bring waste of resources, increased cost and increased pollution of mother liquor (Qian Tingbao. Ion Exchanger Application Technology [M]. Tianjin: Tianjin Science and Technology Press, 1984: 20-35)

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Add 14.0g of polyvinyl alcohol and 1.26g of hydroxypropyl methylcellulose into 1400ml of pure water, stir at room temperature to make them fully dissolve, and then add 560g of monomeric styrene (according to 0.9g / mL Conversion, 622mL), cross-linking agent divinylbenzene 91g (content 55%, 101mL), initiator benzoyl peroxide 7.5g and N,N-dimethyl-p-toluidine 0.7g monomer phase shakes to make it Fully dissolve and pre-polymerize in a constant temperature water bath at 50°C for 20 minutes. After the viscosity of the solution reaches 150% of that before pre-polymerization using an Ubbelohde viscometer, drop it within 25 minutes at a stirring speed of 1000 rpm Add it to the aqueous solution in which the dispersant is dissolved, then raise the temperature to 75°C, 85°C, and 95°C in stages for suspension polymerization for 2 hours, 2 hours, and 5 hours, respectively, cool down and discharge, wash with hot water for several times, and dry.

[0027] Finally, sieving and weighing, ...

Embodiment 2

[0029]Add 14.0g of polyvinyl alcohol and 1.4g of hydroxypropyl methylcellulose into 1400ml of pure water, stir at room temperature to make it fully dissolve, then add 280g of monomer methyl methacrylate (according to 0.9 g / mL conversion, 311mL), methacrylic acid 280g (according to 0.9g / mL conversion, 311mL), crosslinking agent divinylbenzene 98g (content 55%, 108mL), initiator benzoyl peroxide 8.4g and N Shake the monomer phase of 0.84g of N-dimethyl-p-toluidine to fully dissolve, and place it in a constant temperature water bath at 60°C for pre-polymerization for 5 minutes. The viscosity of the solution measured by Ubbelohde viscometer reaches 150% of that before pre-polymerization Afterwards, at a stirring speed of 500 rpm, it was added dropwise to the aqueous solution in which the dispersant was dissolved within 30 minutes, and then the temperature was raised to 75°C, 85°C, and 95°C in stages for suspension polymerization for 2 hours, 2 hours, and 6 hours, respectively. Hou...

Embodiment 3

[0032] Add gelatin 11.3g and hydroxypropyl methylcellulose 1.13g into 1400ml pure water, stir at room temperature and make it fully dissolve, then add monomer methyl methacrylate 490g (according to 0.9g / mL conversion, 544mL), crosslinking agent ethylene glycol dimethacrylate 84g (content 55%, 93mL), cyclohexanol 540gmL (according to 0.9g / mL conversion, 600mL), initiator cumene peroxide 7.0g Shake the monomer phase with 0.48g of N,N-dimethyl-p-toluidine to fully dissolve it, and place it in a constant temperature water bath at 45°C for prepolymerization for 30 minutes, and use an Ubbelohde viscometer to measure the viscosity of the solution before prepolymerization. After 150%, at a stirring speed of 300 rpm, add it dropwise to the aqueous solution in which the dispersant is dissolved within 20 minutes, and then raise the temperature to 75°C, 85°C and 95°C in stages for suspension polymerization for 2 hours and 1 hour respectively And for 5 hours, cool down and discharge, wash...

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PUM

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Abstract

The invention discloses a method for preparing polymer beads for ion exchange resin through step-by-step suspension and polymerization. The method comprises the following steps: pre-polymerizing a monomer by taking a non-polar or polar monomer as a raw material and by adopting a compound dispersant and compound initiator system, performing a suspension polymerization process to prepare gel type polymer beads of an ion exchange resin precursor, or adding a polar or non-polar pore-forming agent in the monomer of the process to prepare macroporous polymer beads for the ion exchange resin precursor. The qualification rate of the beads prepared by the method in the grain size range of 0.3 to 0.8 mm can reach to 92 to 94 percent, the yield of the beads with the grain size of 0.02 to 0.04 mm canreach to 81 to 90 percent, and the uniformity of the while ball grain size can be obviously improved; furthermore, salt is not added in the preparation process, so the revenue can be increased, the cost can be reduced and the economic benefit is very considerable.

Description

technical field [0001] The invention belongs to the technical field of preparation of polymer beads of ion-exchange resin precursors, and in particular relates to a method for preparing ion-exchange resin beads by step-by-step suspension polymerization. Background technique [0002] Since the 1940s, the suspension polymerization process has gradually become one of the most important methods for the synthesis of various polymers, and has been industrialized on a large scale worldwide for more than half a century. Up to now, it is still one of the important synthetic methods of polymers such as polystyrene, polyvinyl chloride and polyacrylates. Among them, especially as polymer bead precursors (commonly known as white balls in the industry) for synthesizing various types of ion exchange resins and macroporous adsorption resins, they are produced by suspension polymerization process almost without exception at home and abroad. [0003] The suspension polymerization process mai...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F212/08C08F212/36C08F222/14C08F220/14C08F220/06C08F2/20C08J9/28B01J47/00
CPCB01J47/00C08F2/20C08F212/08C08F220/14C08J9/28C08J2201/0502C08J2325/08C08J2333/12C08F222/102
Inventor 王亚宁梁洁
Owner SICHUAN UNIV
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