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Process for preparing coarse-grained anion exchange gel

An anion exchanger and gel technology, which is used in the preparation of coarse-grained monodisperse anion-exchange gels, can solve the problems of particle adhesion, difficulty in separation, increased pressure loss, etc., and achieve the effect of high stability and high purity

Inactive Publication Date: 2003-10-15
LANXESS DEUTDCHLAND GMBH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] 1. Due to the addition of monomer, part of the polymer is precipitated from the seed, making the particles adhere to each other, which may interrupt the polymerization of the swollen seed;
[0015] 2. In the reaction solution used for functionalization, the concentration of the dissolved part increases, which may make it more difficult to prepare anion exchangers by functionalization;
[0016] 3. The anion exchanger may contain increased amounts of soluble polymers, which may lead to undesired extraction of the ion exchanger
Debris can enter the solution being treated and contaminate the solution in the application, or make the regenerative separation process more difficult and may result in loss of adsorbent material
Also, damaged anion exchangers are not conducive to functionalization of ion exchangers for column processes
Fragmented material causes increased pressure loss in the column system, thus reducing the throughput of purified liquid through the column, or making separation more difficult during batch processes

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0104] a.) Preparation of seed polymer

[0105] 1960 milliliters of deionized water was added to a 4-L glass reactor, and 630 grams of a microencapsulated mixture consisting of 1.0% by weight of divinylbenzene, 0.2% by weight of ethyl styrene (commercially available The composition of divinylbenzene and ethylstyrene mixture with 80% by weight of divinylbenzene), 0.5% by weight of tert-butyl 2-ethylperoxyhexanoate and 98.8% by weight of styrene, slightly The capsule is composed of formaldehyde-hardening complex polycondensate, wherein the formaldehyde-hardenable complex polycondensate is composed of gelatin and acrylamide-acrylic acid copolymer. The average particle diameter is 300 μm. The mixture was mixed with a solution consisting of 2.4 g of gelatin, 4 g of sodium hydrogen phosphate dodecahydrate, and 100 mg of resorcinol in 80 ml of deionized water, slowly stirred and polymerized, and stirred at 75°C for 10 Hour. The temperature was then increased to 95°C until the poly...

Embodiment 2

[0126] Embodiment 2 (the present invention)

[0127] Preparation of Strongly Basic Type II Anion Exchangers

[0128] Add 1500 mL of deionized water to a 4-neck flask. Dissolve 70 grams of sodium chloride in it. 800 ml of moist chloromethylated bead polymer prepared according to the method of Example 1 and having a chlorine content of 19.51% by weight and 312 g of dimethylaminoethanol were added. The suspension was heated to 90°C within 2 hours, stirred at 90°C for a further 2 hours and at 95°C for 6 hours. After cooling to room temperature, the mother liquor was removed by suction filtration, and then the resin was washed with 1600 ml of deionized water. The product was then stirred in 1600 ml of 3% strength by weight aqueous hydrochloric acid at 70° C. for 4 hours. After cooling, the liquid was separated, the resin was removed from the water and rinsed from the bottom of the column with 6 bed volumes of deionized water.

[0129] Yield: 1710ml filled resin

[0130] Excha...

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Abstract

Preparation of monodisperse gel form anion exchangers by: (a) formation of a suspension of seed in a continuous aqueous phase; (b) swelling in a vinyl monomer mixture; (c) polymerization of this in (a); (d) reswelling of monomer mixture; (e) polymerization of second monomer mixture in the first seed / feed polymerisate; and (f) functionalization of the copolymer obtained by chloromethylation and amination. A method for preparation of monodisperse gel form anion exchangers (I) of high stability and purity comprises: (a) forming in a continuous aqueous phase a suspension of seed poplymerisate with a swelling index of 2.5-7.5, and a content of non-evaporatable extractable portion of less than 1 wt.%; (b) swelling the suspended seed polymerisate in a monomer mixture of vinyl monomer, crosslinker, and radical starter; (c) polymerising the monomer mixture in the seed polymerisate; (d) swelling the polymerisate obtained again in the monomer mixture of vinyl monomer, crosslinker, and radical starter; (e) polymerising a second monomer mixture in the first seed / feed polymerisate; and (f) functionalizing the copolymer obtained, of swelling index 1.5-2 and mean diameter greater than 520 micron, by chloromethylation and amination. The particle size is greater than 800 micron. Independent claims are included for: (1) A process for preparation of the crosslinked seed polymerisate from (wt.%):(i) monomer (96.5-99.0), (ii) crosslinker (0.8-2.5), and (iii) aliphatic peroxyester as polymerization initiator; (2) (I) prepared by the method.

Description

technical field [0001] The invention relates to a method for preparing a coarse particle monodisperse anion exchange gel with high stability and purity. Background technique [0002] Recently, since ion exchange beds of coarse particle size are economically advantageous in many applications, the importance of anion exchanger particle sizes as large and uniform as possible has increased, preferably particle sizes > 800 μm. These advantages arise especially from monodisperse ion exchangers. They can be obtained by functionalizing monodisperse bead polymers. [0003] In particular, coarse-grained materials are suitable for gas adsorption, catalysis, and hydrometallurgy. [0004] Ion exchangers with particle sizes ranging from 300 to 800 [mu]m can be prepared by methods commonly used hitherto. This document discloses various processes for the preparation of ion exchangers having a particle size >800 μm, ie can be relatively referred to as crude exchangers. [0005] US ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D53/02B01J41/04B01J41/14C08F257/00C08F285/00C08F291/00
CPCC08F291/00B01D53/02C08F285/00Y10S526/909B01J41/043B01J41/14B01J41/05C08F212/08C08F2/18
Inventor L·费斯特尔G·沙德H·米塔格
Owner LANXESS DEUTDCHLAND GMBH