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Method for preparing high-temperature and strong alkali resistant type anion exchange resin

A technology of exchange resin and strong base, which is applied in the direction of anion exchange, ion exchange, chemical instruments and methods, etc., and can solve the problems of harsh industrial production, easy to react with water, harsh production conditions, etc.

Active Publication Date: 2016-12-07
PUROLITE (CHINA) CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this method is that metal reagents (Grignard reagents and copper-lithium reagents) are used in the monomer preparation stage, which are active in nature and easy to react with water. The requirements are extremely harsh or even impossible to achieve, and the yield of synthesis is very low
[0008] Based on the above methods of improving heat resistance by adding long-chain spacer groups, it can be seen that this idea has a good effect, but the synthesis routes of these resins reported above are due to various reasons, such as the use of active strong Corrosive or metallic reagents (such as SOCl 2 , PBr 3 , Grignard reagent, etc.), harsh production conditions, low yield, etc., are difficult to achieve in large-scale industrial production, so there are no mature high-temperature-resistant and strong-alkali resin products in the market

Method used

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  • Method for preparing high-temperature and strong alkali resistant type anion exchange resin
  • Method for preparing high-temperature and strong alkali resistant type anion exchange resin
  • Method for preparing high-temperature and strong alkali resistant type anion exchange resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] The preparation of embodiment 1 chlorine ball

[0030] Add 55.75 g of trisodium phosphate dodecahydrate and 1.54 L of water into a 3 L four-necked flask equipped with a stirrer, condenser and thermometer, and stir to raise the temperature to 80°C. Add 55.75 g of anhydrous calcium chloride at 50°C and stir for 10 minutes. At 60°C, a mixture of 4.95 g of hydroxyethyl cellulose and 20 g of sodium chloride was added. At 75°C, a mixture of 7.37 g calcium lignosulfonate and 20 g sodium chloride was added. At 80°C, 157.58 g of sodium chloride was added and stirred for 30 minutes. Then add a mixed solution of 699.68 g styrene, 17.94 g divinylbenzene (content 80%), 444.92 g porogen isobutanol and 7.17 g benzoyl peroxide, stir, adjust to a suitable particle size, and heat to 80°C for reaction After 1.5 hours, the temperature was raised to 82°C for 4 hours, and the temperature was raised to 88°C for 3 hours, and the temperature was continued to rise above 96°C, and the isobutan...

Embodiment 2

[0032] Example 2 Synthesis and Performance Evaluation of Strong Base Anion Exchange Resin with 4-Chlorobutanol as Spacer

[0033] Add 49.5 mL of 4-chlorobutanol, 800 mL of toluene, and 134 mL of 30% trimethylamine aqueous solution to a 1 L four-neck flask equipped with a stirrer, a condenser, and a thermometer, heat to 70°C for 24 hours, and distill the toluene Constantly replenish toluene to 110°C and keep it warm for 2 hours. Cool to room temperature, add the above-mentioned chlorine balls and 93 mL of 30% sodium methoxide solution, heat up to 65°C and react for 24 hours, distill off toluene, and wash to obtain strong base anion exchange resin B. Its volume exchange capacity C0=0.67 mmol / L, strong base content S0=100%.

[0034] Evaluation of High Temperature Resistance of Strong Base Anion Exchange Resin

[0035]Put a certain amount of resin to be tested into the reactor, add an appropriate amount of sodium hydroxide solution of appropriate concentration, stir, keep warm a...

Embodiment 3

[0046] Example 3 Synthesis and performance evaluation of strong base anion exchange resin with 6-chlorohexanol as spacer

[0047] Add 62.5 mL of 6-chlorohexanol, 800 mL of toluene, and 134 mL of 30% trimethylamine aqueous solution to a 1 L four-necked flask equipped with a stirrer, condenser and thermometer, heat to 70°C for 24 hours, and distill the toluene Constantly replenish toluene to 110°C and keep it warm for 2 hours. Cool to room temperature, add the above-mentioned chlorine spheres and 93 mL of 30% sodium methoxide solution, heat up to 65°C and react for 24 hours, distill off toluene, and wash to obtain strong base anion exchange resin C. Its volume exchange capacity C0=0.65 mmol / L, strong base content S0=100%.

[0048] Accurately measure V0 = 40.0 mL of the above resin, transfer it to an autoclave, add 80 mL of 0.1 N sodium hydroxide aqueous solution, seal the autoclave, and raise the temperature to 105 ° C for 168 hours. After cooling and washing, the resin volume...

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Abstract

The invention relates to a method for preparing a high-temperature and strong alkali resistant type anion exchange resin. The method comprises the following steps: 1) allowing styrene polymer to react with chloromethyl ether, then stopping the reaction, washing and drying to obtain chloromethylated beads; 2) mixing C1-C12 long-chain halogenated alcohol with solvent, dropwise adding a trimethylamine aqueous solution to react, and after the reaction is finished, distilling out the solvent; cooling to room temperature, dropwise adding the chloromethylated beads to react, after the reaction, distilling out the solvent, and washing to obtain the strong alkali resistant type anion exchange resin. The method can be used for large-scale industrial production and is economic and environment-friendly, and the product has relatively high heat-resisting stability and can be used in the fields of high-temperature condensation water treatment, high-temperature catalysis and the like.

Description

technical field [0001] The invention relates to a preparation method of a high temperature resistant strong alkali type anion exchange resin. Background technique [0002] Strong base anion exchange resin is mainly used in the field of water treatment, and also has a wide range of uses in the purification, concentration, separation, decolorization and catalyst of substances. The temperature is limited to below 60°C, which greatly limits the application range of strong base anion exchange resins. In recent years, extensive research has been conducted on the thermal stability of strong base anion exchange resins. [0003] At present, the heat resistance of the commercialized strong base anion exchange resin is poor, mainly due to the chemical structure, the bond energy and decomposition activation energy of the quaternary ammonium ion are low, and the strong base group will fall off at a higher temperature and degradation, such as figure 1 shown. These reactions are a form...

Claims

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Application Information

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IPC IPC(8): B01J41/14
CPCB01J41/14
Inventor 耿啸天马志超
Owner PUROLITE (CHINA) CO LTD
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