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A kind of composite functional fluoride removal resin and its preparation method

A composite function, fluorine-removing resin technology, applied in chemical instruments and methods, other chemical processes, adsorption water/sewage treatment, etc., to achieve high adsorption capacity and wide-ranging effects

Inactive Publication Date: 2011-12-07
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Literature search shows that there is no report on the synthesis of amino-modified and metal-loaded composite functional fluorine-removing resins using styrene-divinylbenzene as a substrate through nitration-sulfonation-ammonation-loaded metals

Method used

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  • A kind of composite functional fluoride removal resin and its preparation method
  • A kind of composite functional fluoride removal resin and its preparation method
  • A kind of composite functional fluoride removal resin and its preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] (a) Nitrification reaction

[0027] Put styrene-divinylbenzene resin NDA-150 into a Soxhlet extractor, extract it with ethanol, air-dry it, sieve it, and take the resin with a suitable particle size for use.

[0028] In a 500 mL beaker, add 40 ml of 65% concentrated nitric acid and 80 ml of 85% concentrated sulfuric acid, stir well and cool for later use.

[0029] In a 500 mL three-neck flask, add 10 g of NDA-150 resin, pour into the above mixed solution, stir and react at 50 °C for 0.5 h, after the reaction, pump out the reaction solution, pour it into the ice-water mixture, filter and rinse with distilled water until Neutral, air drying to get resin 150-NO 2 .

[0030] (b) Sulfonation reaction

[0031] In a 500 mL three-neck flask, add the 150-NO prepared in step (a) 2 Resin 10 g, swollen with 20 ml of dichloroethane for 6 h, added 80 ml of 80% concentrated sulfuric acid, then refluxed and heated to 90 ° C, stirred, reacted for 8 h, after the end, distilled dichlo...

Embodiment 2

[0040] In step (a), the concentration of concentrated nitric acid is 60% by weight, and the dosage is 10 times of the amount of resin; the concentration of concentrated sulfuric acid is 98% by weight, and the dosage is 8 times of the amount of resin; the reaction temperature is 40° C., and the reaction time is 2 hours; In step (b), use 40ml of dichloroethane to swell for 9 hours, the concentration of concentrated sulfuric acid is 80% by weight, the amount used is 20 times the amount of resin, the reaction temperature is 70 ° C, and the reaction time is 12 hours; in step (c), SnCl 2 2H 2 The purity of O is 90%, and the dosage is 10 times of the amount of resin; the concentration of concentrated hydrochloric acid is 30% by weight, and the dosage is 10 times of the amount of resin; the purity of ethanol is 90%, and the dosage is 15 times of the amount of resin, and the reaction temperature is 80°C , the reaction time is 12h; step (d) Fe 2 (SO 4 ) 3 The weight percentage concen...

Embodiment 3

[0042] In step (a), the concentration of concentrated nitric acid is 80% by weight, and the dosage is 4 times of the amount of resin, the concentration of concentrated sulfuric acid is 75%, and the dosage is 20 times of the amount of resin, the reaction temperature is 80°C, and the reaction time is 3h; In step (b), use 50ml of dichloroethane to swell for 12h, the concentration of concentrated sulfuric acid is 98% by weight, the amount used is 8 times the amount of resin, the reaction temperature is 120°C, and the reaction time is 16h; in step (c), SnCl 2 2H 2 The purity of O is 100%, and the dosage is 4 times of the amount of resin; the concentration of concentrated hydrochloric acid is 40% by weight, and the dosage is 4 times of the amount of resin; ethanol is absolute ethanol, and the dosage is 5 times of the amount of resin, and the reaction temperature is 100°C , the reaction time is 16h; step (d) Fe 2 (SO 4 ) 3 The weight percentage concentration is 1.0 mol / L, the dosa...

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Abstract

The invention discloses a composite functional fluorine-removing resin, which belongs to the field of resins. The resin is based on styrene-divinylbenzene resin, the structural unit is , contains functional groups -NH2 and -SO3-X (Fe / Al), the particle size is 0.3-0.5mm, and the saturated adsorption capacity for F- is 2.16~8.10mg / g. The preparation method is: take styrene-divinylbenzene resin as the matrix, add 60-80% concentrated nitric acid and 75-98% concentrated sulfuric acid to react at 40-80°C, and stir for 0.5-3 hours to obtain the loaded nitro Resin R-NO2; use dichloroethane as swelling agent, add 80-98% concentrated sulfuric acid to react at 70-120°C, stir and react for 8-16 hours to get nitro-sulfonic acid resin R-NO2 -SO3H; at 60-100°C, add SnCl2·2H2O, concentrated hydrochloric acid, ethanol, and reflux for 8-16 hours to obtain amino-sulfonic acid resin R-NH2-SO3H; at 20-60°C, add 0.1-1.0 mol / L iron salt or aluminum salt solution, stirred and reacted for 18-30 hours, and the composite functional fluorine removal resin R-NH2-SO3-X (Fe / Al) modified by amino groups and supported by metals was prepared. The composite functional fluorine removal resin prepared by the invention can be used for high-efficiency and deep fluorine removal.

Description

technical field [0001] The invention relates to a composite functional fluorine removal resin and a preparation method thereof, in particular to an amino-modified and metal-supported composite functional fluorine removal resin and a preparation method thereof. Background technique [0002] According to the theory of hard and soft acids and bases, fluoride ions are classified as hard bases due to their higher electronegativity and smaller volume. 3+ or Al 3+ Isohard acid has a strong affinity. Numerous studies have shown that conventional Al 2 o 3 The adsorption capacity of bone charcoal to fluorine is only 1.8-3.0mg / g; 3+ or Al 3+ to F - It has been widely studied because of its high binding capacity, and the loading of Fe 3+ or Al 3+ The artificially modified adsorbent can strengthen the ability to remove fluorine, and has a wide application prospect. In addition, due to hydrogen bonding and electrostatic interaction between protonated amino groups and fluorine ion...

Claims

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Application Information

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IPC IPC(8): C08F212/36C08F212/08C08F8/44C08F8/36C08F8/30B01J20/26B01J20/30C02F1/28
Inventor 刘福强刘晶李兰娟鞠佳伟高洁李爱民
Owner NANJING UNIV
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