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A kind of preparation method of calcium-removing resin

A technology of resin and chelating resin, applied in the direction of aluminum halide, aluminum chloride, etc., can solve the problems of poor effect and difficulty in removing calcium ions, improve chelating ability, solve technical bottlenecks, and achieve great economic benefits and social value Effect

Active Publication Date: 2019-12-03
CHINA SHENHUA ENERGY CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the acidic environment of the aluminum chloride solution and the similarity in structure and properties between aluminum ions and calcium ions, it is still very difficult to remove calcium ions with the resin method. Conventional chelating resins, such as aminocarboxylic acid resins, Amino phosphonic acid resins are poor in removing calcium ions, so it is necessary to issue new resins with special pore structures and functional groups to achieve selective removal of calcium ions in aluminum chloride solutions

Method used

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  • A kind of preparation method of calcium-removing resin
  • A kind of preparation method of calcium-removing resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] 1) Add 3L of water, 30g of gelatin, 9g of hydroxymethyl cellulose, and 150g of sodium chloride into a 5L three-necked bottle, stir to dissolve and clear, and obtain an aqueous phase; 230.79g of industrial divinylbenzene, 76.92g of industrial styrene, 426.05 Mix g toluene and 189.35 g 200# gasoline, add 9.23 g benzoyl peroxide, dissolve and clear it by ultrasonication for 20 minutes, and obtain an oil phase; heat the obtained water phase to 55 ° C, add the oil phase, and heat the reaction solution to React at 83°C for 10 hours, filter, extract, wash with water, and dry to obtain resin white balls;

[0045] 2) Mix 350g of resin dry white balls with 1050g of chloromethyl ether, stir and swell at room temperature for 10h, then add 35g of zinc chloride as a catalyst, stir evenly, heat to 45°C for 10h, filter, wash with water to obtain chloromethylated resin, It is the resin chlorine ball. The measured resin chlorine content is 19.2%;

[0046] 3) Mix 300 g of resin chlorine...

Embodiment 2

[0049] The aqueous solution of aminosugar in step 3 in "Example 1" is changed to the diethanolamine aqueous solution that mass concentration is 10%, under the situation that other conditions remain unchanged, obtain and contain amino group and hydroxyl resin (weak base exchange volume: 3.2mmol / g), dry the resin, take 200g of dry resin and mix with 1600g of methanol, swell at room temperature for 3h, then add 34g of sodium methoxide methanol solution with a mass concentration of 15%, and start to drop 62.93g of carbon disulfide after heating to 35°C for 30min. After the addition, react at 45°C for 6 hours, filter, extract, and wash with water to obtain a resin containing amino groups, hydroxyl groups, and mercaptocarboxyl groups. The measured sulfur content is above 1.5 mmol / g.

Embodiment 3

[0051] The aqueous solution of aminosugar in the step 3 of "Example 1" is changed to the o-hydroxyaniline aqueous solution of mass concentration 10%, under the situation that other conditions remain unchanged, obtain and contain amino group and hydroxyl resin (weak base exchange volume: 2.32mmol / g), dry the resin, mix 200g of dry resin with 1000g of dimethyl sulfoxide, swell at room temperature for 3h, then add 50g of dimethyl sulfoxide solution with a mass concentration of 10% tert-butyl sodium, and heat to 80 Begin to add dropwise an aqueous solution of sodium sulfite (containing 90 g of sodium sulfite) with a mass fraction of 24% at ℃, react at 80 ℃ for 10 h after 60 min of dropwise addition, filter, extract, and wash to obtain resins containing amino groups, hydroxyl groups, and mercapto groups, and the sulfur content is measured as 1.62 mmol / g.

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Abstract

The invention provides a preparation method of a chelating resin for removing calcium ions from an aluminum chloride solution. The method comprises the following steps: 1) performing a chloromethylation reaction by using resin dry white balls and a chloromethylation reagent to obtain chlorine balls; 2) performing a nucleophilic substitution reaction on the chlorine balls obtained in the step 1) and an organic amine solution containing hydroxy groups according to a mass ratio of (1:4)-(1:6), and performing drying to obtain a resin containing amino and hydroxy groups; 3) uniformly mixing the resin containing amino and hydroxy groups obtained in the step 2) with a sweller, and performing swelling to obtain a swelling product; and 4) performing an addition reaction on the swelling product obtained in the step 3), an alkaline matter and a sulfur compound to obtain the calcium-removing resin containing amino and hydroxy groups and sulfur. The resin obtained by the method has different functionalized structures, and greatly enhances the adsorption quantity of calcium ions. The obtained calcium-removing resin can satisfy the technical requirements for industrial preparation of aluminum oxide, creates favorable conditions for the resource reutilization of fly ash, and has great economic benefits and social values.

Description

technical field [0001] The invention belongs to the technical field of organic compound preparation, in particular to the preparation of a chelating resin, in particular to the preparation of a chelating resin for removing calcium ions from an aluminum chloride solution. Background technique [0002] As early as the 1950s, foreign scientific and technological workers began to study the technology of extracting alumina from fly ash, and gradually formed three relatively mature processes: limestone sintering method, soda lime sintering method, and fluorine ammonia-assisted dissolution and acid leaching method. , but there are some shortcomings. After 2000, with the development of the domestic coal power industry, the pressure on the environment caused by fly ash is increasing, and the comprehensive utilization of high-value-added products such as alumina extracted from high-alumina fly ash has become a major issue in the coal power industry. A hot topic in alumina industry re...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F212/36C08F212/08C08F8/34C08F8/32C08F8/24C01F7/62
Inventor 郭昭华王宏宾池君洲王永旺寇晓康刘大锐李延军李岁党
Owner CHINA SHENHUA ENERGY CO LTD
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