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Amino nitrogen heterocyclic ring resin and preparation method thereof

A nitrogen heterocycle and nitrogen heterocycle compound technology, applied in the field of organic compound preparation, can solve problems such as low adsorption capacity, poor adsorption selectivity, and reduced resin adsorption capacity

Active Publication Date: 2014-12-24
SUNRESIN NEW METERIALS CO LTD XIAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the main disadvantage of this technology is that the 6-aminopyridine-3-carboxylic acid molecule is relatively large, and it is difficult to combine with the resin. At the same time, the presence of carboxyl groups will reduce the content of pyridine rings and amino groups on the resin, and the resin adsorption capacity will be reduced.
[0024] Although the patent CN102295723A has prepared the aminopyridine functional group, the connection between the pyridine ring and the resin depends on the ester bond, and the functional group is gradually inactivated in a strong acid and strong alkali system, resulting in a decrease in adsorption performance; at the same time, the connection of the ester bond makes the effective functional group account for the proportion of the resin. reduced, the adsorption capacity will be affected
The resins prepared by the methods currently used in the literature have problems such as poor adsorption selectivity and low adsorption capacity.

Method used

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  • Amino nitrogen heterocyclic ring resin and preparation method thereof
  • Amino nitrogen heterocyclic ring resin and preparation method thereof
  • Amino nitrogen heterocyclic ring resin and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0076] Add 500ml of 8% sodium chloride solution configured with tap water into a 1000ml reactor, then add 1g of hydroxyethyl cellulose and 2.5g of gelatin, stir and heat up to 45°C to dissolve evenly, then stop stirring for subsequent use; Weigh 8.8g of 80% divinylbenzene and 91.2g of styrene in the dried beaker, add 80g of toluene and 0.8g of dibenzoyl peroxide, stir evenly, add them into a 1000ml reaction kettle, let stand for 10min, start stirring and Adjust the stirring speed to disperse the oil phase into spherical particles of 0.2-0.7mm, raise the temperature to 80°C and keep it for 3h, and after the balls solidify, raise the temperature to 90°C to continue the reaction for 5h. After the reaction, the solidified balls were filtered out, and the balls were washed with methylal to clean the toluene, and then washed with water until there was no methylal, to obtain 196 g of the resin matrix.

[0077] Put the cured balls prepared above in an oven at 105°C for 3 hours, measur...

Embodiment 2

[0086] Use commercially available 122 resin and dry it with a moisture content of 0.8%. Weigh 80g of dried resin, add it to a 1000ml three-necked glass reactor, add 400ml of ethylene glycol, start stirring, swell for 1h, then add 300ml of ethylenediamine, heat up to 150°C for 15h, filter out the resin and wash with water until neutral , Obtain 267g primary amine phenolic resin.

[0087] Weigh 100g of the above-mentioned primary amine phenolic resin, add it into a 500ml three-necked glass reactor, use 4-chloropiperidine hydrochloride, and add 60g of 35% potassium hydroxide solution into the reactor, stir and heat up to 40°C; Feed a total of 60 g of an aqueous solution containing 32 g of 4-chloropiperidine hydrochloride into a 500 ml reactor, and after 5 hours, the feeding is completed, and then the temperature is raised to 60 ° C, and the reaction is completed for 18 hours. After the end, the resin is filtered out, washed with ethanol, and washed with water to obtain 108g of p...

Embodiment 3

[0093] According to the preparation method of Example 1, the primary amine resin was prepared, but in the preparation process, the raw materials were adjusted as follows: the addition of 80% divinylbenzene was 7.5g, the addition of styrene was 92.5g, the addition of toluene was 100g, other The raw materials are unchanged. The exchange capacity of the obtained primary amine resin was 7 mmol / g, and the water content was 57.23%.

[0094] Add 100 g of the above-prepared primary amine resin into a 500 ml reaction kettle, add 90 g of 50% sodium carbonate, and start stirring; prepare 65.7 g of 2-chloro-1,3-dimethyl imidazoline chloride into a water-saturated The solution was fed into the reaction kettle within 6 hours, and then heated to 30°C for 35 hours of reaction, washed with ethanol, and washed with water to obtain 149 g of imidazole nitrogen-containing heterocyclic resin.

[0095] Take 100g of the above resin, dry it in an oven, put it into a 500ml reaction kettle, add 74g of ...

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Abstract

The invention provides amino nitrogen heterocyclic ring resin and a preparation method thereof. The resin has a structure as shown in the specification, wherein M is a resin matrix, R can be H, also can be a group with hydroxyl, sulfydryl, an ether group, a thioether group, amide or an ester group, and also can be a nitrogen heterocyclic ring functional group which is the same as Q; Q is a nitrogen heterocyclic ring functional group, also can be pyridyl, imidazolyl, piperidyl, indolyl, and the like. The special functional group structure of the amino resin can be used for increasing the selective adsorption capacity of target metal ions more effectively, recycling valuable metals in the industries such as the wet metallurgy industry or the electroplating industry, and has high selection on copper ions.

Description

technical field [0001] The invention relates to an amino nitrogen-containing heterocyclic resin and a preparation method thereof, belonging to the technical field of organic compound preparation. Background technique [0002] In hydrometallurgy, many kinds of ions coexist in most of the feed liquids, especially some ions have similar properties and are difficult to separate. It has always been very difficult to separate target metal ions from such a complex feed liquid environment. The resin method is gradually favored by people due to factors such as environmental protection, simple process, and low cost. It gradually shows more and more advantages in the field of hydrometallurgy, but it still faces many technical bottlenecks. [0003] Patent US-A 4098867 describes a heterodisperse gel-type chelating resin, which is characterized by the following structural formula: [0004] [0005] M is the resin matrix; [0006] Q is a -CH 2 - group; [0007] Y can be H or C 1 ~C...

Claims

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Application Information

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IPC IPC(8): C08F212/08C08F212/36C08F8/34C08F8/32C08G8/28B01J20/26B01J20/30
Inventor 李岁党寇晓康焦鹏伟刘琼
Owner SUNRESIN NEW METERIALS CO LTD XIAN
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