A kind of porous organic framework material, preparation method and application in selective separation of perrhenate

An organic framework, perrhenate technology, applied in the direction of organic anion exchangers, organic cation exchangers, separation methods, etc., can solve problems such as unsatisfactory selective separation effect

Active Publication Date: 2022-07-05
潍坊光华精细化工有限公司 +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although this preparation method can prepare materials with rich porous and macroporous structures, and achieves selective separation of perrhenate, its selective separation effect is not ideal.

Method used

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  • A kind of porous organic framework material, preparation method and application in selective separation of perrhenate
  • A kind of porous organic framework material, preparation method and application in selective separation of perrhenate
  • A kind of porous organic framework material, preparation method and application in selective separation of perrhenate

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preparation example Construction

[0024] The invention provides a preparation method of a porous organic framework material, comprising the following steps:

[0025] Tris(4-imidazolylphenyl)amine, cyanuric chloride and organic solvent are mixed to carry out quaternization reaction to obtain porous organic framework material.

[0026] In the present invention, the substance amount ratio of the tris(4-imidazolylphenyl)amine and cyanuric chloride is preferably (0.6-1.2):(0.4-0.8), more preferably 1:1. In the present invention, the amount ratio of the tris(4-imidazolylphenyl)amine and cyanuric chloride is within the above-mentioned range so that a sufficient quaternization reaction can be performed.

[0027] In the present invention, the organic solvent is preferably N,N'-dimethylformamide, N,N'-dimethylacetamide or N-methylpyrrolidone. In the present invention, the amount of the organic solvent is not particularly limited, as long as the raw material can be dissolved.

[0028] In the present invention, the oper...

Embodiment 1

[0046] Weigh 0.355 g of tris(4-imidazolylphenyl) amine and dissolve it in 20 mL of N,N'-dimethylformamide solvent to obtain the first solution; weigh 0.148 g of cyanuric chloride and dissolve it in 20 mL of N,N'-dimethylformamide In the solvent of base formamide, the second solution was obtained; the ratio of the amount of the tris(4-imidazolylphenyl)amine and the cyanuric chloride was 1:1; then the two solutions were mixed, and the mixture was heated at 100° C. The oil bath reaction was carried out for 24 hours, 0.0016 mol of benzyl bromide was added, and the ratio of the amount of the benzyl bromide to the tris(4-imidazolylphenyl)amine was 1:2, and the oil bath reaction was continued at 80°C for 24 hours. Then, the product obtained by the reaction was washed with N,N'-dimethylformamide, acetonitrile and diethyl ether respectively, and dried under vacuum at 60°C for 12h to obtain a yellow powder, which is a porous organic framework material, and the yield was 60%.

[0047] Th...

Embodiment 2

[0051] Weigh 0.355 g of tris(4-imidazolylphenyl) amine and dissolve it in 20 mL of N,N'-dimethylformamide solvent to obtain the first solution; weigh 0.148 g of cyanuric chloride and dissolve it in 20 mL of N,N'-dimethylformamide In the solvent of base formamide, the second solution was obtained; the ratio of the amount of the tris(4-imidazolylphenyl)amine and the cyanuric chloride was 1:1; then the two solutions were mixed, and the mixture was heated at 100° C. The oil bath reaction was carried out for 24 hours, 0.0016 mol of benzyl bromide was added, and the ratio of the amount of the benzyl bromide to the tris(4-imidazolylphenyl)amine was 1:2, and the oil bath reaction was continued at 80°C for 24 hours. Then, the product obtained by the reaction was washed with N,N'-dimethylformamide, acetonitrile and diethyl ether respectively, and dried under vacuum at 60°C for 12h to obtain a yellow powder, which is a porous organic framework material, and the yield was 52%.

[0052] Th...

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Abstract

The invention provides a preparation method of a porous organic framework material, comprising the following steps: mixing tris(4-imidazolylphenyl)amine, cyanuric chloride and a solvent, and performing a quaternization reaction to obtain a porous organic framework material. In the present invention, tris(4-imidazolylphenyl)amine TIPA and cyanuric chloride are used as raw materials to carry out quaternization reaction, so that the prepared porous material has a special structure of cationic skeleton, and there are free anions such as chloride ions in the pores etc., after mixing with a solution containing perrhenate, the selective separation of perrhenate is carried out by anion exchange in the pores. The experimental results show that the specific surface area of ​​the porous organic framework material provided by this application is 274m 2 , the adsorption rate is as high as 100%, and the maximum adsorption capacity is 442 mg / g.

Description

technical field [0001] The invention belongs to the field of recycling and utilization of scattered elements, and in particular relates to a porous organic framework material, a preparation method thereof, and an application in selective separation of perrhenate. Background technique [0002] Rhenium (Re) is the latest important element found in the rare scattered element (RSE) group. It is a precious rare scattered metal element. It has high hardness, corrosion resistance, wear resistance and good ductility. It is used in national defense, aerospace and ultra-high temperature. It is widely used in emission and so on. Because rhenium is very little in the earth's crust, rhenium and its compounds are expensive, making it more practical to recycle. In weak acid or weak base solution, rhenium is the heptavalent anion ReO 4 - Existence, such as ammonium perrhenate, potassium perrhenate, are generally extracted in the form of anions in hydrometallurgy. [0003] At present, wh...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G73/06B01D15/36
CPCC08G73/0638C08G73/065B01D15/363Y02P10/20
Inventor 王磊焦韶韶刘康李少香马鼎璇杜云梅
Owner 潍坊光华精细化工有限公司
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