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Porous organic framework material and preparation method thereof, and application in selective separation of perrhenate radicals

A technology of organic skeleton and perrhenate, applied in organic anion exchangers, organic cation exchangers, separation methods, etc., can solve problems such as unsatisfactory selective separation effects

Active Publication Date: 2020-12-22
潍坊光华精细化工有限公司 +1
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  • Summary
  • 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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  • Porous organic framework material and preparation method thereof, and application in selective separation of perrhenate radicals
  • Porous organic framework material and preparation method thereof, and application in selective separation of perrhenate radicals
  • Porous organic framework material and preparation method thereof, and application in selective separation of perrhenate radicals

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preparation example Construction

[0024]The present invention provides a method for preparing porous organic framework material, which includes the following steps:

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

[0026]In the present invention, the ratio of the amounts of the tris(4-imidazolylphenyl)amine and cyanuric chloride is preferably (0.6 to 1.2): (0.4 to 0.8), more preferably 1:1. In the present invention, the ratio of the amount of tris(4-imidazolylphenyl)amine and cyanuric chloride within the above-mentioned range enables sufficient quaternization reaction.

[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 operation of mixing the tri...

Embodiment 1

[0046]Weigh 0.355 g of tris(4-imidazolylphenyl)amine and dissolve it in 20mL of N,N'-dimethylformamide solvent to obtain the first solution; weigh 0.148 g of cyanuric chloride and dissolve in 20mL of N,N'-dimethylformamide The second solution is obtained in the base formamide solvent; the ratio of the amount of the tris(4-imidazolylphenyl)amine and cyanuric chloride is 1:1; then the above two solutions are mixed at 100°C Oil bath reaction for 24h, add 0.0016mol benzyl bromide, the ratio of the amount of the benzyl bromide to the tris(4-imidazolylphenyl)amine is 1:2, continue the oil bath reaction at 80°C for 24h ; And then separately with N,N'-dimethylformamide, acetonitrile and ether to wash the product obtained by the reaction, 60 ℃ vacuum drying for 12h, the yellow powder is a porous organic framework material, the yield is 60%.

[0047]The red light spectrum test is performed on the porous organic framework material prepared in this embodiment, such asfigure 2 As shown,figure 2 Is ...

Embodiment 2

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

[0052]The red light spectrum test was performed on the porous organic framework material prepared in this embodiment, and it was proved that the por...

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Abstract

The invention provides a preparation method of a porous organic framework material. The method comprises the following steps: mixing tris(4-imidazolylphenyl)amine, cyanuric chloride and a solvent, andcarrying out a quaternization reaction to obtain the porous organic framework material. According to the preparation method, tris(4-imidazolylphenyl)amine TIPA and cyanuric chloride are used as raw materials for quaternization reaction, so that the prepared porous material has a special structure of a cation skeleton; and after free anions such as chlorine ions and the like exist in pore channelsare mixed with a solution containing perrhenate radicals, and selective separation of perrhenate radicals is carried out through anion exchange in the pore channels. According to the invention, experimental results show that the specific surface area of the porous organic framework material provided by the invention is 274 m<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 specifically relates to a porous organic framework material, a preparation method thereof, and application in the selective separation of perrhenate.Background technique[0002]Rhenium (Re) is the latest important element to be discovered in the Rare Scattered Elements (RSE) group. It belongs to the precious and scattered metal elements. It has high hardness, corrosion resistance, wear resistance and good ductility. Launch and other aspects are widely used. Because rhenium contains very little in the earth's crust, the price of rhenium and its compounds is very expensive, so it is more practical to recycle it. In the weak acid or weak base solution, rhenium is the heptavalent anion ReO4-Exist, such as ammonium perrhenate and potassium perrhenate, which are generally extracted as anions in hydrometallurgy.[0003]At present, the selective separation of perrhenate is usually car...

Claims

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Application Information

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Patent Type & Authority Applications(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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