A polyunsaturated carboxylic acid modified metal organic framework material and its preparation method and application

A metal-organic framework, unsaturated technology, applied in chemical instruments and methods, other chemical processes, water/sludge/sewage treatment, etc., can solve the problem of low adsorption capacity, achieve high adsorption performance, short treatment cycle, and easy operation concise effect

Active Publication Date: 2021-04-13
LIAONING UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The present invention mainly aims at modifying MIL-101 MOF materials
In order to solve the problem of low adsorption capacity, the present invention uses unsaturated carboxylic acid to modify it, and introduces more -COOH adsorption sites, thereby improving the adsorption performance of metal ions

Method used

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  • A polyunsaturated carboxylic acid modified metal organic framework material and its preparation method and application
  • A polyunsaturated carboxylic acid modified metal organic framework material and its preparation method and application
  • A polyunsaturated carboxylic acid modified metal organic framework material and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Example 1 Polyacrylic acid modified metal organic framework material P-AA-MIL-101

[0036] (1) The preparation method is as follows: the synthesis process is as follows figure 1 shown

[0037] 1) Weigh 3.2g of chromium nitrate nonahydrate, 1.32g of terephthalic acid, 2.2mL of glacial acetic acid and 40mL of distilled water in a beaker, stir at room temperature for 30min, add 0.068mL of acrylic acid, stir for 30min, and mix The solution was poured into a hydrothermal reaction kettle, hydrothermally reacted at 200°C for 9 hours, cooled to room temperature, and washed with DMF, ethanol and distilled water in sequence to obtain acrylic acid-modified MIL-101, which was designated as AA-MIL-101.

[0038]2) Dissolve 0.3g AA-MIL-101 in 40mL deionized water, heat up to 60°C, add 0.2mL of acrylic acid to react for 20-30min, add initiator potassium persulfate 0.08g, heat up to 80°C, under nitrogen protection React for 1 h, cool to room temperature, wash with deionized water unti...

Embodiment 2

[0043] Example 2 The adsorption effect of P-AA-MIL-101 on Sc(III) and heavy metal Pb(II) under different acidity

[0044] 1. Method: Weigh 5 parts of 10mgP-AA-MIL-101 respectively, add 10mL to a concentration of 50mg·L -1 The Sc(III) solution, the pH of the Sc(III) solution is 1, 2, 3, 4, 4.5, respectively, shaken at 30°C, 180r / min in a shaking box for 24h. The result is as Figure 5a .

[0045] Depend on Figure 5a It can be seen that with the increase of pH value, the adsorption rate of P-AA-MIL-101 to Sc(III) gradually increases, and at pH=4.5, the adsorption rate of Sc(III) can reach 91%, thus realizing Recovery of rare earth element scandium.

[0046] 2. Method: Weigh 5 parts of 10mgP-AA-MIL-101 respectively, add 10mL to make the concentration 25mg·L -1 The Pb(II) solution, the pH of the Pb(II) solution is 1, 2, 3, 4, 5, shaken at 30°C, 180r / min in a shaking box for 24h. The result is as Figure 5b .

[0047] Depend on Figure 5b It can be seen that with the incr...

Embodiment 3

[0048] Example 3 The separation effect of P-AA-MIL-101 on Sc(III) in the solution of 16 kinds of mixed rare earth ions

[0049] Method: pipette 10mL respectively with a concentration of 20mg·L -1 The mixed solution of 16 kinds of rare earth elements (La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Y, Sc) were adjusted to pH 1, 2, 3, 4, 4.5, add 10mg of adsorbent P-AA-MIL-101, shake at 30°C for 24 hours, then measure the concentration of each rare earth ion in the solution. The result is as Figure 6 .

[0050] Depend on Figure 6 It can be seen that in the whole acidity range, P-AA-MIL-101 has a certain adsorption effect on 16 kinds of rare earth elements, among which the adsorption effect on Sc(III) is the best. When the pH is 3, the adsorption effect on Sc(III) The adsorption rate can reach 95.14%, by Figure 6 It can be seen that the selectivity to Sc(III) is also relatively good.

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Abstract

The invention relates to a polyunsaturated carboxylic acid modified metal organic framework material and its preparation method and application. Take chromium nitrate nonahydrate, terephthalic acid, glacial acetic acid and distilled water, stir at room temperature, add unsaturated carboxylic acid, react in a hydrothermal reaction kettle at 180-230°C for 8-12 hours, cool to room temperature, and wash until Neutral, dissolve the obtained unsaturated carboxylic acid modified MIL-101 in deionized water, heat up to 40-80°C, add unsaturated carboxylic acid to react for 10-40min, add initiator, heat up to 80-100°C °C, react under nitrogen atmosphere for 1-2h, cool, wash until neutral, and dry to obtain the target product polyunsaturated carboxylic acid modified metal organic framework material. The adsorbent prepared by the invention can efficiently recover rare earths and remove heavy metal elements from a solution, and has the advantages of simple synthesis steps, low cost, energy saving and environmental protection, and large adsorption capacity.

Description

technical field [0001] The invention belongs to the technical field of preparation of a modified metal-organic framework adsorption material and the adsorption of rare earth and heavy metal elements. The adsorbent can effectively adsorb rare earth and heavy metal elements from a solution. Background technique [0002] Rare Earth (Rare Earth) is a general term for seventeen metal elements including lanthanides, scandium and yttrium in the chemical periodic table. According to the differences and similarities of their physical and chemical properties, they can be divided into three groups: light rare earth group (lanthanum to promethium), medium rare earth group (samarium to dysprosium), heavy rare earth group (holmium to lutetium plus scandium and yttrium). Almost every 3-5 years, scientists are able to discover new uses of rare earths, and one out of every six inventions is inseparable from rare earths. It is widely used in the field of cutting-edge technology and military ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G83/00B01J20/22C02F1/28C02F101/20
CPCB01J20/226C02F1/285C02F2101/20C08G83/008
Inventor 娄振宁肖欣黄孟楠单炜军熊英
Owner LIAONING UNIVERSITY
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