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Preparation method and application of derivative catalyst based on LDH fixed transition MOF

A transition metal and catalyst technology, applied in the field of catalysts, can solve the problems of low exposure of active centers, limited catalytic activity, large mass transfer resistance, etc., and achieve the effects of simple preparation method, high catalytic activity and low cost

Active Publication Date: 2018-11-16
江阴智产汇知识产权运营有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the currently studied MOF crystals have some problems such as large size, low active center exposure, and high mass transfer resistance, which severely limit the catalytic activity.

Method used

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  • Preparation method and application of derivative catalyst based on LDH fixed transition MOF
  • Preparation method and application of derivative catalyst based on LDH fixed transition MOF
  • Preparation method and application of derivative catalyst based on LDH fixed transition MOF

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] a) Al 2 o 3 Fiber preparation: Soak 1.88 g of absorbent cotton fibers into 150 mL of 0.1 M Al 2 (SO 4 ) 3 In the aqueous solution, after ultrasonication for 4 h, the soaked absorbent cotton fibers were washed with deionized water to remove excess metal ions on the surface. Al 2 o 3 fiber.

[0035] b) Preparation of ZnAl-LDH carrier with fibrous micro-nano hierarchical structure: Zn(NO 3 ) 2 ∙6H 2 O (0.05 M) and hexamethylenetetramine (0.10 M) were dissolved in 25 mL of deionized water. Then 0.083 g of Al prepared in step a) 2 o 3 The fibers were added to the above solution, stirred at room temperature for 30 min, then transferred to a reactor, reacted at 70 °C for 8 h, centrifuged, washed with water and ethanol three times, and dried at 40 °C for 12 h to obtain a ZnAl-LDH carrier with a hierarchical structure.

[0036] c) Preparation of ZnAl-LDH / Co-MOF composite: Disperse 0.075 g of the ZnAl-LDH carrier prepared in step b) in 30 mL of trimesic acid (1.0 M)...

Embodiment 2

[0040] a) Al 2 o 3 Fiber preparation: 2.50 g of absorbent cotton fibers were soaked in 150 mL of 0.13 M Al(NO 3 ) 3 ∙9H 2 In O aqueous solution, after ultrasonication for 4 h, the soaked absorbent cotton fibers were washed with deionized water to remove excess metal ions on the surface. Al 2 o 3 fiber.

[0041] b) Preparation of CuAl-LDH support with fibrous micro-nano hierarchical structure: Cu(NO 3 ) 2 ∙3H 2 O (0.06 M) and hexamethylenetetramine (0.12 M) were dissolved in 25 mL of deionized water. Then 0.089 g of the Al prepared in step a) 2 o 3 The fibers were added to the above solution, stirred at room temperature for 30 min, then transferred to a reaction kettle, reacted at 120 °C for 10 h, centrifuged, washed with water and ethanol three times, and dried at 60 °C for 12 h to obtain a CuAl-LDH carrier with a hierarchical structure.

[0042] c) Preparation of CuAl-LDH / Co-MOF composite: Disperse 0.086 g of the CuAl-LDH carrier prepared in step b) in 30 mL of ...

Embodiment 3

[0046] a) Al 2 o 3 Fiber preparation: 3.75 g of absorbent cotton fibers were soaked in 150 mL of 0.15 M Al(NO 3 ) 3 ∙9H 2 In O aqueous solution, after ultrasonication for 4 h, the soaked absorbent cotton fibers were washed with deionized water to remove excess metal ions on the surface. Al 2 o 3 fiber.

[0047] b) Preparation of NiAl-LDH support with fibrous micro-nano hierarchical structure: Ni(CH 3 COO) 2 ・4H 2 O (0.07 M) and hexamethylenetetramine (0.14 M) were dissolved in 25 mL of deionized water. Then 0.096 g of the Al prepared in step a) 2 o 3 The fibers were added to the above solution, stirred at room temperature for 30 min, then transferred to a reactor, reacted at 110 °C for 10 h, centrifuged, washed with water and ethanol three times, and dried at 80 °C for 12 h to obtain a NiAl-LDH carrier with a hierarchical structure.

[0048] c) Preparation of NiAl-LDH / Ni-MOF composite: Disperse 0.12 g of the NiAl-LDH carrier prepared in step b) in 30 mL of trimes...

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Abstract

The invention belongs to the technical field of catalysts, and relates to a preparation method and application of a derivative catalyst based on a layered double hydroxide (LDH) fixed transition metalorganic framework (MOF). The method comprises the following steps: firstly soaking biomass fibers into an aluminum salt aqueous solution, performing drying, and performing high-temperature calcination to obtain Al2O3 fibers; dissolving a first divalent metal salt (M1<2+>) and hexamethylenetetramine into deionized water, adding the Al2O3 fibers, and performing a hydrothermal method to prepare a M1<2+>Al-LDH carrier with a fibrous micro-nano graded structure; and dispersing the carrier into a trimesic acid methanol solution, adding a second divalent metal salt (M2<2+>) methanol solution, performing drying to obtain an M1<2+>Al-LDH / M2<2+>-MOF complex, finally performing high-temperature calcination in a H2 atmosphere, and performing cooling to obtain the catalyst. According to the method and application disclosed by the invention, the prepared catalyst is applied to hydrogenation reduction of nitro compounds in wastewater; the prepared catalyst has a uniformly-dispersed active center onthe surface of the carrier, a high specific surface area and high catalytic activity, and solves the problems that a traditional catalyst is easy to agglomerate and not easy to recover; and the preparation method is simple and has low costs.

Description

technical field [0001] The invention belongs to the technical field of catalysts, and relates to layered double hydroxide (LDH) nanosheet-immobilized metal-organic framework (MOF) catalysts, in particular to a derivative catalyst based on LDH-immobilized transition metal MOF (M 1 2+ Al-LDO / M 2 ) preparation method and its application. Background technique [0002] In industrial production, a large amount of wastewater containing nitro compounds is directly discharged into the ecosystem without treatment, causing serious water pollution, causing various poisoning, blood diseases, cancer and other diseases. The state has strict regulations on the emission concentration of nitro compounds (≤5mg / L), and nitro compounds have been included in the "China Environmental Priority Pollutants Blacklist". At present, the nitro compounds used to treat wastewater mainly include biochemical methods, chemical oxidation methods, adsorption methods and catalytic hydrogenation reduction met...

Claims

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Application Information

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IPC IPC(8): B01J23/75B01J23/755B01J23/80B01J35/00B01J37/08B01J37/18C02F1/70C02F101/38
CPCC02F1/70B01J23/75B01J23/755B01J23/80B01J37/086B01J37/18C02F2101/38B01J35/399B01J35/393
Inventor 邱凤仙荣坚张涛郭卿朱瑶杨冬亚徐吉成
Owner 江阴智产汇知识产权运营有限公司
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