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Ti-V loaded aluminum-pillared montmorillonite heterogeneous catalyst and application thereof

A heterogeneous catalyst, montmorillonite technology, applied in the direction of organic chemistry, etc., can solve the problems of low conversion rate of reactants, insufficient catalyst activity, increased side reactions, etc., and achieve good development prospects, easy operation, and simple preparation methods.

Active Publication Date: 2013-11-13
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The strong acid center of the catalyst easily leads to an increase in side reactions, which promotes the self-polymerization of aldehydes on the surface of the solid acid, resulting in a decrease in the selectivity of 2,3-cyclopentenopyridine; if the acidity is too weak, the catalyst activity is not enough, and the conversion rate of the reactants is low.

Method used

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  • Ti-V loaded aluminum-pillared montmorillonite heterogeneous catalyst and application thereof
  • Ti-V loaded aluminum-pillared montmorillonite heterogeneous catalyst and application thereof
  • Ti-V loaded aluminum-pillared montmorillonite heterogeneous catalyst and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] (1) Purification of montmorillonite (MMT): Take 40g of Na-based montmorillonite from Linan, Zhejiang, China (Zhejiang Huate Company) and beat it with 1293mL of deionized water to make a suspension with a mass fraction of 3%, let it stand for 20h, discard The floating matter and residue were removed, the suspension was centrifuged and filtered, and the filter cake was dried at 110°C for 4 hours in an air atmosphere to obtain 26.8 g of purified montmorillonite (MMT).

[0032] (2) Preparation of aluminum crosslinking agent: 150mL, 1mol / L NaOH solution and 75mL, 1mol / L AlCl 3 Solution mixing, control of OH in the solution - with Al 3+ The molar ratio of the mixture is 2.0:1, the mixture is vigorously stirred at 80°C for 2h, aged at 40°C for 6h, and cooled to room temperature to obtain an aluminum crosslinking agent.

[0033] (3) Preparation of aluminum pillared montmorillonite (Al-MMT): Disperse 25g of purified montmorillonite (MMT) into 1225mL of deionized water, stir at...

Embodiment 2

[0038] Refer to the above preparation steps

[0039] (1) Purification of montmorillonite (MMT): Take 40g of Na-based montmorillonite from Linan, Zhejiang, China (Zhejiang Huate Company) and beat with 960mL deionized water to make a suspension with a mass fraction of 4%, let it stand for 18h, discard The floating matter and residue were removed, the suspension was centrifuged and filtered, and the filter cake was dried at 110°C for 5 hours in an air atmosphere to obtain 25.6 g of purified montmorillonite (MMT).

[0040] (2) Preparation of aluminum crosslinking agent: 210mL, 1mol / L NaOH solution and 100mL, 1mol / L AlCl 3 Solution mixing, control of OH- and Al in the solution 3+ The molar ratio of the mixture is 2.1:1, the mixture is vigorously stirred at 85°C for 3h, aged at 40°C for 6h, and cooled to room temperature to obtain an aluminum crosslinking agent.

[0041] (3) Preparation of aluminum pillared montmorillonite (Al-MMT): Disperse 25g of purified montmorillonite (MMT) i...

Embodiment 3

[0046] Refer to the above preparation steps

[0047] (1) Purification of montmorillonite (MMT): Take 40g of Na-based montmorillonite in Lin'an, Zhejiang, China (Zhejiang Huate Company) and beat it with 760mL of deionized water to make a suspension with a mass fraction of 5%, let it stand for 20h, discard The floating matter and residue were removed, the suspension was centrifuged and filtered, and the filter cake was dried at 120°C for 5 hours in an air atmosphere to obtain 26g of purified montmorillonite (MMT).

[0048](2) Preparation of aluminum crosslinking agent: 248mL, 1mol / L NaOH solution and 113mL, 1mol / L AlCl 3 Solution mixing, control of OH in the solution - with Al 3+ The molar ratio of the mixture is 2.2:1, the mixture is vigorously stirred at 90°C for 4h, aged at 35°C for 10h, and cooled to room temperature to obtain an aluminum crosslinking agent.

[0049] (3) Preparation of aluminum pillared montmorillonite (Al-MMT): Disperse 25g of purified montmorillonite (M...

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Abstract

The invention discloses a Ti-V loaded aluminum-pillared montmorillonite heterogeneous catalyst which is prepared by using self-made aluminum-pillared montmorillonite as a carrier, respectively using an ethanol solution of titanium tetrachloride and an oxalate solution of ammonium metavanadate as steeping liquor, loading titanium and vanadium oxides into the aluminum-pillared montmorillonite by using an excess impregnation method and drying and roasting the aluminum-pillared montmorillonite. The invention has the following advantages: raw materials are easily available; a preparation method is simple and is easy to operate; and the prepared catalyst has high activity and good stability. When the catalyst is used for a gas-solid phase reaction for synthesis of 2,3-cyclopentenopyridine from the raw materials comprising acrolein, cyclopentanone and ammonia gas, a good effect is obtained, and the catalyst is cheap and has a good development prospect.

Description

(1) Technical field [0001] The invention relates to a preparation method of a heterogeneous catalyst and its application in the synthesis of 2,3-cyclopentenopyridine by gas-solid phase reaction. (2) Background technology [0002] 2,3-cyclopentenopyridine is a pyridine derivative, an important intermediate in the synthesis of cefpirome, and is also widely used in the preparation of plant protection agents, synthetic resins, and plastic products. Cefpirome, as a fourth-generation new cephalosporin, has the characteristics of broad-spectrum, high efficiency, low toxicity, and enzyme resistance. It is the antibiotic with the strongest antibacterial activity against Gram-positive bacteria among known cephalosporins. It was first introduced in 1992 Marketed in Sweden under the trade name Cefrom. Although cefpirome has been on the market and used in developed countries for 20 years, due to the limitations of domestic economic and technological conditions, it has not formed a scale...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/22C07D221/04
Inventor 俞卫华周春晖童东绅张昌盛
Owner ZHEJIANG UNIV OF TECH
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