Tungstenic functional mesoporous molecular sieve catalyst for preparation of glutaric acid based on glutaraldehyde oxidation and preparation method of catalyst

A technology for oxidative production of glutaric acid and catalyst, applied in molecular sieve catalyst, physical/chemical process catalyst, carboxylate preparation, etc., can solve the problems of low activity, high price, harsh synthesis conditions, etc. loss, the effect of excellent catalytic performance

Inactive Publication Date: 2018-08-03
QINGDAO UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chen Hui (Research on Green Synthesis Technology and New Catalyst of Glutaric Acid [D]. Shanghai: Fudan University, 2007) proposed to use 1,2-cyclopentanediol as raw material, hydrogen peroxide as oxidant, and tungsten-containing mesoporous molecular sieve MCM- 41 is a catalyst for the preparation of glutaric acid, but 1,2-cyclopentanediol is expensive and the synthesis conditions are harsh, and the activity of the recyclable tungsten-containing mesoporous molecular sieve MCM-41 catalyst is about 20% lower than that of the homogeneous catalyst tungstic acid

Method used

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  • Tungstenic functional mesoporous molecular sieve catalyst for preparation of glutaric acid based on glutaraldehyde oxidation and preparation method of catalyst
  • Tungstenic functional mesoporous molecular sieve catalyst for preparation of glutaric acid based on glutaraldehyde oxidation and preparation method of catalyst
  • Tungstenic functional mesoporous molecular sieve catalyst for preparation of glutaric acid based on glutaraldehyde oxidation and preparation method of catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Disperse 1g of mesoporous molecular sieve SBA-15 in 10g of benzene, stir at 25°C for 2h, add 0.05g of 3-aminopropyltriethoxysilane, stir, reflux at 110°C for 8h, filter, and dry at 100°C to obtain solid powder a; The solid powder a was subjected to Soxhlet extraction in benzene, dried at 100°C to obtain solid powder b; 18 mL of dichloromethane was added to the solid powder b, stirred for 2 h, 0.1 g of trifluoromethanesulfonic acid was added, and stirred for 6 h , filtered, washed with ethanol, and dried at 100°C to obtain solid powder c; add 66 mL of an aqueous solution containing 0.2 g of sodium tungstate to the solid powder c, stir for 12 hours, filter, wash with water, and dry at 100°C to obtain solid powder d. The solid powder d is the catalyst, numbered #1.

Embodiment 2

[0034] Disperse 1g of mesoporous molecular sieve SBA-15 in 16g of toluene, stir at 29°C for 2.6h, add 0.07g of n-propyltrimethoxysilane, stir, reflux at 122°C for 9.6h, filter, and dry at 100°C to obtain solid powder a; The solid powder a was subjected to Soxhlet extraction in toluene, and dried at 100°C to obtain solid powder b; add 24 mL of dichloromethane to the solid powder b, stir for 2.4 h, add 0.28 g of trifluoromethanesulfonic acid, and stir 7.2h, filter, wash with ethanol, dry at 100°C to obtain solid powder c; add 37.5mL aqueous solution containing 0.15g of 12-phosphotungstic acid to the solid powder c, stir for 19.2h, filter, wash with water, and dry at 100°C to obtain solid Powder d, the solid powder d is the catalyst, numbered #2.

Embodiment 3

[0036]Disperse 1g of mesoporous molecular sieve SBA-15 in 22g of xylene, stir at 33°C for 3.2h, add 0.09g of diphenyldichlorosilane, stir, reflux at 134°C for 11.2h, filter, and dry at 100°C to obtain solid powder a; The solid powder a is subjected to Soxhlet extraction in xylene, dried at 100°C to obtain solid powder b; add 30 mL of dichloromethane to the solid powder b, stir for 3.8 hours, add 0.46 g of trifluoromethanesulfonic acid, and stir 8.4h, filter, wash with ethanol, dry at 100°C to obtain solid powder c; add 30mL aqueous solution containing 0.15g of 18-phosphoditungstic acid to the solid powder c, stir for 26.4h, filter, wash with water, and dry at 100°C to obtain solid Powder d, the solid powder d is the catalyst, numbered #3.

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Abstract

The invention belongs to the technical field of catalysts and relates to a tungstenic functional mesoporous molecular sieve catalyst for preparation of glutaric acid based on glutaraldehyde oxidationand a preparation method of the catalyst. The catalyst is a functional mesoporous molecular sieve SBA-15 supported tungstic catalyst (W-SBA-15), and tungsten is introduced into a framework of a functional mesoporous molecular sieve SBA-15 with a post-synthesis method. The method comprises steps as follows: the mesoporous molecular sieve SBA-15 is dispersed in a solvent and stirred, an organosilaneagent is added, a mixture is stirred, subjected to reflux, filtered, dried, subjected to Soxhlet extraction and dried, dichloromethane is added, stirring is performed, trifluoromethanesulfonic acid is added, stirring, filtering, ethanol rinsing and drying are performed, then a tungsten source is added, stirring, filtering, water washing and drying are performed, and the catalyst is obtained. Themethod is easy to operate. The prepared tungstenic functional mesoporous molecular sieve SBA-15 heterogeneous catalyst is highly ordered in porous structure, tungsten species is highly dispersed, andultrahigh stability is obtained. The prepared W-SBA-15 heterogeneous catalyst is applied to a reaction of preparation of glutaric acid based on glutaraldehyde oxidation, conversion rate of glutaraldehyde can reach 99% or higher, yield of glutaric acid can reach 98% or higher, and the catalyst can be repeatedly used 20 times or more with unchanged activity.

Description

【Technical field】 [0001] The invention relates to a tungsten-containing functionalized mesoporous molecular sieve catalyst for glutaraldehyde oxidation to glutaric acid and a preparation method thereof, belonging to the technical field of catalysts. 【Background technique】 [0002] Glutaric acid is an important chemical raw material and organic intermediate. Such as the preparation of glutaric anhydride, α-ketoglutaric acid, peroxyglutaric acid, B-(4-chlorophenyl) glutaric acid and intermediates for antihypertensive agents; such as synthetic resins, rubber and plasticizers The initiator of the agent; such as materials such as sterilizing solution and cleaning agent. At present, the methods for synthesizing glutaric acid mainly include recovery method and chemical synthesis method. The recovery method is mainly applicable to the industrial production of glutaric acid, which refers to the recovery of glutaric acid from the by-products of adipic acid production. This method re...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/03C07C51/285C07C55/12
CPCB01J29/0341C07C51/285C07C55/12
Inventor 吕志果靳满满郭振美
Owner QINGDAO UNIV OF SCI & TECH
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