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High stability supported heteropoly acid catalyst and its preparation method and use

A high-stability, heteropolyacid technology, applied in the field of catalytic chemistry, can solve problems such as the loss of active components of heteropolyacids, strict requirements for experimental equipment, poor catalyst stability, etc., to achieve continuous catalytic ability, separation and reuse convenience , The effect of long catalytic life

Inactive Publication Date: 2016-12-07
YANCHENG INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the large amount of water vapor generated during the dehydration reaction of glycerin, the force between the heteropolyacid and the carrier is small, and the combination is not strong enough, resulting in the rapid loss of the active components of the heteropolyacid and poor catalyst stability.
[0004] In the prior art, we can use supercritical fluid technology to increase the adhesion rate of heteropolyacids, but such technology requires high temperature and high pressure conditions, which not only adds complicated process conditions to the actual operation, but also has very high requirements for experimental equipment. harsh

Method used

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  • High stability supported heteropoly acid catalyst and its preparation method and use
  • High stability supported heteropoly acid catalyst and its preparation method and use

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preparation example Construction

[0017] The embodiment of the present invention proposes a preparation method of a highly stable supported heteropolyacid catalyst, which comprises the following steps:

[0018] Modification step: uniformly mix the carrier material and the silane coupling agent solution, filter and dry to obtain the modified carrier material.

[0019] Further, the silane coupling agent solution is prepared by mixing a silane coupling agent with an organic solvent, wherein the silane coupling agent is 3-aminopropyltrimethoxysilane (KH-540), N-aminoethyl-γ- At least one of aminopropyltrimethoxysilane (KH-792) and divinyltriaminopropyltrimethoxysilane (NQ-62); the organic solvent is any one of ethanol, toluene and acetone; the used The obtained silane coupling agent and organic solvent can be purchased directly from the market.

[0020] Further, the carrier material is at least one of MCM-41, MCM-48, MCM-50 and FSM-16. MCM-41, MCM-48, MCM-50 and FSM-16 are all molecular sieves, and can be purcha...

Embodiment 1

[0035] This embodiment provides a highly stable phosphotungstic acid / MCM-41 catalyst, the preparation steps of which are as follows:

[0036] Modification steps: Add 0.18g KH-540 to 50ml ethanol, stir and mix evenly; then add 2gMCM-41 to it, reflux and stir at 80°C for 20h, then filter with suction, wash twice with ethanol solution, and Dry for 8 hours;

[0037] Loading step: immerse the above-mentioned modified MCM-41 in phosphotungstic acid solution. The phosphotungstic acid solution used is obtained by dissolving 0.22g of phosphotungstic acid in 40mL water, ultrasonically treated for 2h, then separated and dried at 120°C for 8h. A highly stable phosphotungstic acid / MCM-41 catalyst was obtained.

Embodiment 2

[0039] This embodiment provides a highly stable silicotungstic acid / MCM-41 catalyst, the preparation steps of which are as follows:

[0040] Modification steps: Add 0.22g KH-792 to 50ml ethanol, stir and mix evenly; then add 2gMCM-41 to it, reflux and stir at 80°C for 24h, then filter with suction, wash with ethanol solution 3 times, and heat at 80°C Dry for 10 hours;

[0041] Loading step: immerse the above-mentioned modified MCM-41 in silicotungstic acid solution, which is obtained by dissolving 0.5g silicotungstic acid in 40mL water, ultrasonically treat for 2h, then separate and dry at 80°C for 8h, A highly stable silicotungstic acid / MCM-41 catalyst was obtained.

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Abstract

The invention discloses a preparation method of a high stability supported heteropoly acid catalyst and belongs to the field of catalytic chemistry. The preparation method comprises uniformly mixing a carrier material and a silane coupling agent, filtering and drying the mixture to obtain a modified carrier material, dipping the modified carrier in a heteropoly acid solution and carrying out separation and drying to obtain the high stability supported heteropoly acid catalyst. The preparation method has mild conditions, simple processes, operation safety and reliability and no high temperature and high pressure requirement and is suitable for laboratory synthesis and large-scale industrial production. The invention provides the high stability supported heteropoly acid catalyst. The high stability supported heteropoly acid catalyst has good hydrothermal stability and can keep catalytic activity for a long time. The invention also provides a use of the high stability supported heteropoly acid catalyst in conversion of glycerin into acrolein. The high stability supported heteropoly acid catalyst can keep a high conversion rate and high selectivity for a long time and has a low loss rate.

Description

technical field [0001] The invention relates to the field of catalytic chemistry, and in particular to a high-stability loaded heteropolyacid catalyst and its preparation method and application. Background technique [0002] Biodiesel is a clean and renewable energy with good environmental protection and safety, and it is playing an increasingly important role in the global energy structure. However, in the actual production of biodiesel, bioglycerol, which is one of the main by-products, has not been well utilized, resulting in a great waste of resources. The conversion of glycerol to acrolein, an intermediate in organic synthesis, has always been considered a good solution to the problem. However, there are still problems such as low conversion rate and poor selectivity in this conversion reaction. Finding a suitable catalyst is still an urgent problem to be solved. . [0003] Supported heteropolyacid catalyst is a kind of catalyst with excellent catalytic performance, w...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/04B01J29/78B01J31/26C07C45/52C07C47/22
CPCB01J29/045B01J29/78C07C45/52C07C47/22
Inventor 丁建飞马田林严翠霞邵荣许伟
Owner YANCHENG INST OF TECH
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