Supported heteropolyacid catalyst, preparation method and application thereof

A heteropolyacid and catalyst technology, applied in the field of catalytic chemistry, can solve the problems that the conversion and utilization of bioglycerol have not been well resolved, increase the risk, and require harsh reaction equipment, and achieve separation and reuse. High, meet the effect of industrial production

Inactive Publication Date: 2016-10-12
艾希姆(深圳)科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

As the main by-product in the biodiesel production process, the conversion and utilization of bioglycerol has not been well resolved.
However, the supercritical conditions of the reaction have high requirements on temperature and pressure, which not only imposes strict requirements on the reaction equipment, but also increases the danger in actual operation.

Method used

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  • Supported heteropolyacid catalyst, preparation method and application thereof
  • Supported heteropolyacid catalyst, preparation method and application thereof
  • Supported heteropolyacid catalyst, preparation method and application thereof

Examples

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preparation example Construction

[0020] The embodiment of the present invention proposes a preparation method of a supported heteropolyacid catalyst, comprising the following steps:

[0021] Step A: immerse the carrier material in the heteropolyacid aqueous solution, stir and mix evenly to obtain a slurry.

[0022] Specifically, 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 pure silica molecular sieves, which can be purchased directly from the market. Among them, MCM-41 pure silicon molecular sieve can also be prepared by the following method: after dissolving the template agent in deionized water, add ammonia solution and mix evenly to obtain solution A; slowly add silicon source dropwise to solution A under constant stirring, After stirring at low temperature for 2-5 hours, the solution B was obtained; the solution B was crystallized at 80-110°C for 40-50 hours, filtered after cooling, and the solid part was collected, washed, dried and...

Embodiment 1

[0035] This embodiment provides a supercritical N 2 The phosphotungstic acid / MCM-41 catalyst prepared in the environment, its preparation steps are as follows:

[0036] Dissolve 0.11g of phosphotungstic acid in 20ml of deionized water in the reactor, stir and mix evenly to obtain an aqueous solution of phosphotungstic acid, immerse 1.0g of MCM-41 carrier in the above aqueous solution of phosphotungstic acid, stir and mix evenly to obtain a slurry ; Use temperature program to raise the temperature in the reactor to 60°C, and then use a high-pressure syringe pump to inject N 2 Fill the reaction kettle with gas to make the pressure in the kettle reach 5MPa to reach the supercritical condition, and then maintain the supercritical condition for 2 hours. After the supercritical treatment is completed, lower the temperature, release the pressure, and unload the kettle to obtain the crude catalyst; move the crude catalyst to the centrifuge The tube was centrifuged at 3000r / min for 10...

Embodiment 2

[0039] This embodiment provides a supercritical N 2 The phosphotungstic acid / MCM-41 catalyst prepared in the environment, its preparation steps are as follows:

[0040] Dissolve 0.25g of phosphotungstic acid in 20ml of deionized water in the reaction kettle, stir and mix evenly to obtain an aqueous solution of phosphotungstic acid, immerse 1.0g of MCM-41 carrier in the above aqueous solution of phosphotungstic acid, stir and mix evenly to obtain a slurry ; The temperature in the reactor was raised to 50°C by temperature programming, and then the N 2 Fill the reaction kettle with gas to make the pressure in the kettle reach 6MPa to reach the supercritical condition, and then maintain the supercritical condition for 4 hours. After the supercritical treatment is completed, lower the temperature, release the pressure, and unload the kettle to obtain the crude catalyst; move the crude catalyst to the centrifuge The tube was centrifuged at 5000r / min for 15min, and the solid part of...

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Abstract

Belonging to the field of catalytic chemistry, the invention relates to a preparation method of a supported heteropolyacid catalyst. The method includes the steps of: dipping a carrier material in a heteropolyacid aqueous solution and performing stirring to obtain a pulp; placing the pulp in a N2 environment, raising the temperature and increasing the pressure to make N2 reach a supercritical condition and sustaining the state for 2-6h to obtain a catalyst crude product; and separating and drying the catalyst crude product to obtain the supported heteropolyacid catalyst. In addition, the invention also relates to the supported heteropolyacid catalyst prepared by the method and application thereof in conversion of glycerin to acraldehyde. The method has the advantages of simple operation, mild conditions, and good safety. The prepared supported heteropolyacid catalyst has good dispersibility, high catalytic activity, and is easy to recover. The reaction of conversion of glycerin to acraldehyde under the catalysis of the catalyst achieves excellent conversion rate, selectivity and yield, and effectively alleviates the loss of the catalyst active components.

Description

technical field [0001] The invention relates to the field of catalytic chemistry, and in particular to a supported heteropolyacid catalyst and its preparation method and application. Background technique [0002] Biodiesel, as a clean and renewable energy with good environmental protection and safety, has been paid more and more attention by people. As the main by-product in the biodiesel production process, the conversion and utilization of bioglycerol has not been well resolved. The conversion of glycerol to acrolein, an intermediate in organic synthesis, has always been considered a good method to solve the problem, but the conversion reaction still has problems such as low conversion rate and poor selectivity. [0003] Supported heteropolyacid catalyst is a kind of catalyst with excellent catalytic performance, which can obtain better conversion rate and selectivity in the reaction of converting glycerol into acrolein. However, the supported heteropolyacid prepared by ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/18B01J31/16B01J27/188B01J29/03C07C45/52C07C47/22
CPCB01J27/188B01J27/19B01J29/0341B01J2229/18C07C45/52C07C47/22Y02P20/54Y02P20/584
Inventor 丁建飞马田林严翠霞邵荣许伟
Owner 艾希姆(深圳)科技有限公司
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