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CsPW/Zr-MCM-41 catalyst prepared in supercritical CO2 environment and application of catalyst

A zr-mcm-41, supercritical technology, used in physical/chemical process catalysts, organic compound/hydride/coordination complex catalysts, molecular sieve catalysts, etc. low selectivity issues

Active Publication Date: 2016-04-20
SHANDONG XINGQIANG CHEM IND TECH RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] The technical problem to be solved by the present invention is to provide a supercritical CO 2 The CsPW / Zr-MCM-41 catalyst prepared in the environment, to solve the problem that the conversion rate of glycerol and the selectivity of acrolein in the prior art are low and the service life of the catalyst is short

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Synthesis of Zr-MCM-41 (Si / Zr=5) carrier: 9.1ml of zirconium n-propoxide and 22.8ml of ethyl orthosilicate were mixed and stirred to obtain mixed system I for later use; 12.2g of hexadecyltrimethyl Dissolve ammonium chloride in 100ml of deionized water, and then mix with 110ml of 28wt% ammonia solution to obtain mixed system II for later use; add mixed system I dropwise to mixed system II under constant stirring, and stir at room temperature for 2 hours at 500r / min After the gel is formed, transfer the mixed system to a polytetrafluoroethylene-lined hydrothermal synthesis kettle, place it in an oven at 80°C for 40 hours, and then cool it to room temperature; filter the mixed solution in the reaction kettle , the solid part was washed 3 times with deionized water, and then the solid was dried in an oven at 80°C for 10 h; the dried solid was baked in a muffle furnace at 450°C for 3 h to obtain Zr-MCM-41 ( Si / Zr=5) carrier.

[0045] Synthesis of 20wt% cesium phosphotungst...

Embodiment 2

[0048] Synthesis of Zr-MCM-41 (Si / Zr=7) carrier: 6.5ml of zirconium n-propoxide and 22.8ml of ethyl orthosilicate were mixed and stirred to obtain mixed system I for later use; 12.2g of hexadecyltriethyl Dissolve ammonium bromide in 110ml of deionized water, and then mix with 110ml of 28wt% ammonia solution to obtain mixed system II for later use; add mixed system I dropwise to mixed system II under constant stirring, and stir at room temperature for 3 hours at 500r / min After the gel was formed, the mixed system was transferred to a polytetrafluoroethylene-lined hydrothermal synthesis kettle, and placed in an oven at 100°C for 45 hours, then cooled to room temperature; the mixed solution in the reaction kettle was filtered , the solid part was washed 4 times with deionized water, and then the solid was dried in a drying oven at 100 °C for 12 h; the dried solid was placed in a muffle furnace at 500 °C for 4 h to prepare Zr-MCM-41 ( Si / Zr=7) carrier.

[0049] Synthesis of 30wt%...

Embodiment 3

[0052] Synthesis of Zr-MCM-41 (Si / Zr=10) carrier: 4.5ml of zirconium n-propoxide and 22.8ml of ethyl orthosilicate were mixed and stirred to obtain mixed system I for later use; then 12.2g of hexadecyl trimethyl Ammonium bromide was dissolved in 100ml of deionized water, and then mixed with 110ml of 28wt% ammonia solution to obtain the mixed system II for later use; under constant stirring, the mixed system I was added dropwise to the mixed system II, and stirred at room temperature at 500r / min After 4 hours until the gel was formed, the mixed system was transferred to a polytetrafluoroethylene-lined hydrothermal synthesis kettle, and placed in an oven at 80°C for 50 hours, then cooled to room temperature; the mixed solution in the reaction kettle was Filter, wash the solid part with deionized water for 5 times, then place the solid in a drying oven at 100°C for 10 hours; place the dried solid in a muffle furnace at 550°C for 5 hours to prepare Zr-MCM-41 (Si / Zr=10) support.

...

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Abstract

The invention discloses a CsPW / Zr-MCM-41 catalyst prepared in a supercritical CO2 environment. The preparation method comprises the following steps: Zr-MCM-41 is taken as the carrier, and 10-60% of Cs modified salts is loaded by adopting the supercritical CO2 impregnation technology; with the utilization of the catalyst, the glycerin conversion rate reaches 65.2-100%, the acrolein selectivity reaches 56.8-85.4%; the invention further discloses application of the CsPW / Zr-MCM-41 catalyst to preparation of acrolein through glycerol selective dehydration. Compared with the prior art, the catalyst prepared by adopting the preparation method has the advantages that the dispersion degree of Cs modified salt on the carrier is high, the acting force between the Cs modified salt and the carrier is strong, the hydrothermal stability is high, the acidity loss possibility is low, and meanwhile, when compared with the conventional product, the obtained product is high in glycerin conversion rate and acrolein selectivity, and long in service life.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, in particular to a supercritical CO 2 CsPW / Zr-MCM-41 catalyst prepared in ambient and its application. Background technique [0002] As the world's oil resources become increasingly tense, biodiesel, which can be used as an alternative energy source, is widely favored. Accompanied by its increasing production, a large amount of by-product glycerol has led to a surplus in the market. Glycerol is an important biorenewable resource, which is currently widely used in the fields of medicine, food, tobacco and cosmetics. Therefore, research on converting glycerol into high value-added products has become a hotspot. [0003] Acrolein is an important organic synthesis intermediate, mainly used in pharmaceutical synthesis, paper making, paint, oil field, organic synthesis industry and other fields. The most important use of acrolein is the synthesis of methionine, an animal feed additive, and the pre...

Claims

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Application Information

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IPC IPC(8): B01J31/26C07C47/22C07C45/52
CPCB01J27/188B01J29/041C07C45/52C07C47/22Y02P20/54
Inventor 丁建飞马田林严翠霞邵荣许伟
Owner SHANDONG XINGQIANG CHEM IND TECH RES INST CO LTD
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