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Catalyst for preparing isobutene by dehydrating tertiary butanol and preparation method of catalyst

A catalyst and isobutylene technology, applied in the direction of chemical instruments and methods, physical/chemical process catalysts, organic compounds/hydrides/coordination complex catalysts, etc., can solve the problems of multi-polymerization and temperature-resistant isobutylene, and reduce the use of Grade, overcoming temperature resistance, and reducing the effect of condensing production costs

Active Publication Date: 2014-07-23
WANHUA CHEM GRP CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of the present invention is to provide a catalyst for the preparation of isobutene by a liquid-phase method. The catalyst is used for the reaction of isobutene prepared by a liquid-phase method, which solves the problems of catalyst loading, temperature resistance limitation and isobutene polymerization in the preparation process. , improving the selectivity and atom economy of the reaction

Method used

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  • Catalyst for preparing isobutene by dehydrating tertiary butanol and preparation method of catalyst
  • Catalyst for preparing isobutene by dehydrating tertiary butanol and preparation method of catalyst
  • Catalyst for preparing isobutene by dehydrating tertiary butanol and preparation method of catalyst

Examples

Experimental program
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Effect test

Embodiment 1

[0028] 1070.26g ZrOCl 2 , 210.57gTiCl 2 , 69.24gAlCl 3 After preparing a solution of 0.2mol / L, mix it evenly, under continuous stirring, add 0.5g of polymerization inhibitor THQ and 1.5g of dimethyl dodecyl silicon chloride, stir for 15min after adding, and mix the mixture with 50wt% ammonia water was dripped into the reactor simultaneously for precipitation, and the pH was controlled to be 9.5. After the precipitation was complete, it was aged for 5 hours, and washed with deionized water until there was no Cl - ions, the resulting precipitate was dried at 360K for 12h, and calcined at 853K for 4h to obtain a catalyst precursor, in which the catalyst substrate was 905.98g, and its composition was 15.6wt%TiO 2 , 2.9wt%Al 2 o 3 , 81.4wt%ZrO 2 , the inhibition part is 0.16wt% of the catalyst substrate.

[0029] The obtained catalyst precursor was dispersed in 10 L of 20 wt% (NH 4 )HS 2 o 8 Soak in the solution for 3.5h, filter the solution, rinse the solid with deionized...

Embodiment 2

[0033] 1140.41gZrOCl 2 , 210.57gTiCl 2 , 34.62gAlCl 3 After preparing a 0.2mol / L solution, mix it evenly, under continuous heating and stirring, add 1g of polymerization inhibitor MTBHQ and 4g of methyl ethyl undecyl silicon chloride, stir for 15min after the addition, and mix the mixture Drop into the reactor simultaneously with 50% ammonia water for precipitation, control the pH to 9.85, age for 5 hours after the precipitation is complete, and wash with deionized water until there is no Cl - ions, the resulting precipitate was dried at 360K for 12h and calcined at 815K for 5h to obtain a catalyst precursor, wherein the catalyst substrate was 941.1g, and its composition was 15.1wt%TiO 2 , 1.4wt%Al 2 o 3 , 83.5wt%ZrO 2 , the polymerization inhibition part is 0.25wt% of the catalyst substrate.

[0034] The obtained catalyst matrix was dispersed in 10 L of 25wt% (NH 4 )HSO 3 Soak in the solution for 3h, filter the solution, rinse the solid with deionized water until the ...

Embodiment 3

[0038] 1070.26g ZrOCl 2 , 280.76gTiCl 2 , 34.62gAlCl 3 After preparing a solution of 0.2mol / L, mix it evenly, under continuous heating and stirring, add 2g of polymerization inhibitor DNBP and 7g of dimethyl dodecyl silicon chloride, stir for 15min after adding, mix the mixture with 50% ammonia water was dripped into the reactor at the same time to precipitate, and the pH was controlled to be 9.5. After the precipitation was complete, it was aged for 5 hours, and washed with deionized water until there was no Cl - ions, the resulting precipitate was dried at 360K for 12h, and calcined at 837K for 4h to obtain a catalyst precursor, wherein the catalyst substrate was 940g, and its composition was 20.1%TiO 2 , 1.4%Al2O 3 , 78.5%ZrO 2 , the polymerization inhibition part is 0.42% of the catalyst matrix.

[0039] The obtained catalyst matrix was dispersed in 9 L of 30wt% (NH 4 )HSO 4 Soak in the solution for 1.6h, filter the solution, rinse the solid with deionized water unt...

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Abstract

The invention provides a catalyst for preparing isobutene by a liquid phase method and a preparation method of the catalyst. The formula of the catalyst is [A.B]<+>L<->, wherein A is a catalyst base body, B is a polymerization inhibition part and L is an acidic ion; the content of the acidic ion L is 1wt%-35wt%, preferably 5wt%-15wt%; the polymerization inhibition part B is composed of a polymerization inhibitor and an auxiliary agent by a reaction; the content of the polymerization inhibition part B is 0.01wt%-5wt%, preferably 0.1wt%-1.5wt%; the balance is the catalyst base body A. In the presence of the catalyst, tertiary butanol is rectified and dehydrated by the reaction to prepare isobutene; the selectivity of isobutene can be improved obviously and a polymer is prevented from being generated; the grade of condensed water is lowered; meanwhile, the filling problem of a catalyst in an existing reaction rectification process is solved; the catalyst meets an economical and green chemical idea.

Description

technical field [0001] The invention relates to an alcohol dehydration catalyst and a preparation method thereof, in particular to a liquid-phase method for dehydrating tert-butanol to prepare isobutene and a preparation method thereof, so as to avoid olefin polymerization in the production process. technical background [0002] Isobutylene is an important chemical raw material, which is used to synthesize polyisobutylene rubber, butyl rubber, and the main monomer of isoprene. It is also widely used as medicine, pesticide, antioxidant, synthetic high-grade lubricating oil, gasoline additive and other Raw materials for fine chemical products. [0003] At present, isobutene mainly comes from the separation of C4 fractions in refining and chemical enterprises or the dehydration of tert-butanol by-product of propylene oxide. , isomerization, co-oxidation, etc., among which tert-butanol dehydration is the most simple and effective method to obtain high-purity isobutene. [0004...

Claims

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Application Information

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IPC IPC(8): B01J31/38C07C11/09C07C1/24C07C7/20
Inventor 王中华何岩董如伟吕艳红黎源
Owner WANHUA CHEM GRP CO LTD
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