A kind of supported molybdenum series catalyst, its preparation method and application

A catalyst and supported technology, which is applied in the field of its preparation and supported molybdenum-based catalysts, can solve the problems that the reaction cannot be guaranteed, the preparation method is complicated, and the free hydroxyl group cannot be used, so as to achieve good dissolution effect, increase the number of active sites, and improve The effect of utilization

Active Publication Date: 2020-03-27
北京水木滨华科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the preparation method is relatively complicated, and 12mol / L concentrated hydrochloric acid is needed to convert MoO 3 dissolved, and the method of equal volume impregnation does not guarantee that SiO 2 Free hydroxyl groups on the surface of the support and MoOCl 3 The reaction is complete, SiO 2 The free hydroxyl groups on the surface of the carrier cannot be utilized to the maximum extent

Method used

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  • A kind of supported molybdenum series catalyst, its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Take 0.5g MoO 3 Place in a stainless steel reaction kettle lined with polytetrafluoroethylene, add 10mL, 6mol / L HCl aqueous solution, seal it, and react at 150°C for 2h.

[0040] Add 5.0g SiO to the above reaction kettle 2 Small balls, sealed, reacted at 150°C for 12h, washed, filtered to obtain MoOCl / SiO 2 catalyst.

[0041] to MoOCl / SiO 2 Add 20mL, 46wt.% tert-butyl hydroperoxide solution in tert-butanol to the catalyst, stir at 25°C for 12h, filter, and vacuum-dry at 40°C for 12h to obtain MoO 4 2- / SiO 2 catalyst.

Embodiment 2

[0043] Take 1.0g MoO 3 Place in a stainless steel reaction kettle lined with polytetrafluoroethylene, add 10mL, 6mol / L HCl aqueous solution, seal it, and react at 150°C for 2h.

[0044] Add 5.0g SiO to the above reaction kettle 2 Small balls, sealed, reacted at 150°C for 12h, washed, filtered to obtain MoOCl / SiO 2 catalyst.

[0045] to MoOCl / SiO 2 Add 20mL, 46wt.% tert-butyl hydroperoxide solution in tert-butanol to the catalyst, stir at 25°C for 12h, filter, and vacuum-dry at 40°C for 12h to obtain MoO 4 2- / SiO 2 catalyst.

Embodiment 3

[0047] Take 1.0g MoO 3 Place in a stainless steel reaction kettle lined with polytetrafluoroethylene, add 10mL, 6mol / L HCl aqueous solution, seal, react at 150°C for 12h, and filter.

[0048] The above filtrate was transferred to a polytetrafluoroethylene-lined stainless steel reactor, and 5.55 g of 10 wt% MoO was added 3 SiO 2 Small balls, sealed, reacted at 150°C for 12h, washed, filtered to obtain MoOCl / SiO 2 catalyst.

[0049] To the MoOCl / SiO 2 Add 20mL, 46wt% tert-butyl hydroperoxide solution in tert-butanol to the catalyst, stir at 25°C for 12h, filter, and vacuum-dry at 40°C for 12h to obtain MoO 4 2- / SiO 2 catalyst.

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Abstract

The invention discloses a supported molybdenum-based catalyst, a preparation method and applications thereof, wherein the catalyst is represented by a chemical formula MoO4<2-> / SiO2, and comprises a SiO2 carrier and MoO4<2-> supported on the surface of the SiO2 carrier, and the MoO4<2-> accounts for 2.3-5.5% of the mass of the catalyst. The preparation method of the catalyst comprises: dissolvingMoO3 in a HCl solution under hydrothermal conditions, adding a SiO2 carrier, carrying out a reaction to obtain a MoOCl / SiO2 catalyst, and oxidizing the MoOCl / SiO2 catalyst to obtain the MoO4<2-> / SiO2catalyst. According to the present invention, the free hydroxyl group content on the surface of the SiO2 carrier and the utilization rate of the SiO2 carrier surface are high, and the obtained catalyst can be used for olefin epoxidation reactions.

Description

technical field [0001] The invention belongs to the field of catalysts, and relates to a supported molybdenum-based catalyst, its preparation method and application. Background technique [0002] MoO 4 2- / SiO 2 It is a catalyst with high catalytic activity for olefin epoxidation, and is used to oxidize MoOCl / SiO by tert-butyl hydroperoxide 2 prepared, while MoOCl / SiO 2 MoOCl dissolved in hydrochloric acid solution 3 with SiO 2 Prepared by reaction of free hydroxyl groups on the surface. [0003] Gao Jian et al. (Gao Jian, Zhong Shunhe. Journal of Catalysis. 21(2000) 341-344.) and Zhang Yadong et al. (Zhang Yadong, Wang Zhenxing, Su Yuan. Journal of Chemical Engineering of Universities. 20(2006) 548-553.) will Molybdenum oxide was dissolved in 12mol / L hydrochloric acid solution, and the solution was impregnated in SiO by equal volume impregnation. 2 On the carrier, MoOCl / SiO is obtained after the steps of standing still and vacuum reaction 2 . Zhang Yadong et al. M...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/28C07D301/19C07D303/40
CPCB01J23/28C07D301/19C07D303/40
Inventor 王世华马敏郑虓解淑民
Owner 北京水木滨华科技有限公司
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