A kind of preparation method of olefin epoxidation catalyst of polyaniline supported heteropolyacid

A technology for supporting heteropolyacids and catalysts, which is applied in the direction of physical/chemical process catalysts, chemical instruments and methods, organic compounds/hydrides/coordination complex catalysts, etc. It can solve the problem of large loss of non-supported catalysts and difficulty in industrialization , complex preparation process and other issues, to achieve good catalytic epoxidation effect, easy to scale up and industrialize, and simple preparation process

Active Publication Date: 2021-06-25
JIANGSU YANGNONG CHEM GROUP +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Literature (Li Qianding, Zhang Liang, Xu Haisheng. Research progress on supported phosphotungsten-molybdenum heteropolyacid catalysts[J]. Petrochemical Technology and Application, 2011,29(2):179-185.) and patents (CN201180011178.0, CN201610121435. 0, CN98117816.2, CN201110100126.2, CN02100237.1) Taking phosphotungstomolybdenum heteropolyacid as an example, it is pointed out that the supported catalyst can effectively solve the problems of equipment corrosion and catalyst loss, but the current direct loading method has the distribution of catalyst active groups The problem of unevenness and easy loss; in the grafting method, there is a problem that the active component of the catalyst is easy to interact with the grafted group, which reduces the activity of the catalyst; the sealing method uses zeolite and molecular sieve as the carrier, so that the catalyst is in situ in the channel Formation, no grafted functional groups and more uniform catalyst distribution, the obtained supported catalyst is close to the intrinsic catalyst activity, but there are problems of complex preparation process and difficulty in industrialization
[0003] At present, among heteropolyacid catalysts for olefin epoxidation using hydrogen peroxide as an oxygen source, non-supported catalysts often suffer from large losses and insufficient economic efficiency, while supported catalysts often need to be prepared through steps such as carrier synthesis and catalyst loading, and the process is complicated. Highly affected by the substrate, not very versatile

Method used

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  • A kind of preparation method of olefin epoxidation catalyst of polyaniline supported heteropolyacid
  • A kind of preparation method of olefin epoxidation catalyst of polyaniline supported heteropolyacid
  • A kind of preparation method of olefin epoxidation catalyst of polyaniline supported heteropolyacid

Examples

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Effect test

Embodiment 1

[0024] Catalyst preparation: at room temperature, dissolve 13.24g of sodium tungstate dihydrate (0.04mol) in 20g of water, and add 9.22g of 85% phosphoric acid (0.08mol), 31.56g of 30% H 2 o 2 solution (0.28mol), the resulting clear solution is solution A; slowly add 26.48g aniline (0.28mol) dropwise to 111.45g 25% phosphoric acid solution (0.28mol), and the resulting clear solution is solution B.

[0025] Under ice bath, slowly add solution A dropwise to solution B, control the temperature of the kettle at 5-10°C, stir vigorously for 24 hours, filter, wash the filter cake with water until the washing liquid is neutral, dry the filter cake under vacuum at 60°C for 6 hours, and obtain 28.18g of catalyst , tungsten content 22.31%, load rate 85.16%, marked as PW-PAn.

Embodiment 2-5

[0027] Catalyst preparation: the preparation process is the same as in Example 1, only 0.01mol of different salts are added before the hydrogen peroxide is added dropwise, and the obtained results are as follows:

[0028] metal salt Tungsten loading rate / % Catalyst code Example 2 copper nitrate 84.64 PWCu-PAn Example 3 Sodium vanadate 84.31 PWV-PAn Example 4 Sodium silicate 83.51 PWSi-PAn Example 5 Sodium molybdate 86.21 PWMo-PAn

Embodiment 6

[0030] Catalyst preparation: The preparation process is the same as in Example 5, except that 4.12 g of sodium molybdate (0.02 mol) is added before the hydrogen peroxide is added dropwise, and the tungsten loading rate of the obtained catalyst is 86.25%, which is marked as PWMo-PAn-2.

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Abstract

The invention belongs to the field of catalyst preparation methods in petrochemical industry, and more specifically relates to a preparation method and application of a polyaniline-loaded heteropolyacid-supported olefin epoxidation catalyst. The invention provides a preparation method of an olefin epoxidation catalyst for polyaniline-loaded heteropolyacids. The integrated polyaniline-loaded heteropolyacid catalyst is synthesized by a one-pot method, which has the advantages of simple process and easy scale-up. Its application In the olefin epoxidation reaction, the conversion rate of hydrogen peroxide is ≥ 97%, the yield of epoxidized products is ≥ 85%, and the selectivity is ≥ 90%. The catalyst has the advantages of strong versatility, stable activity and high recovery rate during the use of the catalyst , is a catalyst preparation method that is easy to realize industrialization.

Description

technical field [0001] The invention belongs to the field of catalyst preparation methods in petrochemical industry, and more specifically relates to a preparation method and application of a polyaniline-loaded heteropolyacid olefin epoxidation catalyst. Background technique [0002] Olefin epoxidation is an important organic reaction, and its products have a wide range of applications. For example, styrene oxide is an important intermediate in the pharmaceutical and fragrance industries, ethylene oxide and propylene oxide are key raw materials for the synthesis of polyether polyols, polyurethanes, and surfactants, and epichlorohydrin is a key raw material for the synthesis of epoxy resins. , The base material of chlorohydrin rubber. Taking propylene oxide as an example, the current industrial production methods in my country mainly include chlorohydrin method, co-oxidation method and direct oxidation method. The chlorohydrin method consumes a lot of resources, has serious...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/34C07D303/08C07D303/14
CPCB01J31/34B01J2231/72C07D301/12C07D303/08C07D303/14Y02P20/584
Inventor 王根林丁克鸿徐林王铖王刚殷恒志戚明甫许越
Owner JIANGSU YANGNONG CHEM GROUP
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