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Mesoporous ion liquid heteropolyacid salt catalyst for benzene hydroxylation reaction, preparation method and applications thereof

A technology of ionic liquids and heteropolyacids, which is applied in the preparation of organic compounds, catalysts for physical/chemical processes, catalysts for organic compounds/hydrides/coordination complexes, etc., and can meet the high requirements for control conditions and safety technology , Catalyst recycling difficulties, phenol separation and refining difficulties, etc., to achieve high hydrogen peroxide utilization rate, realize industrial application, and facilitate recycling and reuse.

Inactive Publication Date: 2017-09-22
SHANDONG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the production process of phenol by the cumene method is relatively mature, there are still many defects: the intermediate product cumene hydroperoxide is an unstable peroxide, and it has high requirements for control conditions and safety technology; The production process is long, which makes it difficult to increase the yield of phenol; the separation and purification of phenol is difficult
However, common ionic liquid heteropolyacid salt catalysts are usually easily soluble in H 2 o 2 The benzene hydroxylation system as an oxygen source brings difficulties to the recycling of catalysts

Method used

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  • Mesoporous ion liquid heteropolyacid salt catalyst for benzene hydroxylation reaction, preparation method and applications thereof
  • Mesoporous ion liquid heteropolyacid salt catalyst for benzene hydroxylation reaction, preparation method and applications thereof
  • Mesoporous ion liquid heteropolyacid salt catalyst for benzene hydroxylation reaction, preparation method and applications thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] 1. Preparation of Mesoporous Ionic Liquid Heteropolyacid Salt Catalyst

[0042] (1)H 5 PMo 10 V 2 o 40 Synthesis of Heteropolyacids

[0043] Weigh 16.5g MoO respectively 3 and 2.1g V 2 o 5 , dissolved in 250mL of distilled water, heated the above solution to reflux to 120°C under vigorous stirring, then slowly added 1.33g of 85wt.% phosphoric acid, continued heating after the addition was completed and kept at this temperature for 48h, during this process, cloudy The solution gradually turns into a clear and transparent orange solution; then slowly evaporate the water to dryness in a vacuum oven at 50°C to obtain an orange-red solid; finally dissolve the solid in a small amount of distilled water, slowly precipitate at 0°C, and re- Crystallize 3 times to get H 5 PMo 10 V 2 o 40 Heteropolyacids.

[0044] (2) Synthesis of xylene-coupled imidazolium ionic liquids

[0045] Add 0.2mol of methylimidazole and 0.1mol of α,α'-dichloro-p-xylene into a 100mL three-necke...

Embodiment 2

[0051] Prepare the method for mesoporous ionic liquid heteropolyacid salt catalyst according to embodiment 1, with the imidazolium ionic liquid of xylene coupling and H 5 PMo 10 V 2 o 40 The molar ratio of heteropolyacid is 2:1 to prepare the catalyst [PxyDim] 2 HPMoV 2 , all the other conditions are identical with embodiment 1. The specific method is as follows:

[0052] H 5 PMo 10 V 2 o 40 Heteropolyacid is added in the imidazole ionic liquid aqueous solution of xylene coupling and reacts, wherein the imidazole ionic liquid of xylene coupling and H 5 PMo 10 V 2 o 40 The molar ratio of the heteropolyacid is 2:1, solid precipitation occurs immediately, continue to stir at 25°C for 24h, filter, wash twice with deionized water, and then dry at 80°C for 12h to obtain the catalyst [PxyDim] 2 HPMoV 2 , with a specific surface area of ​​49.3m 2 g -1 , with a total pore volume of 0.44m 3 g -1 , the average pore diameter is 35.6nm.

[0053] According to the applicat...

Embodiment 3

[0056] According to the method for preparing mesoporous ionic liquid heteropolyacid salt catalyst according to embodiment 1, the imidazole ionic liquid of xylene coupling and H 5 PMo 10 V 2 o 40 The mixed solution of heteropolyacid was stirred at 80℃ for 12h to prepare the catalyst [PxyDim] 2.5 PMOV 2 , all the other conditions are identical with embodiment 1. The specific method is as follows:

[0057] H 5 PMo 10 V 2 o 40 Heteropolyacid is added in the imidazole ionic liquid aqueous solution of xylene coupling and reacts, wherein the imidazole ionic liquid of xylene coupling and H 5 PMo 10 V 2 o 40 The molar ratio of the heteropolyacid is 2.5:1, solid precipitation occurs immediately, continue stirring at 80°C for 12h, filter, wash twice with deionized water, and then dry at 80°C for 12h to obtain the catalyst [PxyDim] 2.5 PMOV 2 .

[0058] According to the application of the mesoporous ionic liquid heteropolyacid salt catalyst in Example 1, the catalyst is sel...

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Abstract

The present invention relates to the technical field of chemical catalysis, particularly to a mesoporous ion liquid heteropolyacid salt catalyst for a benzene hydroxylation reaction, a preparation method and applications thereof. The mesoporous ion liquid heteropolyacid salt catalyst is prepared by using a hydrothermal synthesis method, wherein the preparation method comprises: adding H5PMo10V2O40 heteropolyacid to a xylene-coupled imidazole ion liquid aqueous solution, carrying out a reaction, filtering, washing, and drying. According to the present invention, the prepared mesoporous ion liquid heteropolyacid salt catalyst is used in the reaction for phenol preparation through benzene oxidation; the catalysis performance of the mesoporous ion liquid heteropolyacid salt catalyst is improved through the mesoporous structure hydrophobic microenvironment so as to effectively improve the selectivity of phenol; the mesoporous ion liquid heteropolyacid salt catalyst has characteristics of simple preparation, low cost, convenient recovery, and stable reuse performance; and the preparation method has characteristics of rapid reation, mild condition and less environmental pollution, and is suitable for industrial production.

Description

technical field [0001] The invention relates to the technical field of chemical catalysis, in particular to a mesoporous ionic liquid heteropolyacid salt catalyst used for benzene hydroxylation reaction and its preparation method and application. Background technique [0002] Phenol is an important organic chemical product, widely used in the synthesis of various aldehyde resins, phenol derivatives, acids, amines and other compounds. At present, more than 90% of phenol is synthesized by cumene method. Although the production process of phenol by the cumene method is relatively mature, there are still many defects: the intermediate product cumene hydroperoxide is an unstable peroxide, and it has high requirements for control conditions and safety technology; The production process is relatively long, which makes it difficult to increase the yield of phenol; the separation and purification of phenol is difficult. Therefore, scientists at home and abroad have been working har...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D233/58B01J31/02B01J27/199B01J35/10C07C37/60C07C39/04
CPCC07C37/60C07D233/58B01J27/199B01J31/0285B01J31/0298B01J35/613B01J35/633B01J35/647C07C39/04Y02P20/52Y02P20/54
Inventor 赵萍萍崔洪友张云云宋峰孙秀玉
Owner SHANDONG UNIV OF TECH
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