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Mesoporous ionic liquid heteropolyacid salt catalyst for benzene hydroxylation reaction and its preparation method and application

A technology of ionic liquids and heteropoly acid salts, which is applied in the preparation of organic compounds, catalysts for physical/chemical processes, catalysts for organic compounds/hydrides/coordination complexes, etc., which can solve the requirements of control conditions and safety technology. , the difficulty of recycling the catalyst, the difficulty of separating and refining phenol, etc., to achieve the effect of high utilization rate of hydrogen peroxide, industrial application, and convenient recycling and reuse.

Inactive Publication Date: 2019-04-30
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 ionic liquid heteropolyacid salt catalyst for benzene hydroxylation reaction and its preparation method and application
  • Mesoporous ionic liquid heteropolyacid salt catalyst for benzene hydroxylation reaction and its preparation method and application
  • Mesoporous ionic liquid heteropolyacid salt catalyst for benzene hydroxylation reaction and its preparation method and application

Examples

Experimental program
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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 invention relates to the technical field of chemical catalysis, in particular to a mesoporous ionic liquid heteropoly acid salt catalyst for benzene hydroxylation reaction, and a preparation method and application thereof. The mesoporous ionic liquid heteropoly acid salt catalyst is prepared by a hydrothermal synthesis method: the H 5 PMo 10 V 2 O 40 The heteropolyacid was added to the xylene-coupled imidazole ionic liquid aqueous solution for reaction, filtered, washed and dried. Then the prepared mesoporous ionic liquid heteropoly acid salt catalyst was used in the reaction of benzene oxidation to phenol. The mesoporous structure hydrophobic microenvironment of the mesoporous ionic liquid heteropolyacid salt catalyst of the present invention improves its catalytic performance and can effectively improve the selectivity of phenol. In addition, the mesoporous ionic liquid heteropoly acid salt catalyst has the advantages of simple preparation, low cost, convenient recovery, stable reusability, fast reaction speed, mild conditions, less environmental pollution, and easy industrialized 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 Patents(China)
IPC IPC(8): C07D233/58B01J31/02B01J27/199B01J35/10C07C37/60C07C39/04
CPCB01J27/199B01J31/0285B01J31/0298B01J35/1014B01J35/1038B01J35/1061C07C37/60C07D233/58C07C39/04Y02P20/52Y02P20/54
Inventor 赵萍萍崔洪友张云云宋峰孙秀玉
Owner SHANDONG UNIV OF TECH
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