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Catalyst and preparation method for benzene hydroxylation to phenol

A benzene hydroxylation and catalyst technology, which is applied in the field of heteropoly acid catalyst and preparation, can solve the problems of difficult catalyst recovery, low benzene conversion rate and phenol yield, and complicated catalyst preparation process, so as to avoid deep oxidation and improve benzene Conversion rate, effect of promoting reaction

Inactive Publication Date: 2011-12-28
ZHEJIANG NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The most obvious disadvantage of using pure heteropolyacids as homogeneous catalysts to catalyze benzene liquid-phase synthesis of phenol is the difficulty in catalyst recovery. In view of this, Chinese patent CN1788843 uses a sol-gel method to immobilize molybdenum vanadium phosphopolyacids, and finds that in benzene The catalyst prepared in the hydrogen peroxide hydroxylation reaction can be reused many times, but the catalyst preparation process is relatively complicated
[0008] So far, on the publicly reported catalysts, the conversion rate of benzene and the yield of phenol during the hydroxylation of benzene and hydrogen peroxide to phenol are relatively low, and molybdenum vanadium phosphopolyacids are used to modify molybdenum vanadium phosphopolyacids simultaneously with organic and inorganic groups. The hydroxylation process of benzene and hydrogen peroxide has not been reported yet

Method used

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  • Catalyst and preparation method for benzene hydroxylation to phenol
  • Catalyst and preparation method for benzene hydroxylation to phenol
  • Catalyst and preparation method for benzene hydroxylation to phenol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Cs 2.5 (MIMPS) 0.5 HPMo 11VO 40 The preparation and catalytic performance of

[0025] h 4 PMo 11 VO 40 Preparation: Weigh 0.11mol of MoO 3 and 0.005mol of V 2 o 5 were dissolved in water respectively, then the two solutions were mixed and heated to 373K, and 0.01 mol of H was added under stirring 3 PO 4 , and the suspension was reacted at 373K for 24h, and after filtration, the obtained solution was prepared into a 500mL standard solution, and the concentration of the solution was 0.02mol L -1 .

[0026] Cs 2.5 h 1.5 PMo 11 VO 40 Preparation: Weigh 0.005mol of Cs 2 CO 3 Dissolve in water to form a solution, drop by drop into the previously pipetted H 4 PMo 11 VO 40 In 200mL standard solution, heat to 373K, react for 5-7h, centrifuge the obtained suspension, pour the supernatant and dry it in a blast oven at 100°C to obtain Cs 2.5 h 1.5 PMo 11 VO 40 .

[0027] Cs 2.5 (MIMPS) 0.5 HPMo 11 VO 40 Preparation: Weigh the prepared Cs 2.5 h 1.5 PMo...

Embodiment 2

[0030] Cs 2.5 (MIMPS) 0.75 h 0.75 PMo 11 VO 40 The preparation and catalytic performance of

[0031] The preparation method is the same as that of Example 1, except that the amount of MIMPS added is 0.15 mmol.

[0032] Weighed 0.05mmol (ie 0.113g) solid catalyst and applied it to the liquid phase oxidation reaction of benzene, the results are shown in Table 1.

Embodiment 3

[0034] Cs 2.5 (MIMPS)H 0.5 PMo 11 VO 40 The preparation and catalytic performance of

[0035] The preparation method is the same as in Example 1, except that the amount of MIMPS added is 0.2 mmol.

[0036] Weighed 0.05mmol (ie 0.116g) solid catalyst and applied it to the liquid phase oxidation reaction of benzene, the results are shown in Table 1.

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Abstract

The invention relates to a catalyst for preparing phenol by hydroxylation of benzene and a preparation method thereof. The component expression of the catalyst provided by the invention is Cs2.5(MIMPS)nH1.5-nPMo11VO40, wherein MIMPS indicates [N-(3-sulfonic)propyl-imidazolium] and n equals to 0.5-1.5. The preparation method provided by the invention comprises the following steps of: (1) preparingpure vanadium substituted heteropolymolybdates; (2) mixing the pure vanadium substituted heteropolymolybdates obtained from the step (1) with deionized water, adding dropwisely an inorganic cesium salt solution into the above solution with stirring, followed by a reaction, removing water from a suspending liquid obtained after the reaction so as to obtain a solid, drying to obtain a heteropolyacid inorganic cesium salt; (3) mixing the heteropolyacid inorganic cesium salt obtained from the step (2) with deionized water, adding dropwisely an MIMPS aqueous solution with stirring, followed by a reaction, removing the solvent from a suspending liquid obtained after the reaction so as to obtain a solid, and drying to obtain the catalyst for preparing phenol by hydroxylation of benzene. By the adoption of the catalyst provided by the invention, the yield of phenol can be obviously raised; in addition, the catalyst is easy to recover and convenient to repeatedly use.

Description

technical field [0001] The invention relates to an organic-inorganic double-modified heteropolyacid catalyst and a preparation method, in particular to a catalyst and a preparation method for the hydroxylation of benzene to phenol. Background technique [0002] Phenol is an important organic chemical raw material, widely used in petrochemical, agricultural and plastic industries, and the world demand is increasing year by year. At present, the industrial production method of phenol is mainly the cumene method. This method adopts the alkylation of benzene to obtain cumene, the oxidation of cumene to obtain cumene peroxide, and the decomposition of cumene peroxide to produce phenol. The disadvantages of this process are large energy consumption, low phenol yield, the presence of an explosive intermediate product-cumene peroxide, the consumption of national strategic resource propylene, and the production of by-product acetone in an equimolar amount to phenol and acetone The d...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/36C07C39/04C07C37/60
CPCY02P20/52
Inventor 张富民景丽徐文俊钟依均朱伟东
Owner ZHEJIANG NORMAL UNIVERSITY
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