A method for the synthesis of phenol by highly selective oxidation of benzene

A technology of high selectivity and synthesis method, applied in the field of high-selectivity oxidation of benzene to synthesize phenol, can solve the problems of low phenol yield and the like, and achieve the effects of high selectivity, low equipment corrosion and low energy consumption

Active Publication Date: 2019-09-03
HUNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In recent years, the photocatalytic oxidation of benzene to phenol using molecular oxygen as an oxidant has been favored. This method uses solar energy as an energy source, and has the advantages of low reaction temperature, less energy consumption, and simple equipment; however, the yield of phenol is relatively low. Low, need to develop high-efficiency catalyst

Method used

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  • A method for the synthesis of phenol by highly selective oxidation of benzene
  • A method for the synthesis of phenol by highly selective oxidation of benzene
  • A method for the synthesis of phenol by highly selective oxidation of benzene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] The present invention prepares the photocatalyst by changing the molar ratio of cadmium tungstate and bismuth tungstate in the cadmium tungstate-bismuth tungstate composite photocatalyst:

[0025] Preparation of cadmium tungstate nanorods: Dissolve 1.234g of cadmium nitrate and 0.240g of ethylenediamine solution in 20mL of deionized water, stir vigorously for 10min and mix to form solution A; add 20mL of aqueous solution B containing 1.316g of sodium tungstate drop by drop Add to solution A, stir and mix well, adjust the pH to 7 with nitric acid, and continue stirring for 20 minutes to obtain solution C. The resulting solution C was then crystallized at 160°C for 20 hours. Cool and centrifuge, wash with deionized water three times, and dry at 80°C for 4 hours to obtain cadmium tungstate;

[0026] Preparation of composite materials: Dissolve 0.015g sodium tungstate and 0.040g bismuth nitrate in 30mL ethylene glycol solution respectively, stir well and mix to form soluti...

Embodiment 2～5

[0030] For cadmium tungstate and bismuth tungstate composite photocatalysts with different molar ratios, the operation steps are similar to those in Example 1, only the amount of sodium tungstate and bismuth nitrate in the composite material is changed, and the rest of the conditions are unchanged, and the sample number BCW-1, BCW-2, BCW-3, BCW-4, BCW-5. See Table 1 for the composite catalyst conditions and reaction results prepared in Examples 2-5.

[0031] Table 1. Reaction results of bismuth tungstate-cadmium tungstate composite photocatalysts with different molar ratios

[0032]

[0033] As can be seen from Table 1, different benzene conversion rates are obtained under different molar ratios of cadmium tungstate and bismuth tungstate, wherein when the ratio of bismuth tungstate-cadmium tungstate is 4:10, the conversion rate of catalyzed benzene is 5.8%, and that of phenol The selectivity is greater than 99%, and the photocatalytic effect is very good.

Embodiment 6～10

[0035] According to the steps of Example 1 with the best effect, the remaining conditions remain unchanged (the molar ratio of bismuth tungstate and cadmium tungstate is 4:10), only the crystallization temperature during the preparation of the composite photocatalyst is changed to 100°C respectively , 120°C, 140°C, 180°C, 200°C, and the sample numbers are A1, A2, A3, A4, A5. See Table 2 for the composite catalyst conditions and reaction results prepared in Examples 6-10.

[0036] Table 2. Reaction results of bismuth tungstate-cadmium tungstate composite photocatalysts crystallized at different temperatures

[0037]

[0038]

[0039] It can be seen from Table 2 that the conversion rate of benzene obtained at different crystallization temperatures is compared with that of Example 1. The conversion rate of benzene is the highest when the crystallization temperature is 160° C., which has the best photocatalytic effect.

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Abstract

The invention provides a high-selectivity phenol synthesis method by benzoyl oxide. The method has the advantages of high selectivity, small energy consumption, and pollution free. The preparation method includes the steps of taking and dissolving cadmium salt and tungstate in amine solution; after evenly stirring and adjusting pH value, performing hydro-thermal treatment, centrifugation, filtering, washing, drying and other steps to obtain cadmium trngstate; taking and dissolving bismuth salt and tungstate in alcoholic solution; stirring and mixing evenly, and adding the prepared cadmium trngstate; then performing crystallization, cooling, filtering, separation, drying and other steps, and preparing the cadmium trngstate-bismuth tungstate composite photocatalyst; taking and dispersing the cadmium trngstate-bismuth tungstate composite photocatalyst in the solvent and reaction fluid; charging oxygen and lighting to obtain phenol. By controlling the mole ratio of bismuth and cadmium in the catalyst, the conversion rate of benzene is improved, and the selectivity of prepared phenol is more than 99%.

Description

[0001] 【Technical field】 [0002] The invention relates to the field of photocatalytic oxidation, in particular to a method for highly selective oxidation of benzene to synthesize phenol. [0003] 【Background technique】 [0004] As an important organic chemical raw material, phenol is often used in the production of resins, fungicides, preservatives, surfactants, plastics and drugs (such as aspirin). In industry, benzene is often used as raw material, sulfonated with sulfuric acid to generate benzenesulfonic acid, neutralized with sulfurous acid, and then alkali-fused with caustic soda, and phenol is prepared through sulfonation and vacuum distillation. Other preparation methods of phenol include cumene method, chlorobenzene hydrolysis method, Raschig method, etc. The above synthetic methods all have the disadvantages of long production process, complex process, high production cost, and serious equipment corrosion. Therefore, the direct oxidation of benzene to synthesize phe...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/31C07C37/58C07C39/04
CPCC07C37/58B01J23/002B01J23/31B01J2523/00B01J35/39B01J2523/28B01J2523/54B01J2523/69C07C39/04Y02P20/52
Inventor 尹双凤吴敏陈鹏张佳蔚陈浪
Owner HUNAN UNIV
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