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Catalyst used in p-dichlorobenzene hydroxylate for preparing 2,5-dichlorophenol, and preparation method thereof

A technology of dichlorophenylhydroxyl and dichlorophenol is applied in catalyst activation/preparation, physical/chemical process catalysts, chemical instruments and methods, etc. Less, good industrialization prospects, simple operation effect

Active Publication Date: 2016-09-07
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention is: to overcome the shortages of three industrial wastes in the preparation of 2,5-dichlorophenol in the prior art, environmental pollution, and large energy consumption, and not only provide a green 2,5-dichlorophenol hydroxylation system 2 , the catalyst preparation method of 5-dichlorophenol, and save the catalyst preparation process, improve the catalytic conversion rate

Method used

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Examples

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Effect test

preparation example Construction

[0024] Catalyst preparation: Accurately weigh a certain amount of Al 2 o 3 or SiO 2 or TiO 2 , dried in a blast drying oven at 100°C for 1h, and then roasted in a muffle furnace at 550°C for 6h as an impregnated carrier; add a eutectic mixture of choline chloride / urea with a molar ratio of 1:2 to the three-necked flask, Heat and mechanically stir until molten state, add vanadium pentoxide, slowly add phosphoric acid (H 3 PO 4 The mass ratio of vanadium pentoxide to vanadium pentoxide is 8:1) to obtain the impregnating solution; after mixing the above impregnating solution with the impregnating carrier, keep warm and continue mechanical stirring for 72 hours, filter, and dry the filter cake to obtain the catalyst of the present invention.

[0025] By adjusting the concentration of the active components in the impregnation solution and the mass ratio of the impregnation solution to the carrier, a series of catalysts with different vanadium content were prepared: 5% VPO x / A...

Embodiment 1

[0027] In a 250ml flask, dissolve 14.7g p-dichlorobenzene in 100ml acetic acid, stir and heat up to 30°C, after it is completely dissolved, add 5% VPO x / Al 2 o 3 1.2g; slowly add 57ml of 30% hydrogen peroxide dropwise under stirring, finish adding for 10 hours, then react at 30°C for 2 hours, filter with suction, wash the filter cake with acetic acid, combine the filtrates, add sodium bisulfite dropwise to decompose excess hydrogen peroxide; add water, filter with suction , collected the filter cake and dried to obtain unreacted p-dichlorobenzene; the filtrate was extracted 4 times with ethyl acetate, the organic phases were combined, and the ethyl acetate was removed by rotary evaporation, and white needle-like crystals were collected and dried, that is, 2,5-dichlorobenzene Chlorophenol.

Embodiment 2

[0029] With 10% VPO x / Al 2 o 3 Instead of 5% VPO in Example 1 x / Al 2 o 3 , other steps are with embodiment 1.

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Abstract

The invention belongs to the field of fine chemical engineering, relates to a catalyst technology, and concretely relates to a preparation method of a catalyst with vanadium phosphorus oxide supported on an oxide used as a carrier, and an application of the catalyst in synthesis of 2,5-dichlorophenol. The catalyst is prepared through adopting SiO2, Al2O3 or TiO2 as a carrier and introducing an active component VPOx (vanadium phosphorus oxide) by an immersion technology. The catalyst prepared through the method has high activity and selectivity in p-dichlorobenzene hydroxylate for preparing 2,5-dichlorophenol.

Description

technical field [0001] The invention belongs to the field of fine chemical industry and relates to catalyst technology, in particular to the preparation of a catalyst loaded with vanadium phosphorus oxide as a carrier and its application in synthesizing 2,5-dichlorophenol. Background technique [0002] 2,5-Dichlorophenol is mainly used as intermediates of medicines and dyes, herbicide dicamba intermediates, nitrogen fertilizer synergists, leather antifungal agents, etc. Especially the main organic intermediates for the preparation of the pesticide herbicide dicamba. In recent years, with the continuous improvement of greenhouse gas emission reduction and environmental protection requirements, the use of chlorsulfuron and metsulfuron-methyl preparations has been banned and restricted, and the demand for dicamba, a low-toxicity pesticide widely used in crop production, has continued to increase, and the market prospect is good. Therefore, the successful development of 2,5-dic...

Claims

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Application Information

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IPC IPC(8): B01J27/198C07C37/60C07C39/30
CPCB01J27/198B01J37/0213C07C37/60C07C39/30
Inventor 潘飞张伟李明时鲁墨弘
Owner CHANGZHOU UNIV
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