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A kind of preparation method of catalyst for preparing difluoroethanol by hydrogenation of methyl difluoroacetate

A technology of methyl difluoroacetate and difluoroethanol, which is applied in the field of catalyst preparation, can solve the problems of low conversion rate of catalytic reaction, poor catalytic stability of catalyst, difficulty in continuous production control, etc., and achieve the effect of high-efficiency catalytic ability

Active Publication Date: 2016-08-17
格润化学(东营)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Although there are many catalysts for the synthesis of difluoroethanol, most of them require liquid phase reaction at high temperature and high pressure, while the conversion rate of catalytic reaction is low and the catalyst has high requirements for reaction conditions, and the catalytic stability of the catalyst is poor under different reaction conditions. And other shortcomings, making continuous production control difficult, so it is necessary to carry out further research and development

Method used

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  • A kind of preparation method of catalyst for preparing difluoroethanol by hydrogenation of methyl difluoroacetate

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Effect test

Embodiment 1

[0018] A preparation method of a catalyst for preparing difluoroethanol by hydrogenating methyl difluoroacetate, comprising the following steps:

[0019] Step 1, by weight components, 2 parts of vanadium pentoxide (particle size 100 μm) and 2 parts of NbCl 3 Add it into a sodium hydroxide solution with a mass percentage of 6%, heat it to 30°C, then add 0.8 parts of polypropylene glycol and 1 part of tetraethyl orthosilicate under stirring, continue stirring for 20 minutes after the addition, and then remove the precipitate Filter, rinse with deionized water, and dry;

[0020] Step 2, in terms of weight components, add the dried solids in step 1 together with 2 parts of potassium oxide, 0.5 parts of calcium tungstate (particle size 100 μm), 1 part of zinc oxide and 6 parts of zeolite powder (particle size 500 μm) In 10 parts of calcium chloride saturated solution, stir and mix evenly, heat up to 50°C, add 1 part of potassium permanganate solution with a concentration of 7%, st...

Embodiment 2

[0022] A preparation method of a catalyst for preparing difluoroethanol by hydrogenating methyl difluoroacetate, comprising the following steps:

[0023] Step 1, by weight components, 3 parts of vanadium pentoxide (particle size 200 μm) and 3 parts of NbCl 3 Add it into a 7% potassium hydroxide solution by mass, heat it to 33°C, then add 1 part of polypropylene glycol and 2 parts of tetraethyl orthosilicate while stirring, continue stirring for 25 minutes after the addition, and then remove the precipitate Filter, rinse with deionized water, and dry;

[0024] Step 2, in terms of weight components, add the dried solids in step 1 together with 4 parts of potassium oxide, 0.6 parts of calcium tungstate (particle size 150 μm), 3 parts of zinc oxide and 8 parts of zeolite powder (particle size 600 μm) In 12 parts of calcium chloride saturated solution, stir and mix evenly, heat up to 52°C, add 1 part of potassium permanganate solution with a concentration of 5%, stir for 1 hour, c...

Embodiment 3

[0026] A preparation method of a catalyst for preparing difluoroethanol by hydrogenating methyl difluoroacetate, comprising the following steps:

[0027] Step 1, by weight components, 4 parts of vanadium pentoxide (particle size 100 μm) and 3 parts of NbCl 3 Add it into the sodium hydroxide solution with a mass percentage of 8%, heat it to 36°C, then add 1.5 parts of polypropylene glycol and 3 parts of tetraethyl orthosilicate under stirring, continue stirring for 30 minutes after the addition, and then remove the precipitate Filter, rinse with deionized water, and dry;

[0028] Step 2, in terms of weight components, add the dried solids in step 1 together with 5 parts of potassium oxide, 0.8 parts of calcium tungstate (particle size 100 μm), 5 parts of zinc oxide and 12 parts of zeolite powder (particle size 700 μm) In 18 parts of calcium chloride saturated solution, stir and mix evenly, heat up to 60°C, add 2 parts of potassium permanganate solution with a concentration of ...

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Abstract

The invention discloses a preparation method of a catalyst for methyl difluoroacetate hydrogenation to produce difluoroethanol. The method comprises the following specific steps: first adding vanadic anhydride and NbCl3 by weight into an alkali solution, adding with heating and stirring polypropylene glycol and tetraethoxysilane, continuing stirring for 20-30 min, filtering the precipitate, rinsing with deionized water, drying, adding the dried solid with potassium oxide, calcium tungstate, zinc oxide and zeolite powder together into a saturated solution of calcium chloride, stirring to mix well, heating up to 50-60 DEG C, adding a potassium permanganate solution, stirring for 1-2 h, cooling to room temperature, filtering out the precipitate, cleaning with deionized water, and then sintering at 600-700 DEG C, cleaning the cured substances after sintering with deionized water, and drying to constant weight. The catalyst prepared by the invention has high efficiency catalysis capability and catalysis stability under normal pressure.

Description

technical field [0001] The invention belongs to the technical field of chemical catalyst preparation, in particular to a method for preparing a catalyst for hydrogenating methyl difluoroacetate to prepare difluoroethanol. Background technique [0002] Because difluoroethanol contains difluoromethyl groups, it has different properties from other fluorine-containing alcohols. It is mainly used as an intermediate for medicine and pesticides, and for poisoning rodents. Its derivatives can be used as herbicides and insecticides Poison some plants or plant pests. [0003] The hydrogenation of esters to the corresponding alcohols is a very important synthetic link in chemical production, and Cu catalysts and VIIIB metal catalysts are often used. After Christiansen first synthesized alcohol from methyl formate on a copper-based catalyst, researchers began to do a lot of research on this type of catalyst. Although Cu catalysts also have good ester hydrogenation performance, catalys...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/076C07C31/38C07C29/147
Inventor 李海涛李恒滨
Owner 格润化学(东营)有限公司
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