Solid base catalyst, preparation method thereof and application of solid base catalyst in synthesis of anisole

A solid base catalyst and anisole technology, applied in the chemical industry, can solve the problems of unstable loss of active components, short industrial life of catalysts, poor environmental tolerance of catalysts and easy deactivation, etc.

Pending Publication Date: 2021-05-28
YULIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This kind of solid base catalyst has a short industrial life, serious loss of active components due to instability, poor environmental tolerance of the catalyst, easy deactivation, and difficult regeneration. At present, there is no relatively good regeneration method, and its preparation method generally adopts multi-step mixing The melting method, the preparation process is complicated, the preparation conditions are harsh, the reaction needs to be added with components such as liquid ammonia, and the protection of inert gas components is required, the reaction is not a one-time feeding, but multiple feedings are required, and it is not a one-stage reaction, and the reaction conditions need to be adjusted multiple times , the reaction temperature is high, sometimes it can reach about 500°C

Method used

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  • Solid base catalyst, preparation method thereof and application of solid base catalyst in synthesis of anisole
  • Solid base catalyst, preparation method thereof and application of solid base catalyst in synthesis of anisole
  • Solid base catalyst, preparation method thereof and application of solid base catalyst in synthesis of anisole

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preparation example Construction

[0043] Such as figure 1 Shown, the preparation method of solid base catalyst of the present invention comprises the following steps:

[0044] Step 1, N 2 Purge and replace the air and trace moisture in the autoclave (GCF Dalian Automatic Control Equipment Factory) for 0.5-1h;

[0045] Step 2, weigh γ-Al with an analytical balance (FA1104N Shanghai Precision Scientific Instrument Co., Ltd.) 2 o 3 Add 50-150g (4N Shanghai Dibo Chemical Technology Co., Ltd.) into the autoclave, measure CH with a measuring cylinder 3 OH 80-100mL (AR Tianjin Ruijinte Chemicals Co., Ltd.) was slowly added to the γ-Al 2 o 3 moisten

[0046] Step 3, add 10-20g of metal elemental sodium (AR Jining Hengtai Chemical Co., Ltd.), open the high-pressure reactor, and stir the reaction at a temperature of 300-350°C and a pressure of 10-15MPa for 2-4h to obtain Na-CH 3 ONa / γ-Al 2 o 3 (YP / γ-Al 2 o 3 ) solid base catalyst.

preparation Embodiment 1

[0048] Step 1, N 2 Purge and replace the air and trace moisture in the autoclave for 1 hour;

[0049] Step 2, weigh γ-Al with an analytical balance 2 o 3 50g was added to the autoclave, and 80mL of methanol was measured by the graduated cylinder and slowly added to the autoclave;

[0050] Step 3, then add 10g of metal elemental sodium, open the autoclave, and react at a temperature of 300°C and a pressure of 15MPa for 2h to obtain Na-CH 3 ONa / γ-Al 2 o 3 (YP / γ-Al 2 o 3 ) solid base catalyst.

preparation Embodiment 2

[0052] Step 1, N 2 Purge and replace the air and trace moisture in the autoclave for 0.5h;

[0053] Step 2, weigh γ-Al with an analytical balance 2 o 3 80g was added to the autoclave, and 100mL of methanol was measured by the graduated cylinder and slowly added to the autoclave;

[0054] Step 3, then add 15g of metal elemental sodium, open the autoclave, and react for 3 hours at a temperature of 350°C and a pressure of 15MPa to obtain Na-CH 3 ONa / γ-Al 2 o 3 (YP / γ-Al 2 o 3 ) solid base catalyst.

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Abstract

The invention provides a solid base catalyst and a preparation method thereof and application of the solid base catalyst in synthesis of anisole, and the preparation method comprises the following steps: step 1, adding gamma-Al2O3 into a high-pressure reaction kettle, and then adding methanol; and step 2, adding metal elementary substance sodium into the high-pressure reaction kettle, starting the high-pressure reaction kettle, and reacting for 2-4 hours at the temperature of 300-350 DEG C and the pressure of 10-15 MPa to obtain the Na-CH3ON / gamma-Al2O3 solid base catalyst. According to the method, gamma-Al2O3 is selected as a carrier, solid alkali metal elemental sodium is directly loaded on gamma-Al2O3, the Na-CH3ON / gamma-Al2O3 (YP / gamma-Al2O3) solid base catalyst is obtained, the obtained catalyst is good in catalytic effect and easy to regenerate, the preparation method is simple, and the preparation conditions are mild.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and relates to a solid base catalyst, a preparation method thereof and an application in synthesizing anisole. Background technique [0002] At present, there are mainly five kinds of catalysts for synthesizing anisole, which are mainly divided into single inorganic salt catalysts, ionic liquid catalysts, supported catalysts, transition metal carbonyl complex catalysts, and microwave-assisted catalysts according to their catalytic reaction characteristics. [0003] Among them, the single inorganic salt catalyst mainly includes: in 2002, K discovered by Ouk et al. 2 CO 3 Catalyst, under the condition of 150 DEG C, react phenol with dimethyl carbonate for 5 hours, and the yield of anisole can reach 70%. The reaction does not use a solvent, the catalyst can be recycled, and the post-treatment is simple, which has obvious advantages compared with the traditional method. In 2009, various ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/02B01J31/26C07C41/16
CPCB01J31/0212B01J31/26C07C41/16B01J2231/4288C07C43/205
Inventor 张智芳杨鹏任旭张璐陈娟李丽毕文强
Owner YULIN UNIV
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