Preparation method of methyl vinyl ketone

A technology of methyl vinyl ketone and copper-based catalyst, which is applied in the field of preparation of methyl vinyl ketone, can solve problems such as complicated preparation steps, and achieve the effect of easy industrial implementation and large-scale production

Active Publication Date: 2020-06-23
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method adopts a solid alkaline catalyst, avoids the use of dilute sodium hydroxide aqueous solution as a catalyst, and reduces the generation of polymerization products, but the preparation steps are still relatively complicated, and the yield of methyl vinyl ketone products is only increased to about 50%.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] The preparation process of dehydrogenation catalyst DH1 is as follows:

[0028] (1) Weigh 152g of copper nitrate, 80g of ytterbium nitrate and 109g of aluminum nitrate, dissolve them in 1 L of deionized water, and prepare solution A1. Weigh 30 g of potassium hydroxide and 12 g of potassium bicarbonate respectively, dissolve them in 1L of deionized water, and configure solution B1. Add 1L of deionized water into a 5L beaker, raise the temperature and maintain it at 95°C, add solutions A1 and B1 dropwise at the same time under the condition of continuous stirring, control the pH value to maintain around 9.0, and continue stirring for 2 h after the dropwise addition is completed , followed by static aging for 2 h, and filtered to obtain precipitate C1.

[0029] (2) Dry the precipitate C1 at 110°C for 24 h, then bake it at 400°C for 5 h, then add graphite powder with 3% of the weight of the precipitate as a lubricant, press it into a tablet, and then bake it at 400°C for 5...

Embodiment 2

[0033] The preparation process of dehydrogenation catalyst DH2 is as follows:

[0034] (1) Weigh 130g of copper nitrate, 175g of nickel nitrate and 86g of aluminum nitrate respectively, dissolve them in 1 L of deionized water, and prepare solution A2. Weigh 30 g of potassium hydroxide and 12 g of potassium bicarbonate respectively, dissolve them in 1L of deionized water, and configure solution B2. Add 1L of deionized water into a 5L beaker, raise the temperature and maintain it at 95°C, and add solution A2 and B2 dropwise at the same time under the condition of continuous stirring, keep the pH value at about 9.0, and continue stirring for 2 h after the dropwise addition is completed , followed by static aging for 2 h, and the precipitate C2 was obtained by filtration.

[0035] (2) Dry the precipitate C2 at 110°C for 24 h, then bake it at 400°C for 5 h, then add graphite powder with 3% of the weight of the precipitate as a lubricant, press it into a tablet, and then bake it at...

Embodiment 3

[0039] The preparation process of dehydrogenation catalyst DH3 is as follows:

[0040](1) Weigh 121g of copper nitrate, 147g of zinc nitrate and 140g of aluminum nitrate, dissolve them in 1 L of deionized water, and prepare solution A3. Weigh 30 g of potassium hydroxide and 12 g of potassium bicarbonate respectively, dissolve them in 1L of deionized water, and configure solution B3. Add 1L of deionized water into a 5L beaker, raise the temperature and maintain it at 95°C, add solutions A3 and B3 dropwise at the same time under the condition of continuous stirring, control the pH value to maintain around 9.0, and continue stirring for 2 h after the dropwise addition is completed , followed by static aging for 2 h, and the precipitate C3 was obtained by filtration.

[0041] (2) Dry the precipitate C3 at 110°C for 24 h, then roast at 400°C for 5 h, then add graphite powder with 3% of the weight of the precipitate as a lubricant, press into tablets, and then roast at 400°C for 5 ...

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PUM

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Abstract

The invention discloses a preparation method of methyl vinyl ketone. The preparation method comprises the following steps: contacting a raw material containing 1,3-butanediol with a copper-based catalyst to carry out reactions under a dehydrogenation condition, and contacting the reaction effluent with a solid acid catalyst to carry out reactions under a dehydration condition to obtain methyl vinyl ketone. The copper-based catalyst comprises the following components in percentage by weight: 40-50% of copper oxide, 35-45% of at least one of ytterbium oxide, nickel oxide, and zinc oxide, 0.1-1%of potassium oxide and the balance being aluminum oxide. A new preparation method of methyl vinyl ketone is provided, is easy to implement industrially, and is suitable for large scale production.

Description

technical field [0001] The invention relates to a method for preparing methyl vinyl ketone, more specifically, the invention relates to a method for preparing methyl vinyl ketone by using 1,3-butanediol as a raw material. Background technique [0002] Methyl vinyl ketone, that is, 3-buten-2-ketone, has two functional groups of double bond and carbonyl, and is the simplest α, β-unsaturated aldehyde and ketone compound, which is an important raw material for Micheal addition reaction. In addition, methyl vinyl ketone can also be used as a polymer monomer, and as a raw material for the synthesis of cellulose A, anionic resins, and film emulsifiers. [0003] According to literature (Anhui Chemical Industry, 2017, 43(1), 45-48), there are three main preparation methods for methyl vinyl ketone: (1) acetone and formaldehyde high-temperature gasification method, the reaction temperature is higher than 320 ° C, this method The operation safety is very high, and the product state nee...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/66C07C49/205B01J23/83B01J23/78B01J23/80
CPCC07C45/66C07C45/002B01J23/83B01J23/78B01J23/80B01J23/002B01J2523/00C07C49/205C07C49/17B01J2523/13B01J2523/17B01J2523/31B01J2523/3787B01J2523/847B01J2523/27
Inventor 乔凯周峰马会霞翟庆铜张淑梅
Owner CHINA PETROLEUM & CHEM CORP
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