Activation method and reaction device for preparing methyl ethyl ketone catalyst through sec-butyl alcohol dehydrogenation

An activation method, sec-butanol technology, applied in the field of sec-butanol dehydrogenation catalyst activation, can solve the problems of accelerating the condensation reaction rate of alcohol and ketone, decreasing catalyst activity, reducing catalyst activity, etc.

Pending Publication Date: 2020-01-03
ZIBO QIXIANG TENGDA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

There is following shortcoming in above-mentioned patent: adopt high space velocity feeding (>0.5h -1 ) can easily lead to a rise in bed temperature, which in turn leads to a decrease in catalyst activity, and the greater the space velocity, the more significant the bed temperature rise; if a low space velocity feed is used, and the lower the space velocity, the residence time of methyl ethyl ketone and sec-butanol in the reactor The longer it is, the higher the selectivity of alcohol and ketone condensation to generate C8 ketone heavy substances, which will be adsorbed in the active center and pores of the catalyst, which will reduce the catalyst activity; in addition, "CN 1335201A" adopts liquid phase product circulation It is also easy to speed up the reaction rate of alcohol and ketone condensation

Method used

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  • Activation method and reaction device for preparing methyl ethyl ketone catalyst through sec-butyl alcohol dehydrogenation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0067] The catalyst is calculated by weight percentage, and the composition is as follows: CuO 45%, ZnO 35%, Al 2 O 3 17%, K 2 CO 3 3%.

[0068] The catalyst is cylindrical.

[0069] The activation method of the catalyst for the dehydrogenation of sec-butanol to methyl ethyl ketone described in Example 1 consists of the following steps:

[0070] (1) Removal of catalyst physically adsorbed water

[0071] Using nitrogen as the heat carrier, the reactor bed temperature was raised to 190°C at a heating rate of 15°C / h, and the physically adsorbed water of the catalyst was removed by purging. The nitrogen space velocity was 260h -1 .

[0072] (2) Initial stage of reduction

[0073] When the bed temperature of the reactor stabilizes at 190°C, water vapor and nitrogen are introduced before the introduction of sec-butanol, and the nitrogen space velocity is 1400h -1 , The feed molar ratio of steam to nitrogen is 1:10.

[0074] After the steam and nitrogen are introduced and the bed temperature of...

Embodiment 2

[0116] The sec-butanol dehydrogenation device used in Example 2 is the same as that in Example 1. The reactor in Example 2 is an isothermal tube-and-tube reactor with a height-to-diameter ratio of 100:1. There are 10,000 tubes in the reactor. . The column tubes are filled with catalyst, the shell side is heat-conducting oil, and a baffle plate is installed in the shell side.

[0117] The catalyst is calculated by weight percentage, the composition is as follows: CuO 40%, ZnO 40%, Al 2 O 3 18%, K 2 CO 3 2%.

[0118] The catalyst is cylindrical.

[0119] The activation method of the sec-butanol dehydrogenation to methyl ethyl ketone catalyst described in Example 2 consists of the following steps:

[0120] (1) Removal of catalyst physically adsorbed water;

[0121] Using nitrogen as the heat carrier, the reactor bed temperature was raised to 160°C at a heating rate of 10°C / h, and the physically adsorbed water of the catalyst was removed by purging. The nitrogen space velocity was 200h ...

Embodiment 3

[0132] The catalyst is calculated by weight percentage, the composition is as follows: CuO50%, ZnO30%, Al 2 O 3 19%, K 2 CO 3 1%.

[0133] The catalyst is cylindrical.

[0134] The reactor in Example 3 is an isothermal tube-and-tube reactor, with an internal tube height-to-diameter ratio of 200:1, and there are 3000 tube tubes in the reactor. The column tubes are filled with catalyst, the shell side is heat-conducting oil, and a baffle plate is installed in the shell side.

[0135] The activation method of the catalyst for preparing methyl ethyl ketone by dehydrogenation of sec-butanol described in Example 3 consists of the following steps:

[0136] (1) Removal of catalyst physically adsorbed water

[0137] Using nitrogen as the heat carrier, the reactor bed temperature was raised to 180°C at a heating rate of 30°C / h, and the physically adsorbed water of the catalyst was removed by purging. The nitrogen space velocity was 800h -1 .

[0138] (2) Initial stage of reduction

[0139] At th...

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Abstract

The invention belongs to the technical field of sec-butyl alcohol dehydrogenation catalyst activation, and particularly relates to an activation method and a reaction device for preparing a methyl ethyl ketone catalyst through sec-butyl alcohol dehydrogenation. Firstly, catalyst physically adsorbed water is removed, then nitrogen-water vapor is adopted as diluent gas, sec-butyl alcohol is fed at alow air speed to activate the catalyst, and finally, the catalyst is subjected to enhanced reduction through sec-butyl alcohol feeding. According to the activation method for preparing the methyl ethyl ketone catalyst through sec-butyl alcohol dehydrogenation, different reduction methods are adopted in different stages of the activation process of the catalyst, the problems that a traditional alcohol reduction method is large in bed layer temperature rise and prone to carbon deposition can be effectively solved, the one-way service life of the activated catalyst can be effectively prolonged,and use energy consumption is reduced; the sec-butyl alcohol dehydrogenation catalyst reaction device is easy to implement, simple in process and reasonable in design, and the operation process is easy to control.

Description

Technical field [0001] The invention belongs to the technical field of sec-butanol dehydrogenation catalyst activation, and specifically relates to an activation method and a reaction device for a sec-butanol dehydrogenation catalyst to prepare methyl ethyl ketone. Background technique [0002] Methyl ethyl ketone is an important organic solvent with excellent performance. It has the advantages of low toxicity, low boiling point, low viscosity, strong solubility and fast volatilization rate. It is widely used in coatings, dyes, oil refining and other fields. In addition, because methyl ethyl ketone contains a carbonyl group and active hydrogen adjacent to the carbonyl group, it is prone to chemical reactions. It can be used to produce methyl ethyl ketone peroxide, methyl propenyl ketone, methyl amyl ketone and other chemical products. It is an important fine chemical raw material . [0003] At present, the production of methyl ethyl ketone in industry mainly adopts the gas phase d...

Claims

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Application Information

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IPC IPC(8): B01J37/18B01J27/232C07C45/00C07C49/10
CPCB01J37/18B01J27/232C07C45/002C07C49/10Y02P20/584
Inventor 冯伟李永超翟西平郭瑞张路平孙晓明焦卫车平生宋以清赵实柱曲健林谢宝含朱秀清
Owner ZIBO QIXIANG TENGDA CHEM
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