Method for synthesizing mesityl oxide from acetone by one-step process

A technology for mesityl oxide and acetone, which is applied in the field of one-step synthesis of mesityl oxide from acetone, can solve the problems of high equipment investment, side reactions, increased separation cost, etc., and achieves reduced energy consumption, less side reactions, and moderate operating conditions. Effect

Active Publication Date: 2015-02-18
CNOOC TIANJIN CHEM RES & DESIGN INST +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are a small amount of by-products in the product, and if you want to obtain high-purity target product, the subsequent separation cost will increase
In addition, the acetone condensation reaction must adopt a higher pressure condition of 3-10MPa to ensure the conversion rate of acetone, but it will lead to more side reactions and cause high equipment investment.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1～2

[0029] Mix pseudo-boehmite (produced by Shandong Aluminum Factory), extrusion aid and adhesive evenly, add water, knead and extrude to make a cylindrical shape. Dry the extrudate at 130°C, and then bake it at 500°C for 3 hours to obtain γ-Al 2 o 3 carrier. 500ml γ-Al 2 o 3 The carrier was immersed in 500ml of 7.5% calcium nitrate aqueous solution for 4 hours, then dried at 120°C for 4 hours, and calcined at 400°C for 4 hours to obtain the catalyst BTM-I. The physical properties of the catalyst are listed in Table 1.

[0030] Table 1

[0031] Example

1

2

3

4

catalyst

BTM-I

BTM-I

BTM-II

BTM-III

CaO content, %

2.44

2.44

-

4.2

Ba content, %

-

-

3.0

Pore ​​volume, ml / g

0.42

0.42

0.42

0.41

Specific surface area, m 2 / g

220

220

216

208

Lateral compressive strength, N / cm

158

158

164

172

shape

Cylindrical ...

Embodiment 3

[0038] Mix pseudo-boehmite (produced by Shandong Aluminum Factory), extrusion aid and adhesive evenly, add water, knead and extrude to make a cylindrical shape. Dry the extrudate at 130°C, and then bake it at 500°C for 3 hours to obtain γ-Al 2 o 3 carrier. 500ml γ-Al 2 o 3 The carrier was immersed in 500ml of 5.3% barium nitrate aqueous solution for 4 hours, then dried at 120°C for 4 hours, and calcined at 400°C for 4 hours to obtain the catalyst BTM-II. The physical properties of the catalyst are listed in Table 1.

[0039] The bimolecular acetone condensation reactions were carried out in trickle bed reactors, and the loading amount of catalyst in each reactor was 100ml. The reaction conditions are shown in Table 4. The acetone raw material passes through the catalyst bed from top to bottom, and the product enters the molecular sieve adsorption and dehydration tank. The molecular sieve used in the adsorption dehydration tank is 4A molecular sieve.

[0040] The dehydra...

Embodiment 4

[0043] Mix pseudo-boehmite (produced by Shandong Aluminum Factory), extrusion aid and adhesive evenly, add water, knead and extrude to make a cylindrical shape. Dry the extrudate at 130°C, and then bake it at 500°C for 3 hours to obtain γ-Al 2 o 3 carrier. 500ml γ-Al 2 o 3 The carrier was immersed in 500ml of 12.3% calcium nitrate aqueous solution for 4 hours, then dried at 120°C for 4 hours, and calcined at 400°C for 4 hours to obtain the catalyst BTM-II. The physical properties of the catalyst are listed in Table 1.

[0044] The bimolecular acetone condensation reactions were carried out in trickle bed reactors, and the loading amount of catalyst in each reactor was 100ml. The reaction conditions are shown in Table 4. The acetone raw material passes through the catalyst bed from top to bottom, and the product enters the molecular sieve adsorption and dehydration tank. The molecular sieve used in the adsorption dehydration tank is 4A molecular sieve.

[0045] The dehyd...

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PUM

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Abstract

The invention relates to a method for synthesizing mesityl oxide from acetone by a one-step process, which adopts a combination technique of series connection of a fixed-bed reactor and a molecular sieve adsorption dehydration tank. The method comprises the following steps: a reactor is filled with a solid catalyst, and acetone used as a reaction raw material is subjected to condensation reaction to generate mesityl oxide and water; the product enters a first molecular sieve adsorption dehydration tank; the organic oil phase after dehydration enters a second fixed-bed reactor, and the acetone is further subjected to condensation reaction to generate mesityl oxide and water and passes through a second molecular sieve adsorption dehydration tank; the number of stages of series connection of the reactors and dehydration tanks is 2-3; the acetone and mesityl oxide oil phase after dehydration are sent into a rectification separation system, and the unreacted acetone is circulated back to the reactor; and the liquid phase on the tower bottom is separated to obtain the mesityl oxide with the purity of greater than 99%. The method provides a method for producing mesityl oxide from dimolecular acetone by a condensation one-step process, breaks reaction equilibrium, enhances the conversion rate, acquires the high-purity mesityl oxide product, and lowers the energy consumption and production cost of the product.

Description

technical field [0001] The invention relates to a method for synthesizing mesityl oxide from acetone in one step. Background technique [0002] Mesityl oxide (alias: mesityl acetone, 4-methyl-4-pentanone, Mesityl Oxide, referred to as MO) is a medium-boiling strong solvent, mainly used for nitrocellulose and various resins, especially ethylene Solvents for base resins and spray paints; it is also an important organic synthesis intermediate, mainly used in medicines, fine chemicals and pesticides, etc. raw material. [0003] The traditional production method of mesityl oxide is a two-step process: [0004] In the first step, acetone (AC) is compressed and compressed in the presence of a basic catalyst to convert it into diacetone alcohol (DAA). The catalyst is calcium hydroxide or barium hydroxide. [0005] Acetone condensation reaction formula: [0006] 2CH 3 -CO-CH 3 →(CH 3 ) 2 COH-CH 2 -CO-CH 3 . [0007] Second step: dehydration of diacetone alcohol generates m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/203C07C45/74
CPCC07C45/74C07C45/79C07C45/82C07C49/203
Inventor 南军于海斌张景成张玉婷耿姗曲晓龙朱金剑肖寒刘艳姜雪丹张雪梅
Owner CNOOC TIANJIN CHEM RES & DESIGN INST
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