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Device and method for catalytic synthesis of acetyl tri-n-butyl citrate by fixed bed reactor

A technology of acetyl tri-n-butyl citrate and fixed bed reactor, which is applied in chemical instruments and methods, preparation of organic compounds, preparation of carboxylic acid esters, etc., and can solve problems such as catalyst separation and recovery, catalyst loss, and inconvenient operation , to achieve the effect of cheap and easy to obtain catalyst, easy regeneration and simple implementation

Inactive Publication Date: 2008-05-14
ZHEJIANG UNIV
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

[0003] In the catalytic synthesis method of acetyl tri-n-butyl citrate given in the literature, it is all batch production, and the catalyst used is a heterogeneous catalyst, which needs to be stirred during the reaction, and the loss of the catalyst is serious. After the reaction, the catalyst needs to be separated and recovered. Inconvenient to operate

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  • Device and method for catalytic synthesis of acetyl tri-n-butyl citrate by fixed bed reactor

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Experimental program
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Effect test

Embodiment 1

[0018] The inner diameter of the reaction tube of the fixed bed reactor 6 is φ8mm, the outer diameter is φ15mm, and the height is 700mm. The reaction tube is filled with packing section, catalyst section and packing section sequentially from the top to the bottom. 50mm, the catalyst section is filled with macroporous strong acidic cation exchange resin with a particle size ranging from 0.45mm to 1.25mm, the filling height is 540mm, and it operates under normal pressure.

[0019] According to the molar ratio of acetic anhydride to tri-n-butyl citrate as 2.0:1, the temperature of heating circulating water is 70°C, and the temperature is 5.0g.min -1 .cm -2 The flow rate of the reaction material of the above proportion is preheated through the serpentine tube and then passed through the bed to obtain the crude product of acetyl tributyl citrate. The yield is 99.7%, and there is no peak of tri-n-butyl citrate on the gas chromatogram. , indicating that tri-n-butyl citrate has been ...

Embodiment 2

[0021] Using the same fixed-bed reactor as above, the molar ratio of acetic anhydride to tri-n-butyl citrate is 1.6:1, the temperature of the heating circulating water is 70°C, and the temperature is 40.0g.min -1 .cm -2 The flow rate of the reaction material of the above proportion is preheated through the serpentine tube and then passed through the bed to obtain the crude product of acetyl tributyl citrate. The yield is 99.8%, and there is no peak of tri-n-butyl citrate on the gas chromatogram. , indicating that tri-n-butyl citrate has been completely converted. After the crude product obtained by the reaction is suction filtered to recover the catalyst, acetic anhydride and acetic acid are recovered by distillation under reduced pressure, and then washed with deionized water, 2% sodium carbonate aqueous solution, and then washed with water until the water phase is neutral, and the water is removed by distillation under reduced pressure , That is, tri-n-butyl acetyl citrate....

Embodiment 3

[0023] Using the same fixed-bed reactor as above, the molar ratio of acetic anhydride to tri-n-butyl citrate is 2.4:1, and the temperature of the heating circulating water is 40°C. -1 .cm -2 The flow rate of the reaction material of the above-mentioned proportion is passed through the bed layer after being preheated by a serpentine tube, and the crude product of acetyl tri-n-butyl citrate is obtained, and the yield is 99.0%, and there is no tri-n-butyl citrate on the gas chromatogram. peak, indicating that tri-n-butyl citrate has been completely converted. After the crude product obtained by the reaction is suction filtered to recover the catalyst, acetic anhydride and acetic acid are recovered by distillation under reduced pressure, and then washed with deionized water, 4% sodium carbonate aqueous solution, and then washed with water until the water phase is neutral, and the water is removed by distillation under reduced pressure , That is, tri-n-butyl acetyl citrate. Accor...

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Abstract

The invention discloses a method and setting of acetyl tributyl that is catalytic synthesized by solid-bed reactor. The steps are as follows: 1) adding accelerant and filler in solid-bed reactor according to priority by direct filling method, preheating and keeping constant temperature by constant temperature water; 2) preheating acetyl tributyl and acetic anhydride by preheating section, and then entering pipe fixed bed for reaction, getting acetyl tributyl crude product; 3) vacuum distilling the mention crude product to recover acetic anhydride and ethyl acetate, washing by aqueous alkali, and then rinshing to water phase show neutral, removing moisture by vacuum distillation, getting the acetyl tributyl. This invention is easy to accomplish, the setting is few, the operating condition is easy to control, the used accelerant is cheap and easy getted, the catalysis performance is good, the agelimit is long and regenaration is easy. The getted acetyl tributyl is more than 99% by gas-chromatography analysis.

Description

technical field [0001] The invention relates to a device and a method for catalytically synthesizing acetyl tri-n-butyl citrate in a fixed-bed reactor. Background technique [0002] Acetyl tri-n-butyl citrate is a new type of non-toxic additive and plasticizer that can be used in plastic processing industries such as food packaging, medical appliances, children's toys, and personal hygiene products. It has good compatibility, and the plasticized plastic has good low-temperature flexibility, and is heat-stable, light-resistant, water-resistant, and cold-resistant when it is melt-sealed. [0003] In the catalytic synthesis method of acetyl tri-n-butyl citrate given in the literature, it is all batch production, and the catalyst used is a heterogeneous catalyst, which needs to be stirred during the reaction, and the loss of the catalyst is serious. After the reaction, the catalyst needs to be separated and recovered. Inconvenient to operate. Contents of the invention [000...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/716C07C67/313
Inventor 何潮洪谢春和
Owner ZHEJIANG UNIV
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