Synthetic method of tri-n-butyl citrate

A technology of tributyl citrate and a synthesis method, which is applied in the preparation of carboxylate, chemical instruments and methods, preparation of sulfonates, etc., can solve the problems of many side reactions, equipment corrosion, complex post-treatment process and the like

Inactive Publication Date: 2013-12-18
郑桂富
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The traditional production process uses concentrated sulfuric acid as a catalyst, but this catalyst has disadvantages such as many side reactions, dark product color, complicated post-treatment process, serious equipment corrosion, and environmental pollution by waste acid.

Method used

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  • Synthetic method of tri-n-butyl citrate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] A kind of synthetic method of tributyl citrate, comprises the following steps:

[0021] (1) Esterification: Add 192 parts by weight of anhydrous citric acid and 260 parts by weight of n-butanol into a reaction kettle with a stirring and heating device, heat to 90°C under stirring to completely dissolve the citric acid, then add 6 parts by weight of catalyzer, after the reaction at a temperature of 102°C for 3.5h, the esterification reaction is completed to obtain a reaction solution; the catalyzer is a mixture of sulfamic acid and activated carbon with a weight ratio of 15:1;

[0022] (2) Dealcoholization: The reaction solution obtained in step (1) was dealcoholized under the conditions of vacuum degree of 0.09MPa and temperature of 90°C for 20 minutes to obtain a mixture of tributyl citrate, activated carbon and sulfamic acid. The mixture of n-butanol and water is rectified to obtain n-butanol and recycled to step (1) for use;

[0023] (3) Filtration: The filtrate obt...

Embodiment 2

[0027] A kind of synthetic method of tributyl citrate, comprises the following steps:

[0028] (1) Esterification: Add 192 parts by weight of anhydrous citric acid and 410 parts by weight of n-butanol into a reaction kettle with a stirring and heating device, heat to 95°C under stirring to completely dissolve the citric acid, then add 17 parts by weight of catalyzer, after reacting 3.0h under the condition of 135 ℃ of temperature, esterification reaction finishes, obtains reaction liquid; Described catalyzer is the sulfamic acid and activated carbon mixture that weight ratio is 15:1;

[0029] (2) Dealcoholization: dealcoholize the reaction solution obtained in step (1) under the conditions of vacuum degree of 0.09MPa and temperature of 135°C for 30 minutes to obtain a mixture of tributyl citrate, activated carbon and sulfamic acid. The mixture of n-butanol and water is rectified to obtain n-butanol and recycled to step (1) for use;

[0030] (3) Filtration: The filtrate obtain...

Embodiment 3

[0034] A kind of synthetic method of tributyl citrate, comprises the following steps:

[0035] (1) Esterification: Add 192 parts by weight of anhydrous citric acid and 330 parts by weight of n-butanol into a reaction kettle with a stirring and heating device, heat to 93°C under stirring to completely dissolve the citric acid, then add 12 parts by weight of catalyzer, after reacting for 3.5h at a temperature of 115°C, the esterification reaction is completed to obtain a reaction solution; the catalyzer is a mixture of sulfamic acid and activated carbon with a weight ratio of 15:1;

[0036] (2) Dealcoholization: dealcoholize the reaction solution obtained in step (1) under the conditions of vacuum degree of 0.09MPa and temperature of 110°C for 25 minutes to obtain a mixture of tributyl citrate, activated carbon and sulfamic acid. The mixture of n-butanol and water is rectified to obtain n-butanol and recycled to step (1) for use;

[0037] (3) Filtration: Centrifuge the mixture ...

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Abstract

The invention provides a synthetic method of tri-n-butyl citrate, and particularly relates to a method which is used for synthesizing the tri-n-butyl citrate by using activated carbon absorption sulfamic acid as a catalyst and generating nickel sulfamic acid by reacting the reacted catalyst with nickel hydroxide. The synthetic method is characterized in that the activated carbon absorption sulfamic acid is used as the catalyst in a tri-n-butyl citrate synthesis process, and after synthesis reaction, solid activated carbon and sulfamic acid are filtered out from reaction mixture, and then the reaction mixture is dealcoholized, filtered, neutralized and dewatered so as to obtain the tri-n-butyl citrate; the activated carbon and the sulfamic acid which are separated out react with the nickel hydroxide so as to generate electroplating main salt with relatively high additional value, namely the nickel sulfamic acid. The catalyst used in the synthetic method has the advantages of good catalytic selectivity, high catalytic activity, low equipment corrosion, low cost and the like, and is easy to separate. The synthetic method has the characteristics that the conversion rate of the citric acid is high, the esterification reaction time is short, only water is discharged, and the like.

Description

technical field [0001] The present invention relates to a kind of synthetic method of tributyl citrate. Background technique [0002] Plasticizers are an important class of additives used in the polymer material industry. In the past, the plasticizers mainly used in China were phthalate plasticizers. Studies in recent years have shown that phthalate plasticizers are harmful to the human body, especially to children. Therefore, it is imperative to develop non-toxic and highly efficient plasticizers. [0003] As a plasticizer, tributyl citrate (TBC for short) has the advantages of good compatibility, high plasticizing efficiency, non-toxicity, low volatility, light resistance, water resistance, and cold resistance. The raw materials for the production of TBC are citric acid and n-butanol. my country is a big producer of citric acid, which provides raw material guarantee for the production of TBC. Therefore, using abundant citric acid resources to develop and produce tribu...

Claims

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Application Information

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IPC IPC(8): C07C69/704C07C67/08C07C309/14C07C303/32
Inventor郑桂富
Owner郑桂富