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Method for catalytic synthesis of tributyl citrate by utilizing immobilized p-toluenesulfonic acid

A technology of tributyl citrate and p-toluenesulfonic acid, which is applied in the chemical industry, can solve the problems of complex post-treatment process, many catalyst side reactions, complex preparation process, etc., achieve easy recovery and reuse, and improve the efficiency of esterification reaction , The effect of simplifying the post-processing process

Active Publication Date: 2014-06-11
BENGBU BBCA MEDICINE SCI DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The traditional production process uses concentrated sulfuric acid as a catalyst, but this catalyst has many side reactions, difficult refining, serious equipment corrosion, complicated post-treatment process, and waste acid pollution. Its application has been greatly restricted.
Some catalysts that have been studied more later, such as solid superacids, have good catalytic activity for this reaction, but their preparation process is complicated and costly, which is not conducive to industrial production.

Method used

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  • Method for catalytic synthesis of tributyl citrate by utilizing immobilized p-toluenesulfonic acid
  • Method for catalytic synthesis of tributyl citrate by utilizing immobilized p-toluenesulfonic acid
  • Method for catalytic synthesis of tributyl citrate by utilizing immobilized p-toluenesulfonic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] 1) Preparation of immobilized p-toluenesulfonic acid

[0023] Add 2.5g of sodium alginate, 5g of polyvinyl alcohol and 1.5g of p-toluenesulfonic acid into 100mL of deionized water, mix well, heat in a constant temperature water bath at 80°C to dissolve completely, cool to about 45°C, and use a constant temperature The flow pump drips it into 100mL of calcium chloride solution with a mass percentage of 1.5% at a speed of 60rpm and continuously stirs at a slow speed. After the calcium chloride solution is dripped, stop stirring, and place it at 4°C for crosslinking for 24 hours. After that, it was taken out and filtered to obtain immobilized p-toluenesulfonic acid.

[0024] 2) Esterification reaction

[0025] Add 308g of n-butanol, 200g of citric acid, and the immobilized p-toluenesulfonic acid obtained in step 1) into a 500mL three-neck flask equipped with electromagnetic stirring, a thermometer, a reflux condenser, and a water separator, and heat and reflux at 130°C. ...

Embodiment 2-4

[0029] Only change n-butanol consumption, all the other are with embodiment 1. The results are shown in Table 1.

[0030] Table 1

[0031]

Embodiment 5-7

[0033] Only change the esterification reaction temperature, all the other are with embodiment 1. The results are shown in Table 2.

[0034] Table 2

[0035]

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Abstract

The invention provides a method for catalytic synthesis of tributyl citrate by utilizing immobilized p-toluenesulfonic acid, comprising the steps of taking the immobilized p-toluenesulfonic acid as a catalyst, carrying out esterification reaction on citric acid and n-butyl alcohol and synthetizing the tributyl citrate. The method provided by the invention has the advantages that: the immobilized p-toluenesulfonic acid adopted as the catalyst has no obvious corrosivity and is easy to recover and repeatedly utilize, the activity of the recovered catalyst basically remains unchanged; the esterification reaction efficiency is increased and the product yield can be up to 97.2-99.6%; adopting the reactant n-butyl alcohol as a water-carrying agent not only avoids the use of toxic solvents such as toluene and the like but also simplifies the aftertreatment process; the esterification reaction is mild in condition and simple in process, and the method is suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of chemical industry, in particular to a method for catalytically synthesizing tributyl citrate with immobilized p-toluenesulfonic acid. Background technique [0002] Tributyl citrate is a new type of non-toxic plasticizer, which has the characteristics of good compatibility, high plasticizing efficiency, non-toxicity, low volatility, cold resistance, mildew resistance, light resistance and water resistance. At present, the plasticizers commonly used in industry are phthalates. Because they can induce cancer, their use has been strictly controlled abroad. my country has also formulated relevant laws and regulations, and will gradually phase out their use in food packaging materials, medical appliances, and toys. However, tributyl citrate is used as a new substitute, so it has excellent development and application prospects. [0003] Tributyl citrate is usually formed by the esterification of citric acid and n-butanol ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/704C07C67/08
Inventor 陶涛汪洪湖张亚孙建华韦亚锋李亚龙
Owner BENGBU BBCA MEDICINE SCI DEV
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