Method for synthesizing tributyl citrate

A technology of tributyl citrate and synthesis process, which is applied in the preparation of carboxylate, chemical instruments and methods, preparation of organic compounds, etc., can solve problems such as equipment corrosion, complicated post-treatment, and pollute the environment, and achieve mild reaction conditions. , The effect of small amount of catalyst and large specific surface area

Inactive Publication Date: 2011-05-25
SHAOXING UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The traditional method of synthesizing tributyl citrate is to use concentrated sulfuric acid as a catalyst [Edited by Song Qihuang, Fine Chemical Technology, Beijing: Chemical Industry Press, 1995: 95]. This catalyst has many side reactions, difficult refining, and serious equipment corrosion , complicated post-processing, producing industrial "three wastes", polluting the environment and other shortcomings, its application has been greatly restricted
Some catalyzers that develop later are as catalyzer [Xie Wenlei etc., fine petrochemical industry, 1998, (4): 7-9] with p-toluenesulfonic acid, all have good catalytic activity to this reaction, but catalyzer is expensive, and Cannot be reused

Method used

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  • Method for synthesizing tributyl citrate

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Embodiment 1, the preparation of tributyl citrate

[0028] (1) Gelatinized starch-based carbon-based solid acid: Add 10g of starch into 50ml of water, heat and stir at 70°C for 4 hours to obtain starch sol, place it in an oven at 85°C for drying, and finally add 5g of isethionic acid for After stirring and mixing, place it in a quartz tube muffle furnace, replace the air with nitrogen, and heat to 200°C in a nitrogen atmosphere for carbonization reaction for 12 hours to obtain a black solid. After the solid is cooled to room temperature, add 80°C The above hot water is washed and filtered until the filtrate is clear and acidic, and then the solid is placed in an oven at 120°C for 1 day to obtain an acid value of 2.3mmol / g and a thermal decomposition temperature of 2.3mmol / g. 180°C;

[0029] (2) Esterification reaction: Add 0.1mol citric acid and 0.45mol n-butanol to a 100mL three-necked bottle equipped with electromagnetic stirring, a thermometer, a reflux condenser, a...

Embodiment 2-4

[0032] The preparation method is the same as in Example 1, except that the amount of gelatinous starch-based carbon-based solid acid is 0.3 g, the amount of citric acid is 0.1 mol, the amount of n-butanol is according to the ratio in Table 1, and the reaction is 4 hours.

[0033] Table 1. Productivity comparison under different acid-alcohol ratios

[0034] Example

Embodiment 5-7

[0036] The preparation method is the same as that in Example 1, except that the gelatinous starch-based carbon-based solid acid is used in the amounts shown in Table 2.

[0037] Table 2, the yield contrast under different gelatinous starch-based carbon-based solid acid dosages

[0038] Example

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Abstract

The invention discloses a method for synthesizing tributyl citrate, in particular relates to a method for synthesizing the tributyl citrate through the catalysis of gel starch-based carbon-based solid acid, and belongs to the technical field of organic chemical synthesis. The method is characterized by comprising the following steps of: performing ester synthesis by taking the gel starch-based carbon-based solid acid as a catalyst; filtering the catalyst out of the reaction mixture after the reaction is finished; and performing water-washing and alkali-washing, distilling and the like to obtain the tributyl citrate. The method has the advantages of high yield, small using amount of catalyst, mild reaction condition, short reaction time, environmental friendliness and the like.

Description

Technical field: [0001] The invention relates to a method for synthesizing tributyl citrate, in particular to a method for catalyzing the synthesis of tributyl citrate with gelatinous starch-based carbon-based solid acid, which belongs to the technical field of organic chemical synthesis. Background technique: [0002] Tributyl citrate is a non-toxic and tasteless "green" environmental plastic plasticizer, widely used in food and medical instrument packaging, cosmetics, daily necessities, toys, military supplies, etc., with good compatibility, high plasticizing efficiency, no It has the advantages of toxicity, easy biodegradation and low volatility, excellent cold resistance, light resistance and water resistance, and has mildew resistance in the resin, and does not grow mold. The combination of tributyl citrate and other non-toxic plasticizers can increase the hardness of the product, especially for soft fiber ether. At the same time, it can improve the anti-ultraviolet ab...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/704C07C67/08B01J31/02
Inventor 梁学正
Owner SHAOXING UNIVERSITY
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