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Method for synthesizing trioctyl lemon acid

A technology of trioctyl citrate and citric acid, applied in the field of organic chemical synthesis, can solve the problems of complicated post-processing, difficult refining, serious equipment corrosion, etc., and achieves the effects of small catalyst dosage, no environmental pollution, and mild reaction conditions

Inactive Publication Date: 2008-08-20
EAST CHINA NORMAL UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The traditional method of synthesizing trioctyl citrate uses 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 trioctyl lemon acid
  • Method for synthesizing trioctyl lemon acid
  • Method for synthesizing trioctyl lemon acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] The preparation of the first step naphthalenesulfonic acid methylal

[0015] Heat 10g of naphthalene to 160°C, then slowly add 10ml of concentrated sulfuric acid dropwise, then heat and stir at 140°C for 5h, then cool to 100°C, add 2ml of water, dropwise add 10ml of formaldehyde solution, keep heating at 100°C for 4h, to obtain black solid, then add boiling water to wash, filter with suction, and dry at 120°C to obtain methylal of naphthalenesulfonic acid.

[0016] Step 2 esterification reaction

[0017] Add 0.1mol citric acid, 0.45mol n-octanol, and 10ml water-carrying agent toluene into a 100mL three-necked bottle equipped with electromagnetic stirring, a thermometer, a reflux condenser, and a water separator, and heat and stir. After the citric acid is completely dissolved, add 0.3g of naphthalenesulfonic acid methylal is heated under reflux and stirred to separate the water generated by the reaction from the water separator, and the reaction is stopped when there i...

Embodiment 2-4

[0022] Except for the following differences, all the other are the same as in Example 1. The amount of naphthalenesulfonic acid methylal is 0.3 g, the amount of citric acid is 0.1 mol, and the ratio of n-octanol in Table 1 is used for 4 hours.

[0023] Table 1

[0024]

Embodiment 5-7

[0026] Except following difference, all the other are identical with embodiment 1, and the consumption of naphthalenesulfonic acid methylal is respectively by table 2.

[0027] Table 2

[0028]

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PUM

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Abstract

The invention discloses a method for synthesizing trioctyl citrate, which adopts critric acid and n-octanol as reactants, in the process of ester synthesis, naphthalene sulfonic acid methylal is used as catalyst; after the reaction, the catalyst is filtered out from the materials left after the reaction, and after water washing, caustic washing and distillation, trioctyl citrate can be gained from filter liquid; the method has the advantages that, first, the high yield is high and is about 97.5 to 99.6 percent; second, the catalyst is cheap, and the amount of catalyst which takes up 0.1 to 2.0 percent of the total weight of reaction materials is little; third, the reaction conditions are mild, and the reaction time is short; fourth, the catalyst can be used repeatedly and fifth, no environmental pollution exists.

Description

technical field [0001] The invention relates to the technical field of organic chemical synthesis, in particular to a method for synthesizing trioctyl citrate. Background technique [0002] Trioctyl citrate is a non-toxic, odorless "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 trioctyl 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 ability of nitrocellulose, and is a solvent for various spices, and can also be used as a defoamer for protein solutions. Therefore, tri...

Claims

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Application Information

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IPC IPC(8): C07C69/704C07C67/08B01J31/02
Inventor 杨建国王有菲高珊王箭权南南张敬鲍少华何鸣元
Owner EAST CHINA NORMAL UNIVERSITY
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