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A kind of method of synthesizing tributyl citrate

A technology of tributyl citrate and citric acid, which is applied in the preparation of carboxylic acid esters, chemical instruments and methods, and the preparation of organic compounds, etc., can solve the problems of high cost, toxicity and degradability of ionic liquids, and achieve short reaction time , low cost, and mild reaction conditions

Active Publication Date: 2016-05-18
XIAN ORIGIN CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

A series of studies have shown that conventional ionic liquids such as imidazole and pyridine have high cost, certain toxicity and poor degradability, and are not easy to degrade through the most widely used biological treatment process or biological self-purification.

Method used

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  • A kind of method of synthesizing tributyl citrate
  • A kind of method of synthesizing tributyl citrate
  • A kind of method of synthesizing tributyl citrate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Step 1. Preparation of choline chloride-based acidic ionic liquid: Add 0.5 mol of choline chloride into a 500 mL flask, then add 0.5 mol of citric acid, heat and stir at 100° C. for 1.5 h under a nitrogen atmosphere , obtain choline chloride acidic ionic liquid after cooling;

[0029] Step 2, esterification reaction: add 2.0mol n-butanol and the choline chloride acidic ionic liquid described in step 1 to a four-necked flask with mechanical stirring, thermometer, reflux condenser and water separator, and heat to reflux and stir , the water produced by the reaction is separated from the water separator, and the reaction is stopped when the reaction reaches anhydrous and then enters the water separator, and choline chloride is separated out from the reaction system; the temperature of the heating and reflux stirring is 110° C. 1500rpm;

[0030] Step 3, separation of choline chloride: filter the reaction system after the reaction in step 2 to obtain solid choline chloride ...

Embodiment 2

[0033] The method of embodiment 2 and embodiment 3 is all identical with embodiment 1, wherein difference is that the molar consumption of citric acid is respectively 0.25mol and 1mol, and the molar consumption of n-butanol is respectively 1mol and 4mol, see table 1.

[0034] Conversion rate and productive rate of table 1 embodiment 1 to embodiment 3

[0035] Example

Embodiment 4

[0037] Step 1. Preparation of choline chloride-based acidic ionic liquid: add 0.5 mol of choline chloride into a 500 mL flask, then add 0.25 mol of citric acid, heat and stir at 120° C. for 1 h under a nitrogen atmosphere, Obtain choline chloride acidic ionic liquid after cooling;

[0038] Step 2, esterification reaction: add 1.0mol n-butanol and the choline chloride acidic ionic liquid described in step 1 to a four-necked flask with mechanical stirring, thermometer, reflux condenser and water separator, and heat to reflux and stir , the water produced by the reaction is separated from the water separator, and the reaction is stopped when the reaction reaches anhydrous and then enters the water separator, and choline chloride is precipitated from the reaction system; the temperature of the heating and reflux stirring is 160 ° C, and the stirring rate 800rpm;

[0039] Step 3, separation of choline chloride: filter the reaction system after the reaction in step 2 to obtain soli...

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Abstract

The invention discloses a method for synthesizing tributyl citrate. The method comprises the following steps: I, preparing a choline chloride acidic ionic liquid; II, performing esterification reaction; III, filtering the reaction system after reaction, thereby obtaining solid choline chloride and a liquid phase product; and IV, performing atmospheric distillation on the liquid phase product, washing residues generated after atmospheric distillation by using an alkali solution, adding activated carbon to decolor, filtering to remove the activated carbon, performing reduced pressure distillation on residues generated after filtration, and collecting fraction of 197-200 DEG C, thereby obtaining tributyl citrate. According to the method, choline chloride and citric acid are adopted to synthesize the acidic ionic liquid, the synthesized acidic ionic liquid is both a raw material and a catalyst, the acidic ionic liquid has esterification reaction with n-butyl alcohol to synthesize n-butyl alcohol, the efficiency of the esterification reaction is improved, the conversion rate can be greater than 90%, the choline chloride after esterification can be recycled and utilized, and the cost is low.

Description

technical field [0001] The invention belongs to the technical field of organic chemical synthesis, in particular to a method for synthesizing tributyl citrate. Background technique [0002] Tributyl citrate is a non-toxic, odorless, green and environmentally friendly new plasticizer. It has received widespread attention due to its excellent properties such as non-toxic, light resistance, heat resistance, good stability, and durability. At present, it has become a "green substitute" for traditional phthalate plasticizers, and can be used in food packaging, medical appliances, children's toys and personal hygiene products. Tributyl citrate has excellent compatibility with all kinds of cellulose, and also has good solubility for vinyl resin and some natural resins. It can be used as a solvent-based plasticizer for vinyl acetate and other kinds of cellulose. agent. In addition, due to its low solubility in oils, it can also be used in oil-resistant formulations. As a new type...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C67/08C07C69/704B01J31/02
CPCC07C67/08C07C69/704
Inventor 王宪沛刘卫涛李小安李潇雷东卫张辉辉李文张立龙闫俊
Owner XIAN ORIGIN CHEM TECH
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