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Method for preparing glycerol triacetate by utilizing polymer-supported mesoporous catalyst

A technology of triacetin and polymer loading, which is applied in chemical instruments and methods, preparation of organic compounds, separation/purification of carboxylic acid esters, etc., to achieve the effects of no catalyst residue, improved production efficiency, and improved production efficiency

Inactive Publication Date: 2017-07-14
JIANGSU RUICHEN CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] There are many documents on the preparation method of glyceryl triacetate, but there is no document that uses polymer-supported mesoporous catalysts to replace sulfuric acid and phosphoric acid to prepare glycerol triacetate.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Embodiment 1: a kind of method utilizing macromolecule supported mesoporous catalyst to prepare glycerol triacetate, described method comprises the following steps:

[0028] (a) Glycerol, acetic acid and water-carrying agent are pre-mixed, preheated, and then enter a fixed-bed reactor filled with a polymer-supported mesoporous catalyst for esterification; the polymer-supported mesoporous catalyst is a mesoporous size The catalyst of high molecular polymer loaded heteropolyacid; described high molecular polymer is the polymer of p-stilbene, chloromethylstyrene and three (2-aminoethyl) amine; described heteropolyacid is At least one of heteropoly acids such as phosphotungstic acid and silicotungstic acid;

[0029] (b) sending the above-mentioned esterification reaction product into a dehydration tower for distillation and dehydration, and the temperature at the top of the tower is between 80°C and 100°C;

[0030] (c) Send the above-mentioned dehydrated material into an a...

Embodiment 2

[0039] Embodiment 2: a kind of method utilizing macromolecule supported mesoporous catalyst to prepare glycerol triacetate, specifically:

[0040] Mix 10kg glycerin, 22kg acetic acid and 6kg water-carrying agent, preheat, and then enter a fixed-bed reactor filled with a polymer-loaded mesoporous catalyst for esterification; send the esterification reaction product into a dehydration tower for distillation and dehydration. The top temperature is controlled between 85°C and 95°C; the dehydrated material is sent to the acylation kettle, and acetic anhydride is added for acylation reaction; the acylation temperature is controlled between 145°C and 155°C and kept for 1 hour; acylation After the reaction is completed, deacidification, high vacuum distillation, decolorization, deodorization and refining are carried out to obtain triacetin product.

[0041] The macromolecule supported mesoporous catalyst adopted in the present embodiment is the catalyst of the macromolecule polymer su...

Embodiment 3

[0042] Embodiment 3: a kind of method utilizing macromolecule supported mesoporous catalyst to prepare glycerol triacetate, specifically:

[0043] Glycerin, acetic acid and water-carrying agent are mixed and preheated, and then enter a fixed-bed reactor filled with a polymer-loaded mesoporous catalyst for esterification reaction; the esterification reaction product is sent to a dehydration tower for distillation and dehydration, and the temperature at the top of the tower is controlled Between 90°C and 95°C; send the dehydrated material into the acylation kettle, and add acetic anhydride to carry out the acylation reaction; the acylation temperature is controlled between 150°C and 155°C, and the temperature is kept for 1.5h; the acylation reaction is completed Finally, carry out deacidification, high vacuum distillation, then decolorization, deodorization and refinement to obtain triacetin product.

[0044] The polymer loaded mesoporous catalyst adopted in the present embodime...

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Abstract

The invention discloses a method for preparing glycerol triacetate by utilizing a polymer-supported mesoporous catalyst. The method comprises the following steps of (a) pre-mixing glycerinum, acetic acid and a water-carrying agent, preheating, then feeding in a fixed bed reactor filled with the polymer-supported mesoporous catalyst for carrying out esterification reaction; (b) feeding the esterification reaction product into a dehydrating tower for carrying out distillation dehydration, wherein the tower top temperature ranges from 80 DEG C to 100 DEG C; (c) feeding the dehydrated material into an acylation kettle, and adding acetic anhydride for carrying out acylation reaction, wherein the acylation temperature ranges from 140 DEG C to 160 DEG C, and the warm is kept for 1 to 3h; (d) after finishing acylation reaction, carrying out deacidification and high vacuum distillation, and then decoloring, deodorizing and refining to obtain a glycerol triacetate finished product. Through the manner, the method provided by the invention is not only high in catalytic activity, good in selectivity and good in recycling, but also environmental-friendly, the production efficiency is greatly improved, and the discharge of the three wastes is reduced.

Description

technical field [0001] The invention relates to the field of preparation of chemical products, in particular to a preparation method of glycerol triacetate. Background technique [0002] Glyceryl triacetate, also known as glycerol triacetate, is a colorless, odorless, oily liquid, non-toxic and non-irritating. Its English name is Glycerol Triacetate, and its molecular formula is C 9 h 14 o 6 , with a molecular weight of 218.21. Solubility: Soluble in alcohol, ether, benzene, chloroform and castor oil, but insoluble in linseed oil. It can dissolve nitrocellulose, cellulose acetate, acrylic resin, polyvinyl acetate, etc. It is a good solvent and plasticizer, and is widely used in food, spices, printing and dyeing and tobacco industries. The method for preparing triacetin in traditional industry is to use glycerin and acetic acid as raw materials, mainly adopt inorganic liquid acids such as sulfuric acid and phosphoric acid as catalysts, carry out esterification under the ...

Claims

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Application Information

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IPC IPC(8): C07C67/08C07C69/18C07C67/48
CPCC07C67/08C07C67/48C07C69/18
Inventor 陈祥宋宇飞钱建强张勇钱冬
Owner JIANGSU RUICHEN CHEM