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Method for preparing triacetin by catalysis of solid superacid

A technology of triacetin and solid super acid, which is applied in the preparation of carboxylate, chemical instruments and methods, preparation of organic compounds, etc. The effect of reducing side reactions, causing secondary pollution and reducing production costs

Inactive Publication Date: 2011-04-20
CHANGSHA ECONOMIC TECH DEV ZONE ZHONGCHENG INDAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although concentrated sulfuric acid or p-toluenesulfonic acid can make the reaction obtain a relatively ideal esterification rate, and the price is low, but the reaction is often accompanied by side reactions such as oxidation, carbonization, polymerization, rearrangement, etc., the selectivity is poor, and the product has a darker color. Perform complex post-treatment processes such as deacidification, acylation, neutralization, and filtration
At the same time, concentrated sulfuric acid severely corrodes equipment and is difficult to recycle, resulting in high production costs, some emissions are serious environmental pollution, and environmental protection pressure is high, making it difficult to further improve

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Take a certain amount of TiO 4 Dilute with water until there is no white smoke, add the same amount of ZrOCl 2 ·8H 2 O, stir to dissolve, adjust PH=10-11 with ammonia water, filter the precipitate after aging for 10h, wash the precipitate with distilled water until there is no Cl - (with 0.1mol / L AgNO 3 test). After drying the precipitate, it is pulverized, then impregnated with a certain concentration of sulfuric acid solution for a period of time, filtered, dried, and roasted to obtain the solid super acid SO 4 2- / ZrO 2 -TiO 2 catalyst.

[0026] Add a certain amount of glycerin and proportional glacial acetic acid into the reactor, and add 2% solid superacid SO 4 2- / ZrO 2 -TiO 2 Catalyst, adding isopropanol with 15% glycerin mass as water-carrying agent, heating and controlling at 130°C for reflux reaction, rectifying water during the reaction, when there is no water in the rectifying device, add the same molar glacial acetic acid as the initial glycerin ...

Embodiment 2

[0029] Will Fe 2 (SO 4 ) 3 solution and Ti(OC 4 h 9 ) 4 The solution was mixed according to a certain ratio, and NaOH solution was added dropwise to adjust the pH=8.0, aged for 4 hours, filtered and washed, dried, crushed until it could pass through a 80-mesh sieve, and then mixed with 0.15mol / L H 2 SO 4 The solution is immersed for a certain period of time, filtered, dried, and roasted to obtain the solid super acid SO 4 2- / Fe 2 o 3 -TiO 2 catalyst.

[0030] Modified solid superacid SO 4 2- / Fe 2 o 3 -TiO 2 It is catalyst, and its optimized synthetic condition is the mol ratio of the glacial acetic acid of initial reaction and added glacial acetic acid total amount and glycerin 1: 4.0, and catalyst consumption is 8% (in 0.12mol glycerol) of glycerin quality, isopropanol consumption It is 20% of the mass of glycerin. In the heating and reflux reaction, glacial acetic acid and water with a lower boiling point pass through the rectification device, and the aceti...

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PUM

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Abstract

The invention relates to a method for preparing triacetin by catalysis of solid superacid. The method is as follows: mixing a proper amount of glacial acetic acid and glycerin in proportion; adding a proper amount of solid superacid used as a catalyst in mixing solution; heating to 125-135 DEG C and then carrying out reflux reaction; in the reaction, leading the glacial acetic acid with a low boiling point and water to pass through a rectification device; leading the acetic acid in which water is removed by rectification to enter a reactor to continuously react; and replenishing a proper amount of glacial acetic acid and continuously controlling the temperature at 125-135 DEG C for reaction. The solid superacid can be recycled, and the highest yield of glycerin after reaction can be up to 96%. The invention provides an economical and environment-friendly method for producing the glycerin, which ensures that the yield of the glycerin is greatly improved. The catalyst is small in corrosion and can be recycled at the same time, thereby providing dual benefits in the aspects of process optimization and environmental protection for an enterprise.

Description

technical field [0001] The invention relates to a method for preparing glycerol triacetate by catalyzing a solid superacid, in particular to a production technology for preparing glycerol triacetate by catalyzing a solid superacid with low corrosiveness, strong acidity and high selectivity. Background technique [0002] Glyceryl triacetate, also known as glycerol triacetate. English name Glycerol Triacetate, molecular formula C 9 h 14 o 6 , Molecular weight 218.21, colorless and odorless oily liquid, non-toxic and non-irritating. Triacetin is soluble in alcohol, ether, benzene, chloroform, and castor oil, but not in linseed oil. Can dissolve nitrocellulose, acrylic resin, polyvinyl acetate, etc. Glyceryl triacetate has good gelling effect and physiological inertness, and is widely used as a plasticizing and curing agent for cellulose acetate in cigarette filters, food additives, cosmetic fixatives and lubricating bases. Glyceryl triacetate is widely used in tobacco, fo...

Claims

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Application Information

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IPC IPC(8): C07C69/18C07C67/08
CPCY02P20/584
Inventor 罗伟
Owner CHANGSHA ECONOMIC TECH DEV ZONE ZHONGCHENG INDAL
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