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Preparation method of glyceryl triacetate

A technology of glycerol acetate and glycerol, which is applied in the field of preparation of glycerol triacetate, can solve the problem that the quality standard of glycerol triacetate cannot be reached, the production of high quality glycerol triacetate, the yield of glycerol triacetate and the The problem of low purity, etc., achieves the effect of good catalytic effect, reduction of side reaction polymerization products, and shortening of esterification time.

Active Publication Date: 2016-01-06
MILE KANGHE GLYCERIDE CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This is currently the most important industrial route for synthesizing glyceryl triacetate, but the reaction time of this process is longer, and the yield and purity of glyceryl triacetate obtained are all low, which cannot reach the quality standard of glycerol triacetate for cigarettes (99.50% pure)
[0008] At present, there are many routes for synthesizing triacetin, but the existing routes have low yield and high cost, are not suitable for industrial production, and cannot produce high-quality triacetin

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Step (1): Stir 1.0ml of concentrated sulfuric acid (1.84g) and 1.84g of activated carbon with pH=1 and raise the temperature to 180°C, keep it warm for 20min, cool it naturally, and place it at room temperature for 17 days to prepare the catalyst.

[0037]Step (2): Mix the catalyst prepared in step (1) and stir with 50ml of glycerin, 150ml of acetic acid and 20ml of ethyl acetate and heat up to 100°C. After 20 hours of reaction, the water content is 0.019%, and the reaction is stopped. Add 1.5g of activated carbon for decolorization, pump acid for 3 hours at a steam pressure of 0.45MPa and a temperature of 120°C, add saturated aqueous soda ash for neutralization, dehydrate at a temperature of 60-70°C, dehydrate at a steam pressure of 0.3MPa, dehydrate for 4 hours, and filter with suction to obtain Glyceryl triacetate, the recovery rate is 96%, the purity of glyceryl triacetate detected by GC is 99.79%, the moisture content is 0.016%, the color is No. 10 (platinum-cobalt)...

Embodiment 2

[0039] Step (1): Stir 0.5ml of concentrated sulfuric acid (0.92g) and 1.0g of activated carbon with pH=1 and raise the temperature to 180°C, keep it warm for 20min, cool it naturally, and place it at room temperature for 15 days to prepare the catalyst.

[0040] Step (2) Heat the catalyst prepared in step (1) with 50ml of glycerin, 180ml of acetic acid and 30ml of ethyl acetate to 130°C. After 18 hours of reaction, the water content is 0.029%, and the reaction is stopped. Add 1.85g of activated carbon for decolorization, pump acid for 3 hours at a steam pressure of 0.35MPa and a temperature of 140°C, add a saturated aqueous solution of soda ash for neutralization, dehydrate at a temperature of 80~90°C, and a steam pressure of 0.25MPa, dehydrate for 4 hours, and filter to obtain Glyceryl triacetate, the recovery rate is 95%, the purity of glyceryl triacetate detected by GC is 99.71%, the moisture content is 0.018%, the color is No. 10 (platinum-cobalt), the acidity is 0.004%, an...

Embodiment 3

[0042] Step (1) Stir 1.0ml of concentrated sulfuric acid (1.84g) and 2.2g of activated carbon with a pH of 1 and raise the temperature to 180°C, keep it warm for 30 minutes, cool it naturally, and place it at room temperature for 20 days to prepare the catalyst.

[0043] Step (2): Heat the catalyst prepared in step (1) with 50ml of glycerin, 200ml of acetic acid and 50ml of cyclohexane to 120°C. After 19 hours of reaction, the water content is 0.018%, and the reaction is stopped. Add 1.25g of activated carbon for decolorization, pump acid for 4 hours at a steam pressure of 0.45MPa and a temperature of 130°C, add saturated aqueous soda ash for neutralization, dehydrate at a temperature of 70°C, dehydrate at a steam pressure of 0.20MPa, and dehydrate for 4 hours, and filter to obtain three Glyceryl acetate. The yield was 96%, the purity of triacetin detected by GC was 99.80%, the moisture content was 0.022%, the chromaticity was No. 10 (platinum-cobalt), the acidity was 0.0036%,...

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Abstract

The invention discloses a preparation method of glyceryl triacetate. The preparation method comprises the following steps: 1, mixing and stirring concentrated sulfuric acid and activated carbon, wherein the pH value of the activated carbon is 1, the mass ratio of the sulfuric acid to the activated carbon is 1: 0.5-2, raising the temperature to 150-190 DEG C, preserving the temperature for 10-30 minutes, conducting natural cooling, then placing the mixture at the normal temperature, and obtaining a catalyst; 2, mixing the catalyst obtained in step 1 with glycerin, acetic acid and dehydrating agents, raising the temperature to 100-150 DEG C, getting the mixture to react, and obtaining glyceryl triacetate through post-treatment, wherein the volume mass ratio of glycerin to the catalyst is 1: 0.004-0.10. According to the preparation method, a novel catalytic reaction is adopted, esterification time is shortened by about 10 hours, energy is saved, and the cost is lowered; compared with a method in which concentrated sulfuric acid serves as a catalyst, the novel catalyst is used for preparing glyceryl triacetate, side reaction polymerization products are reduced, and product purity is raised to above 99.7% from 98.0-99.0%.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a preparation method of glycerol triacetate. Background technique [0002] The molecular formula for triacetin is C 9 h 14 o 6 , CAS No. 102-76-1, a colorless oily liquid with a faint fruity, sweet meaty taste and a bitter taste at low concentrations. Glyceryl triacetate is an intermediate of many fine chemical products, and can be used as soil hardener, casting hardener, fungicide, fixative, wetting agent, food additive, cleaning disinfectant, ignition aid and adhesive It is a very popular chemical raw material with a consumption of more than 10,000 tons in our country. [0003] Glyceryl triacetate can also be used to form cigarette filter rods, rolled into filter rods, and then packaged into cigarettes. When consumers smoke cigarettes, the harmful components in glycerol triacetate will enter the human body through the mouth, affecting the health of co...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/18C07C67/08B01J27/02
CPCB01J27/02C07C67/08C07C69/18
Inventor 杨崇光
Owner MILE KANGHE GLYCERIDE CO LTD
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