Preparation of Triacetin CAS 102-76-1
(1) The molar ratio of glycerol to methyl acetate is 1:1.2, which is added into the reactor with reflux device, and the potassium hydroxide solution with the concentration of 3 ~ 5wt% is added as the catalyst for reaction for 1 ~ 2.5 hours to obtain the reaction product, which is a mixture containing glycerol triacetate, methyl acetate, glycerol, methanol and alkali catalyst;
(2) Distilling the mixture obtained in step (1) at 70 ~ 80 ℃, separating the mixture of methyl acetate and methanol, and obtaining the mixture of glycerol triacetate, glycerol and alkali catalyst; The obtained mixture of methyl acetate and methanol is separated by water, methyl acetate is separated, and methanol aqueous solution is obtained, which is used to produce glass water. The separated methyl acetate is refluxed to step (1) and used as raw material.
(3) Extracting the mixture of glycerol triacetate, glycerol and alkali catalyst obtained in step (2) with an extractant, separating the mixture of alkali catalyst and glycerol, and obtaining the mixture of glycerol triacetate and extractant; The separated mixture of alkali catalyst and glycerol is refluxed to step (1) as raw material and alkali catalyst.
(4) The mixture of glycerol triacetate and extractant obtained in step (3) is distilled at the temperature of 80 ~ 90 ℃, and the extractant is separated to obtain the final product glycerol triacetate. The separated extractant is refluxed to step (3) and used as extractant.
Test of Triacetin CAS 102-76-1
Glyceryl triacetate is a common plasticizer for acetate fiber filter rod. Its dosage directly affects the hardness, pressure drop and shrinkage of the filter rod, and then affects the filtration efficiency of the filter rod and the suction quality of cigarettes. Therefore, the tobacco industry promulgated and implemented the standard of glyceryl triacetate for tobacco (yc144-2008) in 2008. The standard requires the purity of glyceryl triacetate for tobacco to reach more than 99%. At the same time, it is recommended to use the normalization method to detect the content of glyceryl triacetate products.
- Using ethanol as solvent, trans anisole as internal standard, polar capillary column was used for chromatographic separation, and gas chromatograph with FID detector was used for detection. An internal standard quantitative method of glycerol triacetate in plasticizer was established. The results show that this method can accurately determine the purity of tobacco triacetate compared with the quantitative method recommended in tobacco triacetate (yc144-2008). The linear regression coefficient of glycerol triacetate was > 0.999 in the content range of 33% - 110%; The recovery was 95.4% - 105%, and the RSD was less than 1%. Compared with the normalization method recommended by YC / t144-2008, the method established in this paper can improve the accuracy of judging whether the product meets the requirements, so as to reduce the misjudgment of product quality.
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