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Method for synthesizing long-chain alkyl carbonate by transesterification

A technology for long-chain alkyl carbonates and long-chain alkanols, applied in the field of synthesizing long-chain alky Carbonate yield is unknown and other problems, to achieve good stability, high catalytic activity, good selectivity effect

Inactive Publication Date: 2008-09-03
CHENGDU ORGANIC CHEM CO LTD CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] There are relatively few studies on heterogeneous catalysts for synthesizing long-chain alkyl carbonates by transesterification, and the yields of existing solid base catalysts for long-chain alkyl carbonates are low; solid acid catalysts have complex preparation steps, and high-carbon alcohol carbonic acid The yield of the ester is unknown

Method used

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  • Method for synthesizing long-chain alkyl carbonate by transesterification

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Carrier Al 2 o 3 Roast at 600°C for 4h, according to KNO 3 10%, Al 2 o 3 Weigh a certain KNO for 90% composition (mass percentage) 3 Prepared as an aqueous solution, the Al 2 o 3 Add it into the above aqueous solution and stir for 2 hours, then let it stand for 10 hours, dry the obtained sample in an oven at 110°C for 5 hours, and roast it in a muffle furnace at 500°C for 4 hours, take it out and grind it to get a supported catalyst. In a three-necked beaker connected with a nitrogen inlet tube, a constant pressure dropping funnel, a thermometer and a rectification column, 0.84 g of the prepared catalyst and 74.5 g of lauryl alcohol were added. When the temperature rises to 140°C, start to add dimethyl carbonate dropwise. The total amount of dimethyl carbonate added is 9.07g. Calculate the reaction time from the start of adding dimethyl carbonate dropwise, and react for 4 hours; Azeotrope of Methanol and Dimethyl Carbonate. The reaction liquid was analyzed by ga...

Embodiment 2

[0032] The preparation and evaluation method of the catalyst are the same as in Example 1, the number of carbon atoms of the long-chain alcohol is adjusted, and n-octanol is used as a raw material, in a three-necked beaker connected with a nitrogen inlet pipe, a constant pressure dropping funnel, a thermometer and a rectifying column , 0.59 g of the prepared catalyst and 50.09 g of n-octanol were added. When the temperature rises to 140°C, start to add dimethyl carbonate dropwise. The total amount of dimethyl carbonate added is 9.07g. Calculate the reaction time from the start of adding dimethyl carbonate dropwise, and react for 4 hours; Azeotrope of Methanol and Dimethyl Carbonate. The reaction solution was analyzed by a gas chromatograph, and the quantitative analysis was carried out by the calibration normalization method. It was found that the conversion rate of dimethyl carbonate was 82.56%, the yield of di-n-octyl carbonate was 80.65%, and the selectivity was 97.69%.

Embodiment 3

[0034]The preparation and evaluation method of the catalyst is the same as in Example 1, the number of carbon atoms of the long-chain alcohol is adjusted, and n-hexadecanol is used as a raw material, in a three-necked beaker connected with a nitrogen inlet pipe, a constant pressure dropping funnel, a thermometer and a rectifying column 1.06 g of the prepared catalyst and 96.98 g of n-hexadecanol were added. When the temperature rises to 160°C, start to add dimethyl carbonate dropwise. The total amount of dimethyl carbonate added is 9.07g. Calculate the reaction time from the start of adding dimethyl carbonate dropwise, and react for 4 hours; Azeotrope of Methanol and Dimethyl Carbonate. The reaction solution was analyzed by a gas chromatograph, and quantitatively analyzed by the calibration normalization method. It was found that the conversion rate of dimethyl carbonate was 79.37%, the yield of di-n-hexadecyl carbonate was 76.05%, and the selectivity was 95.82%.

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Abstract

The invention provides a method for preparing long-chain alkyl carbonic ester by ester interchange under the existing condition of supported catalyst and using methyl carbonate and long chain alkyl alcohol as raw material, wherein the catalyst is loaded on kinds of carriers by isovolumetric impregnation method by soluble alkaline metal and alkali salt, the range of mass ratio between alkaline metal or soluble salt of alkaline metal and the carrier is: 0. 05-0. 25, the sintering temperature is 400-900 degree C. the catalyst for the reaction synthesizing long-chain alkyl carbonic ester by ester interchange has good catalytic activity and high selectivity, the yield of long-chain alkyl carbonic ester can reach more than 75, and the selectivity reaches more than 95 More particularly, the catalyst causes no pollution to environment and no corrosion to the equipment, and is easy for separating, reclaiming and preparing.

Description

technical field [0001] The invention relates to a method for synthesizing long-chain alkyl carbonate by transesterification using dimethyl carbonate and long-chain alkyl alcohol as raw materials in the presence of a loaded catalyst. Background technique [0002] Long-chain alkyl carbonate is a transparent liquid or oil with low pour point, good lubricity, wear resistance, self-cleaning property, corrosion resistance and good solubility in hydrocarbon oils. High thermo-oxidative stability, it is a good lubricating oil base material, can be widely used in the metal processing manufacturing industry, high-end equipment, automobiles, etc.; can also be used in textiles, cosmetics, metal degreasing, leather processing industries. At present, there are relatively few studies on this kind of long-chain alkyl carbonate, and the synthesis methods mainly include phosgene method, oxidative carbonylation method, urea alcoholysis method, transesterification method and so on. The phosgen...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/96C07C68/06
Inventor 王公应范燕平杨先贵王庆印姚洁
Owner CHENGDU ORGANIC CHEM CO LTD CHINESE ACAD OF SCI