2,2,4-trimethyl pentanediol monoester synthesizing method
A technology of trimethylpentanediol monoester and synthesis method, which is applied in chemical instruments and methods, preparation of carboxylic acid esters, preparation of organic compounds, etc., can solve the problems of dehydration reaction of synthetic raw materials and low selectivity of synthesis reaction, etc. Improve selectivity and inhibit dehydration reaction
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[0019] A kind of synthetic method of 2,2,4-trimethylpentanediol monoester, described synthetic method comprises the following steps:
[0020] In the presence of an acidic catalyst, the alkyl aldehyde compound undergoes a condensation reaction for 1-5 hours;
[0021] The obtained mixture is separated and purified to obtain 2,2,4-trimethylpentanediol monoester;
[0022] The acidic catalyst is a mixture of oxalic acid and molecular sieve, the molecular sieve is a zeolite molecular sieve, and the surface of the zeolite molecular sieve has proton acid sites;
[0023] The structure of the alkyl aldehyde compound is as follows:
[0024]
[0025] The structure of the 2,2,4-trimethylpentanediol monoester is as follows:
[0026]
[0027] The R 1 , R 2 For methyl.
[0028] The molecular sieve of the present invention is a porous body having pores with uniform pore diameters. Among them, the form of molecular sieve zeolite and molecular sieve activated carbon is not particular...
Embodiment 1
[0054]In a reactor equipped with a condenser, a stirring device, and a thermometer, add 2g of 2,2,4-trimethylpentanediol monoester HY type zeolite (H-ZSM-52,2,4-trimethylpentanediol Monoester, exchange degree 90%, SiO2 / Al2O3 molar ratio 18) and 0.05g oxalic acid, add 200g isobutyraldehyde for condensation reaction, control the reaction temperature at 70-80 degrees Celsius, react at 70-80 degrees Celsius for 25 minutes, heat up To 100 degrees Celsius, the reaction temperature is controlled at 100-110 degrees Celsius, and the reaction is carried out at 100-110 degrees Celsius for 50 minutes to prepare a synthetic liquid. Under reduced pressure distillation under the condition of -0.097MPa, 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate was obtained. Analyzing the synthesis solution, the conversion rate of isobutyraldehyde was 86.9%, and the selectivity of 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate was 96.9%.
Embodiment 2
[0056] In a reactor equipped with a condenser, a stirring device, and a thermometer, add 2g of 2,2,4-trimethylpentanediol monoester HY type zeolite (H-ZSM-52,2,4-trimethylpentanediol Monoester, exchange degree 90%, SiO2 / Al2O3 molar ratio 23) and 0.1g oxalic acid, add 200g isobutyraldehyde for condensation reaction, control the reaction temperature at 70-80 degrees Celsius, react at 70-80 degrees Celsius for 25 minutes, heat up To 100 degrees Celsius, the reaction temperature is controlled at 100-110 degrees Celsius, and the reaction is carried out at 100-110 degrees Celsius for 40 minutes to prepare a synthetic liquid. Under reduced pressure distillation under the condition of -0.097MPa, 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate was obtained. Analyzing the synthesis liquid, the conversion rate of isobutyraldehyde was 88.3%, and the selectivity of 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate was 96.2%.
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