A kind of synthetic method of 2,2,4-trimethylpentanediol diester
A technique for the synthesis of trimethylpentanediol diester, which is applied in chemical instruments and methods, preparation of ester groups and hydroxyl groups, organic compound/hydride/coordination complex catalysts, etc., can solve complex process, Low production efficiency, many side reactions, etc., to achieve high catalytic efficiency, reduced production cost, and good catalytic effect
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[0018] A kind of synthetic method of 2,2,4-trimethylpentanediol diester, described synthetic method comprises the following steps:
[0019] In the presence of a catalyst, 2,2,4-trimethylpentanediol monoester undergoes an esterification reaction at 120-170°C for 1-3 hours to prepare 2,2,4-trimethylpentanediol bis esters and 1,3-diols;
[0020] Separating 2,2,4-trimethylpentanediol diester and 1,3-diol to obtain 2,2,4-trimethylpentanediol diester;
[0021] The catalyst is a benzothiazole ionic liquid.
[0022] As a preferred embodiment, the benzothiazole ionic liquid is selected from benzothiazole hydrogen sulfate, benzothiazole dihydrogen phosphate, benzothiazole perchlorate, benzothiazole nitrate, 3-(3 - sulfonic acid) propyl benzothiazole hydrogen sulfate, 3-(3-sulfonic acid) propyl benzothiazole perchlorate, 3-(3-sulfonic acid) propyl benzothiazole dihydrogen phosphate one or several.
Embodiment approach
[0023] As a preferred embodiment, the synthetic method of the benzothiazole ionic liquid is:
[0024] Add 13.6g of benzothiazole compounds and 50ml of absolute ethanol into the reaction vessel, fully stir and drop 150g of inorganic acid aqueous solution under the condition of ice-water bath, continue to react at room temperature for 2-5 hours after the addition is completed, and filter to remove After solvent, it was washed with ethyl acetate, filled and crystallized under absolute ethanol to obtain benzothiazole ionic liquid.
[0025] As a preferred embodiment, the benzothiazole compound is selected from one or both of benzothiazole and 3-(3-sulfonic acid)propylbenzothiazole.
[0026] As a preferred embodiment, the mass content of the inorganic acid in the aqueous inorganic acid solution is 10-50%.
[0027] As a preferred embodiment, the aqueous inorganic acid solution is selected from one or more of nitric acid solution, sulfuric acid solution, and perchloric acid solution....
Embodiment 1
[0034] In the reaction vessel with stirring device and temperature control system, add 100 parts by weight of 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate, add 2 parts by weight of benzothiazole Bisulfate ionic liquid, controlled reaction temperature 140°C under full stirring, carried out transesterification reaction for 2 hours to obtain 2,2,4-trimethyl-1,3-pentanediol diisobutyrate and 2,2, 4-Trimethyl-1,3-pentanediol. After separating the ionic liquid catalyst, control the temperature between 170-190° C., and carry out rectification and separation at a pressure of -0.003 MPa to obtain 2,2,4-trimethyl-1,3-pentanediol diisobutyrate. The yield of 2,2,4-trimethyl-1,3-pentanediol diisobutyrate was 79.0%.
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