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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

Active Publication Date: 2020-05-08
RUNTAI CHEM TAIXING CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The problem of the above method is that after the reaction, the catalyst used needs to be removed by alkali neutralization, and the method has many side reactions, strong corrosion, complex process, low production efficiency, and produces a large amount of solid waste and waste water to pollute the environment.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[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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Abstract

The invention relates to a synthetic method of 2, 2, 4-trimethylpentanediol diester. The synthetic method includes following steps: at presence of a catalyst, allowing 2, 2, 4-trimethylpentanediol monoester to be in transesterification at 120-170 DEG C for 1-3h to obtain 2, 2, 4-trimethylpentanediol diester and 1, 3-diol; separating 2, 2, 4-trimethylpentanediol diester and 1, 3-diol to obtain 2, 2, 4-trimethylpentanediol diester, wherein the catalyst is benzothiazole ion liquid which is selected from one or multiple of benzothiazole hydrosulfate, benzothiazole dihydric phosphate, benzothiazoleperchlorate, benzothiazole nitrate, 3-(3-sulfonic acid) propyl benzothiazole hydrosulfate, 3-(3-sulfonic acid) propyl benzothiazole perchlorate and 3-(3-sulfonic acid) propyl benzothiazole dihydric phosphate. The benzothiazole ion liquid is adopted as the catalyst of transesterification, so that catalytic effect is good; the catalyst is simple and efficient in separation.

Description

technical field [0001] The invention relates to a synthesis method of 2,2,4-trimethylpentanediol diester. Background technique [0002] 2,2,4-Trimethylpentanediol diester is a new type of plasticizer. It is a green and non-toxic plasticizer with oil resistance, migration resistance, aging resistance and volatility resistance. It is an advantageous product with economic, social and environmental benefits. It has the characteristics of low viscosity, low density, low freezing point, hydrolysis resistance, colorless and transparent, high stability, safety and non-toxicity, etc. It is widely used in various PVC resin products, including PVC dipped gloves, toys, wallpaper, floor leather, artificial leather , Conveyor belts, etc. In addition, 2,2,4-trimethylpentanediol diester can also be used in inks, pigments and EVA emulsions. [0003] There are few public reports about the preparation method of 2,2,4-trimethylpentanediol diester. US Patent No. 4110539A discloses a synthesis...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C67/03C07C69/28C07D277/62B01J31/02
CPCB01J31/0277B01J2231/49C07C67/03C07C69/28C07D277/62
Inventor 张海飞张润赟王小伟张世元
Owner RUNTAI CHEM TAIXING CO LTD