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Preparation method of 2, 2, 4-trimethyl-1, 3-pentanediol monoisobutyrate

A technology of pentanediol monoisobutyrate and trimethyl, applied in the field of preparation of 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate, can solve the problem of no industrial scale-up , isobutyraldehyde instant heat release and other problems, to achieve the best catalytic effect, the best water absorption effect

Active Publication Date: 2021-03-02
广州联普新材料科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The preparation method of alcohol ester 12, the domestic application patent is more, for example CN 1260204C discloses a kind of step-by-step heating, two-stage reaction synthesis method, isobutyl Aldehydes undergo condensation reaction at low temperature, the reaction temperature is 10-60°C, and then directly heated up, the second stage reaction temperature is 60-150°C, this method uses solid or liquid alkali as the catalyst, but it is only the result of a small laboratory test , without industrial amplification
In the prior art, the preparation method of alcohol ester twelve is scaled up from small laboratory test to industrial production, and there is a problem of instantaneous and violent exotherm during the condensation reaction of isobutyraldehyde

Method used

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  • Preparation method of 2, 2, 4-trimethyl-1, 3-pentanediol monoisobutyrate

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preparation example Construction

[0027] The invention provides a preparation method of 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate, comprising:

[0028] (1) Alkali metal hydroxide, alkaline earth metal oxide and alcohol ester twelve are added to reaction vessel, stir evenly;

[0029] (2) adding isobutyraldehyde and controlling the feed rate of isobutyraldehyde, controlling the temperature to be 20-70° C., carrying out the first-stage isobutyraldehyde condensation reaction to obtain an intermediate product;

[0030] (3) After the addition of isobutyraldehyde is completed, the control temperature is 40~70° C., and it is incubated for 1~5 hours to carry out the Cannizzaro reaction of the second stage to obtain the alcohol ester twelve crude product;

[0031] (4) Purifying the crude product of the alcohol ester twelve to obtain the finished product of the alcohol ester twelve.

[0032] The preparation method of 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate provided by the present invention mainly involves ...

Embodiment 1

[0048] Pump 2000kg of alcohol ester twelve finished products into 20m through the delivery pump 3 In the first reactor, 75kg of barium oxide and 75kg of potassium hydroxide are added at one time through the star feeder on the first reactor. Stirring was started, and the inner and outer coils of the first reaction kettle were fed with -5°C ethylene glycol-water solution to cool the materials.

[0049] Cool the material in the first reaction kettle to about 20°C, pump isobutyraldehyde into the first reaction kettle at a speed of 1 to 5 tons / hour through the isobutyraldehyde delivery pump, and control the isobutyraldehyde pump The input speed and the ethylene glycol-water solution inside and outside the first reaction kettle are coiled, and the temperature of the reaction materials is controlled at 20-70°C. The amount of adding isobutyraldehyde is 15 tons.

[0050] After the addition of isobutyraldehyde is completed, the first stage of isobutyraldehyde condensation reaction is ...

Embodiment 2

[0063] 3000kg alcohol ester twelve finished products are pumped into the 20m 3 In the first reaction kettle, 250kg of barium oxide and 400kg of sodium hydroxide were added at one time through the star feeder on the first reaction kettle. Stirring was started, and the inner and outer coils of the reaction kettle were fed with ethylene glycol-water solution at -5°C to cool the materials.

[0064] Cool the material in the first reaction kettle to about 20°C, pump isobutyraldehyde into the first reaction kettle at a speed of 1 to 5 tons / hour through the isobutyraldehyde delivery pump, and control the isobutyraldehyde pump The input speed and the ethylene glycol-water solution inside and outside the first reaction kettle are coiled, and the temperature of the reaction materials is controlled at 20-70°C. The amount of isobutyraldehyde added is 13 tons.

[0065] After the addition of isobutyraldehyde is completed, the first stage of isobutyraldehyde condensation reaction is complet...

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Abstract

The invention relates to a preparation method of 2, 2, 4-trimethyl-1, 3-pentanediol monoisobutyrate, which comprises the following steps: (1) adding alkali metal hydroxide, alkaline earth metal oxideand alcohol ester-12 product into a reaction container, and uniformly stirring the materials; (2) adding isobutyraldehyde, controlling the feeding speed of isobutyraldehyde, controlling the temperature to be 20-70 DEG C, and carrying out a first-stage isobutyraldehyde condensation reaction to obtain an intermediate product; (3) after the isobutyraldehyde is completely added, controlling the temperature to be 40-70 DEG C, keeping the temperature for 1-5 hours, and carrying out a second-stage Canichalro reaction to obtain an alcohol ester-12 crude product; and (4) purifying the alcohol ester-12crude product to obtain an alcohol ester-12 finished product. According to the invention, alkali metal hydroxide is used as a catalyst, alkaline earth metal oxide is added to remove moisture in the material, and alcohol ester-12 is added and the feeding speed of isobutyraldehyde is controlled in the reaction process, so that the temperature of the condensation reaction of isobutyraldehyde is controlled, and the preparation method of alcohol ester-12 is enlarged to industrial production from laboratory lab test.

Description

technical field [0001] The invention belongs to the field of synthetic chemistry, and in particular relates to a preparation method of 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate. Background technique [0002] 2,2,4-Trimethyl-1,3-pentanediol monoisobutyrate, referred to as alcohol ester twelve, is a colorless, transparent, non-toxic, high boiling point, low freezing point, low volatility alcohol ester solvent. Alcohol ester twelve is a film-forming aid widely used in high-end architectural water-based coatings around the world. It is mainly used to help latex paint form a film, which can significantly improve the coalescence of latex paint at low temperatures, and is beneficial to the stability of paint viscosity. and pigment dispersion. Alcohol ester twelve is an excellent film-forming aid for latex paint. It can reduce the minimum film-forming temperature of latex paint. The minimum film-forming temperature decreases gradually with the increase of the amount added. ...

Claims

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Application Information

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IPC IPC(8): C07C45/72C07C49/17C07C67/08C07C69/28C07C51/00C07C51/16C07C53/124B01J23/04B01J23/06
CPCC07C45/72C07C67/08C07C51/00C07C51/16B01J23/04B01J23/06C07C49/17C07C69/28C07C53/124
Inventor 冯春凤
Owner 广州联普新材料科技有限公司
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