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Method for preparing 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate by condensation of isobutyraldehyde

A technology of pentanediol monoisobutyrate and isobutyraldehyde, which is applied in the preparation of aldehyde redox, separation/purification of carboxylate, organic chemistry, etc., can solve the problem of high quality requirements of raw material isobutyraldehyde and complex reaction process , the catalyst is toxic and other problems, to achieve the effect of environmental friendliness, high yield and less impurities in the synthesis process

Active Publication Date: 2021-08-17
ZHONGRONG TECH CORP LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Chinese patent CN201010283690.8 discloses a preparation method of alcohol ester-12, the catalyst used is sodium alkoxide, thereby avoiding the shortcomings of inorganic alkali catalyst two-stage reaction process complexity, high energy consumption, etc., and also avoiding Ba(OH) 2 Disadvantages such as catalyst toxicity and high quality requirements for raw material isobutyraldehyde
[0007] As can be seen from the above, the preparation part of alcohol ester-12 adopts Ba(OH) 2 It is a catalyst, but it has the disadvantages that the catalyst itself is poisonous and has high requirements on the quality of the raw material isobutyraldehyde
Part of the prior art is prepared by a two-stage method, which has the disadvantages of complex reaction process and high energy consumption, and the problem of wastewater treatment in aqueous sodium hydroxide solution

Method used

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  • Method for preparing 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate by condensation of isobutyraldehyde
  • Method for preparing 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate by condensation of isobutyraldehyde
  • Method for preparing 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate by condensation of isobutyraldehyde

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Experimental program
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Effect test

Embodiment 1

[0031] In this embodiment, a 100mL reaction kettle was used and heated in an oil bath. Add 50g of isobutyraldehyde to the reaction kettle, then add 0.5g of 1-methyl-3-butyl-imidazolium tetrafluoroborate, seal the reaction kettle, heat to 100°C, react for 20h, cool down after the reaction is completed , the measured yield of alcohol ester-12 was 71.8%, and the total impurity content was 1.56%.

Embodiment 2

[0033] Use a 1000L reactor and use steam heating. Add 500Kg isobutyraldehyde in the reactor, add 10Kg tetrabutylammonium hydroxide again, seal the reactor, heat to 80 ℃, react for 24h, after the reaction is completed, the reaction material is cooled down, and the yield of alcohol ester-12 is measured as 75.6%, and the total impurity content is 1.28%.

[0034] The reaction materials are sent to three rectification towers in series for rectification, and alcohol ester-12 is extracted from the top of the third rectification tower. The mass spectrometry test results are shown in figure 1 As shown in Figure A, with figure 1 Figure B is completely consistent with a purity of 99.5%. The ionic liquid catalyst remaining in the tower kettle is recovered.

Embodiment 3

[0036] In this embodiment, a 100mL reaction kettle was used and heated in an oil bath. Add 50g isobutyraldehyde in reactor, and add the ionic liquid catalyst (tetrabutylammonium hydroxide) that 0.25g embodiment 2 reclaims, be heated to 200 ℃, react 20h, measure the yield of alcohol ester-12 after completion of reaction is 73.6%, and the total impurity content is 1.18%.

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Abstract

The invention relates to a method for preparing 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate by condensation of isobutyraldehyde. The method uses isobutyraldehyde as a raw material, and the raw material is mixed with a catalyst Mixing and heating together, so that the raw materials undergo two chemical reaction processes of aldol condensation and Cannizzaro reaction in one stage of reaction; wherein the catalyst is an ionic liquid. With the method of the invention, the reaction conditions are mild, the amount of impurities is small, and the yield is high; the ionic liquid can be recycled, and the synthesis process is environmentally friendly. The product can be purified by using the method of the invention to obtain a product with a purity greater than or equal to 99.5%.

Description

technical field [0001] The invention relates to the technical field of chemical product synthesis, in particular to a method for preparing 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate by condensation of isobutyraldehyde. Background technique [0002] The product 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate, referred to as dodecyl alcohol ester or alcohol ester-12, is an ideal film-forming aid for water-based systems. Emulsion polymers have the effect of good film formation and lower minimum film formation temperature. It is suitable for various emulsions, latex paints, adhesives, etc. synthesized from (meth)acrylate, styrene, and vinyl acetate. Water-based coatings can help the film-forming of various commercial emulsions and effectively reduce their minimum film-forming temperature. The production of alcohol ester-12 can not only meet the needs of the current society, make green and environmentally friendly coatings more widely used, but also reduce the import of coa...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/28C07C67/44C07C67/48
CPCC07C67/44C07C67/48C07C69/28
Inventor 吴超勇代淑梅李秋园
Owner ZHONGRONG TECH CORP LTD
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