Method for preparing 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate through condensation of isobutylaldehyde

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

Active Publication Date: 2019-02-05
ZHONGRONG TECH CORP LTD
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  • 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

Method used

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  • Method for preparing 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate through condensation of isobutylaldehyde
  • Method for preparing 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate through condensation of isobutylaldehyde
  • Method for preparing 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate through condensation of isobutylaldehyde

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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 through condensation of isobutylaldehyde. The method takes the isobutylaldehyde as a raw material; the raw material and a catalyst are mixed and commonly heated so that the raw material is subjected to two chemical reaction processes including aldol condensation reaction and cannizzaro reaction in one section of reaction, wherein the catalyst is ionic liquid. The method provided by the invention has the advantages of moderate reaction conditions, less impurity content and high yield; the ionic liquid can be recycled and a synthesis technology is environmentally friendly. By adopting the method provided by the invention, a product can be purified and the product with the purity greater than or equal to 99.5 percent is obtained.

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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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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