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Method for synthesizing triethylene glycol di-2-ethylhexoate

A technology of isooctanoate and triethylene glycol diethylene glycol, which is applied in the field of synthesizing triethylene glycol diisocaprylate, can solve the problems of restricting production scale and low technical yield, and achieve the improvement of overall acidity, increase of reaction yield, The effect of strong chemical electrophilicity

Active Publication Date: 2016-03-30
SHENYANG ZHANGMING CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The yield of triethylene glycol diisocaprylate preparation technology in the prior art is low, which restricts the production scale, and it is necessary to find a new catalytic synthesis route with higher catalytic effect for improvement

Method used

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  • Method for synthesizing triethylene glycol di-2-ethylhexoate

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Experimental program
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Effect test

Embodiment 1

[0020] (1) Pretreatment of catalyst:

[0021] Add 100Kg of stannous oxide, 0.2Kg of zinc bis(trifluoromethylsulfonyl)imide, and 0.2Kg of boron trifluoride ether solution into a 500L high-speed mixer and mix evenly to prepare the catalyst.

[0022] (2) Synthesis reaction:

[0023] Add 100Kg triethylene glycol and 336Kg isooctanoic acid into a 1000L reactor, add 8.72Kg of the catalyst prepared in the above steps into the reactor, react at a temperature of 220°C, and react for 5 hours. After the reaction, the crude product triethylene glycol diisocaprylate is obtained. , the crude triethylene glycol diisocaprylate is washed again, purified by distillation, and excess isooctanoic acid is removed to obtain the final product triethylene glycol diisocaprylate. Numbered M-1.

Embodiment 2

[0025] (1) Pretreatment of catalyst:

[0026] Add 100Kg of stannous oxide, 0.1Kg of zinc bis(trifluoromethylsulfonyl)imide, and 0.1Kg of boron trifluoride ether solution into a 500L high-speed mixer and mix evenly to prepare the catalyst.

[0027] (2) Synthesis reaction:

[0028] Add 100Kg triethylene glycol and 240Kg isooctanoic acid into a 1000L reactor, add 3.4Kg of the catalyst prepared in the above steps into the reactor, react at a temperature of 180°C, and react for 10 hours. After the reaction, the crude product triethylene glycol diisocaprylate is obtained. , the crude triethylene glycol diisocaprylate is washed again, purified by distillation, and excess isooctanoic acid is removed to obtain the final product triethylene glycol diisocaprylate. Numbered M-2.

Embodiment 3

[0030] (1) Pretreatment of catalyst:

[0031] Add 100Kg of stannous oxide, 0.5Kg of zinc bis(trifluoromethylsulfonyl)imide, and 0.5Kg of boron trifluoride ether solution into an 800L high-speed mixer and mix evenly to prepare the catalyst.

[0032] (2) Synthesis reaction:

[0033] Add 100Kg triethylene glycol and 480Kg isooctanoic acid into a 1000L reactor, add 29Kg of the catalyst prepared in the above steps into the reactor, and react at a temperature of 250°C for 3 hours. After the reaction, the crude product triethylene glycol diisocaprylate is obtained. The crude triethylene glycol diisocaprylate is washed again, purified by distillation, and excess isooctanoic acid is removed to obtain the final product triethylene glycol diisocaprylate. Numbered M-3.

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Abstract

The present invention discloses a method for synthesizing triethylene glycol di-2-ethylhexoate. The method comprises the following steps of: adding triethylene glycol and isocaprylic acid into a reactor; adding a catalyst into the reactor, wherein in the molar ratio of the triethylene glycol to the isocaprylic acid of 1:(2.5-5), the addition amount of the catalyst accounts for 1-5% of the total mass of the triethylene glycol and the isocaprylic acid; performing a reaction for 3-10 hours at the reaction temperature of 180-250 DEG C; obtaining a crude product of triethylene glycol di-2-ethylhexoate after the reaction; performing washing and distillation purification on the crude product of triethylene glycol di-2-ethylhexoate to remove the redundant isocaprylic acid; and obtaining the final product of triethylene glycol di-2-ethylhexoate.

Description

technical field [0001] The invention relates to a method for synthesizing esters, in particular to a method for synthesizing triethylene glycol diisocaprylate. Background technique [0002] Triethylene glycol diisocaprylate is a solvent-based cold-resistant and environmentally friendly plasticizer, which has excellent low-temperature performance, durability, oil resistance, ultraviolet radiation resistance and antistatic properties, and has low viscosity and certain lubricity. This product is a special effect plasticizer for polyvinyl butyral (PVB safety glass) and synthetic rubber, which can make it produce low temperature performance and low volatility. It can also be used in polyester cloth, adhesives and sealing materials, and is a plasticizer for PVC, PS, ethyl cellulose, nitrocellulose, etc. When used in polyvinyl butyral cloth-based coatings containing castor oil, it can improve the flexibility in severe cold conditions. It is also used in the formulation of butadie...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08C07C69/33
CPCC07C67/08C07C69/33
Inventor 张明何延胜王娟
Owner SHENYANG ZHANGMING CHEM
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