Preparation method of triethylene glycol di-2-ethylhexoate
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A technology of isooctanoate and triethylene glycol diethylene glycol is applied in the field of plasticizers to achieve the effects of inhibiting side reactions, simple methods, and improving product quality
Inactive Publication Date: 2015-04-22
天元航材(营口)科技股份有限公司
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[0003] For above-mentioned situation, the purpose of the present invention is to provide a kind of improved Claisen condensation reaction method, adopt
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Embodiment 1
[0017] Take a 500ml four-neck flask, equipped with mechanical stirring, oil bath heating device, install a condenser, a distillation head, and a thermometer, add 75g of triethylene glycol, 225g of isooctanoic acid, and 0.5g of activated clay, heat and stir, when the temperature rises to 40 ° C ~ 80 °C, add 1.5 g of catalyst and stir for 2 hours.
[0018] Continue to raise the temperature, control the temperature at 80°C-90°C, dehydrate under negative pressure, control the vacuum degree at 10mmHg-15mmHg, and react for 6 hours to obtain the esterification mixture;
[0019] The above-prepared esterification mixture was lowered to room temperature, and 100 g of 1.0% sodium hydroxide aqueous solution was added dropwise within 1 hour, and 5.0 g of decolorizing agent (activated carbon) was added. Distill under the condition of 1mmHg to remove excess isooctanoic acid, and then filter to obtain triethylene glycol diisocaprylate.
Embodiment 2
[0021] Take a 1000ml four-neck flask, equipped with mechanical stirring, oil bath heating device, install a condenser, distillation head, thermometer, add 75g triethylene glycol, 200g isooctanoic acid, 0.5g activated carbon, heat and stir, when the temperature rises to 40 ℃ ~ 80 ℃ When, add 1.5g catalyst, stir 2 hours.
[0022] Continue to raise the temperature, control the temperature at 90°C to 105°C, dehydrate under negative pressure, control the vacuum at 10mmHg to 15mmHg, and react for 4.5 hours to obtain an esterification mixture;
[0023] The esterification mixture prepared above was lowered to room temperature, and 100 g of 1.2% sodium hydroxide aqueous solution was added dropwise within 1 hour, and 4.5 g of decolorizing agent (activated carbon) was added. Distill under the condition of 1mmHg to remove excess isooctanoic acid, and then filter to obtain triethylene glycol diisocaprylate.
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Abstract
The invention discloses a preparation method of triethylene glycol di-2-ethylhexoate and relates to a method for preparing a plasticizer from triethylene glycol and isocaprylic acid serving as initial raw materials through processes such as Claisen condensation reaction, neutralization and distillation. The preparation method comprises the steps of adding isocaprylic acid and triethylene glycol serving as the raw materials into a reactor, stirring while heating to dissolve isocaprylic acid and triethylene glycol, keeping the temperature at 40-80 DEG C, and adding an adsorbent and a catalyst; reacting under the conditions that the temperature is 80-110 DEG C and the vacuum degree is 1-15mmHg, then, cooling, and dropwise adding a sodium hydroxide water solution with the concentration of 1-2.5%; and then, adding a decolorizing agent, distilling under the conditions that the temperature is 80-150 DEG C and the vacuum degree is 0.5-1mmHg, and filtering to obtain triethylene glycol di-2-ethylhexoate. The preparation method disclosed by the invention is simple and is easily implemented. The preparation method has the characteristics that raw materials are available, and negative pressure and low-temperature reaction is adopted, so that the production cost is greatly reduced. In addition, an adsorbent is added to inhibit side reaction and adsorb colored impurities, so that the quality of triethylene glycol di-2-ethylhexoate is improved, and the heat resistance of triethylene glycol di-2-ethylhexoate is greatly improved. The prepared triethylene glycol di-2-ethylhexoate has the chroma of less than 30 which is superior to the chroma of a domestic product (more than 50) if being detected after being heated at the temperature 180 DEG C for 2 hours. Problems existing in the existing production method are solved.
Description
technical field [0001] The invention relates to a method for preparing a plasticizer by taking triethylene glycol and isooctanoic acid as initial raw materials through Claisen condensation reaction, neutralization, distillation and other processes. Background technique [0002] Triethylene glycol diisocaprylate is a special-purpose plasticizer for the manufacture of automotive glass films. It has excellent low temperature resistance, durability, oil resistance, UV resistance and antistatic properties, and has low viscosity and certain lubricity. . At present, most of the products in the domestic market are imported from abroad. At present, the production method adopted by domestic and foreign production enterprises is the traditional esterification reaction. The reaction temperature is generally around 200 ° C, which consumes a lot of energy and high production costs. Moreover, the process is relatively complicated, and the product must be obtained through processes such as...
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