A reaction device for the synthetic production of Diisooctyl Sebacate, the device comprises an esterification kettle, an esterification tower, an esterification condenser, a separator, a rectification kettle, a rectification tower, a rectification condenser, an alcohol receiving tank, an ester receiving tank, Vacuum system and pump conveying system, the outer surfaces of the esterification kettle and the rectification kettle are equipped with a heat conduction oil heating system for heating the materials in the esterification kettle or rectification kettle, and the heat conduction oil heating system is set In the rest of the esterification tank and rectification tank except the top, and avoid the outlet at the bottom of the esterification tank and rectification tank;
The esterification tower is arranged on the top of the esterification kettle, the outlet end of the esterification tower is connected with the inlet end of the esterification condenser, the outlet end of the esterification condenser is connected with the inlet end of the separator, and on the side of the separator The wall is also provided with an alcohol recovery pipeline in circulation with the esterification tank, the discharge port of the esterification tank is connected to the feed port of the rectification tank through the material pump in the pump delivery system, and the rectification tower is set At the top of the rectification tank, the outlet end of the rectification tower is connected with the inlet end of the rectification condenser, and the outlet end of the rectification condenser is connected with the alcohol receiving tank and the ester receiving tank.
The heat transfer oil heating system is provided with a heat transfer oil inlet and a heat transfer oil outlet, and the heat transfer oil inlet and the heat transfer oil outlet are respectively installed on the top of one side of the outer surface of the heat transfer oil heating system and the bottom of the other side. The heat transfer oil heating system is also provided with a thermometer socket for installing a thermometer to measure the temperature in the esterification tank or rectification tank. An acid feed port, an alcohol feed port, a catalyst inlet and a vent port are arranged on the top of the esterification kettle.
A synthetic process for Diisooctyl Sebacate, comprising the following steps:
Step 1. According to the ratio of isooctyl alcohol to sebacic acid molar ratio of 2:1, take sebacic acid for later use, and take excess isooctyl alcohol and add it to the esterification kettle, after that, start the stirring in the esterification kettle System and heat conduction oil heating system, adjust the temperature of the heat conduction oil in the heat conduction oil heating system of the esterification kettle to 70-80°C, when the temperature in the esterification kettle rises to 60°C, start the vacuum system to vacuum the esterification kettle treatment to keep the vacuum degree in the esterification kettle at -0.04～-0.06Mpa;
Step 2. Add the weighed sebacic acid and the catalyst tetrabutyl titanate with a mass of 0.5% to 1% of the added sebacic acid into the esterification kettle of step 1. After that, close the vacuum system, and the esterification kettle The material starts to react. When the temperature in the esterification tank rises to 90-100°C, adjust the temperature of the heat-conducting oil in the heat-conducting oil heating system of the esterification tank to 200°C. When the temperature in the esterification tank rises to 165-175°C , open the esterification condenser to condense the materials entering it, when the esterification condenser refluxes, control the temperature of the heat transfer oil in the heat conduction oil heating system of the esterification kettle to rise to 230°C at a heating rate of 10-20°C/h , when the temperature in the esterification tank rises to 220°C, control the material in the esterification tank to perform heat preservation and pressure reaction at this temperature for 25-35 minutes, and then turn off the heat transfer oil heating system of the esterification tank to complete the esterification reaction;
Step 3. The material that has completed the esterification reaction in step 2 is transported to the rectification kettle through the material pump in the pump delivery system. After that, the vacuum pumping system is used to vacuumize the rectification kettle to keep the vacuum degree in the rectification kettle At -0.0985～-0.099Mpa, and adjust the temperature of the heat transfer oil in the heat transfer oil heating system of the rectification kettle to 200°C, open the rectification condenser to condense the materials entering it;
Step 4. When the temperature at the top of the rectification tower rises to 140-160°C, open the valve of the alcohol receiving tank, so that the alcohol receiving tank can collect the isooctyl alcohol distilled out at a temperature of 140-160°C at the top of the rectification tower. When there is no more liquid flowing into the alcohol receiving tank, adjust the temperature of the heat-conducting oil in the heat-conducting oil heating system of the rectifying kettle to 290°C, so that the alcohol receiving tank can continue to collect the distillate from the rectifying tower. When the temperature at the top of the tower rises to 240-250°C, close the valve of the alcohol receiving tank and open the valve of the ester receiving tank, so that the ester receiving tank can collect the distillate distilled when the top temperature of the rectification tower exceeds 240-250°C , the material collected in the ester receiving tank is the finished product Diisooctyl Sebacate.
In Step 3, the material that has completed the esterification reaction in Step 2 needs to be transported by the material pump when the temperature of the esterification tank drops below 180°C.
Fig. 1 is a schematic diagram of the structure; reference numerals: 1, esterification tank, 101, acid feed port, 102, alcohol feed port, 103, catalyst inlet, 104, vent port, 2, esterification tower, 3, esterification Condenser, 4. Separator, 5. Rectification kettle, 6. Rectification tower, 7. Rectification condenser, 8. Alcohol receiving tank, 9. Ester receiving tank, 10. Heat transfer oil heating system, 1001, Heat transfer oil Import, 1002, heat transfer oil outlet, 1003, thermometer socket, 11, material pump.
