Hydroxyalkanoate zinc polyester catalyst, its preparation method and the application of the catalyst
A technology of polyester catalyst and zinc hydroxyalkanoate, applied in carboxylate preparation, organic chemistry, etc., can solve the problems of unstable product performance, poor compatibility, high catalytic activity, etc., and achieve low cost and good dispersibility , the effect of moderate catalytic efficiency
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Embodiment 1
[0023] 200 g of 1% glycolic acid aqueous solution was prepared. Under a nitrogen atmosphere, the glycolic acid aqueous solution was reacted with 1.31 g of zinc hydroxide at 15° C. for 30 hours. After the reaction was completed, the temperature was lowered to 0° C., and the crystalline product was filtered and separated, washed with deionized water, and finally in After drying at 40° C. and 0.01 kPa for 6 hours, the target product zinc glycolate catalyst was obtained with a yield of 56%.
[0024] In a 3L stainless steel reaction kettle, add 1kg methyl glycolate and 23.88g of the zinc glycolate catalyst prepared above, repeatedly feed and emit nitrogen to replace the air in the kettle, then start heating and stirring, and the temperature is set at 190°C, react for 2 hours, until no methanol is discharged, then increase the reaction temperature to 230°C, reduce the pressure in the reactor to 30Pa, continue to react for 1.5 hours, and discharge after the reaction is completed. Th...
Embodiment 2
[0026] Prepare 200g of 80% 4-hydroxybutyric acid aqueous solution. Under a nitrogen atmosphere, the 4-hydroxybutyric acid aqueous solution was reacted with 4.17 g of zinc oxide at 95°C for 0.1 hour. After the reaction was completed, the temperature was lowered to 15°C, and the crystalline product was filtered and separated, and then washed with deionized water , and finally dried at 80° C. and 80 kPa for 0.1 hour to obtain the target product zinc 4-hydroxybutyrate catalyst with a yield of 73%.
[0027] In a 3L stainless steel reaction kettle, add 1kg of hydroxybutyric acid and 2.60g of the zinc 4-hydroxybutyrate catalyst prepared above, repeatedly feed and release nitrogen to replace the air in the kettle, then start heating and stirring, and set the temperature Set at 160°C, react for 2.5 hours, until no water is discharged, then increase the reaction temperature to 190°C, reduce the pressure in the reactor to 20Pa, continue to react for 2 hours, and discharge after the react...
Embodiment 3
[0029] Prepare 200g of 50% 3-hydroxypropionic acid aqueous solution by mass percentage. Under a nitrogen atmosphere, the 3-hydroxypropionic acid aqueous solution was reacted with 11.04 g of zinc hydroxide at 80°C for 9 hours. After the reaction was completed, the temperature was lowered to 5°C, and the crystalline product was filtered and separated, and then washed with deionized water , and finally dried at 60° C. and 1 kPa for 4 hours, the target product 3-hydroxypropionate zinc catalyst was obtained, and the yield was 87%.
[0030] In a 3L stainless steel reaction kettle, add 1kg lactide and 0.017g of the 3-hydroxypropionate zinc catalyst prepared above, repeatedly feed and release nitrogen to replace the air in the kettle, then start heating and stirring, and set the temperature Set at 190°C, when the reaction temperature is reached, start timing, and react at normal pressure for 30 minutes. After the normal pressure reaction is completed, turn on the vacuum pump, reduce t...
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