Method for refining crude glycerol
A crude glycerin and glycerol technology, applied in chemical instruments and methods, preparation of hydroxyl compounds, preparation of organic compounds, etc., can solve the problems of high manufacturing cost, complicated process and high production cost, and achieve reduced production cost, high reactivity, The effect of not easy to carbonize
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Embodiment example 1
[0048] Add 250g of crude glycerin and 25g of A15 resin catalyst into a 1000mL round bottom flask, heat to 75°C, slowly feed 410g of isobutylene gas, and continue the reaction at 75°C for 8 hours. After the temperature drops to room temperature, unreacted isobutene is recovered, the catalyst is filtered off, and glycerin tert-butyl ether is obtained by distillation under reduced pressure.
[0049] Glycerin tert-butyl ether was transferred to the cracking reaction kettle, and 25g of cracking catalyst A15 resin catalyst was added, and the reaction temperature was 110°C, and the reaction was carried out for 2 hours, and then lowered to room temperature, and the isobutylene obtained by cracking was recovered, and the catalyst was filtered off. Dilute with methanol, obtain the effluent through the filter membrane, add acid clay with 2% glycerin mass to the effluent, stir at 90°C for 2 hours, then filter the acid clay, distill the filtrate under normal pressure and distill the methano...
Embodiment example 2
[0052] Add 500g of crude glycerin, 383g of methyl tert-butyl ether and 25g of A35 resin catalyst into a 1000mL round-bottomed flask for ether formation reaction, heat to 80°C, and continue the reaction at 80°C for 8 hours. After the temperature drops to room temperature, the unreacted isobutene cracked is recovered, the catalyst is filtered off, and glycerol tert-butyl ether is obtained by distillation under reduced pressure.
[0053] Glycerol tert-butyl ether is transferred to the cracking reactor, and 25g cracking catalyst SO is added 3 H-MCM-41, the reaction temperature is 90°C, react for 4 hours, cool down to room temperature, recover the isobutene obtained by cracking, filter off the catalyst, dilute the obtained glycerin with 0.5 times the mass of methanol, obtain the effluent through the filter membrane, and pour it into the effluent Add acid clay with 3% glycerin mass to the liquid, stir at 80°C for 2 hours, then filter the acid clay, and distill the filtrate to obtain...
Embodiment example 3
[0056] In a 1000mL round bottom flask, add 500g of crude glycerin, 643g of tert-butanol and 35g of SO 4 2- / SiO 2 The resin catalyst undergoes ether-forming reaction, is heated to 70°C, and continues to react at 70°C for 20 hours. After the temperature drops to room temperature, the unreacted isobutene cracked is recovered, the catalyst is filtered off, and glycerol tert-butyl ether is obtained by distillation under reduced pressure.
[0057] Glycerol tert-butyl ether is transferred to the cracking reactor, and 25g cracking catalyst SO is added 4 2- / ZrO 2 -MnO 3 , the reaction temperature is 90°C, react for 4 hours, lower to room temperature, recover the isobutene obtained by cracking, filter off the catalyst, dilute the obtained glycerin with 0.2 times the mass of methanol, obtain the effluent through the filter membrane, and add the mass of glycerin to the effluent 3% acid clay, stirred at 80°C for 2 hours, then filtered the acid clay, distilled the filtrate under nor...
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