Natural benzaldehyde preparation method
A benzaldehyde, natural technology, applied in the field of preparation of natural benzaldehyde, can solve the problem of low ozone utilization rate, and achieve the effect of high ozone utilization rate, good selectivity and simple process
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Embodiment 1
[0027] 1. Prepare 0.1 mol / L hydrochloric acid solution, weigh 5 g of columnar activated carbon, grind it into powder, soak activated carbon in the above hydrochloric acid solution for 24 h, wash, 110 o C dry at 250 o C activation yields acid-activated activated carbon.
[0028] 2. In the bubbling reactor, respectively add 4 g cinnamaldehyde (cinnamaldehyde content above 95%), 12.00 g absolute ethanol, 0.02 g activated carbon catalyst activated by 0.1 mol / L hydrochloric acid, press 0.1 g (ozone) / g (cinnamaldehyde) / h flow rate, the ozone is passed into the bubble reactor, and the ozonation reaction is carried out at 0 °C for 2 h to obtain the ozonide intermediate.
[0029] 3. Dissolve 3.00 g of thiourea and 0.4 g of oxalic acid in 50 mL of deionized water, slowly drop the ozonated intermediate into the thiourea aqueous solution, perform a reduction reaction at below 10 °C for 3 h, centrifuge, and take out the organic phase.
[0030] 4. Molecularly distill the organic phase at...
Embodiment 2
[0032] 1. Prepare 0.2 mol / L hydrochloric acid solution, weigh 5 g of columnar activated carbon, grind it into powder, soak the activated carbon in the above hydrochloric acid solution for 24 h, wash, 110 o C dry at 250 o C activation yields acid-activated activated carbon.
[0033] 2. In the bubbling reactor, add 4 g cinnamaldehyde (the content of cinnamaldehyde is more than 95%), 12.00 g absolute ethanol, 0.04 g activated carbon catalyst activated by 0.2 mol / L hydrochloric acid, press 0.1 g (ozone) / The flow rate of g (cinnamaldehyde) / h is to pass ozone into the bubbling reactor, and perform an ozonation reaction at 0 °C for 0.5 h to obtain an ozonide intermediate.
[0034] 3. Dissolve 3.00 g of thiourea and 0.4 g of oxalic acid in 50 mL of deionized water, slowly drop the ozonated intermediate into the thiourea aqueous solution, perform a reduction reaction at below 10 °C for 3 h, centrifuge, and take out the organic phase.
[0035] 4. Molecularly distill the organic phase...
Embodiment 3
[0037] 1. Prepare 0.3 mol / L hydrochloric acid solution, weigh 5 g of columnar activated carbon, grind it into powder, soak the activated carbon in the above hydrochloric acid solution for 24 h, wash, 110 o C dry at 250 o C activation yields acid-activated activated carbon.
[0038]2. In the bubbling reactor, add 4 g of cinnamaldehyde (the content of cinnamaldehyde is more than 95%), 12.00 g of absolute ethanol, and 0.16 g of activated carbon catalyst activated by 0.3 mol / L hydrochloric acid, and press 0.2 g (ozone) / The flow rate of g (cinnamaldehyde) / h is to pass ozone into the bubbling reactor, and perform an ozonation reaction at 30 °C for 1 h to obtain an ozonide intermediate.
[0039] 3. Dissolve 3.00 g of thiourea and 0.4 g of oxalic acid in 50 mL of deionized water, slowly drop the ozonated intermediate into the thiourea aqueous solution, perform a reduction reaction at below 10 °C for 3 h, centrifuge, and take out the organic phase.
[0040] 4. Molecularly distill th...
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