Method for preparing propyl propionate by using recycled n-propanol
A technology of propyl propionate and n-propanol, which is applied in the field of preparing propyl propionate by recovering n-propanol, can solve the difficulty of separating propyl propionate, the low yield of propyl propionate, the decline in utilization rate, etc. problems, to achieve the effect of reduced dosage, high safety and increased productivity
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[0028] The invention provides a kind of preparation method of reclaiming n-propanol to prepare propyl propionate, comprising the following steps:
[0029] Under anhydrous conditions, the recovered n-propanol, anhydrous aluminum trichloride and aluminum flakes are mixed for a reflux reaction to obtain a reflux reaction product, which includes aluminum n-propoxide;
[0030] The reflux reaction product is mixed with propionaldehyde to carry out the Tischenko, V. reaction to obtain the Tischenko, V. reaction product;
[0031] The Tischenko, V. reaction product was distilled and rectified in sequence to obtain propyl propionate.
[0032] In the present invention, unless otherwise specified, the raw materials used are conventional commercially available products in this field.
[0033] In the present invention, under anhydrous conditions, the recovered n-propanol, anhydrous aluminum trichloride and aluminum flakes are mixed for reflux reaction to obtain a reflux reaction product, a...
Embodiment 1
[0049] Put 100g of n-propanol into the dry reaction bottle, replace the air with nitrogen three times, and then put in 1.33g of aluminum flakes with a specific surface area of 1.1cm 2 / g, and 0.3g of aluminum trichloride, at a heating rate of 2°C / min, the temperature was raised from 25°C to 97°C for reflux reaction for 3h, the temperature was lowered to 10°C, and the cooling rate was 2°C / min, and 600g of acrylic acid was added dropwise Aldehyde, and Tischenko, V. reaction at 10°C for 3h, atmospheric distillation at 80-99°C, reflux ratio 3:1 for 5h, recovery of n-propanol and crude propyl propionate, and crude Propyl propionate was rectified for 5 hours at 100-130°C with a reflux ratio of 5:1 to obtain 570g of propyl propionate product.
[0050] In this embodiment, based on the quality of propionaldehyde, it can be seen through calculation that the yield of propyl propionate is 95%, and the purity is 99%.
Embodiment 2
[0052] Drop into and reclaim n-propanol 107g (93% of the low-boiling fraction propanol content of propyl propionate, 7% of propyl propionate content) in the reaction bottle of drying, replace air with nitrogen three times, then drop into aluminum sheet 1.33g, The specific surface area is 1.1cm 2 / g, and 0.3g of aluminum trichloride, at a heating rate of 2°C / min, the temperature was raised from 25°C to 97°C for reflux reaction for 3h, the temperature was lowered to 10°C, and the cooling rate was 2°C / min, and 600g of acrylic acid was added dropwise Aldehyde, and Tischenko, V. reaction at 10°C for 3h, atmospheric distillation at 80-99°C, reflux ratio 3:1 for 5h, recovery of n-propanol and crude propyl propionate, and crude Propyl propionate was rectified for 5 hours at 100-130°C with a reflux ratio of 5:1 to obtain 595.5g of propyl propionate product.
[0053] In this embodiment, based on the quality of propionaldehyde, it can be known through calculation that the yield of propy...
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Abstract
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