Method for synthesizing n-butyl alcohol

Abstract

The invention relates to a method for synthesizing n-butyl alcohol, and particularly relates to the method for preparing n-butyl alcohol through catalyst solid-liquid reaction without a catalyst. The method comprises steps of putting calcium ethoxide and ethyl alcohol into an airtight reactor, raising temperature to 130-500 DEG C in inert gas atmosphere, heating and reacting, then cooling to room temperature, collecting a solid-liquid mixture in the reactor, separating then collecting liquid, thereby obtaining n-butyl alcohol. The method does not use precious metals or rear metal catalysts, is low in cost and is simple; under the condition that the catalyst is not used, the yield of n-butyl alcohol in the product reaches 43%, so that the method has industrial application prospect.

Description

Technical field

[0001] The invention relates to a method for synthesizing n-butanol, in particular to a method for preparing n-butanol by solid-liquid reaction without a catalyst. Background technique

[0002] As an important chemical raw material, the demand for n-butanol in my country reached 720,000 tons in 2008. At present, the main industrial methods for synthesizing n-butanol include propylene carbonyl synthesis and acetaldehyde aldol condensation. Propylene carbonyl synthesis method uses propylene and synthesis gas (CO+H 2 ) Is the raw material, the two first react to produce n-butyraldehyde and isobutyraldehyde, and then hydrogenate to produce n-butanol. The reaction uses noble metals (cobalt, rhodium complex, nickel, etc.) as a catalyst, the temperature is 130-160°C, the pressure is about 7.0MPa, and the selectivity is about 68%. Aldol condensation of acetaldehyde is obtained by condensation and dehydration of two molecules of acetaldehyde to produce crotonaldehyde. Th...

Examples

Embodiment 1

[0018] Weigh 2g of calcium ethoxide solid powder and place it in a quartz sleeve, add anhydrous ethanol with a molar ratio of 1:15 to calcium ethoxide, place the sleeve in a 50ml high-temperature and high-pressure reaction vessel and seal, and purge the vessel with argon gas In the air, heat at 3°C / min to 390°C under normal pressure, react for 9 hours, cool the reactor to room temperature at 18°C / min, take out the solid-liquid mixture in the sleeve and transfer it to the centrifuge tube, centrifuge at 7900r / min The product was collected after 5 minutes, and the yield of n-butanol was measured to be 41%.

Embodiment 2

[0020] Weigh 2g of the prepared calcium ethoxide solid powder into a quartz sleeve, add anhydrous ethanol with a molar ratio of 1:25 to the calcium ethoxide, place the sleeve in a 50ml high-temperature and high-pressure reactor, seal it, and purge it out with argon gas The air in the kettle was heated to 390°C under normal pressure and reacted for 1 hour. After the kettle was cooled to room temperature, the solid-liquid mixture in the sleeve was taken out and transferred to a centrifuge tube. After centrifugation at 7900r / min for 5 minutes, the product was collected. The yield of alcohol is 35%.

Embodiment 3

[0022] Weigh 2g of the prepared calcium ethoxide solid powder into a quartz sleeve, add anhydrous ethanol with a molar ratio of 1:15 to the calcium ethoxide, place the sleeve in a 50ml high-temperature and high-pressure reactor, seal it, and purge it out with argon gas The air in the kettle was heated to 390°C under normal pressure and reacted for 6 hours. After the kettle was cooled to room temperature, the solid-liquid mixture in the sleeve was taken out and transferred to a centrifuge tube. After centrifugation at 7900r / min for 5 minutes, the product was collected. The yield of alcohol was 43%.

Technical field

[0001] The invention relates to a method for synthesizing n-butanol, in particular to a method for preparing n-butanol by solid-liquid reaction without a catalyst. Background technique

[0002] As an important chemical raw material, the demand for n-butanol in my country reached 720,000 tons in 2008. At present, the main industrial methods for synthesizing n-butanol include propylene carbonyl synthesis and acetaldehyde aldol condensation. Propylene carbonyl synthesis method uses propylene and synthesis gas (CO+H 2 ) Is the raw material, the two first react to produce n-butyraldehyde and isobutyraldehyde, and then hydrogenate to produce n-butanol. The reaction uses noble metals (cobalt, rhodium complex, nickel, etc.) as a catalyst, the temperature is 130-160°C, the pressure is about 7.0MPa, and the selectivity is about 68%. Aldol condensation of acetaldehyde is obtained by condensation and dehydration of two molecules of acetaldehyde to produce crotonaldehyde. Th...

Examples

Embodiment 1

[0018] Weigh 2g of calcium ethoxide solid powder and place it in a quartz sleeve, add anhydrous ethanol with a molar ratio of 1:15 to calcium ethoxide, place the sleeve in a 50ml high-temperature and high-pressure reaction vessel and seal, and purge the vessel with argon gas In the air, heat at 3°C / min to 390°C under normal pressure, react for 9 hours, cool the reactor to room temperature at 18°C / min, take out the solid-liquid mixture in the sleeve and transfer it to the centrifuge tube, centrifuge at 7900r / min The product was collected after 5 minutes, and the yield of n-butanol was measured to be 41%.

Embodiment 2

[0020] Weigh 2g of the prepared calcium ethoxide solid powder into a quartz sleeve, add anhydrous ethanol with a molar ratio of 1:25 to the calcium ethoxide, place the sleeve in a 50ml high-temperature and high-pressure reactor, seal it, and purge it out with argon gas The air in the kettle was heated to 390°C under normal pressure and reacted for 1 hour. After the kettle was cooled to room temperature, the solid-liquid mixture in the sleeve was taken out and transferred to a centrifuge tube. After centrifugation at 7900r / min for 5 minutes, the product was collected. The yield of alcohol is 35%.

Embodiment 3

[0022] Weigh 2g of the prepared calcium ethoxide solid powder into a quartz sleeve, add anhydrous ethanol with a molar ratio of 1:15 to the calcium ethoxide, place the sleeve in a 50ml high-temperature and high-pressure reactor, seal it, and purge it out with argon gas The air in the kettle was heated to 390°C under normal pressure and reacted for 6 hours. After the kettle was cooled to room temperature, the solid-liquid mixture in the sleeve was taken out and transferred to a centrifuge tube. After centrifugation at 7900r / min for 5 minutes, the product was collected. The yield of alcohol was 43%.