Method for preparing n-butanol from ethanol by using hydrothermal technique

A technology of n-butanol and ethanol, which is applied in the field of synthesizing n-butanol by hydrothermal technology, can solve the problems of high reaction temperature, high cost, and difficult operation, and achieve the effects of mild reaction conditions, low equipment requirements, and low cost

Inactive Publication Date: 2013-07-10
JILIN UNIV
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  • Summary
  • Abstract
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Problems solved by technology

The catalyst used in this method is not simply to mix magnesia and alumina, but to adopt a co-precipitation method and calcined to obtain magnesium-aluminum oxide. The preparation process is tedious and complicated, and as the reaction proceeds, the catalyst will gradually lose Live, and can not be recycled; at the same time, using this method to synthesize n-butanol, there are problems such as high reaction temperature, low selectivity of n-butanol (only up to 40%), complicated equipment, difficult operation and high cost

Method used

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  • Method for preparing n-butanol from ethanol by using hydrothermal technique
  • Method for preparing n-butanol from ethanol by using hydrothermal technique

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Put 0.295g (0.005mol) of metal cobalt powder, 0.84g (0.01mol) of sodium bicarbonate, 8.76mL (0.15mol) of absolute ethanol and 1.242mL (0.069mol) of distilled water into a 30mL autoclave to make The filling degree reaches 33%, react at 240°C for 3 days, and filter after the reactor is cooled.

[0019] The obtained solution was detected by gas chromatography-mass spectrometry (TRACE DSQ GC-MS) (the column model was TR-wax-ms, the temperature of the injection port was 200°C, the temperature of the ion source was 250°C, the temperature of the transfer line was 250°C, and the sample injection The volume is 0.4μL, the split ratio is 10, the initial temperature of the programmed temperature rise is 80°C, and it is kept for 1 minute. The heating rate is 15°C / min, and the temperature is raised to 200°C, and it is kept for 6 minutes. mL / min). Compared with the retention time of the butanol standard sample chromatogram and the molecular ion peak and each fragment peak of the mass...

Embodiment 2

[0021] Add 0.295g (0.005mol) of metal cobalt powder, 0.84g (0.01mol) of sodium bicarbonate, 8.76mL (0.15mol) of absolute ethanol and 11.24mL (0.624mol) of distilled water into a 30mL autoclave to fill the The temperature reached 67%, reacted at 200°C for 30 days, and filtered after the reactor was cooled.

[0022] Gained solution is detected by gas chromatography-mass spectrometry (GC-MS), and according to the concentration-peak area standard curve and the product peak area, the concentration of n-butanol in the product of Example 2 can be calculated to be 0.36mol / L, selectivity 72%.

Embodiment 3

[0024] Add 0.42g (0.005mol) of sodium bicarbonate, 23.35mL of absolute ethanol (0.40mol) and 5.15mL (0.286mol) of distilled water into a 30mL autoclave, so that the filling degree reaches 95%, and react at 140°C for 30 Days, after the reaction kettle was cooled, it was filtered and the product was a colorless transparent liquid.

[0025] The resulting solution was detected by gas chromatography-mass spectrometry (GC-MS). No cobalt powder was added in Example 3, and n-butanol could be reacted to synthesize n-butanol, but the yield of n-butanol was low and the selectivity was low.

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Abstract

The invention provides a method for preparing n-butanol from ethanol, and belongs to the technical field of hydrothermal chemistry. Ethanol and water are subjected to a hydrothermal reaction catalyzed by sodium bicarbonate and a metal cobalt powder in common. n-Butanol is prepared by reacting at 140-300 DEG C for 1-30 days. The present invention provides a novel mild reaction route for n-butanol synthesis from ethanol, simple catalysts are used, and n-butanol can be synthesized under mild conditions. The catalyst includes the metal cobalt powder and sodium bicarbonate, raw materials are readily available, and the cost is low. The catalyst is prepared by simply mixing without special treatment. The cobalt powder does not change after the reaction and can be reused. The method of the present invention is low in reaction temperature, has low requirement on equipments, only needs a sealed reactor, is easy to operate, and has selectivity for butanol up to 87%.

Description

technical field [0001] The invention belongs to the technical field of hydrothermal chemistry, and in particular relates to a method for synthesizing n-butanol through hydrothermal technology under the co-catalysis of sodium bicarbonate and metallic cobalt powder. Background technique [0002] The use of renewable resources to produce chemicals and fuels has received much attention over the past few decades due to a number of reasons including global warming, fluctuations in oil supply, increasing crude oil prices and existing regulations restricting the use of non-renewable resources. With the continuous development of bioethanol technology, ethanol, as a renewable resource, has become an important industrial raw material, and the catalysis of ethanol to synthesize more valuable products (such as n-butanol or 1,3-butadiene) has attracted much attention. focus on. [0003] Butanol is an important chemical raw material, mainly used in dimethyl phthalate, butyl aliphatic diba...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C31/12C07C29/34
Inventor 田戈张显龙冯守华刘紫微徐兴良
Owner JILIN UNIV
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