Method for directly preparing gamma-valerolactone from acetylpropionic acid and aminic acid
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A technology of levulinic acid and valerolactone, applied in directions such as organic chemistry, to achieve the effects of simple and convenient operation process, improved environmental friendliness, and avoided energy consumption
Active Publication Date: 2009-03-04
UNIV OF SCI & TECH OF CHINA
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[0009] However, the patent WO 03085071 pointed out that the biggest problem in the production process of levulinic acid lies in its separation process, especially the separation from the by-product formic acid!
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Embodiment 1～7
[0025] In the autoclave of 150mL, add 0.2mmol trihydrate ruthenium trichloride, 0.6mmol triphenylphosphine (PPh 3 ), 20mmol sodium hydroxide, 200mmol formic acid and 79.4mmol levulinic acid, sealed and stirred evenly. Heat to 100, 150 or 200°C, keep for 4, 6, 8 or 12 hours, finish the reaction and cool to room temperature, slowly depressurize to atmospheric pressure, open the autoclave, take samples, send to GC-MS for detection, specific experimental temperature, reaction The time and test results are listed in Table 1 with serial numbers 1-7.
Embodiment 8～11
[0027] Add 0.2mmol ruthenium trichloride trihydrate, 0.6mmol triphenylphosphine, 20mmol triethylamine or pyridine, 200mmol formic acid and 79.4mmol levulinic acid into a 150mL autoclave, seal it, and stir well. Heat to 150°C, keep for 6 or 12 hours, finish the reaction and cool to room temperature, slowly depressurize to atmospheric pressure, open the autoclave, take samples at different temperatures and reaction times, send them to GC-MS for detection, and the test results are listed in Table 1 The serial numbers are 8-11.
Embodiment 12～15
[0029] Add 0.2mmol ruthenium trichloride trihydrate, 0.6mmol triphenylphosphine, 20mmol triethylamine or pyridine, 200mmol formic acid and 200mmol levulinic acid into a 150mL autoclave, seal it, and stir well. Heat to 150°C, keep for 6 or 12 hours, finish the reaction, cool to room temperature, slowly depressurize to atmospheric pressure, open the autoclave, take samples, take samples at different temperatures and reaction times, send them to GC-MS for detection, and the test results are listed in the table The serial number in 1 is 12~15.
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Abstract
The invention discloses a method for preparing GAMMA-valerolactone from levulinic acid and formic acid, which is characterized in that the levulinic acid is in situ reduced at 100-200 DEG C in the presence of ruthenium catalyst and formic acid contained in a system as reducer, and distillation is carried out to obtain mixture containing the product GAMMA valerolactone and used catalyst; and mother liquor containing the used catalyst and raw material are mixed to realize circulation of the catalyst, thereby greatly improving environmental friendliness. The method avoids the energy source consumption during valerolactone purification process, avoids hydrogen source acquired from the system exterior, and improves the economy and security of a production system, with the advantages of simple operation process. The formic acid is decomposed to generate large amount of carbon dioxide besides hydrogen, which is convenient for collection and utilization.
Description
technical field [0001] The invention belongs to the technical field of methods for producing vehicle fuel from biomass, in particular to a method for preparing gamma-valerolactone by in-situ hydrogenation reduction and lactonization of biomass carbohydrates. Background technique [0002] The use of carbohydrates derived from biomass to produce vehicle fuel was first proposed in the 1970s. But so far, only one kind of bioethanol has been industrialized. However, the production of bioethanol from starch will cause food problems, and there are still obstacles in engineering using cellulose as raw material. Therefore, the production of other biofuels from carbohydrates is receiving increasing attention. [0003] γ-valerolactone is one of the candidate compounds, which is an ideal natural product not only for the production of fuels, but also for the production of chemicals and polymer materials. γ-valerolactone has the following excellent properties: [0004] 1. Low toxicity...
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