Method for catalytic preparation of gamma-butyrolactone by using supported nano-gold catalyst
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A nano-gold and catalyst technology, which is applied in the chemical industry, can solve problems that have not been reported, and achieve the effects of simple process, high catalytic activity and low cost
Inactive Publication Date: 2008-03-12
FUDAN UNIV
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At present, domestic and foreign literatures on gold-catalyzed liquid phase oxidation mostly focus on the selective oxidation of alcohols to prepare aldehydes or acids such as benzyl alcohol, glycerol and glucose, although the selective epoxidation of 1,4-butanediol Butyrolactone is of great significance, but has not been reported
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Embodiment 1
[0017] Example 1: Add 12.6ml of 0.024mol / L HAuCl to 40ml of deionized water 4 Solution, 3.67g of urea, stirred to dissolve, 2g of P25 was added to the solution, electromagnetically stirred in a water bath at 80°C for 2h, then the stirring was stopped, filtered with suction, washed with deionized water three times, washed with ethanol three times, and dried at room temperature to obtain Au / TiO 2 Catalyst, recorded as 1# catalyst. Reaction conditions: Add 20ml tributyl phosphate as solvent, 1.4g 1,4-butanediol and 0.5g 1# catalyst in the autoclave, seal the autoclave, fill with 1.3Mpa air, 120°C oil bath, electromagnetic stirring reaction 9 hours.
Embodiment 2
[0018] Example 2: Add 12.6ml of 0.024mol / L HAuCl to 40ml of deionized water 4 solution, adding sodium hydroxide solution dropwise to adjust the pH value to 7, adding 2g of P25 to the solution, stirring electromagnetically in a water bath at 20°C for 24h, then stopping the stirring, filtering with suction, washing with deionized water, and drying at 95°C to obtain Catalyst is recorded as 2# catalyst. Reaction conditions: 20ml tributyl phosphate, 1.4g 1,4-butanediol, 0.5g 2# catalyst, 1.3Mpa air, 120°C oil bath, electromagnetic stirring for 9 hours.
Embodiment 3
[0019] Example 3: Add 12.6ml of 0.024mol / L HAuCl to 40ml of deionized water 4 Solution, add sodium hydroxide solution dropwise to adjust the pH value to 14, add 2g P25 to the solution, stir electromagnetically in a water bath at 80°C for 2h, then stop stirring, filter with suction, wash with deionized water, dry at 95°C, and dry at 200°C Lower roasting 4 hours, the catalyst obtained is denoted as 3# catalyst. Reaction conditions: 20ml tributyl phosphate, 1.4g 1,4-butanediol, 0.5g 3# catalyst, 1.3Mpa air, 120°C oil bath, electromagnetic stirring for 9 hours.
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Abstract
The present invention belongs to the field of chemical engineering and technology and is a method of using the loading nano-sized gold catalyst in the air for the direct oxidation of gamma-butyrolactone. The catalyst used in the present invention is prepared in a deposition and aggradation method. Specifically, the gold is deposited on the nano-sized titanium dioxide; the nano-sized Au/TiO2 catalyst can be got after roasting. The catalyst is good in dispersion, small in gold particles and good in stability, and can catalyze the air for the direct oxidation of 1, 4-butanediol to prepare the gamma-butyrolactone; the catalyst shows the excellent activity (the conversion rate of the 1, 4-butanediol is 100 percent; the collection rate of the gamma-butyrolactone is 99 percent). The present invention realizes the one-step oxidation of the 1, 4-butanediol to prepare the gamma-butyrolactone. In the oxidation process of the 1, 4-butanediol, the clean and easily accessible air is used as the oxidant to replace the strong oxidant in the traditional method such as the peracid, halogen oxide, nitrogen oxide and so on; the method avoids the production of the pollutants, and meets the requirements of the green chemistry. The catalyst can be repeatedly used and the relatively high activity can still be maintained; the method has the relatively high value for the industrial application.
Description
technical field [0001] The invention belongs to the technical field of chemical industry and relates to a method for preparing gamma-butyrolactone in one step by using nano-scale gold as a catalyst to catalyze air to directly oxidize 1,4-butanediol. Background technique [0002] γ-butyrolactone is an important solvent, extractant and intermediate of drugs, fibers and pesticides, and can be used in the synthesis of fuels and dyes, so it is widely used in petrochemical, agricultural, pharmaceutical, fiber and resin fields Has a wide range of uses. γ-butyrolactone can be synthesized by using 1,4-butanediol as a raw material. In the traditional process, some strong oxidants are often used, or a co-oxidant is added. The operation is dangerous, the price is expensive, and the reaction generates a large amount of pollutants, which does not meet the requirements Green chemistry and sustainable development requirements. From the point of view of green chemistry, a clean oxidant mus...
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