Method for catalytic preparation of delta-valerolactone 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 the problems of difficult catalyst recovery, high reaction temperature, and difficult purification of products, and achieve good catalytic oxidation activity, mild reaction conditions, and good industrial prospects.
Inactive Publication Date: 2008-04-09
FUDAN UNIV
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Problems solved by technology
There are two kinds of catalysts commonly used in the process of preparing δ-valerolactone from 1,5-pentanediol. One is a ruthenium complex catalyst. Expensive, not suitable for industrial production; the other is copper-based catalyst, but generally need to add chromium to achieve higher activity, chromium is a highly toxic substance, does not meet the requirements of green chemistry, and the reaction temperature is higher
Gold has alw
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Embodiment 1
[0016] 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, 0.8g 1,5-pentanediol and 0.5g 1# catalyst in the autoclave, seal the autoclave, fill with 1.3Mpa air, 120°C oil bath, electromagnetic stirring reaction 1 hour.
Embodiment 2
[0017] Example 2: 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 20°C for 24h, then the stirring was stopped, filtered with suction, washed with deionized water, dried, and calcined at 100°C for 24h to obtain the catalyst. It is 2# catalyst. Reaction conditions: 10ml tributyl phosphate, 0.8g 1,5-pentanediol, 0.5g 2# catalyst, 1.3Mpa air, 120°C oil bath, electromagnetic stirring for 2 hours.
Embodiment 3
[0018] Example 3: Add 12.6ml of 0.024mol / L HAuCl to 40ml of deionized water 4 Solution, 3.67g urea, stirred to dissolve, 2g 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, dried at 95°C, and calcined at 200°C for 4 hours , The catalyst obtained is designated as 3# catalyst. Reaction conditions: 10ml tributyl phosphate, 0.8g 1,5-pentanediol, 0.5g 3# catalyst, 1.3Mpa air, 120°C oil bath, electromagnetic stirring for 4 hours.
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Abstract
The invention pertains to the technical field of chemical industry, in particular to a preparation method of delta-valerolactone by using the load-type nano-gold catalyst. The using catalyst of the invention adopts a deposition precipitation method for preparation, in particular to the Au/TiO2 catalyst with the nano size after the calcination synthesis at certain temperature and the deposition of gold on the titanium dioxide. The catalyst is characterized by good dispersion of activity, small particles of gold and good stability, and can be used for catalytic air direct oxidation of 1, 5-pentanediol for the preparation of delta-valerolactone, so as to realize the one-step oxidation of 1, 5-pentanediol, further to generate the delta-valerolactone. The air is used as the oxidant during the oxidation process of 1, 5-pentanediol to replace the strong oxidants in the traditional methods, such as peracid, halogen oxides, nitrogen oxides and so on, thus avoiding the violent reaction conditions and the pollution substances generated by oxidants, which is in line with the requirements of green chemistry. The catalyst has the advantages of easy recovery and regeneration, can maintain a higher activity after a plurality of repeated uses and has higher industrial application value.
Description
technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a method for directly oxidizing 1,5-pentanediol with a supported nano-gold catalyst to prepare delta-valerolactone in one step. Background technique [0002] δ-valerolactone is an important organic intermediate widely used in the synthesis of various biochemical products such as fibers, drugs, spices and pesticides. δ-valerolactone can be synthesized by using 1,5-pentanediol as a raw material. In the traditional process, strong oxidants such as peracids, halogen oxides, nitrogen oxides or composite oxides are often used. The operation is dangerous, expensive, and reactive. A large amount of pollutants are generated, which does not meet the requirements of green chemistry and sustainable development. From the point of view of green chemistry, a clean oxidant must be selected. Air is an ideal oxidant because it is cheap and easy to obtain, and does not produ...
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