Method for preparation of cycloaliphatic carboxylic acid ester
A production method and a technology for aromatic carboxylic acid esters are applied in the field of producing alicyclic carboxylic acid esters, and can solve the problems of high catalyst cost, insufficient catalytic effect of pyromellitic acid ester hydrogenation, corrosion and the like
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Embodiment 1
[0063] 1.35 g of ruthenium chloride (Ru content 37%) was dissolved in 40 mL of water. 9.5g powdered SiO 2 Disperse in 60g of water and stir for 20min, add the aqueous solution of ruthenium to SiO 2 The suspension was stirred for 1 hour. The pH value of the solution was adjusted to 10 with NaOH aqueous solution (20% by mass). Thereafter, 10 mL of NaBH was added 4 The aqueous solution (10% by mass) was stirred for 0.5 hours. Filtration and washing to obtain Ru / SiO with a mass fraction of 5% 2 catalyst.
Embodiment 2
[0065] 1.35 g of ruthenium chloride (Ru content 37%) was dissolved in 40 mL of water. Disperse 9.5g of activated carbon powder in 60g of water and stir for 20min, then add the aqueous solution of ruthenium dropwise to SiO 2 The suspension was stirred for 1 hour. The pH of the solution was adjusted to 11 with NaOH aqueous solution (20% by mass). Thereafter, 5 mL of aqueous formaldehyde solution (30% by mass) was added, the temperature was raised to 90° C., the temperature was kept constant for 2 hours, and then cooled. Filter and wash to obtain a Ru / C catalyst with a mass fraction of 5%.
[0066] Its XRD such as figure 1 shown. There is no obvious diffraction peak of ruthenium.
Embodiment 3
[0068] 1.35 g of ruthenium chloride (Ru content 37%) and 0.83 g of palladium chloride were dissolved in 60 mL of deionized water. Add 50 g of alumina particles (30-40 mesh) to the above solution. Heating in a water bath at 60°C and rotary steaming, so that the ruthenium chloride and palladium chloride are supported on the alumina. The alumina containing noble metal salt was dried at 150°C for 2 hours, calcined at 400°C for 4 hours in an air atmosphere, and finally reduced with hydrogen at 250°C for 4 hours to obtain a ruthenium-palladium co-supported catalyst (1% by weight Ru-1% by weight Pd / Al 2 o 3 ).
[0069] Transmission electron microscopy images of the ruthenium-palladium co-supported catalyst prepared by this method are shown in figure 2 . There are no obvious particles on the surface of the carrier. Analyze the coexistence state of ruthenium and palladium in the particles with EDX, and the results are shown in image 3 .
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