Method for preparing 1,3 propylene glycol by using glycerol method
A technology of propylene glycol and glycerol, applied in chemical instruments and methods, preparation of hydroxyl compounds, preparation of organic compounds, etc., can solve the problems of high equipment investment, high reaction pressure, harsh production process, etc., and achieve good economic benefits and mild reaction conditions. , the effect of large market competitiveness
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Embodiment 1
[0029] Add 100ml of aqueous solution (prepared by dissolving the corresponding salt in water at 70°C) containing chromium nitrate hydrate (1.0M Cr), potassium tungstate (0.5M W) and copper acetate (0.25M Cu) into a 500ml flask . An aqueous solution of sodium hydroxide (0.5M) was then added dropwise. A reddish-brown gel formed within 15-30 minutes. The gel material was repeatedly washed with ammonium nitrate solution (1mol / L) to pH=8-9. After removing the water by using a rotary evaporator, the solid material was further dried overnight in a vacuum oven at 25°C, and then calcined. (Calcination is carried out in this way, the solid matter is placed in an air atmosphere, then heated to 275° C. at a rate of 10° C. / min and kept in an air atmosphere of 275° C. for 1 hour; then the air atmosphere is changed to argon and The material was heated from 275°C to 600°C at a rate of 2°C / min and the material was kept at 600°C under argon for 2 hours.) The nominal composition of the final ...
Embodiment 2
[0032]Add 100ml of aqueous solution (prepared by dissolving the corresponding salt in water at 70°C) containing chromium nitrate hydrate (1.0M Cr), potassium tungstate (0.5M W) and copper acetate (0.25M Cu) into a 500ml flask . An aqueous solution of sodium hydroxide (0.5M) was then added dropwise. A reddish-brown gel formed within 15-30 minutes. Stand in a dark place at 20°C for 72 hours. The gel material was repeatedly washed with ammonium nitrate solution (1mol / L) to pH=8-9. After removing water by using a rotary evaporator, the solid matter was further dried overnight in a vacuum oven at 25° C., and 34 g of a solid catalyst precursor were recovered. 17 g of this solid catalyst precursor were then calcined. Calcination is carried out by placing the solid substance in an air atmosphere, then heating it to 275°C at a rate of 10°C / min and maintaining it in an air atmosphere at 275°C for 1 hour; then changing the air atmosphere to argon and drying the substance Heat from 2...
Embodiment 3
[0035] An additional 17 g of solid catalyst precursor prepared in Example 2 was calcined in the following manner: the solid material was placed in an air atmosphere, then heated to 275° C. at a rate of 10° C. / min and held in an air atmosphere at 275° C. for 1 hours; the air atmosphere was then changed to argon and the mass was heated from 275°C to 600°C at a rate of 2°C / min and the mass was maintained at 600°C under argon for 5 hours. The nominal composition of the final catalyst is Cr 1 W 0.5 Cu 0.25 o x .
[0036] 10 grams of glycerol with a purity of 95% and 30 milliliters of hydrogen peroxide with a concentration of 30 percent were added to a 200 milliliter round-bottomed flask respectively, a condenser tube and a drying tube were installed, and the temperature was raised to 100° C. for 2 hours under stirring, and the reaction was stopped to obtain 9.0 grams Acetol. Add it into a 500 ml autoclave with 0.25 g of the catalyst prepared in advance, and continuously feed h...
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