A kind of synthetic method of 1,2-propanediamine
A synthetic method and technology of propylenediamine, applied in the first field, can solve problems such as unfavorable industrial production, difficult separation, difficult operation, etc., and achieve the effects of easy separation, high selectivity and simple operation
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
preparation example Construction
[0028] The preparation of the metal-loaded catalyst in the present invention can be carried out using conventional catalyst steps, such as the following steps: the carrier is dried in a vacuum oven at 150° C. to 300° C. for 2 hours, and then mixed with a solution containing Ni or Co metal salt and a metal additive Re or non-metallic additive B, fully immersed in ultrasonic waves for 1.5h; filter off excess liquid to obtain a carrier with adsorbed metal ions, dry in a vacuum oven at 150°C to 300°C for 3h, and then continue to immerse in the remaining solution 2h; the carrier impregnated twice is calcined in a box-type resistance furnace at 300° C. to 400° C. for 6 hours to prepare a catalyst precursor.
[0029] The catalyst precursor is reductively activated in a tubular reactor, heated to 250°C to 300°C for about 4 hours and kept for 1 hour, while H 2 and N 2 6:1 (volume ratio) gas flow through the reaction tube, continue to heat to 350 ℃ ~ 350 ℃ and constant temperature acti...
Embodiment 1
[0034] The catalyst is a nickel-based supported catalyst, and the carrier is Al 2 o 3 , Ni is Al 2 o 3 15% of the mass of the carrier, and the non-metallic additive B is 3% of the mass of the carrier.
[0035] With 110g of isopropanolamine, 3.3g supported catalyst, 55g water, 0.55gNa 2 CO 3 The auxiliary agent is added into the autoclave, the air in the autoclave is replaced by hydrogen, and then evacuated, 42g of liquid ammonia is introduced, the hydrogen is continuously introduced to 2MPa, the temperature is raised to 185°C, and the reaction is carried out for 8h. After the reaction, the reaction solution was cooled to room temperature, and the reaction solution was filtered to recover the catalyst. Based on the consumption of isopropanolamine per unit weight, the conversion rate is 38.2%, and the selectivity of 1,2-propylenediamine is 99.6%. The reaction filtrate was analyzed by GC, and no 2,5-dimethylpiperazine was detected.
[0036] The reaction solution is distill...
Embodiment 2
[0038] The catalyst is a nickel-based supported catalyst, and the carrier is Al 2 o 3 , Ni is Al 2 o 3 20% of the mass of the carrier, and the metal additive Re is 1% of the mass of the carrier.
[0039] With 95g of isopropanolamine, 2.9g nickel-based supported catalyst, 95g water, 4.75gK 2 CO 3 The auxiliary agent is added into the autoclave, the air in the autoclave is replaced by hydrogen, and then vacuumized, 45g of liquid ammonia is introduced, the hydrogen is continuously introduced to 3MPa, the temperature is raised to 195°C, and the reaction is carried out for 8h. After the reaction, the reaction solution was cooled to room temperature, and the reaction solution was filtered to recover the catalyst. Based on the consumption of isopropanolamine per unit weight, the conversion rate is 59.5%, and the selectivity of 1,2-propylenediamine is 97.3%. The reaction solution was distilled to remove water, and further rectified to obtain the pure product of 1,2-propanediamin...
PUM
| Property | Measurement | Unit |
|---|---|---|
| boiling point | aaaaa | aaaaa |
Abstract
Description
Claims
Application Information
Login to View More