Catalytic preparation method of isopropanolamine
A technology of isopropanolamine and catalyst, applied in the field of preparation of isopropanolamine products, can solve problems such as multiple reactors, unfavorable industrialization promotion and application, increase in investment amount of synthetic equipment and complexity of process control, etc. Side reactions, stable and efficient catalysis, the effect of improving yield
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preparation example 1
[0057] Preparation of Pd / Au / La-ZSM Catalyst
[0058] S1: Dissolve chloroauric acid and ammonium chloropalladate in deionized water to make solutions with a concentration of 5 mM respectively, and set aside;
[0059] S2: Put 200mL of ZSM-5 zeolite into a beaker, add 500mL of 20% ethanol solution, and add 5M hydrochloric acid to make the hydrochloric acid content about 20g, activate at 40°C for 2 hours;
[0060] S3: Disperse the activated ZSM-5 zeolite in ethanol aqueous solution of mercaptoethylamine, let it stand at 40°C overnight, filter, wash with deionized water 3 times, and dry at 50°C for 4 hours;
[0061] S4: Put the ZSM-5 zeolite obtained in the previous step into the reaction bottle, add 500 mL of deionized water to the bottle, pass nitrogen gas into the reaction bottle for 2 minutes to remove oxygen, add 50 mL of the chloroauric acid solution prepared above and chloropalladium acid Ammonium solution 50mL, incubate under ultrasound for 10min, continue to sonicate, and...
Embodiment 1
[0068] Preparation of isopropanolamine products based on triisopropanolamine
[0069] (S1): 1 kg of liquid ammonia was prepared at room temperature into saturated ammonia water and added to the autoclave, which was filled with 200 g of Pd / Au / La-ZSM catalyst prepared by the method described in Preparation Example 1 and 50 g of montmorillonite in advance. Loaded phosphotungstic acid (Keggin type, tungsten load 0.5wt%) and 35g ammonium carbonate;
[0070] (S2): Close the reactor, pass nitrogen into the reactor to remove the air, pressurize 10.7kg of propylene oxide from the metering tank to 0.15Mpa, then pour it into the reactor from the feed port, raise the temperature to 60°C, and stir for 2 hour; then heat up to 70°C, continue to spray 1.8kg of saturated ammonia water at about 5°C through the atomization spray feeding port, and the spray feeding time is 10-12min. Reaction solution 1;
[0071] (S3): Cool the reaction solution, send the reaction solution 1 to the deamination t...
Embodiment 2
[0074] Same as Example 1, the difference is that the amount of catalyst used in step S1 is: 300g of Pd / Au / La-ZSM catalyst, 110g of phosphotungstic acid supported by montmorillonite, other preparation materials and methods are the same as in Example 1, and the prepared product contains three The content of isopropanolamine is 95.2%.
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