Preparation method of 1,3-butadiene catalyst from butene
A catalyst, butadiene technology, applied in catalyst activation/preparation, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of low activity, poor dispersion of active metals, etc., achieve simple process, stable product properties, The effect of short reaction time
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[0043] The preparation process of the catalyst of the present invention is as follows: ammonia and the salt solution of Fe, Zn and M are continuously sprayed into the impeller 2 rotating at high speed from the feed ports 4 and 5 provided on the impeller cover respectively, and the slurry generated by the reaction is passed around the impeller 2 Falling into the reactor, the generated part of the slurry enters the circulation pipe 7 through the circulation pipe inlet 6, and the circulating material is sprayed into the high-speed rotating impeller 2 from the circulating material outlet 6 provided on the impeller cover 3, and the generated slurry is discharged from the top of the reactor. The overflow port 8 is continuously discharged, and the catalyst is obtained by filtering, drying and roasting. Among them, the reaction temperature is controlled at 10~40°C, the residence time is 5~20min, the pH value of the slurry discharged from the overflow port is controlled to be 7~9, and t...
Embodiment 1
[0047] (1) Weigh 146.6g Fe(NO 3 ) 2 . 9H 2 O, 166.4g Zn(NO 3 ) 2 . 6H 2 O and 4.7gCr(NO 3 ) 3 . 9H 2 O is prepared into 200mL metal solution, ready for use; measure 44mL of the above solution and dilute to 90mL, add 12g polyethylene glycol and mix evenly, take 100g of alumina carrier for solution impregnation, after impregnation, dry at 120°C for 4 hours, and the drying is completed After that, roasting is carried out, wherein, the heating rate before 140°C is 2.0°C / min, the heating rate at 140~170°C is 1.3°C / min, the heating rate at 170~210°C is 0.7°C / min, and the heating rate at 210~270°C is 5.5°C / min, 270~600°C heating rate of 2.0°C / min, 600°C constant temperature for 3 hours, to obtain granular precursor a 1 , and its particle size distribution is shown in Table 1;
[0048] (2) Add the granular precursor obtained in step (1) and 200mL water into the reactor for circulation, take 156mL of the metal salt solution prepared in step (1) and dilute it to 500mL, and m...
Embodiment 2
[0050] Other conditions are the same as embodiment 1, just 4.8g Cr(NO 3 ) 3 . 9H 2 O was changed to 11.6Mg(NO 3 ) 2 . 6H 2 O, the quality of polyethylene glycol was changed to 11g. During the catalyst roasting process in step (1), the heating rate before 140°C was 1.8°C / min, the heating rate was 1.2°C / min at 140~175°C, and the heating rate was 175~215°C 0.4°C / min, 215~275°C heating rate is 6.0°C / min, 275~600°C heating rate is 1.8°C / min, the granular precursor a 2 , in step (2), change the diameter of the nozzle to 18mm, the volume ratio of the circulation volume of the slurry to the feed volume is 2.5:1, the temperature of the precipitation reaction is 35°C, and the pH value of the slurry at the overflow port is 8.2, and the catalyst A is obtained 2 , and its physical and chemical properties are listed in Table 1.
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