Preparation method of 1,3,3,3-tetrafluoropropene
A technology of tetrafluoropropene and tetrafluoropropane, which is applied in the field of preparation of hydrofluoroolefins, can solve the problems of harsh reaction conditions, expensive raw materials, and expensive prices, and achieve the effects of mild reaction conditions, cheap and easy-to-obtain raw materials, and easy operation
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[0027] Example 1:
[0028] Add trichloropropene (20.0g, 0.15mol) and 120mL chloroform to the 250mL dry three-necked flask equipped with magnetic stirring, thermometer and condenser. Under constant stirring, add anhydrous aluminum trichloride ( 2.0g, 0.015mol), and then gradually heated to 60℃, reacted for 12h, the reaction liquid was cooled to about 30℃, filtered, and the filtrate was distilled under reduced pressure. The vacuum degree was 5kPa, and the fraction at 120~125℃ was collected. 1,1,1,2,3,3-hexachloropropane (HCC-230da), the conversion rate is 85.7%, and the selectivity is 90.4%.
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[0029] Example 2:
[0030] Preparation of the catalyst: a certain proportion of Zn(NO 3 ) 2 ·6H 2 O, FeCl 3 , La(NO 3 ) 3 ·6H 2 O was mixed into a 2mol / L aqueous solution, and 15% by mass ammonia was added dropwise under constant stirring at 20°C-40°C, adjusted to pH 8.0, reacted for 8h, filtered, and dried at 120°C for 2h , Then mix a certain amount of magnesia with it uniformly, and then roast at 200℃ for 1h, 5℃ / min to 320℃, roast for 2h, then 10℃ / min to 450℃, roast for 4h, and finally heat it with hydrogen fluoride at 200 The Zn-Fe-La-Mg composite catalyst was obtained by activation treatment at ℃-380℃ for about 36h.
[0031] A fixed-bed tubular reactor with an inner diameter of 38 mm was filled with 50 ml of Zn-Fe-La-Mg composite catalyst, where the molar ratio of Zn, Fe, La, and Mg was 0.5:2:0.5:7, and the catalyst Dry, and then at 250 ℃, HF and CCl 3 CHClCHCl 2 (HCC-230da, abbreviated as 230da) into the first reactor R1, control the molar ratio of the two to 10:1, the contac...
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[0032] Examples 3 to 5:
[0033] Examples 3 to 5 prepared HCFC-234da according to the same method in Example 2, except that the reaction temperatures of R1 and R2 in Example 2 were 250°C and 300°C, respectively, while in Examples 3 to 5, R1, The reaction temperature and reaction results of R2 and R3 are shown in Table 1.
[0034] Table 1
[0035]
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