Method for producing trans-1-chloro-3,3,3-trifluoropropene
A manufacturing method and technology of trifluoropropene, applied in chemical instruments and methods, preparation of halogenated hydrocarbons, preparation of dehydrohalogenation, etc., capable of solving heating and other problems
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preparation example 1
[0108] Introduce 4.1g / min of 1,1,1,3,3-pentachloropropane (240fa) and 3.4g / min of hydrogen fluoride ( Molar ratio: 240fa / hydrogen fluoride = about 1 / 9), and the autoclave was heated to 150°C. When the pressure exceeds about 4 MPa, the reaction product gas is discharged from the needle valve at the outlet of the condenser so as to maintain about 4 MPa. The exhausted gas was cooled in an ice water bath, and the acid was absorbed by a fluororesin gas cleaning bottle filled with ice water, and the reaction organic matter was recovered by passing through a glass trap of a dry ice acetone bath. When the liquid volume in the autoclave reached about 1000 ml, the reaction liquid was discharged from a dip tube through a needle valve so as to maintain about 1000 ml. The discharged reaction liquid was collected in a gas cleaning bottle made of fluororesin which was cooled in an ice-water bath and filled with ice water. After continuing the reaction for 24 hours, all the reaction liquid ...
Embodiment 1
[0112] The temperature was raised while flowing nitrogen gas at a rate of 10 ml / min through a cylindrical stainless steel (SUS316L) reaction tube with an inner diameter of 2.7 cm and a length of 40 cm equipped with an electric furnace. When the temperature of the reaction tube reached 320°C, as the reaction raw material, the vaporized reaction solution (halogenated hydrocarbon compound with 3 carbon atoms) was supplied at a flow rate of about 0.32 g / min, and the gasified reaction liquid (halogenated hydrocarbon compound with 3 carbon atoms) was supplied at a flow rate of about 0.12 g / min. Hydrogen fluoride is supplied at a flow rate of 0.8 ml / min, and chlorine gas is supplied at a flow rate of about 0.8 ml / min (molar ratio: halogenated hydrocarbon compound with 3 carbon atoms / hydrogen fluoride / chlorine gas=1 / 3.4 / 0.02, contact time: about 50 seconds) , when the flow is stable, stop the nitrogen supply. The generated gas flowing out of the reactor is passed through a fluororesin...
Embodiment 2
[0114] Regarding the supply amount of the reaction raw material, in addition to supplying the gasified reaction liquid (halogenated hydrocarbon compound with 3 carbon atoms) at a flow rate of about 0.47 g / min, hydrogen fluoride at a flow rate of about 0.10 g / min, In addition to supplying chlorine gas at a flow rate of about 0.8ml / min (molar ratio: halogenated hydrocarbon compound / hydrogen fluoride / chlorine gas with 3 carbon atoms=1 / 2.0 / 0.02, contact time: about 50 seconds), the same as in Example 1 The reaction was carried out in the same manner. The results are shown in Table 3.
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