Production method of synthetising HFC-152a using two-step method reaction
A production method and technology of hfc-152a, which are applied in the production field of synthesizing HFC-152a by two-step reaction
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Embodiment 1
[0031] According to the above process and steps, 1Kg TiCl is charged into 50L No. 1 Reactor 1. 4 And input 1.5Kg HF to activate for 5 hours, input HF to 10Kg, vinyl chloride to 10Kg, the reaction temperature is controlled at about 15°C, and the reaction pressure is controlled at about 0.22MPa. Half an hour No. 1 reactor 1 gas sampling and chromatographic analysis gave the crude product composition shown in Table 1. Put 0.5KgSnCl in 50L No. 2 reactor 4 4 And put in 0.8KgHF to activate for 6 hours, then put the materials and anhydrous hydrofluoric acid steamed into the layerer 3 in No. 1 reactor at 2Kg / hour and 650g / hour respectively, and control the reaction temperature to about 45℃, pressure About 0.6MPa, the top temperature of the reaction reflux tower 5 is about 10°C. After the reaction is stable, a sample is taken for analysis, and the crude product composition is shown in Table 2.
[0032] Table I
[0033]
[0034] Table II
[0035]
[0036] Conclusion: CH can be calculate...
Embodiment 2
[0038] According to the operation steps of Example 1, 5Kg of HF and 10Kg of vinyl chloride were put into No. 1 Reactor 1, and other conditions were unchanged. The crude product sampled and chromatographic analysis of the first reaction gave the crude product composition shown in Table 3. In the second step, the crude product was sampled and analyzed by chromatography to give the composition of the crude product as shown in Table 4.
[0039] Table Three
[0040]
[0041] Table Four
[0042]
[0043] Conclusion: CH can be calculated from the data in Tables 3 and 4 2 = The selectivity of final conversion of CHCl to HFC-152a is 99.6%. But when the reaction time of the first step is unchanged, when the molar ratio of hydrogen fluoride to vinyl chloride is less than 2, the content of CH2=CHCl in the crude product HCFC-151a cannot reach ≤100ppm. It also leads to the content of CH2=CHCl in the crude product HFC-152a of the second step reaction not reaching ≤10ppm. Therefore, the first...
Embodiment 3、4
[0045] According to the operation steps of Example 1, the first step of the reaction is under the reaction conditions of temperature 3~8℃, pressure 0.05~0.1MPa and temperature 35~40℃, pressure 0.4~0.6MPa, and other conditions remain unchanged. Sampling and chromatographic analysis of the crude reaction product showed the composition of the crude product in Table 5.
[0046] Table 5
[0047]
[0048] Conclusion: The above data shows that when the reaction temperature of the first step is lower than 10℃, the conversion of vinyl chloride is not complete; when the temperature is higher than 25℃, the formation of high boilers increases; therefore, the optimal reaction temperature is 10-25 ℃.
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