Process for producing 2,3,3,3-tetrafluoropropene
A technology of trifluoropropene and tetrafluoropropane, which is applied in the field of preparation of fluorinated organic compounds, and can solve the problems of industrial-scale hydrogen treatment, such as danger and high cost
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Embodiment 1
[0064] Example 1: Fluorination of 1230xa using 1230xa as starting material
[0065] Load 3 cc of high surface area BASF chromium oxide into a 1 / 2 inch Hastelloy Nickel C 276 reactor. A 6-inch Hastelloy nickel-based corrosion-resistant and heat-resistant B 1 / 8" distillation packing was packed on the top of the catalyst as an evaporation zone. First, the catalyst was activated with HF, and then from the top of the reactor at 275°C and atmospheric pressure to Add 1230xa at a flow rate of 0.54 ml / hr along with 18 sccm of HF and 3 sccm of N 2 . The flow from the reactor was analyzed by GC and GC-MS. Show the results of the test in figure 1 middle. Catalysts show degradation over time.
[0066]
Embodiment 2
[0067] Example 2: Fluorination of 1230xa using 1232xf-1230xa (molar ratio 1:1) mixture as starting material
[0068] 3 cc of high surface area BASF chromia was loaded into a 1 / 2 inch Hastelloy Nickel C 276 reactor. A 6-inch Hastelloy nickel-based corrosion-resistant and heat-resistant B 1 / 8" distillation packing was packed on the top of the catalyst as an evaporation zone. First, the catalyst was activated with HF, and then from the top of the reactor at 275°C and atmospheric pressure to A flow rate of 0.53 ml / hr was added to the 1232xf-1230xa mixture along with 18 sccm of HF and 3 sccm of N 2 . The flow from the reactor was analyzed by GC and GC-MS. Show the results of the test in figure 1 middle. The results show that catalyst life is improved by using a mixture of 1232xf-1230xa (1:1 molar ratio) as feedstock.
[0069]
Embodiment 3
[0070] Example 3: Fluorination of 1230xa using a mixture of 10 wt% 1233xf - 90 wt% 1230xa as starting material
[0071] The 1230xa used in this example contained 5 ppm of diisopropylamine. A mixture of 10% by weight 1233xf-90% by weight 1230xa was used as starting material. Load 6.5 L of pre-fluorinated chromia catalyst into a 4-inch Monel 400 reactor. The reactor was heated up to about 180°C in a nitrogen flow. Then, the feed of anhydrous HF was started at a flow rate of 1.9 lb / h. After passing through the Mol Sieve 3A column at a flow rate of 1.1 lb / h, the organic feed was mixed with the HF feed. The mixed HF and organic feed are introduced into the gasifier for gasification, and then introduced into the reactor for reaction. Once the reaction started, the reaction temperature (hot spot temperature) increased to about 200°C. The reactor pressure was set at 70 psig. During the reaction, samples were taken from the product stream periodically and analyzed by GC and GC-...
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