Process for producing 2,3,3,3-tetrafluoropropene
A technology of tetrachloropropene and trifluoropropene is applied in the field of preparing fluorinated organic compounds, and can solve the problems of high cost and high cost
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Embodiment 1
[0054] The HCO-1230xa feed used in Example 1 had a purity of 99.2 GC (gas chromatography) area % and contained 100 ppm moisture.
[0055] used by N 2 , HF and organic feed system, feed vaporizer, superheater, 2-inch ID Monel reactor, acid scrubber, dryer and product collection system constituted of a continuous gas-phase fluorination reaction system to study the reaction. Load the reactor with 1.8 liters of Cr fluoride 2 o 3 catalyst. Then after installing the reactor in a constant temperature sand bath, the N 2 The reactor was heated to a temperature of approximately 180°C while purging the catalyst. HF feed as N 2 The co-feed was introduced into the reactor (via vaporizer and superheater) for 15 minutes, at which time the N 2 flow. The HF flow rate was adjusted to 1.9 lb / hr before starting to feed 1,1,2,3-tetrachloropropene (HCO-1230xa) to the reactor (via vaporizer and superheater). The HCO-1230xa feed contained 5 ppm diisopropylamine. The feed rate of HCO-1230xa w...
Embodiment 2
[0060] The HCO-1230xa feed used in Example 2 had a purity of 99.2 GC (gas chromatography) area % and contained 100 ppm moisture.
[0061] by N 2 , HF and organic feed systems, a steam vaporizer, a ½” OD U-shaped superheater (submerged in a sand bath) and an acid scrubber were used in this study. In N 2 The U-shaped superheater was heated to a temperature of about 180°C in the flow. HF and HCO-1230xa were introduced into the steam vaporizer and then the U-shaped superheater at feed rates of 2.0 lb / h and 1.0 lb / h, respectively. The HCO-1230xa feed contained 5 ppm diisopropylamine. The pressure in the U-shaped superheater was then built to 70 psig. After 8 hours, the entire process stream from the U-shaped superheater was introduced into the DIT (Dry Ice Trap) and collected for 15 minutes. Then 50 mL of CH 2 Cl 2 and 530 ml DI H 2 O sucked into the DIT. The contents of the DIT were transferred to a Sep funnel after thawing for phase separation. The fraction of the separa...
Embodiment 3
[0063] This example demonstrates the efficiency of 3A molecular sieves for the removal of moisture from HCO-1230xa feed. The HCO-1230xa feed used in Example 1 had a purity of 99.2 GC (gas chromatography) area % and contained 100 ppm moisture. The HCO-1230xa feed contained 5 ppm diisopropylamine. The HCO-1230xa feed was passed through a 2” ID column loaded with 2 liters of 3A molecular sieve at a rate of 1.0 lb / h and a sample was taken from the sampling port behind the drying column. Moisture content was measured using a Mitsubishi hygrometer (Model CA-100) is 12 ppm, indicating that 3A molecular sieve is an effective desiccant for HCO-1230xa.
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