Method for preparing fluorine hydride addition reaction catalyst and fluorine-containing alkane
A fluorine-containing alkanes and addition reaction technology, which is applied in the field of hydrogenation and fluorination of fluoroolefins to synthesize saturated fluorine-containing alkanes, can solve the problems of high conversion rate of raw materials and product selectivity, low equipment requirements, high reaction pressure, etc. The effects of high conversion and product selectivity, ease of industrial-scale production, and low reaction temperature and pressure
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Embodiment 1
[0036] In a 500ml three-necked flask, add about 209.6g of tri-n-butylamine, and then slowly introduce HF about 54.2g~67.7g at room temperature, accompanied by stirring, and react to prepare the binary system catalyst tri-n-butylamine·2.4~ 3.0HF, that is, the molar ratio of tri-n-butylamine:HF is 1:2.4~3.0.
[0037]In a 500ml stainless steel autoclave, add about 107.3g of the prepared tri-n-butylamine 2.6HF, 4.5g of potassium fluoride, about 19.3g of 18-crown-6, and then add hexafluoro at the liquid phase port of the autoclave at room temperature Propylene 53g. Stirring was started and the temperature was rapidly raised to 85°C, and the reaction was carried out for about 1 hour. The sample was analyzed by GC, and the results showed that the content of hexafluoropropylene was 7.03%, and the content of 2H-heptafluoropropane was 92.97%. The self-pressure generated in the reaction process is 0.7-0.8Mpa, and the method of the invention does not produce the highly toxic substance oc...
Embodiment 2
[0039] In a 500ml stainless steel autoclave, add about 95g of the prepared tri-n-butylamine 3.0HF, 21ml of ethanol, 4.5g of potassium fluoride, about 19.3g of 18-crown-6, and then add it into the liquid phase port of the autoclave at room temperature Hexafluoropropylene 50g. Stirring was started and the temperature was rapidly raised to 85° C., and the reaction was carried out for about 1 hour. The sample was analyzed by GC, and the result showed that the content of 2H-heptafluoropropane was 87.79%. The self-pressure generated by the reaction process is 0.6-0.7 MPa.
Embodiment 3
[0041] In a 500ml three-necked flask, add about 101.19g of tri-n-butylamine, and then slowly introduce about 100.05g of HF at room temperature, accompanied by stirring, to react to obtain the catalyst tri-n-butylamine·5.0HF of the binary system, which is The molar ratio of tri-n-butylamine:HF is 1:5.0.
[0042] In a 500ml stainless steel autoclave, add the prepared tri-n-butylamine 5.0HF, add 2.6g of lithium fluoride and about 22g of 15-crown (ether)-5 at room temperature, and then add tetrahydrofuran at the liquid phase port of the autoclave at room temperature 20ml, tetrafluoroethylene 500g. Stirring was started and the temperature was rapidly raised to 90° C., reacted for about 1 hour, and a sample was taken for GC analysis, and the result showed that the content of pentafluoroethane was 93.52%. The self-pressure generated in the reaction process is 0.5-0.6 MPa.
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