Catalytic conversion method for hexachlorobutadiene
A technology for hexachlorobutadiene and butene, applied in the field of catalytic conversion of hexachlorobutadiene, can solve the problems of inability to recycle, low reactivity, poor thermal stability, etc., and achieves high industrial application prospects and low reactivity , the effect of high thermal stability
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Embodiment 1
[0019] Add 45 grams of alum pentoxide, 50 grams of anhydrous hydrogen fluoride, 20 grams of potassium fluoride and 10 grams of anhydrous sulfuric acid into a 300mL stainless steel belt stirred autoclave. Vacuum to remove excess water.
[0020] Add 52 grams of hexachlorobutadiene and 40 grams of anhydrous hydrogen fluoride into the kettle, then raise the temperature to 150°C for 3-4 hours, control the pressure at 1.5-1.7 MPa, and collect the discharged material with a cold trap.
[0021] After the product was separated by rectification, the NMR detection showed the following data:
[0022] 1 H NMR (500MHz, CDCl 3 )δ6.64(q,1H,J=6.5Hz);
[0023] 13 C NMR (500MHz, CDCl 3 )δ132.0(qq, J=39.3Hz, J=5.4Hz), 121.9(q, J=37.5Hz), 120.6(q, J=270Hz), 119.1(q, J=272.5Hz);
[0024] 19 F NMR (470MHz, CDCl 3 )δ-71.3(m, CF 3 ),-61.3(m, CF 3 ).
[0025] The above data prove that the product obtained is 2-chloro-1,1,1,4,4,4-hexafluoro-2-butene.
[0026] 1 H NMR (500MHz, CDCl 3 )δ6.60...
Embodiment 2～8
[0031] Examples 2-8 Prepare 2-chloro-1,1,1,4,4,4-hexafluoro-2-butene according to the same preparation method in Example 1, the difference is that the catalyst in Example 1 is Alum pentoxide, and the ratio of telomerization in Examples 2 to 8 is titanium dioxide, niobium pentoxide, tantalum pentoxide, titanium tetrachloride, alum pentachloride, niobium pentachloride, and tantalum pentachloride. The reaction results of Examples 2-8 are shown in Table 1.
[0032] Table 1 Catalyst Screening
[0033]
[0034]
Embodiment 9～13
[0036] Examples 9 to 13 were prepared according to the same preparation method in Example 1, 2-chloro-1,1,1,4,4,4-hexafluoro-2-butene, the difference is that the catalyst Agent is potassium fluoride, and in embodiment 9~13, be respectively tripropylamine, tributylphosphine, potassium bisulfate, potassium chlorosulfonate, potassium benzenesulfonate. The reaction results of Examples 9-13 are shown in Table 2.
[0037] Table 2 Screening of catalytic promoters
[0038] Example Catalyst Yield (%) 9 Tripropylamine 52.8 10 Tributylphosphine 44.2 11 Potassium bisulfate 62.6 12 Potassium chlorosulfonate 66.6 13 Potassium benzenesulfonate 57.6
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