[NHR3] 3 [Pt (SnCl3) 5] metal cluster single crystal, synthesis method and application of [NHR3] 3 [Pt (SnCl3) 5] metal cluster single crystal in catalytic dehydrogenation of low-carbon alkane
A synthesis method and metal cluster technology are applied in the application field of dehydrogenation of low-carbon alkanes to olefins, which can solve the problems of reduced interaction probability and insufficient modulation effect, so as to promote interaction, improve stability and regeneration performance, Make up clear effects
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Embodiment 1
[0037] Single crystal preparation: prepared in 3mol / L hydrochloric acid solution [NHR 3 ] 3 [Pt(SnCl 3 ) 5 ] The single crystal preparation method of subnano metal clusters and recrystallization is as follows:
[0038] S1 Weigh 80mg of chloroplatinic acid hexahydrate and 60mg of triethylamine hydrochloride fully dissolved in 1mL 3mol / L hydrochloric acid aqueous solution to obtain solution A; another weigh 170mg of stannous chloride dihydrate fully dissolved in 1mL 12mol / L concentrated hydrochloric acid In a water bath at 25°C, add 3 mL of deionized water at 600 rpm to dilute concentrated hydrochloric acid to 3 mol / L, and stir for 15 minutes to obtain solution B;
[0039] S2 Slowly add the above solution A to solution B dropwise to form an orange-red precipitate, stir for 5 minutes, filter under reduced pressure, wash with 10mL 3mol / L hydrochloric acid aqueous solution, and vacuum dry at 2-10°C for 24h to obtain [NHEt 3 ] 3 [Pt(SnCl 3 ) 5 ] Subnanometer metal cluster cru...
Embodiment 2
[0042] Pt@Sn-S-Al 2 o 3 Catalyst preparation and the method for the dehydrogenation of low-carbon alkanes are as follows:
[0043] 2.1 Preparation of carrier
[0044] Pseudoboehmite powder was roasted in a muffle furnace, raised from room temperature to 600 °C at a rate of 1 °C / min, kept for 2 hours, and finally cooled to room temperature to obtain granular Al 2 o 3 (Al 2 o 3 -SB-600);
[0045] 2.2 Catalyst preparation
[0046] Weigh the Al prepared in Example 2.1 2 o 3 Carrier 300mg, quickly weigh 250mg after oven drying at 120°C for 4h; weigh the [NHR 3 ] 3 [Pt(SnCl 3 ) 5 ] Dissolve 10.5 mg of subnano metal cluster single crystal in 0.22 mL of 1mol / L hydrochloric acid / ethanol impregnation solution, shake for 1 min and then impregnate equal volume into the above Al 2 o 3 On the carrier, let it stand at room temperature for 2h; dry at 50°C overnight, bake in air at 500°C for 4h, and finally in 20%H 2 / N 2 Pt@Sn-S-Al was obtained by reduction at 590°C for 2h in ...
Embodiment 3
[0062] The preparation of a KPt@Sn-Beta zeolite catalyst and the method for producing propylene from propane dehydrogenation are as follows:
[0063] 3.1 Catalyst carrier treatment
[0064] H-beta molecular sieve, SiO 2 / Al 2 o 3 =25, pickled with 13M (20ml / g) concentrated nitric acid at 80-100°C for 12h, centrifuged and washed with deionized water until neutral, dried at 120°C and dried in a vacuum oven at 150-200°C for 18-48h to obtain Beta-no-Al .
[0065] 3.2 Preparation of KPt@Sn-Beta-no-Al catalyst
[0066] Take by weighing 250mg of carrier in embodiment 3.1, take by weighing [NHR in embodiment 1 3 ] 3 [Pt(SnCl 3 ) 5 ] Subnanometer metal cluster single crystal 10.5mg dissolved in 0.175mL 1M HCl / C 2 h 5 The mixed solution of OH was shaken for 1 min, then impregnated with an equal volume on the above-mentioned molecular sieve carrier, left at room temperature for 1-2 h, then dried in a vacuum oven at 50°C for 24 h, then taken out and recorded as sample A. Weigh ...
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