High yield preparation method of paraxylene by methanol/dimethyl ether conversion
A technology of p-xylene and dimethyl ether, which is applied in the field of methanol/dimethyl ether conversion to produce p-xylene with high yield, which can solve the problems of low market value and complicated products
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[0029] The present invention uses the preparation method of catalyst, wherein the siloxane compound is shown in the following formula:
[0030]
[0031] where R 1 , R 2 , R 3 and R 4 is an alkyl group of 1-10 carbon atoms.
[0032] The invention uses a catalyst preparation method, wherein the siloxane-based compound is ethyl silicate.
[0033] The reaction mode of the present invention is the contact reaction between the reaction material and the catalyst, the reaction temperature is 350-550°C, preferably 400-500°C; the reaction pressure is 0-2MPa, preferably 0-1MPa; the methanol / dimethyl ether feed weight The air speed is 0.1-20h -1 , preferably 1-10h -1 . When the content of toluene or benzene in the methanol / dimethyl ether raw material is not more than 10wt%, the content of aromatics in the reaction product can reach more than 50wt%, wherein the content of p-xylene in aromatics is greater than 80wt%, and p-xylene is in xylene isomers The selectivity is greater th...
Embodiment 1
[0035] Embodiment 1 fixed-bed catalyst preparation
[0036] 1) 500g ZSM-5 zeolite molecular sieve former powder (Nankai University Catalyst Factory) (SiO 2 / Al 2 o 3 =50) Roast at 550°C to remove the template agent, exchange 4 times with a 0.5 molar equivalent ammonium nitrate solution in a water bath at 80°C, dry in air at 120°C after the exchange, and roast at 550°C for 3 hours to obtain HZSM- 5 Zeolite molecular sieves.
[0037] 2) Take 20 g of the HZSM-5 zeolite molecular sieve prepared in step 1) for tablet molding, obtain a 40-60 mesh sample after crushing and screening, and use a mass concentration of 9% zinc nitrate [Zn(NO 3 ) 2 ] solution at room temperature for 4 hours, after drying at 120°C, roasting in air at 550°C for 6 hours; using orthoethyl silicate (TEOS) to impregnate zinc-modified HZSM-5 zeolite molecular sieve at room temperature for 24 hours, and pour out the upper liquid for 120 ℃ drying, 550 ℃ air roasting for 6 hours to obtain the HZSM-5 catalyst jo...
Embodiment 2
[0038] Embodiment 2 fixed-bed catalyst preparation
[0039] Get 20g of the HZSM-5 zeolite molecular sieve prepared in step 1) of Example 1 for tablet molding, obtain a 40-60 mesh sample after crushing and screening, use molybdenum nitrate [Mo(NO 3 ) 3 ] The solution was impregnated with HZSM-5 molecular sieve at room temperature for 4 hours, and after drying at 120°C, it was roasted in air at 550°C for 6 hours; the HZSM-5 zeolite molecular sieve after molybdenum modification was impregnated with orthoethyl silicate (TEOS) at room temperature for 24 hours, and poured out After the upper liquid was dried at 120°C and baked in air at 550°C for 6 hours, a HZSM-5 catalyst jointly modified by molybdenum and silanization was obtained. The Mo content in the catalyst was about 3wt%, and the catalyst was named MTA-07.
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