Preparation method of 2,6-DiMethylnaphthalene (DMN) by using SAPO-11 molecular sieve
A technology of SAPO-11 and dimethylnaphthalene, applied in molecular sieve catalysts, chemical instruments and methods, condensation between hydrocarbons and non-hydrocarbons, etc., can solve the problems that catalysts cannot have high activity at the same time, catalysts are easy to deactivate, etc. , to facilitate large-scale production, good catalytic stability, and reduce synthesis costs
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specific Embodiment approach 1
[0022] Specific embodiment one: the method for preparing 2,6-dimethylnaphthalene by a kind of SAPO-11 molecular sieve of the present embodiment is to carry out according to the following steps: one, SAPO-11 molecular sieve is put into the catalyst bed layer of fixed bed reactor , activate at 500°C~600°C for 2h; 2. Mix naphthalene, alkylating agent and solvent evenly to obtain the raw material liquid, and use a metering pump to continuously inject the raw material liquid into the catalyst bed of the fixed-bed reactor in step 1 , and at a temperature of 350°C~450°C, a pressure of 2~5MPa, and a mass space velocity of 0.5~2h -1 , under the condition that the carrier gas flow rate is 20~60mL / min, carry out the alkylation reaction for 1~24h to obtain 2,6-dimethylnaphthalene; wherein, the molar ratio of naphthalene to alkylation reagent is 1:2~ 4. The molar ratio of naphthalene to solvent is 1:6~12.
[0023] This embodiment includes the following beneficial effects:
[0024] 1. The...
specific Embodiment approach 2
[0029] Specific embodiment two: the difference between this embodiment and specific embodiment one is that the prepared SAPO-11 molecular sieve described in step 1 is synthesized in the water system by means of microwave heating, and the specific steps are as follows: 2 o 3 :SiO2 2 :P 2 o 5 :DPA:H 2 The O molar ratio is 1:0.2~1.2:1:1:40 and the ratio is evenly stirred to obtain a gel. Put the polytetrafluoroethylene lining with the gel into the ceramic outer lining, and then put it into a microwave oven. With a power of 600W and a temperature of 160°C~180°C, crystallize for 0.5~4h to obtain a solid-liquid mixture; then wash the solid phase obtained by filtration and dry it at a temperature of 110°C for 12h. Then calcined at 650°C for 7 hours to obtain SAPO-11 molecular sieve. Others are the same as in the first embodiment.
specific Embodiment approach 3
[0030] Specific embodiment three: the difference between this embodiment and specific embodiment one or two is that the SAPO-11 molecular sieve described in step 1 is synthesized in alcohol-water system by traditional electric heating method, and the specific steps are as follows: press Al 2 o 3 :SiO2 2 :P 2 o 5 :DPA:C 2 h 5 OH:H 2 O molar ratio is 1:0.2~1.2::1:1:10:(10~100) Stir evenly to get gel, put the polytetrafluoroethylene lining with gel into the stainless steel outer lining, Then put it into an oven, and crystallize for 12-48 hours at a temperature of 160°C~180°C to obtain a solid-liquid mixture; then wash the solid phase obtained by filtration, and dry it at a temperature of 110°C 12h, and then calcined at 650°C for 7h to obtain SAPO-11 molecular sieve. Others are the same as in the first or second embodiment.
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