Method for preparing 2,6-dimethylnaphthalene by catalyzing naphthalene alkylation reaction with CoAPO-11 molecular sieve

A technology for catalyzing naphthalene and alkylation reactions with molecular sieves, applied in molecular sieve catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of not being able to have high activity at the same time, and achieve good redox performance and high catalytic activity , Ease of mass production

Inactive Publication Date: 2012-10-24
HEILONGJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to solve the problem that existing catalysts cannot simultaneously have high activity and high 2,6-dimethylnaphthalene selectivity, and provide a CoAPO-11 molecular sieve to catalyze the alkylation reaction of naphthalene to prepare 2, 6-Dimethylnaphthalene method

Method used

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  • Method for preparing 2,6-dimethylnaphthalene by catalyzing naphthalene alkylation reaction with CoAPO-11 molecular sieve
  • Method for preparing 2,6-dimethylnaphthalene by catalyzing naphthalene alkylation reaction with CoAPO-11 molecular sieve
  • Method for preparing 2,6-dimethylnaphthalene by catalyzing naphthalene alkylation reaction with CoAPO-11 molecular sieve

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specific Embodiment approach 1

[0020] Specific embodiment one: a kind of CoAPO-11 molecular sieve of this embodiment catalyzes the alkylation reaction of naphthalene to prepare the method for 2,6-dimethylnaphthalene is carried out according to the following steps: one, CoAPO-11 molecular sieve is put into fixed The catalyst bed of the bed reactor is activated at 550°C for 2 hours; 2. Mix naphthalene, alkylating agent and solvent evenly to obtain the raw material liquid, and inject the raw material liquid into the catalyst of the fixed-bed reactor in step 1 with a metering pump Bed, 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 6~24h to obtain 2,6-dimethylnaphthalene; wherein, the molar ratio of naphthalene to alkylation reagent is 1:(2 ~4), the mol ratio of naphthalene and solvent is 1:(6~12).

[0021] The present embodiment adopts CoAPO-n molecular siev...

specific Embodiment approach 2

[0022] Specific embodiment two: the difference between this embodiment and specific embodiment one is that the CoAPO-11 molecular sieve described in step one is synthesized by electric heating method, and the specific steps are: pseudoboehmite, cobalt source, mass The percentage content is 85% phosphoric acid, di-n-propylamine and deionized water according to the mass ratio of 5.7: (0.2~0.6): 7.8:3.5: (22.1~26.2) after stirring evenly to make a gel, the gel will be installed Put the polytetrafluoroethylene lining of the glue into the stainless steel outer lining, and then put it in an oven at 180 ° C for 48 hours of crystallization to obtain a solid-liquid mixture; then wash the solid phase obtained by filtration, and put it in a temperature of Dry it in an oven at 110°C for 12h, then put it into a muffle furnace at 650°C and bake it for 7h to get CoAPO-11 molecular sieve; the cobalt source is Co(CH 3 COO) 2 4H 2 O or Co (NO 3 ) 2 ·6H 2 O. Others are the same as in the f...

specific Embodiment approach 3

[0023] Specific embodiment three: the difference between this embodiment and specific embodiment one or two is that the CoAPO-11 molecular sieve described in step one is synthesized by microwave radiation heating, and the specific steps are: pseudoboehmite, cobalt source , the mass percentage content is 85% phosphoric acid, di-n-propylamine, and deionized water according to the mass ratio of 5.7: (0.2~0.6):7.8:3.5: (22.1~26.2) and stir evenly to make a gel, then put the Put the polytetrafluoroethylene lining with gel into the ceramic outer lining, then put it into a microwave oven, and crystallize it for 3 hours at a power of 600W and a temperature of 160-180°C to obtain a solid-liquid mixture; then put After washing the solid phase obtained by filtration, put it into an oven with a temperature of 110° C. to dry for 12 hours, and then put it into a muffle furnace with a temperature of 650° C. and roast it for 7 hours to obtain CoAPO-11 molecular sieve; wherein the cobalt source...

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Abstract

The invention provides a method for preparing 2,6-dimethylnaphthalene by catalyzing naphthalene alkylation reaction with CoAPO-11 molecular sieve, relates to a method for preparing 2,6-dimethylnaphthalene, and is used for solving the problems that the traditional catalyst cannot simultaneously have high activity and high selectivity of 2,6-dimethylnaphthalene. The method comprises the steps of: activating the CoAPO-11 molecular sieve synthesized by an electrical heating method or microwave heating method for 2h, then mixing with naphthalene, alkylation reagents and solvent to prepare raw material liquid, and carrying out alkylation reaction to obtain 2,6-dimethylnaphthalene. According to the invention, the synthesized CoAPO-11 molecular sieve has higher catalytic reaction activity on naphthalene alkylation reaction, and higher selectivity of 2,6-dimethylnaphthalene; and the method is suitable for preparing 2,6-dimethylnaphthalene.

Description

technical field [0001] The invention relates to a method for preparing 2,6-dimethylnaphthalene. Background technique [0002] Polyethylene naphthalate (PEN) is one of the fastest-growing polymer materials in recent years. It is widely used due to its heat resistance, naphthalene corrosion, strong mechanical properties, and good radiation protection. 2,6-Dimethylnaphthalene (2,6-DMN) is an important monomer raw material for the preparation of PEN, but its large-scale entry into the market is severely restricted due to its complex production process and high cost. At present, the preparation of 2,6-DMN is mainly through one-step synthesis, but one-step preparation of 2,6-DMN can produce ten isomers, and the boiling points of these ten isomers are similar, so it is difficult to separate, especially The difference between the boiling point of 2,6-DMN and 2,7-DMN is only 0.3°C, so how to improve the selectivity of 2,6-DMN and the ratio of 2,6- / 2,7-DMN in DMN products is the key ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C15/24C07C2/88B01J29/83
Inventor 吴伟刘敏肖林飞张瑞
Owner HEILONGJIANG UNIV
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