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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

Inactive Publication Date: 2015-01-21
HEILONGJIANG UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention solves the problem that existing catalysts cannot have high activity and high 2,6-DMN selectivity at the same time, and the catalyst is easily deactivated, and a kind of SAPO-11 molecular sieve is provided to prepare 2,6-dimethylnaphthalene Methods

Method used

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  • Preparation method of 2,6-DiMethylnaphthalene (DMN) by using SAPO-11 molecular sieve
  • Preparation method of 2,6-DiMethylnaphthalene (DMN) by using SAPO-11 molecular sieve
  • Preparation method of 2,6-DiMethylnaphthalene (DMN) by using SAPO-11 molecular sieve

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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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Abstract

The invention relates to a preparation method of the 2,6-DMN, in particular to a preparation method of the 2,6-DMN by using a SAPO-11 molecular sieve. The preparation method mainly solves the problems that catalysts cannot be provided with high activity and 2,6-DMN selectivity simultaneously, and the catalysts are easy to inactivate. The method includes activating the SAPO-11 molecular sieve synthesized by microwave radiation and heating, mixing naphthalene and alkylation reagents with a solvent according to a molar ratio of 1:(2-4):(6-12), and performing alkylation reaction to obtain the 2,6-DMN at a temperature of 350 DEG C to 450 DEG C, at a pressure of 2 MPa to 5 MPa, at a quality airspeed of 0.5-2h-1 and at a carrier gas flow rate of 20-60 mL / min. According to the preparation method, the synthesized SAPO-11 molecular sieve can shorten the crystallization time greatly, and has high catalytic activity to the alkylation reaction of the naphthalene and high selectivity and good anti-carbon deposition competence to the 2,6-DMN.

Description

technical field [0001] The invention relates to a method for preparing 2,6-dimethylnaphthalene. Background technique [0002] In 1973, Japan's Teijin Corporation first developed a new type of polyester material polyethylene naphthalate, referred to as PEN. Because of its heat resistance, corrosion resistance, good dimensional stability and strong mechanical properties, it is widely used in many fields such as aerospace, atomic energy materials and electronic components. 2,6-Dimethylnaphthalene is an important monomer raw material for the preparation of PEN, but the complex production process and high production cost of 2,6-DMN seriously restrict the large-scale entry of PEN into the market. At present, my country's 2,6-DMN is basically dependent on imports, so developing a simple 2,6-DMN production method and reducing its production cost are of great significance to promote the development of my country's PEN polyester materials. [0003] At present, the synthesis of 2,6-D...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C15/24C07C2/88B01J29/85
Inventor 吴伟刘敏武光赵爱娟
Owner HEILONGJIANG UNIV
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