Preparation method of coronene compound

A compound and benzene technology, applied in the field of organic chemistry, can solve problems such as complicated operation, unsuitable for large-scale production, expensive raw materials, etc., and achieve the effect of simple preparation process, suitable for large-scale production, and easy-to-obtain raw materials

Active Publication Date: 2020-10-16
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0013] In order to solve the problems of expensive raw materials, complex operation and unsuitability for large-scale produc

Method used

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  • Preparation method of coronene compound
  • Preparation method of coronene compound
  • Preparation method of coronene compound

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Experimental program
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Effect test

Embodiment 1

[0053] Embodiment 1: the synthesis of DNL-6 molecular sieve catalyst

[0054] Initial gel molar composition ratio 2N-methylbutylamine (as organic structure directing agent): 0.3SiO 2 : 0.4P 2 o 5 : 0.5Al 2 o 3 : 50H 2 O: 0.2 (20%) cetyltrimethylammonium bromide (as seed crystals) Mix measured amounts of organic structure directing agent, silica sol, phosphoric acid, aluminum isopropoxide, deionized water, and seed crystals in a beaker , fully stirred to form a gel, then loaded into a stainless steel autoclave lined with polytetrafluoroethylene, and rotated and crystallized at a constant temperature of 200°C at a speed of 75r / min for 24h. After crystallization, use a centrifuge at 3000 rpm for 3 minutes, wash the separated solid product with deionized water to neutrality, and dry it overnight in air at 120°C. The results of XRD analysis are as follows: figure 1 shown. From the results in Figure 1, it can be seen that the synthesized product is the raw powder of DNL-6 mol...

Embodiment 2

[0055] Embodiment 2: the synthesis of SAPO-42 molecular sieve catalyst

[0056] Based on the initial gel molar composition ratio of 1.85 2,2-dimethyl-2,3-dihydro-1H-phenyl[de]isoquinoline (as an organic structure-directing agent): 0.296SiO 2 : 0.85P 2 o 5 : 1Al 2 o 3 : 60H 2 O Mix the metered organic structure-directing agent, silica sol, phosphoric acid, pseudoboehmite and deionized water in a beaker, stir well to form a gel, and then put it into a stainless steel autoclave lined with polytetrafluoroethylene. Constant temperature crystallization at 175℃ for 120h. After crystallization, use a centrifuge at 3000 rpm for 3 minutes, wash the separated solid product with deionized water until it is neutral, and dry it overnight in air at 100°C. The results of XRD analysis are as follows: figure 2 shown. from figure 2 It can be seen from the results that the synthesized product is SAPO-42 molecular sieve raw powder, and the raw powder was calcined at 600°C for 5 hours to ...

Embodiment 3

[0057] Embodiment 3: the synthesis of ZK-21 molecular sieve catalyst

[0058] 6.1g sodium aluminate (1.11Na 2 O·Al 2 o 3 3.5H 2 0) mix with a small amount of deionized water, add 23g concentration of 85% phosphoric acid, be made into 220ml aqueous solution, add 10.3g sodium metasilicate pentahydrate and 80ml deionized water while stirring, the gel obtained after fully stirring, then Put it into a stainless steel autoclave lined with polytetrafluoroethylene, and crystallize at a constant temperature of 100°C for 69h. After crystallization, use a centrifuge at 3000 rpm for 3 minutes, wash the separated solid product with deionized water until it is neutral, and dry it overnight in air at 100°C. The results of XRD analysis are as follows: image 3 shown. from image 3 It can be seen from the results that the synthesized product is the original powder of ZK-21 molecular sieve, and the original powder was calcined at 600°C for 5 hours to obtain ZK-21 molecular sieve, which is...

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Abstract

The invention discloses a preparation method of a coronene compound. The method comprises the following steps of: (1) pretreating a catalyst containing an SAPO molecular sieve; and (2) filling a reactor with a raw material containing non-cyclic olefin, and carrying out contact reaction with the catalyst pretreated in the step (1) to obtain the coronene compound, wherein the pretreatment refers toactivation of the catalyst. The method does not need expensive raw materials or complex operation, and is suitable for large-scale production.

Description

technical field [0001] The application relates to a method for preparing coronene compounds from acyclic olefins, which belongs to the field of organic chemistry. Background technique [0002] Because it can be used as a fluorescent material, the research of coronene and its derivatives has always attracted people's attention. In recent years, it has been found that coronene and its derivatives are excellent organic fluorescent materials for making UV-CCD. The maximum emission wavelength of coronene is 520nm, the maximum absorption wavelength is 255nm, and it also has high quantum efficiency. Coronene is a very ideal UV-CCD material. [0003] At present, the preparation methods about coronene mainly include the following three kinds: [0004] The first is the preparation method disclosed by Joost T.M.van Dijk in J.Org.Chem.1996,61,1136-1139, and the chemical reaction equation of the method is as follows: [0005] [0006] In this method, the temperature needs to be lo...

Claims

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Application Information

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IPC IPC(8): C07C2/42C07C15/20C09K11/06B01J29/85B01J37/08C01B37/08C01B39/54
CPCB01J29/85B01J37/0018B01J37/08C01B37/08C01B39/54C07C2/42C09K11/06C07C2603/54C07C15/20
Inventor 王男郅玉春魏迎旭刘中民
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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