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Method for preparing coronene compound by using molecular sieve catalyst

A molecular sieve and catalyst technology, applied in the field of chemical preparation, can solve the problems of unstable intermediate products and inconvenient industrialization, and achieve the effect of being suitable for large-scale production, low cost, 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

AI Technical Summary

Problems solved by technology

Although this method overcomes the disadvantage of expensive raw material perylene, the process involves multiple anhydrous, oxygen-free and low-temperature operations, and the intermediate product is extremely unstable, which brings inconvenience to industrialization

Method used

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  • Method for preparing coronene compound by using molecular sieve catalyst
  • Method for preparing coronene compound by using molecular sieve catalyst
  • Method for preparing coronene compound by using molecular sieve catalyst

Examples

Experimental program
Comparison scheme
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 figure 1 It can be seen from the results that the synthesized product is the raw powder of DNL-6 m...

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 the original powder of SAPO-42 molecular sieve, and the original powder was calcined at 600°...

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 ZK-21 molecular sieve raw powder, and the raw powder is calcined at 600°C for 5 hours to obtain ZK-21 molecular sieve, which is designated as cat...

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Abstract

The invention relates to a method for preparing a coronene compound by using a molecular sieve catalyst. Specifically, the method disclosed by the invention comprises the following steps of: (1) activating a molecular sieve catalyst; wherein the molecular sieve catalyst comprises an SAPO molecular sieve catalyst; and (2) carrying out contact reaction on a raw material and the molecular sieve catalyst activated in the step (1) in a reactor to obtain the coronene compound, wherein the raw material comprises an alcohol compound.

Description

technical field [0001] The invention relates to the preparation of chemicals, more specifically to a method for preparing coronene compounds from alcohol raw materials. Background technique [0002] Coronene is an organic fluorescent material. The maximum absorption wavelength of coronene is 255nm, the maximum emission wavelength is 520nm, and has high quantum efficiency. Therefore, coronene can be used in ultraviolet-charge coupled devices and radar. [0003] The preparation methods of coronene mainly include three kinds, namely, Wurtz-Fittig reaction synthesis method, Diels-Alder reaction synthesis method and anion reaction synthesis method. [0004] 1. Wurtz-Fittig reaction synthesis method: In 1951, Wilson Baker et al. started from 2,7-dimethylnaphthalene, and synthesized coronene under the action of Na and palladium black reduction. Its synthetic route is shown below. In this preparation method, the final yield of coronene is 4%, the reaction time is long, the condit...

Claims

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Application Information

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IPC IPC(8): C07C1/20C07C15/20
CPCC07C1/20C07C2529/84C07C2529/85C07C2603/54C07C15/20
Inventor 王男郅玉春魏迎旭刘中民桑石云
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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