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A kind of naphthalene liquid-phase oxidation catalyst, its preparation method and application

A liquid-phase oxidation and catalyst technology, which is applied in the preparation of oxidized quinones, physical/chemical process catalysts, molecular sieve catalysts, etc., can solve the problems of chromium-containing wastewater, low selectivity of 1,4-naphthoquinone, environmental pollution, etc., and achieve improvement conversion rate effect

Active Publication Date: 2020-10-09
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

[0010] For a long time, the liquid-phase oxidation of naphthalene requires the participation of heavy metal-based catalysts such as stoichiometric chromium oxide, so a large amount of industrial wastewater containing heavy metals is produced in industrial production. The treatment process of these wastewater is difficult and complicated, which will cause very serious pollution to the environment.
Since the 1970s, researchers have tried to develop new catalysts to solve the problem of chromium-containing wastewater. Although this type of research has achieved some visible results in pollution, the conversion rate of naphthalene and 1,4- Naphthoquinones are less selective
[0011] In general, the naphthalene-based liquid phase oxidation method avoids the use of chromium salts and other environmentally polluting catalysts, but in order to improve the yield and selectivity of the target product, it is still unavoidable to use environmentally unfriendly catalysts or oxidants

Method used

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  • A kind of naphthalene liquid-phase oxidation catalyst, its preparation method and application
  • A kind of naphthalene liquid-phase oxidation catalyst, its preparation method and application
  • A kind of naphthalene liquid-phase oxidation catalyst, its preparation method and application

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Embodiment 1

[0045] After mixing the TEAOH solution with 10 g of deionized water, add hydrofluoric acid, stir the mixture evenly with a magnetic stirring bar, and then add ferric nitrate, ethyl orthosilicate and aluminum sulfate. Stir the mixture for 4h under the condition of constant temperature water bath at 60°C to obtain a composition ratio of 0.5TEAOH:1.0SiO 2 : 0.005Al 2 o 3 : 0.01Fe 2 o 3 :0.65HF:5H 2 O solution. The solution was transferred to a stainless steel synthesis kettle equipped with a polytetrafluoroethylene liner, and placed in an oven at 110° C. for 10 days for crystallization. After the crystallization, the product in the kettle was suction-filtered, dried, and calcined in a muffle furnace at 550° C. for 5 hours to obtain a Beta molecular sieve catalyst containing transition metal oxide particles. The XRD spectrum of the Beta molecular sieve catalyst prepared in this embodiment is shown in figure 1 The spectrum of No. 1 in the electron microscope photo is shown i...

Embodiment 2

[0048] After mixing the TEAOH solution with 10 g of deionized water, hydrofluoric acid was added. After the mixture was stirred evenly with a magnetic stirring bar, ferric nitrate, tetraethyl orthosilicate and aluminum sulfate were added. Stir the mixture for 4h under the condition of constant temperature water bath at 60°C to obtain a composition ratio of 0.5TEAOH:1.0SiO 2 : 0.002Al 2 o 3 : 0.05Fe 2 o 3 :0.65HF:5H 2 O solution. The solution was transferred to a stainless steel synthesis kettle equipped with a polytetrafluoroethylene liner, and placed in an oven at 120° C. for 7 days for crystallization. After the crystallization, the product in the kettle was suction-filtered, dried, and calcined in a muffle furnace at 550° C. for 5 hours to obtain a Beta molecular sieve catalyst containing transition metal oxide particles. The XRD spectrum of the Beta molecular sieve catalyst prepared in this embodiment is shown in figure 1 The spectrum of No. 2 in the electron micro...

Embodiment 3

[0051] After mixing the TEAOH solution with 10 g of deionized water, add hydrofluoric acid, stir the mixture evenly with a magnetic stirring bar, and then add ferric nitrate, ethyl orthosilicate and aluminum sulfate. Stir the mixture for 4h under the condition of constant temperature water bath at 60°C to obtain a composition ratio of 0.5TEAOH:1.0SiO 2 : 0.003Al 2 o 3 : 0.01Fe 2 o 3 :0.65HF:5H 2 O solution. The solution was transferred to a stainless steel synthesis kettle equipped with a polytetrafluoroethylene liner, and placed in an oven at 140° C. for 7 days for crystallization. After the crystallization, the product in the kettle was suction-filtered, dried, and calcined in a muffle furnace at 550° C. for 5 hours to obtain a Beta molecular sieve catalyst containing transition metal oxide particles. The XRD spectrum of the Beta molecular sieve catalyst prepared in this embodiment is shown in figure 1 The spectrum of No. 3 in the electron microscope photo is shown in...

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Abstract

The present application discloses a naphthalene liquid-phase oxidation catalyst, the catalyst includes a Beta molecular sieve containing transition metal oxide particles, and a preparation method thereof, the preparation method comprising: a) gel preparation: structure-directing agent, aluminum source, The silicon source, transition metal precursor, fluoride ion source and water are mixed and stirred to form a gel. The molar ratio of each component in the gel is: SiO 2 / Al 2 o 3 =10~1000, M / Si=0.01~2, wherein M is a transition metal; b) crystallization: transfer the gel obtained in step a) into a synthesis kettle, and crystallize at 110~220°C for 0.5~10 sky. The application also discloses the application of the above-mentioned catalyst in catalyzing the oxidation reaction of naphthalene in an organic solvent, which effectively improves the conversion rate of naphthalene and the selectivity of the target product. The reaction condition is mild, the operation is simple, the catalyst is easy to prepare, is pollution-free and can be recycled.

Description

technical field [0001] The invention relates to a naphthalene liquid-phase oxidation catalyst, a preparation method and an application thereof, and belongs to the field of chemistry and chemical engineering. Background technique [0002] Naphthalene is the most important fused-ring aromatic hydrocarbon in industry, and oxygen-containing organic chemicals synthesized by oxidation reactions occupy an important position in petrochemical products. Naphthalene can be converted into oxygen-containing compounds such as naphthol, 1,4-naphthoquinone, and phthalic anhydride by oxidation reaction. These oxygen-containing compounds are important organic chemical raw materials and important intermediates and raw materials for organic synthesis. Therefore, The catalytic oxidation of naphthalene is one of the important ways to produce various high-value chemicals from naphthalene. [0003] In the presence of a catalyst, naphthalene can be first oxidized to naphthol, then deeply oxidized t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/76C07C46/06C07C50/12C07D307/89
Inventor 许磊张晓敏赵晓炜陈磊
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI