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Catalyst for preparing 1,4-naphthoquinone through liquid-phase oxidation of naphthalene as well as preparation method and application of catalyst

A catalyst and catalyst quality technology, applied in the direction of catalyst activation/preparation, oxidized quinone preparation, physical/chemical process catalyst, etc., can solve the problems of difficult and complicated treatment process, difficult separation of naphthoquinone, strong corrosion, etc., and achieve good industrial application foreground effect

Active Publication Date: 2019-06-14
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

In addition, glacial acetic acid is often used as a solvent in the reaction system, which is highly corrosive and requires high material requirements for equipment.
The liquid-phase oxidation method is adopted, the reaction conditions are mild, and the selectivity to naphthoquinone is good. The main disadvantage of the current liquid-phase oxidation method is that in this reaction system, heavy metal-based catalysts such as stoichiometric chromium oxide are required to participate. Therefore, in industrial production A large amount of industrial wastewater containing heavy metals is produced. The treatment process of these wastewater is difficult and complicated, which will cause very serious pollution to the environment. great difficulty

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Weigh 10g of HY molecular sieve carrier, at room temperature 0.5mol / L Fe(NO 3 ) 3 9H 2 Immerse in O aqueous solution for 0.5h, and the volume of the solution is measured according to the mass content of iron oxide on the molecular sieve being 10%. Dry at room temperature, after drying at 120°C for 10h, place in a muffle furnace and raise the temperature to 500°C, and roast in air for 4h to obtain Fe 2 o 3 / HY. Weigh a certain amount of Fe 2 o 3 / HY, after excessive immersion in diluted concentrated sulfuric acid solution for 12h, dried and roasted to obtain concentrated sulfuric acid modified Fe 2 o 3 / HY, denoted as Catalyst 1.

[0029] Catalyst 1 prepared above was used in the liquid-phase oxidation of naphthalene to prepare 1,4-naphthoquinone. The specific implementation process is: in a 250mL round bottom flask, add 0.8g of naphthalene, 25mL of acetic acid, and 0.2g of catalyst. Heat up to 60°C, add 2 mL of 30% hydrogen peroxide dropwise, and react at cons...

Embodiment 2

[0031] Weigh 10g of HY molecular sieve carrier, at room temperature 0.5mol / L Fe(NO 3 ) 3 9H 2 Immerse in O aqueous solution for 0.5h, and the volume of the solution is measured according to the mass content of iron oxide on the molecular sieve being 15%. Dry at room temperature, after drying at 120°C for 10h, place in a muffle furnace and raise the temperature to 500°C, and roast in air for 4h to obtain Fe 2 o 3 / HY. Weigh a certain amount of Fe 2 o 3 / HY, after excessive immersion in diluted concentrated sulfuric acid solution for 12h, dried and roasted to obtain concentrated sulfuric acid modified Fe 2 o 3 / HY, denoted as Catalyst 2.

[0032] Catalyst 2 prepared above was used in the liquid-phase oxidation of naphthalene to prepare 1,4-naphthoquinone. The specific implementation process is: in a 250mL round bottom flask, add 0.8g of naphthalene, 25mL of acetic acid, and 0.2g of catalyst. Heat up to 60°C, add 2 mL of 30% hydrogen peroxide dropwise, and react at cons...

Embodiment 3

[0034] Weigh 10g HY molecular sieve carrier, at room temperature 0.5mol / L Fe(NO 3 ) 3 9H 2 Immerse in the O aqueous solution for 0.5h, and measure the volume of the solution according to the mass content of the iron oxide on the molecular sieve being 20%. Dry at room temperature, after drying at 120°C for 10h, place in a muffle furnace and raise the temperature to 500°C, and roast in air for 4h to obtain Fe 2 o 3 / HY. Weigh a certain amount of Fe 2 o 3 / HY, after excessive immersion in diluted concentrated sulfuric acid solution for 12h, dried and roasted to obtain concentrated sulfuric acid modified Fe 2 o 3 / HY, recorded as catalyst 3.

[0035] Catalyst 3 prepared above was used in the liquid-phase oxidation of naphthalene to prepare 1,4-naphthoquinone. The specific implementation process is: in a 250mL round bottom flask, add 0.8g of naphthalene, 25mL of acetic acid, and 0.2g of catalyst. Heat up to 60°C, add 2 mL of 30% hydrogen peroxide dropwise, and react at co...

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PUM

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Abstract

The invention discloses a catalyst. The catalyst comprises a carrier and an active component, wherein the carrier is a molecular sieve; the active component is a transition metal oxide modified by strong acid; the mass percentage content of the active component is 0.5%-50% based on the mass of the catalyst. The catalyst is used for preparing 1,4-naphthoquinone by liquid-phase oxidation of naphthalene. The invention also discloses a preparation method of the catalyst and application of the catalyst to preparation of 1,4-naphthoquinone by liquid-phase oxidation of naphthalene, the conversion rate of naphthalene and the selectivity of 1,4-naphthoquinone are effectively improved, the reaction conditions are mild, the operation is simple, and the catalyst is easy to prepare, pollution-free andrecyclable.

Description

technical field [0001] The invention relates to a catalyst for preparing 1,4-naphthoquinone by liquid-phase oxidation of naphthalene, a preparation method and application thereof, and belongs to the field of chemical engineering. Background technique [0002] 1,4-Naphthoquinone is an important raw material in fine chemicals, an intermediate of medicines, dyes, spices, pesticides, plasticizers, etc., and a polymerization regulator for synthetic rubber and resins. raw material. In addition, 1,4-naphthoquinone has excellent ultraviolet absorption properties and visible and near-infrared reflection functions, making it of great significance in textile functional dyes. [0003] Synthesis of 1,4-naphthoquinone from naphthalene is mainly carried out by catalytic oxidation. According to different oxidants, it can be divided into gas phase oxidation method and liquid phase oxidation method. Gas-phase catalytic oxidation of naphthalene produces 1,4-naphthoquinone with low cost. Exc...

Claims

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Application Information

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IPC IPC(8): B01J29/14B01J29/24B01J29/46B01J37/02B01J37/08C07C46/02C07C50/12
CPCY02P20/584
Inventor 张晓敏许磊赵晓炜陈磊
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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