A kind of production method of 1,4-naphthoquinone, adopted catalyst and its application

A production method and catalyst technology, which is applied in the field of fine chemical synthesis, can solve the problems of low naphthalene conversion rate, high yield, and low cost, and achieve the effects of simple post-treatment process, low difficulty in operation control, and reduced cost

Active Publication Date: 2019-07-30
上海谷雨医药科技有限公司
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Problems solved by technology

[0006] The purpose of the present invention is to solve defects such as the low conversion rate of naphthalene and the low production yield of 1,4 naphthoquinone in the prior art, and the three wastes are easy to produce, and provide a fixed-bed reactor catalytic oxidation system for vaporizing naphthalene below the boiling point temperature. , the production method of 4-naphthoquinone, on the premise that the naphthalene air ratio is 0.02~0.04, using the principle of variable partial pressure of the mixture gas vapor, the liquid naphthalene below the boiling point temperature is directly mixed with hot air, vaporized and catalyzed to produce 1,4-naphthoquinone The advanced production method (including naphthalene feeding method, first reactor, catalyst, water capture, second reactor waste gas treatment and post-treatment process), is suitable for industrial production, with high yield, low cost and environmental friendliness

Method used

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  • A kind of production method of 1,4-naphthoquinone, adopted catalyst and its application
  • A kind of production method of 1,4-naphthoquinone, adopted catalyst and its application
  • A kind of production method of 1,4-naphthoquinone, adopted catalyst and its application

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preparation example Construction

[0039] The preparation method of the first catalyst is to adopt 11~15% vanadium pentoxide, 20-30% potassium sulfate, 10~20% auxiliary agent (potassium pyrosulfate or potassium bisulfate or a mixture of the two) and 45% ~50% carrier (SiO 2 、Al 2 o 3 , SiO 2 -Al 2 o 3 、Al 2 o 3 -TiO 2 Any one of them or any mixture of two or more) mixed, dried at 60~100°C in different periods (at least 2 times of drying), kept at 100~150°C for 2~4 hours to ensure that the dehydration is complete, and prepared into a diameter of ¢4~ 8mm, 4~8mm high ring-shaped catalyst, activated by calcination at 150~500°C and a small amount of air (providing oxygen to increase the valence state of vanadium) in different periods, and at 450~500°C for 4~6 hours to improve the thermal stability of the catalyst The first catalyst of the present invention is obtained by natural cooling.

[0040] In the first catalyst, the addition of potassium sulfate may lead to an increase or decrease in the yield of naph...

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Abstract

The invention discloses a production method of 1,4-naphthoquinone, the catalyst used and its application. The method comprises: step 1, mixing liquid naphthalene with hot air, heating and vaporizing to obtain a naphthalene-air mixture; step 2 , the naphthalene-air mixture is input into the first reactor, and the catalytic oxidation reaction is carried out at 350-400°C by the first catalyst, and the gas residence time is 1-1.5 seconds; The aqueous solution of the product; Step 4, performing solid-liquid separation treatment, collecting the solid mixture and the liquid mixture respectively; Step 5, separating the solid mixture through solvent extraction and recrystallization to obtain 1,4-naphthoquinone. The production method of the present invention has low difficulty in controlling the concentration of naphthalene, high safety, low degree of deep oxidation, and high yield. The conversion rate of naphthalene is 95.5~99.7%, and the yields of the main reaction products 1,4-naphthoquinone and phthalic anhydride are 44% respectively. ~58%, total reaction yield ≥ 102%, total product yield ≥ 95%, broad application prospects.

Description

technical field [0001] The invention belongs to the field of fine chemical synthesis, and relates to a production method for preparing 1,4-naphthoquinone by catalytic oxidation in a fixed-bed reactor, a catalyst used and an application thereof. Background technique [0002] As an important new fine chemical product and organic synthesis intermediate, 1,4 naphthoquinone is mainly used in the synthesis of pharmaceuticals, pesticides, spices, dyes and other intermediates; in the fields of national defense, aviation and aerospace, it can be used for carbon fiber ablation-resistant compounding Raw materials for materials; in the field of large-scale integrated circuit semiconductors, the introduction of naphthoquinones has a unique regulator effect on the performance of high-end heat-resistant novolak epoxy resins and carbon-carbon composite materials; in the field of synthesizing pharmaceutical compounds with biological activity, it is very important The role of antibiotics, ant...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C50/12C07C46/04B01J23/22C07D307/89
Inventor 沈秋钟沈静燕
Owner 上海谷雨医药科技有限公司
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