Method for preparing 1-naphthol by using pigment green B catalysis

A technology for catalytic preparation and pigment green, which is applied in the direction of chemical instruments and methods, preparation of organic compounds, physical/chemical process catalysts, etc., can solve the problems of large process pollution, poor safety, complex process, etc., and achieve simple operation and low pollution , Ease of industrial production

Active Publication Date: 2010-06-09
南通新丰威机械科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This technology overcomes the shortcomings of the previous process, such as heavy pollution, long process, complex process

Method used

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  • Method for preparing 1-naphthol by using pigment green B catalysis

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Effect test

Embodiment 1

[0015] In a 100 mL four-necked flask equipped with a thermometer and a stirring device, 0.26 g of naphthalene, 18 g of acetonitrile, and 0.01 g of Pigment Green B catalyst were added. Heat up to 75°C, add dropwise 30% H over 0.5h 2 o 2 2g, keep warm for 5h. Filter, take the filtrate and measure the content of naphthalene and 1-naphthol with gas chromatography external standard method. The conversion rate of naphthalene was 30.2%, and the yield of 1-naphthol was 18.3%.

Embodiment 2

[0017] In a 100 mL four-necked flask equipped with a thermometer and a stirring device, 0.256 g of naphthalene, 30 g of acetonitrile, and 0.03 g of Pigment Green B catalyst were added. Heating to 45°C, adding 30% H 2 o 2 5g, with 2h, heat preservation reaction 18h. After cooling, the catalyst was filtered off, and the filtrate was measured by gas chromatography external standard method. The conversion rate of naphthalene was 40.3%, and the yield of 1-naphthol was 15.3%.

Embodiment 3

[0019] In a 100 mL four-necked flask equipped with a thermometer and a stirring device, add 0.256 g of naphthalene, 13 g of acetonitrile, and 0.005 g of Pigment Green B catalyst. Heat up to 55°C, add 30% H 2 o 2 1.5g, use time 0.5h, heat preservation reaction 15h. After cooling, the catalyst was filtered off, and the filtrate was measured by gas chromatography external standard method. The conversion rate of naphthalene was 38.7%, and the yield of 1-naphthol was 17.2%.

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Abstract

The invention provides a method for preparing 1-naphthol by using pigment green B catalysis. The method comprises the following steps: mixing naphthalene, acetonitrile solvent and pigment green B catalyst, heating the mixture to between 45 and 75 DEG C, dripping H2O2 into the mixture for 0.5 to 3 hours, and reacting the mixture for 4 to 18 hours to generate the 1-naphthol; and filtering the solution to remove the catalyst after cooling, and reclaiming the solvent to obtain a 1-naphthol product, wherein the mass ratio of the naphthalene to the H2O2 to the acetonitrile to the pigment green B is 0.26: 1.5-5: 13-30: 0.005-0.03. Compared with the prior process, the method has the advantages of cheap and easily obtained catalyst, little pollution, short line, simple operation, and easiness for industrial production.

Description

technical field [0001] The invention belongs to the preparation method of hydroxyl-substituted aromatic ring compounds, and particularly proposes a method for preparing 1-naphthol by catalyzing pigment green B. Background technique [0002] 1-Naphthol is an important intermediate widely used in organic synthesis of fine chemicals, and there are three main production methods for 1-Naphthol. Sulfonated alkali fusion method: naphthalene is sulfonated with concentrated sulfuric acid, hydrolyzed, neutralized, alkali fused, acidified, and refined. This process has defects such as complex process, long process, serious equipment corrosion, more three wastes, and large environmental pollution. Naphthol-acetone co-production method: using naphthalene and propylene as raw materials, catalyzed isopropylation to produce 1-isopropylnaphthalene, then oxidized to produce 1-isopropylnaphthalene peroxide, and finally acid decomposition to obtain 1- naphthol and acetone. The production pro...

Claims

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Application Information

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IPC IPC(8): C07C39/14C07C37/60B01J31/22
Inventor 张天永杨秋生史慧贤
Owner 南通新丰威机械科技有限公司
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