Photocatalytic method for preparing 3,4-dichloroaniline

A technology of dichloroaniline and photocatalysis, applied in chemical instruments and methods, preparation of amino compounds, preparation of organic compounds, etc., can solve the high cost of alkali sulfide reduction method, large amount of three wastes in iron powder reduction method, and corrosion resistance requirements Advanced problems, to achieve the effect of low unit product cost, good environmental benefits, and high selectivity

Active Publication Date: 2013-12-18
德兴市德邦化工有限公司
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

The iron powder reduction method produces a large amount of three wastes and serious pollution; the catalytic hydrogenation reduction method requires high temperature and high pressure equipment, high requirements on the pressure resistance and corrosion resistance of the equipment, and there are many unsafe factors in operation; the alkali sulfide reduction method is high in cost, Low yield, large amount of three wastes and serious pollution

Method used

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  • Photocatalytic method for preparing 3,4-dichloroaniline
  • Photocatalytic method for preparing 3,4-dichloroaniline
  • Photocatalytic method for preparing 3,4-dichloroaniline

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preparation example Construction

[0020] The photocatalytic method for preparing 3,4-dichloroaniline of the present invention is illustrated in conjunction with examples.

[0021] The photocatalytic method for preparing 3,4-dichloroaniline of the present invention is based on the following inventive idea: when the semiconductor used as a catalyst is irradiated with light having a wavelength smaller than the forbidden band width of the semiconductor, the electrons on the valence band of the semiconductor are excited to transition to the conduction band , creating holes in the valence band. Conduction band electrons have a strong reduction ability, which can reduce the electron acceptor adsorbed on the semiconductor surface, such as conduction band electrons, which can reduce the aromatic nitro substances adsorbed on the semiconductor surface. TiO 2 The 3,4-dichloronitrobenzene on the surface of the catalyst is reduced to 3,4-dichloroaniline.

[0022] Preparation of 3 of the present invention, the reaction rou...

Embodiment 1

[0027] Example 1 Weigh 0.5g of 3,4-dichloronitrobenzene, 0.3g of solid powdery porous TiO with an average particle diameter of 10-15nm 2 Catalyst and 0.25g surfactant subwet159, put it into a photocatalytic reactor with a magnetic rotor, add 50mL of anhydrous methanol solution, that is, the concentration of 3,4-dichloronitrobenzene is 10g / L, the concentration of the catalyst The concentration is 6g / L, the concentration of the surfactant subwet159 is 5g / L, start the magnetic stirrer 2, in an inert gas nitrogen atmosphere, under the stirring of the magnetic stirrer 2, first perform dark adsorption for 10min, and then turn on 250W , radiation intensity 4120μW / cm 2 UV lamp, after irradiating for 20h, the reaction is terminated, and the solid powdery TiO is filtered out. 2 Catalyst, the resulting filtrate was analyzed by Aglient1100 high performance liquid chromatography (HPLC), and the yield of 3,4-dichloroaniline was 71.30%. The total time of the whole reaction ultraviolet lamp...

Embodiment 2

[0028] In Example 2, except that isopropanol was used instead of anhydrous methanol as a solvent, other reaction conditions were the same as in Example 1. As a result, the yield of 3,4-dichloroaniline was 34.20%.

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Abstract

The invention provides a method for preparing 3,4-dichloroaniline by photocatalytic reduction, which comprises the following steps: selecting a photocatalytic reactor which is required to have a gas inlet, a gas outlet and a cooling water feeding and discharging system and of which the wall is required to allow ultraviolet light with a wavelength of less than 387.5 nanometers to transmit, filling an organic solvent into the photocatalytic reactor and dissolving 3,4-dichloronitrobenzene in the organic solvent; adding solid powdered TiO2 into the 3,4-dichloronitrobenzene containing solvent as a catalyst, and also adding a surfactant subwet159 as an additive; in an atmosphere of inert nitrogen, performing the dark absorption of the 3,4-dichloronitrobenzene and solid powdered TiO2, which are dissolved in the organic solvent, for 10 minutes; and in the atmosphere of inert nitrogen, irradiating the transparent reactor containing the 3,4-dichloronitrobenzene and solid powdered TiO2 to obtain 3,4-dichloroaniline. The preparation method provided by the invention is green, environment-friendly, safe and nontoxic, the product yield of the preparation method is high, and the cost of the preparation method is low.

Description

technical field [0001] The invention relates to an organic synthesis process method, in particular to a photocatalytic method for preparing 3,4-dichloroaniline. Background technique [0002] 3,4-Dichloroaniline (3,4-Dichloroaniline) is an important intermediate of various pesticides, medicines, dyes, pigments, and fine chemical products, and is also a biologically active intermediate with a wide range of uses. The large demand for raw materials in my country's herbicide market has laid the foundation for the widespread use of 3,4-dichloroaniline, so the development of this product has a good market prospect. [0003] The commonly used synthesis method of 3,4-dichloroaniline is the reduction method of 3,4-dichloronitrobenzene, which can generally be reduced by iron powder, catalytic hydrogenation reduction, and alkali sulfide reduction. The iron powder reduction method produces a large amount of three wastes and serious pollution; the catalytic hydrogenation reduction method...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C211/52C07C209/36
Inventor 费学宁刘玉茹曹凌云陈佳俊夏媛
Owner 德兴市德邦化工有限公司
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