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A method for sodium borohydride reduction of aromatic hydrocarbons or derivatives thereof

A technology of sodium borohydride and derivatives, which is applied in hydrogenation hydrocarbon production, chemical instruments and methods, carbon compound catalysts, etc., can solve problems such as cumbersome operation, safety hazards, and expensive platinum, and achieves avoiding safety hazards and controllable reduction Effect

Active Publication Date: 2020-02-21
河南郑大催化技术研究院有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the relatively stable benzene ring, the reduction of aromatic hydrocarbons and their derivatives by traditional hydrogenation catalysts is usually carried out at high temperature and high pressure. The yield of hexane is 70% (J. Wang, Q. Li, J. Yao, Applied Catalysis A: Genreal. 184 (1999) 181); Chinese patent CN1457923A discloses a method for preparing cyclohexane by hydrogenation of benzene, using Platinum catalyst, reaction temperature 150~400 ℃, hydrogen pressure 2~5 MPa, benzene conversion rate and cyclohexane selectivity above 90%, platinum is expensive, and the operation is cumbersome, and there are potential safety hazards; Chinese patent CN1298760 discloses a The method for preparing cyclohexane by hydrogenation of benzene, using amorphous Ni-B or Ni-M-B catalyst, the reaction temperature is above 100 °C, the hydrogen pressure is 4.0 MPa, and the stirring rate is 1000 r / min
[0004] However, the use of high-pressure reactors and hydrogen cylinders in the laboratory has serious safety hazards

Method used

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  • A method for sodium borohydride reduction of aromatic hydrocarbons or derivatives thereof
  • A method for sodium borohydride reduction of aromatic hydrocarbons or derivatives thereof
  • A method for sodium borohydride reduction of aromatic hydrocarbons or derivatives thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0026] A method for sodium borohydride reduction of benzene, the steps are as follows:

[0027] (1) Transfer 10 mL of benzene, 40 mL of deionized water, and catalyst NiB nano-amorphous alloy with a mass fraction of 0.5 wt% of benzene into a three-necked flask, and mechanically stir at 25 °C under normal pressure and control the stirring speed to 600 r / min;

[0028] (2) Weigh 3.20 g NaBH 4 and 0.40 g NaOH were dissolved in a beaker containing 60 mL of deionized water, and transferred to an Erlenmeyer flask for ice bath;

[0029] (3) Use a peristaltic pump to feed the NaBH stored in the ice bath in step (2) 4 The alkaline aqueous solution of the solution was added dropwise into the three-necked flask in step (1). After the dropwise addition was completed, the stirring was continued for 0.5 h, and the product was detected by gas chromatography mass spectrometry.

Embodiment 2

[0031] The difference from Example 1 is that in step (1), the reaction temperature is changed to 30 °C, and the others are the same as in Example 1.

Embodiment 3

[0033] The difference from Example 1 is that in step (1), the reaction temperature is changed to 10°C, and the others are the same as in Example 1.

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PUM

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Abstract

The invention belongs to the field of chemical engineering, and particularly discloses a method for reducing arene or derivative of arene by sodium borohydride. The method comprises the following steps of stirring the arene or derivative of arene, water and a catalyst at normal pressure and temperature of 10 to 150 DEG C, and controlling stirring rate to 400 to 900r / min; dissolving NaBH4 (sodium borohydride) and NaOH (sodium hydroxide) into water, so as to prepare an alkaline water solution of NaBH4; placing into ice bath, and storing for further use; dripping the alkaline water solution of NaBH4 into a reaction system, and continuing to stir after dripping is finished. The method has the advantages that the reaction system contains three phases of oil (arene or derivative thereof), water, and solid (catalyst), so that the multi-phase catalyzing method is adopted, and the reaction is realized by the simple experiment device; the arene or derivative of arene can be converted into cyclohexane or derivative of cyclohexane under the moderate conditions, the safety hidden hazards due to use of high-pressure hydrogen steel cylinders in a laboratory are avoided, and the controllable reduction on the arene or derivative of arene is realized by controlling the usage amount of the NaBH4.

Description

technical field [0001] The invention belongs to the field of chemistry and chemical engineering, and in particular relates to a method for reducing aromatic hydrocarbons or derivatives thereof with sodium borohydride. Background technique [0002] Cyclohexane is a colorless and transparent liquid. Cyclohexane and its derivatives are important chemical intermediates and important raw materials for organic synthesis. They are widely used in aerospace, daily chemicals, pharmaceuticals, pesticides, flavors and fragrances, etc. Many fields. [0003] As early as more than 100 years ago, the reductive hydrogenation process of unsaturated organic compounds in the presence of nickel-based catalysts was studied. However, due to the relatively stable benzene ring, the reduction of aromatic hydrocarbons and their derivatives by traditional hydrogenation catalysts is usually carried out at high temperature and high pressure. The yield of hexane is 70% (J. Wang, Q. Li, J. Yao, Applied C...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C5/10C07C13/18C07C13/28
CPCC07C5/10C07C2523/755C07C13/18C07C13/28
Inventor 刘仲毅苗亚磊李保军刘寿长
Owner 河南郑大催化技术研究院有限公司
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