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Method for preparing 2, 6-ditertiary butyl-4-methylphenol by electrochemically degrading lignin

A technology of di-tert-butyl and methyl phenol, which is applied in the direction of electrolysis, organic chemistry, electrolysis components, etc., can solve the problems of high cost, serious pollution, high energy consumption, etc., and achieve the effect of low cost, high efficiency and simple process

Inactive Publication Date: 2013-05-01
HEBEI UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] The purpose of the present invention is to provide a method for electrochemically degrading lignin to prepare 2,6-di-tert-butyl-4-methylphenol for the shortcomings of current technologies such as high cost, high energy consumption, and serious pollution. Using Pb / PbO 2 The electrode is used as the working electrode, the Cu sheet electrode is used as the auxiliary electrode, and the standard saturated calomel electrode is used as the reference electrode to form an electrolytic cell to electrochemically degrade lignin

Method used

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  • Method for preparing 2, 6-ditertiary butyl-4-methylphenol by electrochemically degrading lignin
  • Method for preparing 2, 6-ditertiary butyl-4-methylphenol by electrochemically degrading lignin
  • Method for preparing 2, 6-ditertiary butyl-4-methylphenol by electrochemically degrading lignin

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Embodiment 1

[0023] (1) Dissolve 12g lignin in 150mL NaOH solution (0.5M), then add 0.50g NaOH solid to adjust the solution to pH=10, the lignin concentration is 80g / L, put it in the electrolytic cell as the electrolyte use.

[0024] (2) Take 12 (3×2×2) cm 2 Lead sheet, prepared Pb / PbO according to the relevant electrodeposition method (Chemosphere, 2005, (61): 1327-1335) 2 electrode. Take a copper sheet with the same area and use it after surface grinding.

[0025] (3) Use self-made Pb / PbO 2 The electrode is the working electrode, the Cu sheet electrode is the auxiliary electrode, magnetic stirring, the standard saturated calomel electrode is the reference electrode, the electrolytic cell and the reference cell are connected by a salt bridge, and the lignin is electrocatalytically degraded by a constant current with a current density of 25mA / cm 2 , electrolyzed for 4.5h, and the resulting electrolyte was further analyzed after the electrolysis was completed.

[0026] (4) Take the ele...

Embodiment 2-10

[0032] Embodiment 2~10 is at current density 25mA / cm 2 , pH=10, and lignin concentration of 80g / L, the effect of different reaction times on the concentration of product BHT (see Table 1), and other operating steps are the same as in Example 1.

[0033] Table 1 Effect of reaction time on BHT concentration

[0034] project Reaction time (h) BHT concentration (g / L) Example 2 0.5 0.56 Example 3 1 5.23 Example 4 1.5 4.52 Example 5 2 4.07 Example 6 2.5 4.20 Example 7 3 5.61 Example 8 3.5 3.85 Example 9 4 5.13 Example 10 5 1.12

Embodiment 11-17

[0036] In Examples 11 to 17, the reaction time is 3h, pH=10, and the lignin concentration is 80gL. The effect of different current densities on the concentration of the product 2,6-di-tert-butyl-4-methylphenol (see Table 2), Other operating steps are the same as in Example 1.

[0037] Table 2 The influence of current density on the concentration of 2,6-di-tert-butyl-4-methylphenol

[0038] project Current density (mA / cm 2 ) BHT concentration (g / L) Example 11 10 0.86 Example 12 15 2.98 Example 13 20 2.22 Example 14 25 5.24 Example 15 30 4.23

[0039] Example 16 35 4.33 Example 17 40 1.80

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Abstract

The invention provides a method for preparing 2, 6-ditertiary butyl-4-methylphenol by electrochemically degrading lignin. According to the method, a Pb / PbO2 electrode is used as a work electrode, a Cu piece is used as an auxiliary electrode, and a standard saturated calomel electrode is used as a reference electrode to form an electrolytic tank so as to electrochemically degrade lignin. According to the method for degrading lignin by catalytic oxidation by means of electrochemical technique, the method is mild in reaction condition, environmentally friendly and higher in efficiency. The raw material lignin selected is a reproducible high polymer with a wide source, and the lignin is used as the raw material to prepare BHT (Butylated Hydroxytoluene), so that not only is sewage discharged by a paper mill treated, but also a certain economic value is obtained. The method for preparing BHT by electrochemically degrading lignin is simple in process, lower in cost and environment-friendly, and has good development prospect and industrial application value.

Description

technical field [0001] The invention relates to providing a method for preparing 2,6-di-tert-butyl-4-methylphenol by electrochemically catalyzing and oxidizing lignin, and belongs to the technical field of biomass energy chemical industry. Background technique [0002] Lignin is the second largest natural polymer material after cellulose in nature. It is regenerated at a rate of 600 trillion tons per year. It is one of the renewable resources with great potential. Its structure is complex, mainly composed of three The three-dimensional network formed by the basic structural units (guaiacylpropyl, syringylpropyl and p-hydroxyphenylpropyl), the lignin structure (Coordination Chemistry Reviews, 2010, 254:1854-1870) is shown in the figure below . If it can be effectively degraded, many useful organic compounds will be generated. [0003] [0004] As a major waste product of the pulp and paper industry, lignin is rarely used efficiently. With the recognition of environmenta...

Claims

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Application Information

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IPC IPC(8): C25B3/00C07C39/06
Inventor 黎钢张一鸣杨芳尹小莲彭莹
Owner HEBEI UNIV OF TECH
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