Preparation of metal-loaded catalyst with bean dreg-derived nitrogen-doped carbon base as carrier and method for catalyzing hydrodeoxygenation of p-nitrophenol

A technology of p-nitrophenol and supported catalysts, which is applied in the preparation of organic compounds, preparation of amino hydroxyl compounds, chemical instruments and methods, etc., to achieve the effects of simple preparation process, resource saving, and low toxicity of reagents

Inactive Publication Date: 2020-01-21
LANZHOU UNIVERSITY +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In order to solve the problems in the preparation of existing metal-loaded catalysts and the method of catalyzing the hydrodeoxygenation of p-nitrophenol, the present invention provides a preparation of a metal-loaded catalyst based on a nitrogen-doped carbon base derived from soybean dregs and catalyzes p-nitrophenol Method for Hydrodeoxygenation of Phenol

Method used

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  • Preparation of metal-loaded catalyst with bean dreg-derived nitrogen-doped carbon base as carrier and method for catalyzing hydrodeoxygenation of p-nitrophenol
  • Preparation of metal-loaded catalyst with bean dreg-derived nitrogen-doped carbon base as carrier and method for catalyzing hydrodeoxygenation of p-nitrophenol
  • Preparation of metal-loaded catalyst with bean dreg-derived nitrogen-doped carbon base as carrier and method for catalyzing hydrodeoxygenation of p-nitrophenol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] A method for preparing a metal-supported catalyst based on a nitrogen-doped carbon base derived from okara and catalyzing the hydrodeoxygenation of p-nitrophenol, comprising the following steps:

[0027] S1. Wash, dry and grind the bean dregs and pass through a 40-mesh sieve. Under the condition of nitrogen protection, roast the treated bean dregs in a tube furnace at 300°C for 2 hours, collect the roasted bean dregs and add potassium hydroxide solution , stirred at room temperature for 30 minutes and then filtered. The filtered bean dregs were washed with water, and the pH was adjusted to neutral to obtain a crude product. The crude product was dried naturally and ground to obtain a crude product. After weighing, it was placed in a tube under nitrogen protection. Roasting in a furnace at 800°C for 2 hours, grinding the product after the roasting treatment to obtain a nitrogen-carbon carrier;

[0028] S2. Disperse the nitrogen-carbon carrier in methanol at room temperat...

Embodiment 2

[0032] According to embodiment 1, adopt field emission scanning electron microscope (SEM) to characterize the morphology and particle distribution of sample; Adopt elemental analysis (EDS) to determine the kind and content of the element contained in catalyst; Adopt X-ray diffractometer (XRD) to measure sample The structure, composition and crystallinity of the sample were tested and analyzed by X-ray photoelectron spectroscopy (XPS).

[0033] figure 2 It is the SEM topography image of the Pd / NC catalyst, and Table 1 shows the element distribution results of the nitrogen-doped carbon-based support. It can be seen from the table that the heteroatom nitrogen was successfully introduced into the carbon base by the method of okara calcination, and the nitrogen content exceeded 11%. achieved the intended purpose.

[0034] Table 1 Element distribution results on the surface of Pd / NC catalyst

[0035]

[0036] image 3 It is the XRD characteristic diffraction pattern of metal...

Embodiment 3

[0043] Effect of Metal Content on Reaction

[0044] According to Application Example 1, this experiment used the nitrogen-carbon material prepared from bean dregs as the carrier and metal Pd as the load to investigate the catalytic reaction time required for the metal Pd-supported catalyst with different mass fractions under the same conditions. The results are shown in Figure 7 As shown, it can be seen that with the continuous increase of the mass fraction of Pd contained in the catalyst, the required reaction time is constantly decreasing, indicating that within a certain range (this experiment is a Pd content of 2% to 10%), the same Under the reaction conditions (Pd is the supported metal and the carrier is the carbon-nitrogen material derived from bean dregs), the catalytic effect of 4-NP hydrogenation is the best when the Pd content is 10%.

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Abstract

The invention provides preparation of a metal-loaded catalyst with a bean dreg-derived nitrogen-doped carbon base as a carrier and a method for catalyzing hydrodeoxygenation of p-nitrophenol and relates to the technical field of catalyst production and application. The preparation method comprises the following steps: S1, roasting treated bean dregs in a tubular furnace, adding a potassium hydroxide solution, adjusting the pH value to be neutral, and roasting the bean dregs in the tubular furnace under the protection of nitrogen to obtain a nitrogen-carbon carrier; S2, dispersing the nitrogen-carbon carrier into methanol at room temperature, treating the nitrogen-carbon carrier in an ultrasonic instrument, adding a PdCl2 solution, carrying out condensation reflux operation on the liquid, dropwise adding a sodium borohydride aqueous solution, stirring the mixture at room temperature, and carrying out suction filtration, water washing and drying to obtain the metal-loaded nitrogen-carbonmaterial catalyst; S3, sequentially mixing the p-nitrophenol aqueous solution, the sodium borohydride aqueous solution and the catalyst aqueous solution, and detecting the catalytic hydrogenation reduction progress of p-nitrophenol by adopting an ultraviolet spectrophotometer. The preparation method has the advantages of resource saving, simple operation, small environmental pollution and strongrepeatability.

Description

technical field [0001] The invention belongs to the technical field of catalyst production and application, and relates to the preparation of a metal-loaded catalyst with a nitrogen-doped carbon base derived from bean dregs as a carrier and a method for catalyzing the hydrodeoxygenation of p-nitrophenol. Background technique [0002] The energy crisis is one of the major problems faced by human beings, and converting the huge reserves of renewable biomass into fuel energy that can be used efficiently is one of the effective ways to solve the current fossil energy crisis. However, a large number of lignin-derived phenolic compounds are the most difficult class of substances to convert during biomass upgrading. It is an effective way to solve this problem to construct efficient and environmentally friendly catalysts to catalyze the hydrodeoxygenation conversion of phenolic compounds with high selectivity. Early related work used industrial catalysts such as CoMoS and NiMoS, b...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24C07C213/02C07C215/76
CPCB01J27/24C07C213/02C07C215/76
Inventor 于桂琴董正平刘相黄国生董翔牛雁宁万元蒋伟李静
Owner LANZHOU UNIVERSITY
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