Temperature programming-infrared spectroscopy combined device and application thereof in catalyst preparation

A temperature-programmed, combined technology, applied in catalyst activation/preparation, physical/chemical process catalysts, measurement devices, etc., can solve the problems of inability to realize qualitative research on catalyst preparation, and inability to provide physical and chemical changes of solid catalyst surface reactants.

Active Publication Date: 2021-06-29
TIANJIN UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This patented technology cannot give the characteristic reaction on the surface of the solid catalyst and the physical and chemical changes of the reactants during the reaction process, and this patent focuses on the reaction process on the surface of the catalyst, but cannot achieve qualitative research on the catalyst preparation process

Method used

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  • Temperature programming-infrared spectroscopy combined device and application thereof in catalyst preparation
  • Temperature programming-infrared spectroscopy combined device and application thereof in catalyst preparation
  • Temperature programming-infrared spectroscopy combined device and application thereof in catalyst preparation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] (1) Use the infrared system alone: ​​the temperature-programmed-infrared combined device includes a temperature-programmed reaction system and a detection system ( Figure 2a ). The temperature-programmed reaction system includes: more than two gas paths, each gas path is equipped with a pressure reducing valve 1, a pressure gauge 2, a stop valve 3, a mass flow meter 4, and the gas paths are in parallel; the mass flow meter outlet and the reaction tube 5 inlet Connection, the reaction tube is heated by the heating furnace 6, and the outlet of the reaction tube is divided into two channels, one leads to the atmosphere, and the other leads to the detection system; the gas channel entering the detection system is connected with the inlet of the gas sample pool 8 of the infrared spectrometer 7, and the gas passes through the infrared After spectral detection and recording, it flows out from the outlet of the gas sample cell and leads to the atmosphere.

[0035] (2) Tempera...

Embodiment 2

[0038] Preparation of Ni 2 Phosphate precursors for P catalysts

[0039] 6.6g of nickel nitrate (Ni(NO 3 ) 2 ·6H 2 O) was dissolved in 15 mL of deionized water, and 3 g of diammonium hydrogen phosphate ((NH 4 ) 2 HPO 4 ) was dissolved in 10 mL of deionized water, and the diammonium hydrogen phosphate aqueous solution was added dropwise to the continuously stirred (200 rpm) nickel nitrate aqueous solution at room temperature, and the stirring was continued for 30 min after the dropwise addition. The mixture was placed on the electric furnace, and the water was evaporated by stirring with a glass rod while heating. When a large amount of water was evaporated, it was transferred to a blast drying oven at 120°C for drying for 12 hours. The dried samples were ground and pulverized, then transferred to a muffle furnace and calcined at 500 °C for 3 h in an air atmosphere to obtain Ni. 2 Phosphate precursor for P catalysts.

[0040] Preparation of Ni from Nickel Phosphate Prec...

Embodiment 3

[0044] Preparation of Phosphate Precursors for MoP Catalysts

[0045] 4 g of ammonium molybdate ((NH 4 ) 6 Mo 7 O 24 ·4H 2 O) was dissolved in 15 mL of deionized water, and 3 g of diammonium hydrogen phosphate ((NH 4 ) 2 HPO 4 ) was dissolved in 10 mL of deionized water, the diammonium hydrogen phosphate aqueous solution was added dropwise to the (200 rpm) ammonium molybdate aqueous solution continuously stirred at room temperature, and the stirring was continued for 30 min after the dropwise addition. The mixture was placed on the electric furnace and heated while stirring with a glass rod to evaporate the water. When a large amount of water was evaporated, it was transferred to a blast drying oven for drying at 120°C for 12 hours. The dried samples were ground and pulverized, and then transferred to a muffle furnace for calcination at 500 °C in an air atmosphere for 3 h to obtain the phosphate precursor of the MoP catalyst.

[0046] Preparation of MoP catalysts from ...

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PUM

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Abstract

The invention relates to a temperature programming-infrared spectroscopy combined device and application thereof in catalyst preparation, and the device comprises a temperature programming reaction system and a Fourier transform infrared spectrum detection system, and can also be additionally provided with a thermal conductivity cell detector. The temperature programming reaction system is composed of a heating furnace, a reaction tube, more than two gas path modules with flow control and a temperature programming control module. The Fourier transform infrared system is composed of a gas sample cell and an infrared detector. The gas from the temperature programming reaction tube can directly enter a detection system or be discharged to the atmosphere through a bypass. The gas entering the detection system can directly enter the gas sample cell of the Fourier transform infrared spectrometer or enter the gas sample cell of the Fourier transform infrared spectrometer after being detected by the thermal conductivity cell detector through a split / non-split gas path. The temperature programming and infrared combined device is used for researching the reduction process of a catalyst, and is beneficial to comprehensively understanding the reduction process and the reaction mechanism.

Description

technical field [0001] The invention belongs to the technical field of instruments and meters, and in particular relates to a thermal analysis instrument for characterizing solid materials, especially solid catalysts, and its application in the research of the preparation process of solid catalysts. Background technique [0002] The temperature-programmed analysis technique is to study the change of the gas composition during the temperature-raising process of a solid material or a solid material that has been pre-treated by a specific method under a specific gas flow atmosphere, and take this change as a function of temperature or time. A technique for studying its laws. It is an automatic dynamic tracking measurement, so compared with the static method, it has the advantages of continuous, fast and simple, and is widely used in inorganic chemistry, organic chemistry, polymer chemistry, biochemistry, metallurgy, petrochemistry, mineralogy and geology various academic field...

Claims

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Application Information

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IPC IPC(8): G01N21/3504G01N25/20B01J27/185B01J27/19B01J27/188B01J37/28B01J37/08B01J37/18
CPCG01N21/3504G01N25/20B01J27/1853B01J27/19B01J27/188B01J37/28B01J37/088B01J37/18
Inventor 盛强李翔刘春静陈绍章
Owner TIANJIN UNIVERSITY OF SCIENCE AND TECHNOLOGY
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