Method for measuring content of free carbon in molybdenum carbide

A detection method and technology for free carbon, applied in the field of chemical analysis, can solve the problems of inability to evaluate the total free carbon content of molybdenum carbide catalysts, difficulty in detecting free carbon in molybdenum carbide, and difficulty in free carbon content, etc., and achieve low cost and small pore size. , The effect of easy filtration and separation

Inactive Publication Date: 2014-01-15
NORTHWEST INSTITUTE FOR NON-FERROUS METAL RESEARCH
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

The carbon and sulfur analyzer can only detect the total carbon content. Since molybdenum carbide has high carbon content and contains impurities such as oxides, as well as free C, direct analysis of C without treatment will cause large analysis deviations.
However, because molybdenum carbide is easily oxidized in air, it is difficult to detect free carbon in molybdenum carbide
In addition, because there is no standard sample, the carbon-sulfur analyzer has a large error in the test results for carbides containing a small amount (less than 0.5%) of free carbon, and it is difficult to evaluate the content of free carbon
[0004] X-ray photoelectron spectroscopy can be used to analyze the atomic valence state and element composition of the solid surface, but it can only detect the chemical composition in the range of a few nanometers on the surface, and cannot evaluate the overall free carbon content in the molybdenum carbide catalyst

Method used

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  • Method for measuring content of free carbon in molybdenum carbide
  • Method for measuring content of free carbon in molybdenum carbide
  • Method for measuring content of free carbon in molybdenum carbide

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Embodiment 1

[0022] The detection method of free carbon content in the present embodiment molybdenum carbide comprises the following steps:

[0023] Step 1. Add molybdenum carbide powder into nitrohydrochloric acid and stir, so that molybdenum carbide is dissolved in nitrohydrochloric acid, and free carbon is dispersed in nitrohydrochloric acid as an insoluble substance; the volume V of said nitrohydrochloric acid satisfies: V≥20m 0 , where m 0 is the mass of molybdenum carbide powder, m 0 The unit of V is g, and the unit of V is mL; the quality m of molybdenum carbide powder described in the present embodiment 0 is 1.0012g, and the volume V of nitrohydrochloric acid is 20mL;

[0024] Step 2. Put the filter paper in a drying box, and heat it at 150°C for 30 minutes to carry out the first drying treatment. After the first drying treatment, the mass of the filter paper is m 1 It is 0.0922g; The filter paper is a binder-free glass fiber filter paper with a filter aperture of 1.2 μm;

[00...

Embodiment 2

[0028] The detection method of free carbon content in the present embodiment molybdenum carbide comprises the following steps:

[0029] Step 1. Add molybdenum carbide powder into nitrohydrochloric acid and stir, so that molybdenum carbide is dissolved in nitrohydrochloric acid, and free carbon is dispersed in nitrohydrochloric acid as an insoluble substance; the volume V of said nitrohydrochloric acid satisfies: V≥20m 0 , where m 0 is the mass of molybdenum carbide powder, m 0 The unit of V is g, and the unit of V is mL; the quality m of molybdenum carbide powder described in the present embodiment 0 is 10.0008g, and the volume V of nitrohydrochloric acid is 200mL;

[0030] Step 2. Put the filter paper in a drying box, and heat it at 180°C for 20 minutes to carry out the first drying treatment. After the first drying treatment, the mass of the filter paper is m 1 It is 0.2422g; The filter paper is a binder-free glass fiber filter paper with a filter aperture of 0.7 μm;

[...

Embodiment 3

[0034] The detection method of free carbon content in the present embodiment molybdenum carbide comprises the following steps:

[0035] Step 1. Add molybdenum carbide powder into nitrohydrochloric acid and stir, so that molybdenum carbide is dissolved in nitrohydrochloric acid, and free carbon is dispersed in nitrohydrochloric acid as an insoluble substance; the volume V of said nitrohydrochloric acid satisfies: V≥20m 0 , where m 0 is the mass of molybdenum carbide powder, m 0 The unit of V is g, and the unit of V is mL; the quality m of molybdenum carbide powder described in the present embodiment 0 is 0.5003g, and the volume V of nitrohydrochloric acid is 15mL;

[0036] Step 2. Place the filter paper in a drying oven, and heat it at 120°C for 60 minutes to carry out the first drying treatment. The mass of the filter paper after the first drying treatment is m 1 It is 0.0923g; The filter paper is a binder-free glass fiber filter paper with a filter aperture of 3.0 μm;

[...

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Abstract

The invention provides a method for measuring the content of free carbon in molybdenum carbide. The method comprises the following steps: (1) adding molybdenum carbide powder into nitro-hydrochloric acid and stirring to dissolve molybdenum carbide in nitro-hydrochloric acid and allowing free carbon to disperse in an undissolved state in nitro-hydrochloric acid, the mass and unit of the molybdenum carbide powder being m0 and g respectively; (2) performing first drying treatment on filter paper, the mass and unit of the filter paper subjected to first drying treatment being m1 and g respectively; the filter paper being binder-free glass fiber filter paper; (3) performing filtration treatment on nitro-hydrochloric acid using filter paper, performing secondary drying treatment after washing with deionized water, and the mass and unit of the filter paper subjected to secondary drying treatment being m2 and g; (4) calculating the mass percentage content x of free carbon in the molybdenum carbide powder. The content of free carbon is detected and analyzed using nitro-hydrochloric acid and binder-free glass fiber filter paper. The design is reasonable, the operation is convenient and easy, the detection error is less, and the result accuracy is high.

Description

technical field [0001] The invention belongs to the technical field of chemical analysis, in particular to a method for detecting free carbon content in molybdenum carbide. Background technique [0002] Molybdenum carbide (Mo 2 C) Belonging to transition metal carbides, it is a group of mesenchymal compounds with metallic properties formed by carbon entering the transition metal lattice. Studies have shown that this kind of material has good catalytic activity and selectivity for hydrofining, desulfurization and denitrogenation of oil products, and is a new catalytic material with great application prospects. The electronic properties of molybdenum are close to those of platinum group metals, resulting in the catalytic performance of molybdenum carbide similar to that of platinum group metals. Molybdenum carbides have some properties of noble metals, especially molybdenum carbides are cheaper than noble metals, and have excellent resistance to sulfur poisoning, so molybden...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N5/02
Inventor 梁静张新林小辉杨健
Owner NORTHWEST INSTITUTE FOR NON-FERROUS METAL RESEARCH
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