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A kind of solid catalyst and its preparation method and application

A solid catalyst and solid technology, applied in the direction of catalyst activation/preparation, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of unsatisfactory efficiency and low graphite yield, and achieve good results and high graphite yield High, chemically stable effect

Active Publication Date: 2022-07-12
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

From the various reaction examples reported in the literature, it can be seen that the efficiency of the above-mentioned traditional catalysts in converting the carbon dioxide obtained by oxidation of the sample into graphite is not ideal, and the yield of graphite is relatively low, so it is not suitable for processing a small amount of samples, or the carbon content is low. s material

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  • A kind of solid catalyst and its preparation method and application
  • A kind of solid catalyst and its preparation method and application

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preparation example Construction

[0031] A second aspect of the present invention provides a preparation method of the above-mentioned solid catalyst, the preparation method comprising:

[0032] (1) mixing the solution of Group VIII metal soluble precursor with the adsorbent, dispersing uniformly to obtain a mixed system;

[0033] (2) remove the liquid phase and roasting in the mixed system to obtain the treated solid;

[0034] (3) the solid after described treatment is carried out contact reaction with hydrogen, obtains the solid after reduction;

[0035] (4) Co-grinding the reduced solid and a carbon-free grinding aid to obtain the solid catalyst.

[0036] In the present invention, the solvent in the solution of the group VIII metal soluble precursor can be any solvent suitable for dissolving the group VIII metal precursor, such as water, ethanol and the like.

[0037] According to the present invention, preferably, the calcination temperature in step (2) is 100-800°C; the contact reaction temperature in s...

Embodiment 1

[0065] 1) Weigh 7.2g Fe (NO 3 ) 3 ·9H 2 O (analytical pure), add an appropriate amount of deionized water to dissolve;

[0066] 2) Weigh 10 g of diatomaceous earth, add it to the solution obtained in step 1), ultrasonically treat it to form a dispersion system, and stir overnight;

[0067] 3) Under the stirring state, slowly evaporate the mixed suspension system obtained in step 2) to dryness, collect the solid remaining after evaporation to dryness, transfer the solid to a porcelain boat, place it in a muffle furnace, and bake it at 200° C. for 3 hours;

[0068] 4) The solid roasted in step 3) is transferred to the tube furnace together with the porcelain boat, and the heating tube is passed into nitrogen. After the air in the container is exhausted, the nitrogen flow is replaced with hydrogen, and the nitrogen is exhausted side by side, and the system is heated. to 250°C for 2h; after cooling, the hydrogen flow was replaced with nitrogen, the hydrogen was exhausted, and t...

Embodiment 2

[0073] 1) Weigh 0.5 g of chloroplatinic acid (analytical grade, platinum content 38%), add an appropriate amount of deionized water, and stir until completely dissolved;

[0074] 2) Weigh 10 g of γ-alumina, add it to the solution obtained in step 1), ultrasonically treat it to form a dispersion system, and stir overnight;

[0075] 3) filter the mixed suspension system obtained in step 2) to collect solid;

[0076] 4) Weigh 0.5 g of chloroplatinic acid (analytical purity, platinum content 38%), add an appropriate amount of deionized water, and stir until completely dissolved;

[0077] 5) adding the solid obtained in step 3) to the solution obtained in step 4), ultrasonically treating it to form a dispersion system, and stirring overnight;

[0078] 6) filter the mixed suspension system obtained in step 5) to collect the solid; transfer the solid to a porcelain boat, place it in a muffle furnace, and bake at 250° C. for 2 hours;

[0079] 7) The solid roasted in step 6) is trans...

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Abstract

The present invention belongs to 14 In the field of C detection, a solid catalyst and a preparation method and application thereof are disclosed. Based on the total weight of the solid catalyst, the solid catalyst comprises: 1-40% by weight of group VIII metal nanoparticles, 60-98% by weight of adsorbent and 1-20% by weight of carbon-free grinding aid, and the sum of the weight percentages of each component is 100wt%. The catalyst of the invention has good catalytic reduction effect of carbon dioxide gas, high graphite yield, and can efficiently solve the problem that the total amount of carbon dioxide is generated when the sample carbon content is very low or the total amount of the sample is small; the catalyst itself does not contain any form The carbon element will not pollute the resulting graphite product and will not affect the measurement results.

Description

technical field [0001] The present invention relates to 14 The field of C detection, more specifically, relates to a solid catalyst and a preparation method thereof, and the use of the solid catalyst in an accelerator mass spectrometer 14 Application of sample graphitization pretreatment in C measurement. Background technique [0002] 14 C is an important radioactive isotope of carbon and widely exists in various organisms, environmental samples and organic and polymer products. right 14 The measurement of C is of great significance in the fields of archaeology, geology, meteorology, medicine, biology, materials, and energy. available to measure 14 The methods of C content include proportional scintillation method (PSM), beta ionization (BI) and accelerated mass spectrometry (AMS). Among them, the proportional scintillation method needs to convert C in the sample into benzene series and then detect it, which requires a large amount of sample, and the converted benzene ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/24B01J23/745B01J23/42B01J37/18C01B32/205
CPCB01J27/24B01J23/745B01J23/42B01J37/18C01B32/205B01J35/393B01J35/23
Inventor 高昂高静范彦如李红玉薛燕波
Owner CHINA PETROLEUM & CHEM CORP
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