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A kind of manganese-based molecular sieve deoxidizer and its preparation method and application

A sieve deoxidizer and molecular sieve technology, applied in the field of deoxidizers, can solve the problems of insufficient removal depth, incomplete utilization of active components, and low oxygen adsorption capacity

Active Publication Date: 2021-02-02
JILIN UNIV +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In summary, the existing chemical adsorption deoxidizers are prepared by loading copper, manganese and other metal oxides with porous supports through traditional mechanical mixing or traditional impregnation; this inevitably makes it difficult to effectively disperse the active metal oxide components , leading to the incomplete utilization of active components; resulting in low oxygen adsorption capacity, insufficient removal depth and other shortcomings
In addition, the existing manganese-based deoxidizer also has a disadvantage that it is easy to cause overheating during the reduction process, which affects the service life of the deoxidizer

Method used

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Examples

Experimental program
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Effect test

preparation example Construction

[0025]The invention provides a method for preparing a manganese-based molecular sieve deoxidizer, which comprises the following steps:

[0026]Mix Y-type molecular sieve with water to obtain Y-type molecular sieve solution;

[0027]Subjecting the Y-type molecular sieve solution and the water-soluble manganese salt to a spontaneous co-precipitation reaction to obtain a first precursor;

[0028]Subjecting the first precursor to gradient vacuum roasting to obtain a second precursor;

[0029]In a hydrogen-containing atmosphere, the second precursor is subjected to a reduction reaction to obtain a manganese-based molecular sieve deoxidizer; the temperature of the reduction reaction is 150-300°C.

[0030]In the present invention, unless otherwise specified, all raw material components are commercially available products well known to those skilled in the art.

[0031]In the present invention, Y-type molecular sieve and water are mixed to obtain Y-type molecular sieve solution.

[0032]In the present invention...

Embodiment 1

[0056]Under the conditions of 60℃ water bath heating and 200rpm, 10g NaY molecular sieve and 40mL deionized water were stirred uniformly, 5g manganese nitrate was slowly added within 50min, and then heated in a 60℃ water bath, stirred at 300rpm for 30min, and the resulting reaction system proceeded Suction filtration, drying the obtained solid product at 80°C to obtain the first precursor;

[0057]The first precursor was placed in a vacuum muffle furnace, heated to 500°C at a temperature increase rate of 10°C / min, and kept for 4h, where the vacuum degree was -95kPa, and the calcined product obtained was subjected to tableting and grinding treatments To the particle size of 0.5~1.0mm, the second precursor is obtained;

[0058]In a hydrogen-containing atmosphere (hydrogen volume fraction is 50%), the space velocity is 500h-1At 250°C, the second precursor is reduced for 5 hours to obtain a manganese-based molecular sieve deoxidizer (marked as S1), in which the MnO content is 14.5%; the tempe...

Embodiment 2

[0061]Under the conditions of 80℃ water bath heating and 100rpm, 15g NH4Y-type molecular sieve and 300mL deionized water are stirred uniformly, 15g manganese chloride is slowly added within 45min, and then stirred for 50min, the resulting reaction system is suction filtered, and the resulting solid product is dried at 90°C to obtain the first precursor ;

[0062]Put the first precursor in a vacuum muffle furnace, heat it up to 400°C at a heating rate of 5°C / min, and then keep it for 6 hours, where the vacuum degree is -96kPa, and the resulting calcined product is subjected to tableting and grinding treatments To the particle size of 0.5~1.0mm, the second precursor is obtained;

[0063]In hydrogen atmosphere (hydrogen volume fraction is 100%), space velocity is 1000h-1At 150°C, the second precursor is reduced for 10 hours to obtain a manganese-based molecular sieve deoxidizer (marked as S2), in which the MnO content is 19.6%; the temperature rise during the reduction is 1.6°C.

[0064]Use the...

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Abstract

The invention provides a manganese-based molecular sieve deoxidizer, its preparation method and application, and belongs to the technical field of deoxidizers. The preparation method of the manganese-based molecular sieve deoxidizer provided by the present invention, firstly, the generated manganese hydroxide nano-colloid is evenly deposited on the outer surface of the Y-type molecular sieve by the method of spontaneous co-precipitation; 2 o 3 The nanoparticles are highly dispersed in the cavity of the Y-type molecular sieve with twelve-membered ring channels, and finally the MnO‑Y-type molecular sieve deoxidizer with excellent deoxidation performance at room temperature is prepared after hydrogen reduction. Because the highly dispersed active MnO has a higher contact efficiency with oxygen, the deoxidizer has the advantages of high deoxidation depth, large deoxidation capacity at room temperature, and the reduction process is not easy to overheat. In addition, the highly dispersed active manganese oxide greatly reduces the amount of precursor manganese salt used. available for N 2 , Ar, H 2 , CO, hydrocarbons and other raw material gas deep deoxidation.

Description

Technical field[0001]The invention relates to the technical field of deoxidizers, in particular to a manganese-based molecular sieve deoxidizer, and a preparation method and application thereof.Background technique[0002]The oxygen content in the ultrapure gas is a very important indicator. Many industries require it to be carried out in an oxygen-free atmosphere, and the volume percentage of impurity oxygen is required to be as low as 0.1×10-6Or lower, which puts forward higher requirements on the performance of the deoxidizer.[0003]The existing deoxidizers are mainly divided into two categories. (1) Catalytic deoxidizers. Most of these deoxidizers use precious metals such as Pt, Pd, Ru as active components. The principle of deoxidation is to pass H2Or CO chemically react with trace oxygen in the target mixture to produce water or carbon dioxide, thereby achieving the purpose of deoxygenation; this type of deoxidizer has the advantages of high activity and high deoxygenation efficie...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/18B01D53/02B01J20/30
CPCB01D53/02B01D2257/104B01J20/06B01J20/186
Inventor 闫文付蒋涛许紫洋宫本希胡有坤白璞
Owner JILIN UNIV