CN112717685B - Purifying agent for removing trace impurities in high-purity gas and preparation method and application thereof - Google Patents

Purifying agent for removing trace impurities in high-purity gas and preparation method and application thereof Download PDF

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CN112717685B
CN112717685B CN202011508500.8A CN202011508500A CN112717685B CN 112717685 B CN112717685 B CN 112717685B CN 202011508500 A CN202011508500 A CN 202011508500A CN 112717685 B CN112717685 B CN 112717685B
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purifying agent
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CN112717685A (en
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杜霞茹
徐卫
侯蕾
李楠
于志日
肖菲
吴熠
李宏涛
刘振峰
刘金刚
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Dalian Samat Chemicals Co ltd
DALIAN CATALYTIC ENGINEERING TECHNOLOGY Ltd
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Dalian Samat Chemicals Co ltd
DALIAN CATALYTIC ENGINEERING TECHNOLOGY Ltd
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    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34Chemical or biological purification of waste gases
    • B01D53/74General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/86Catalytic processes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/26Drying gases or vapours
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34Chemical or biological purification of waste gases
    • B01D53/46Removing components of defined structure
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34Chemical or biological purification of waste gases
    • B01D53/46Removing components of defined structure
    • B01D53/62Carbon oxides
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34Chemical or biological purification of waste gases
    • B01D53/74General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/86Catalytic processes
    • B01D53/8671Removing components of defined structure not provided for in B01D53/8603 - B01D53/8668
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    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
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    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/76Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
    • B01J23/84Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
    • B01J23/889Manganese, technetium or rhenium
    • B01J23/8892Manganese
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    • B01J23/00Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/76Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
    • B01J23/84Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
    • B01J23/889Manganese, technetium or rhenium
    • B01J23/8898Manganese, technetium or rhenium containing also molybdenum
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2257/00Components to be removed
    • B01D2257/10Single element gases other than halogens
    • B01D2257/104Oxygen
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2257/00Components to be removed
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    • B01D2257/108Hydrogen
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2257/00Components to be removed
    • B01D2257/50Carbon oxides
    • B01D2257/502Carbon monoxide
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2257/00Components to be removed
    • B01D2257/50Carbon oxides
    • B01D2257/504Carbon dioxide
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2257/00Components to be removed
    • B01D2257/80Water
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2523/00Constitutive chemical elements of heterogeneous catalysts

Abstract

The invention relates to a gas purification technology in chemical industry, in particular to a purifying agent for removing trace impurities in high-purity gas by a one-step method, a preparation method and application thereof. The purifying agent consists of an active component, a carrier and a binder; wherein, the active component accounts for 60 to 90 percent of the total weight of the catalyst, the carrier accounts for 9 to 20 percent of the total weight of the catalyst, and the binder accounts for 1 to 20 percent of the total weight of the catalyst; the active components are three or more compounds of Ni, cu, mn, fe and Mo, and the carrier is SiO 2 Or SiO 2 A composite oxide with MOx. The product of the invention is suitable for purifying nitrogen, hydrogen, oxygen, argon, helium, methane and organic gas, can be widely applied to the industries of semiconductors, optical fibers, steel and petrochemical industry, has high impurity removal capacity and long service life, and is suitable for large-scale industrial use.

Description

Purifying agent for removing trace impurities in high-purity gas, and preparation method and application thereof
Technical Field
The invention relates to a gas purification technology in chemical industry, in particular to a purifying agent for removing trace impurities in high-purity gas by a one-step method, a preparation method and application thereof.
Background
The high-purity gas can be used as carrier gas and protective gas in the manufacturing and production processes of large-scale integrated circuits, liquid crystal displays, polycrystalline silicon and thin-film solar cells, novel electric light sources, photoelectric semiconductor devices and optical fiber communication devices so as to manufacture electronic elements with reliable performance. The purity of the industrially produced high-purity gas usually contains 5N (99.999%) or even 4N (99.99%), and also contains impurities such as hydrogen, oxygen, carbon monoxide, carbon dioxide, water and the like, and the high-purity gas needs to be purified and removed until the gas purity reaches 7N (99.99999%) to meet the requirements of manufacturing electronic devices.
The purificant/catalyst for removing impurities applied in related patent documents and industrial production is divided into two main types, the first type is a catalytic type deoxidizer, the working principle is that hydrogen or carbon monoxide in a gas source is utilized to generate a chemical reaction under the action of a catalyst to generate water or carbon dioxide, then a molecular sieve, silica gel, alumina and other traditional adsorbents are used for dehydration, and finally a 13X molecular sieve is used for removing carbon dioxide. The purification process needs three purification materials, uses three purification devices and occupies a large area. The second category is metal getters, usually based on titanium, which react with many elements and compounds at high temperatures, 300-500 ℃, for example, titanium getters react with carbon, hydrogen, nitrogen, oxygen at high temperatures. The method has the problems of high operation temperature, low safety, low capacity, high cost and the like. Therefore, it is necessary to develop a purifying agent capable of removing trace impurities in high-purity gas in one step.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provides a purifying agent for removing trace impurities in high-purity gas by a one-step method and a preparation method and application thereof.
In order to achieve the purpose, the invention adopts the technical scheme that:
micro-device for removing high-purity gasA purifying agent for measuring impurities, which consists of an active component, a carrier and a binder; wherein, the active component accounts for 60 to 90 percent of the total weight of the catalyst, the carrier accounts for 9 to 20 percent of the total weight of the catalyst, and the binder accounts for 1 to 20 percent of the total weight of the catalyst; the active components are three or more compounds of Ni, cu, mn, fe and Mo, and the carrier is SiO 2 Or SiO 2 A composite oxide with MOx.
The weight ratio of Cu/Ni in the active component is 0.1-1.6; the weight ratio of Mn to Ni is 0.2-1.8; the weight ratio of Mo to Ni is 0.01-0.35; the weight ratio of Fe to Ni is 0.05-1.
M in the MOx is Al or Ti, and x is 1-2.
The carrier SiO 2 Is SiO 2 One or more of powder, silica sol and diatomite.
The binder is one or more of kaolin, high alumina cement, pseudo-boehmite or silica sol.
A preparation method of a purifying agent for removing trace impurities in high-purity gas,
(1) Mixing and dissolving soluble metal salt of an active component precursor in deionized water, adding a carrier under the condition of stirring, and heating to 60-85 ℃ for later use;
(2) Adding a sodium carbonate solution into the system in the step (1) under the condition of stirring until the pH value of the system is 8-10, and then aging for 1-8 hours at the temperature of 60-85 ℃;
(3) Centrifuging the aged system, collecting precipitate, dispersing the precipitate in 60-85 deg.C water, repeatedly washing to neutrality, drying, and roasting to obtain active component powder;
(4) And fully mixing the obtained active component powder with a binder, and airing and roasting overnight at room temperature to obtain the purifying agent.
The soluble metal salt of the active component precursor in the step (1) comprises nickel nitrate/nickel acetate, manganese nitrate/manganese acetate and ferric nitrate/ferric acetate; cobalt nitrate/acetate, ammonium molybdate;
collecting the precipitate, drying at the low temperature of 80-150 ℃, and then roasting at the temperature of 300-500 ℃ for 2-4 hours to obtain active component powder;
and (3) fully mixing the powder in the step (4) with a binder, forming, airing at room temperature overnight, roasting at 300-500 ℃ for 2-4 hours, and cooling to room temperature to obtain the nano-composite material.
The application of a purifying agent for removing trace impurities in high-purity gas, wherein the purifying agent is applied to the purification of nitrogen, hydrogen, oxygen, argon, helium, methane and organic gas.
The application method of the purifying agent comprises the steps of activating the purifying agent by using hydrogen-containing atmosphere before use, removing gas to be treated containing impurities of oxygen, hydrogen, carbon monoxide, carbon dioxide and water through a purifying agent bed layer, and reducing and regenerating the purifying agent when the impurity content at the outlet of the purifying agent bed layer exceeds 10 ppb. The purifying agent of the invention can be reduced and regenerated on site and can be reused.
The invention has the beneficial effects that:
1. the purifying agent of the invention adopts the domestic metal mineral resources with rich resources as the raw materials, and the price is low, thus having stronger market competitiveness.
2. The purifying agent can remove trace H in high-purity gas by one-step method 2 、O 2 、CO、CO 2 、H 2 O and other impurities are removed to 1ppb at room temperature, and the requirements of the semiconductor industry, the electronic industry, the steel industry and the chemical industry on the content of the impurities in the high-purity gas are met.
3. The purifying agent has high impurity removing capacity and high removing precision, can be repeatedly regenerated and used, can effectively purify various impurities in one operation unit, simplifies the gas purification process and reduces the operation energy consumption. Can be widely applied to the purification of bulk gases such as oxygen, hydrogen, helium, argon, nitrogen and the like and organic gases such as low-carbon small-molecular hydrocarbons such as methane, ethylene, propylene and the like.
Detailed Description
The following examples are presented to further illustrate embodiments of the present invention, and it should be understood that the embodiments described herein are for purposes of illustration and explanation only and are not intended to limit the invention.
Example 1
Taking 106gCu (NO) 3 ) 2 .3H 2 O、1012gNi(NO 3 ) 2 .6H 2 O、138gMn(NO 3 ) 2 (50 wt.%) and 126gFe (NO) 3 ) 3 .9H 2 Dissolving O in 2600ml deionized water, adding 69g metatitanic acid (less than 200 meshes) and 60g SiO while stirring 2 Forming suspension A (smaller than 200 meshes), and heating to 70 ℃ for later use; preparing 2mol/L sodium carbonate solution B; and dripping the suspension A into the suspension B under the stirring state until the pH value is 9, aging for 1 hour at 70 ℃, filtering, washing, drying, and roasting for 2 hours at 300 ℃ to obtain active component powder.
The powder obtained above was ground to 300 mesh or less, and 67ml (28% SiO) 2 pH value of 8), 25g of pseudo-thin powder are fully and uniformly mixed, extruded by a strip extruder to be formed, kept stand in the air and dried, roasted at 300 ℃ for 4 hours and naturally cooled to room temperature for later use.
Example 2
Taking 152gCu (NO) 3 ) 2 .3H 2 O、1265gNi(NO 3 ) 2 .6H 2 O、378gMn(NO 3 ) 2 Dissolving 50wt% of the mixture in 2500ml of deionized water, adding 50g of diatomite (smaller than 200 meshes) while stirring to form a suspension A, and heating to 80 ℃ for later use; preparing 2mol/L sodium carbonate solution B; and dripping the solution B into the solution A under the stirring state until the pH value is 9, aging for 5 hours at 80 ℃, then filtering, washing, drying, and roasting for 4 hours at 300 ℃ to obtain active component powder.
Grinding the obtained powder to below 300 meshes, adding 85g of kaolin, fully and uniformly mixing, rolling and molding by using a sugar coating machine, standing in air, airing, roasting at 300 ℃ for 4 hours, and naturally cooling to room temperature for later use.
Example 3
Taking 455gCu (NO) 3 ) 2 .3H 2 O、389gNi(NO 3 ) 2 .6H 2 O、441gMn(NO 3 ) 2 (50 wt%) was dissolved in 2300ml of deionized water, and 268ml of alkaline silica sol (28% SiO) was added with stirring 2 pH value of 8) to form a suspension A, and heating to 70 ℃; preparation of 2mol/LSodium carbonate solution B; and dripping the solution B into the solution A under the stirring state until the pH value is 9, aging for 8 hours at 70 ℃, then filtering, washing, drying, and roasting for 3 hours at 450 ℃ to obtain active component powder.
The powder obtained above was ground to 300 mesh or less, and 50g of diatomaceous earth (SiO) was added 2 Content is more than or equal to 90 percent), 75g of pseudo-thin powder is fully and uniformly mixed, rolled and molded by a sugar coating machine, kept stand in air and dried, roasted at 450 ℃ for 4 hours and naturally cooled to room temperature for later use.
Example 4
Take 61g (NH) 4 ) 6 Mo 7 O 24 .4H 2 O、304gCu(NO 3 ) 2 .3H 2 O、584g Ni(NO 3 ) 2 .6H 2 O、315gMn(NO 3 ) 2 (50 wt.%) was dissolved in 2400ml of deionized water and 25g of TiO was added with stirring 2 179ml of basic silica sol (28% SiO) 2 pH value of 8) to form a suspension A, and heating to 60 ℃; preparing 2mol/L sodium carbonate solution B; and dripping the solution B into the solution A under the stirring state until the pH value is 8, aging for 1 hour at 60 ℃, then filtering, washing, drying, and roasting for 2 hours at 500 ℃ to obtain active component powder.
The powder obtained above was ground to 300 mesh or less, and 50g of diatomaceous earth (SiO) was added 2 Content is more than or equal to 90 percent), 105g of high-alumina cement is fully and uniformly mixed, rolled and molded by a sugar coating machine, kept stand in the air and dried, roasted at 500 ℃ for 4 hours and naturally cooled to room temperature for later use.
Example 5
Taking 379gFe (NO) 3 ) 3 .9H 2 O、76gCu(NO 3 ) 2 .3H 2 O、292gNi(NO 3 ) 2 .6H 2 O、694gMn(NO 3 ) 2 (50 wt%) was dissolved in 2000ml of deionized water, and 45g of pseudo-thin powder and 25g of SiO were added under stirring 2 Forming a suspension A and heating to 70 ℃; preparing 2mol/L sodium carbonate solution B; dripping the solution B into the solution A under stirring to pH 8.5, aging at 70 deg.C for 3 hr, filtering, washing, oven drying, and roasting at 350 deg.C for 2 hr to obtain active component powder.
100ml (28% SiO) was added 2 pH value of 8), 50g of metatitanic acid are fully and uniformly mixed, extruded by a bar extruder for forming, kept stand in air and dried, roasted at 350 ℃ for 4 hours, and naturally cooled to room temperature for later use.
Example 6
Taking 227gCu (NO) 3 ) 2 .3H 2 O、265gNi(NO 3 ) 2 .6H 2 O、189gMn(NO 3 ) 2 (50 wt%) was dissolved in 1400ml of deionized water, and 89ml of alkaline silica sol (28% SiO) was added with stirring 2 pH value of 8) to form a suspension A, and heating to 85 ℃; preparing 2mol/L sodium carbonate solution B; and dripping the solution B into the solution A under the stirring state until the pH value is 9, aging for 4 hours at 85 ℃, then filtering, washing, drying, and roasting for 3 hours at 400 ℃ to obtain active component powder.
The powder obtained above was ground to 300 mesh or less, and 50g of diatomaceous earth (SiO) was added 2 Content is more than or equal to 90%), 75g of pseudo-powder is fully and evenly mixed, rolled and formed by a sugar-coating machine, kept stand in air and dried, roasted at 400 ℃ for 4 hours and naturally cooled to room temperature for standby.
Example 7
The purifiers of examples 1 to 6 were measured for impurity removal capacity and removal depth. The measurement method is as follows: taking 20ml of sample, loading the sample into a stainless steel reactor with the diameter of 15mm, introducing nitrogen with the volume proportion of 2 percent of hydrogen at the temperature of 250 ℃, and keeping the volume space velocity for 500h -1 Reducing for 12h and cooling to room temperature. Introducing balance gases of argon, methane and helium at normal pressure and 25 ℃; nitrogen, with an impurity composition of 200ppmO 2 -200ppmH 2 、-200ppmCO-200ppmCO 2 -200ppmH 2 The gas volume space velocity of the mixed feed gas of O is 5000h -1 . The impurity content in the reacted gas was detected on-line during the test, and the experiment was stopped when the impurity concentration after the reaction exceeded 10ppb (v/v).
Figure BDA0002845625990000041
Figure BDA0002845625990000051
The data in Table 1 show that the purifiers of examples 1-6 are directed to impurity O in high purity gas feed gas 2 、H 2 、CO、CO 2 And H 2 O has good adsorption capacity and purification depth.
Example 8
The scavenger prepared in example 5 was subjected to a multiple "regeneration activation-cycle test". The measurement method is as follows: taking 20ml of sample, loading the sample into a stainless steel reactor with the diameter of 15mm, introducing nitrogen with the volume proportion of 2 percent of hydrogen at the temperature of 250 ℃, and keeping the volume space velocity for 500h -1 Reducing for 12h and then cooling to room temperature. (1) At normal pressure and 25 ℃, the composition of 200ppmO is introduced 2 -200ppmH 2 -200ppmCO-200ppmCO 2 -200ppmH 2 O and the balance of nitrogen, wherein the gas volume space velocity is 5000h -1 . The impurity content in the reacted gas was detected on-line during the test, and the experiment was stopped when the impurity concentration after the reaction exceeded 10ppb (v/v). (2) Switching to high-purity nitrogen for system purging, heating to 250 ℃, introducing nitrogen with 2% hydrogen volume ratio, and keeping the volume space velocity for 500h -1 Reducing for 12H, then cutting in high-purity nitrogen to continuously purge H in tail gas 2 The content is less than 10ppb, and the raw material gas is cut into the raw material gas after being cooled to room temperature for the second evaluation test. The above steps (1) and (2) are repeated, and the experimental results are summarized in the following table 2.
Figure BDA0002845625990000052
As can be seen from the data in the table, the purifying agent prepared in example 5 still maintains higher adsorption capacity and lower purification depth after 50 purification-regeneration cycle tests, and still has adsorption capacity not lower than 80% compared with the experimental result of the first test.

Claims (4)

1. A purifying agent for removing trace impurities in high-purity gas is characterized in that:
taking 106gCu (NO) 3 ) 2 ·3H 2 O、1012gNi(NO 3 ) 2 ·6H 2 O 、138g 50wt%Mn(NO 3 ) 2 And 126gFe (NO) 3 ) 3 ·9H 2 Dissolving O in 2600ml deionized water, adding 69g of metatitanic acid with less than 200 meshes and 60g of SiO with less than 200 meshes while stirring 2 Forming a suspension A, and heating to 70 ℃ for later use; preparing 2mol/L sodium carbonate solution B; dripping the suspension A into the suspension B under stirring until the pH value is 9, aging at 70 ℃ for 1 hour, filtering, washing, drying, and roasting at 300 ℃ for 2 hours to obtain active component powder;
grinding the above obtained active ingredient powder to below 300 mesh, adding 67ml of 28% SiO% 2 The pH value of the alkaline silica sol is 8, 25g of pseudo-thin powder is fully and uniformly mixed, a strip is extruded by a strip extruding machine for forming, the mixture is stood in the air for airing, and the mixture is roasted at 300 ℃ for 4 hours and naturally cooled to the room temperature, so that the purifying agent is obtained.
2. A purifying agent for removing trace impurities in high-purity gas is characterized in that:
take 61g (NH) 4 ) 6 Mo 7 O 24 ·4H 2 O、304gCu(NO 3 ) 2 ·3H 2 O、584g Ni(NO 3 ) 2 ·6H 2 O 、315g 50wt%Mn(NO 3 ) 2 Dissolved in 2400ml of deionized water and stirred with 25g of TiO 2 179ml 28% SiO 2 The pH value of the alkaline silica sol is 8 to form a suspension A, and the suspension A is heated to 60 ℃; preparing 2mol/L sodium carbonate solution B; dripping the solution B into the solution A under stirring until the pH value is 8, aging for 1 hour at 60 ℃, then filtering, washing, drying, and roasting for 2 hours at 500 ℃ to obtain active component powder;
grinding the obtained active component powder to below 300 mesh, adding 50g SiO 2 Fully and uniformly mixing diatomite with the content of more than or equal to 90 percent and 105g of high-alumina cement, rolling and molding by using a sugar coating machine, standing and airing in the air, roasting at 500 ℃ for 4 hours, and naturally cooling to room temperature to obtain the purifying agent.
3. A purifying agent for removing trace impurities in high-purity gas is characterized in that:
taking 379gFe (NO) 3 ) 3 ·9H 2 O 、76gCu(NO 3 ) 2 ·3H 2 O、292gNi(NO 3 ) 2 ·6H 2 O、694g 50wt%Mn(NO 3 ) 2 Dissolving in 2000ml deionized water, adding 45g of pseudo-thin powder and 25g of SiO while stirring 2 Forming a suspension A and heating to 70 ℃; preparing 2mol/L sodium carbonate solution B; dripping the solution B into the solution A under stirring until the pH value is 8.5, aging at 70 ℃ for 3 hours, then filtering, washing, drying, and roasting at 350 ℃ for 2 hours to obtain active component powder;
adding 100ml of SiO in a concentration of 28% 2 The pH value of the alkaline silica sol is 8, 50g of metatitanic acid is fully and uniformly mixed, the mixture is extruded by a strip extruder to be formed, is kept stand in the air and dried, and is roasted at 350 ℃ for 4 hours and naturally cooled to the room temperature, so that the purifying agent is obtained.
4. Use of a scavenger for the removal of trace impurities from a high purity gas according to any one of claims 1 to 3, characterized in that: the use of said scavenger for the purification of nitrogen, hydrogen, oxygen, argon, helium and organic gases.
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CN114146685A (en) * 2021-12-09 2022-03-08 大连圣迈化学有限公司 Nickel-based purifying agent and preparation method and application thereof

Family Cites Families (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1667129C3 (en) * 1967-06-20 1978-06-29 Messer Griesheim Gmbh, 6000 Frankfurt Process for removing homogeneously dissolved impurities, in particular oxygen, from gases or liquids
DE3618942A1 (en) * 1986-06-05 1987-12-10 Messer Griesheim Gmbh DIMENSIONS FOR REMOVAL BY CHEMICAL SORPTION OF HOMOGENEOUSLY SOLVED ADDITIVES, IN PARTICULAR OXYGEN, FROM GASES OR LIQUIDS
CN1031746C (en) * 1993-12-24 1996-05-08 华东理工大学 Preparation of effective Mo-family deoxidiser
US7160360B2 (en) * 2003-12-08 2007-01-09 Air Products And Chemicals, Inc. Purification of hydride gases
US8637723B2 (en) * 2010-09-09 2014-01-28 Guido Henze Process for the activation of a copper-, zinc- and zirconium oxide-comprising adsorption composition
CN103127821A (en) * 2011-11-30 2013-06-05 中国石油化工股份有限公司 Gas purification method
US20180333676A1 (en) * 2017-05-22 2018-11-22 Pure Air Filtration, LLC Adsorbent materials, apparatus, and methods for removal of hydrogen sulfide from gases
CN109539284B (en) * 2018-11-27 2020-06-16 中国科学院大连化学物理研究所 Oxygen carrier for purifying inert gas and preparation and application thereof
EP3967396A4 (en) * 2019-05-06 2023-04-12 China Petroleum & Chemical Corporation Catalyst for dehydrogenating organic hydrogen storage raw material, carrier for catalyst, hydrogen storage alloy, and method for providing high purity hydrogen
CN111893360B (en) * 2019-05-06 2022-10-21 中国石油化工股份有限公司 AB 5 Hydrogen storage alloy, preparation method and application thereof, and method for purifying hydrogen containing organic matters
CN110280206A (en) * 2019-08-05 2019-09-27 大连中鼎化学有限公司 A kind of multi-functional adsorbent and preparation method thereof, application

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