CN117101375A - Inert gas purification material and preparation method thereof - Google Patents

Inert gas purification material and preparation method thereof Download PDF

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CN117101375A
CN117101375A CN202311233982.4A CN202311233982A CN117101375A CN 117101375 A CN117101375 A CN 117101375A CN 202311233982 A CN202311233982 A CN 202311233982A CN 117101375 A CN117101375 A CN 117101375A
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catalyst
inert gas
gas purification
purification material
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CN117101375B (en
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李志超
孙林
陈应培
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Yingde Xizhou Gas Co ltd
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    • 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
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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
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    • B01D53/34Chemical or biological purification of waste gases
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    • B01D53/34Chemical or biological purification of waste gases
    • B01D53/74General processes for purification of waste gases; Apparatus or devices specially adapted therefor
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    • B01D53/78Liquid phase processes with gas-liquid contact
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    • B01D53/34Chemical or biological purification of waste gases
    • B01D53/74General processes for purification of waste gases; Apparatus or devices specially adapted therefor
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    • B01D53/74General processes for purification of waste gases; Apparatus or devices specially adapted therefor
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Abstract

The application relates to the technical field of inert gas purification, and particularly discloses an inert gas purification material and a preparation method thereof. An inert gas purification material comprising the following components: deionized water, sodium hydroxide, sodium peroxyacetate, barium carbonate, a catalyst and a thickener; the catalyst is a compound of cobalt catalyst, iridium catalyst and platinum catalyst. The preparation method of the inert gas purification material comprises the following steps: step 1), mixing deionized water and sodium hydroxide to obtain a premix; and 2) cooling to room temperature, adding sodium peroxyacetate, barium carbonate, a catalyst and a thickening agent into the premix, and uniformly stirring to obtain the inert gas purification material. The application has the advantages of simplifying the inert gas purification process and reducing the cost.

Description

Inert gas purification material and preparation method thereof
Technical Field
The application relates to the field of inert gas purification, in particular to an inert gas purification material and a preparation method thereof.
Background
With the development of technology, the use of inert gas in the manufacturing process is more and more widely used, especially in the semiconductor production process, when manufacturing a semiconductor device, plasma is generated by ionization energy of the inert gas, ion sputtering, plasma CVD film growth, ion etching and the like are important parts in the semiconductor device production process, with the rapid development of the semiconductor industry, the demand for inert gas is more and more increased, wherein helium is the most used one of the inert gases, but the inert gas is also called rare gas, the inert gas is very rare in resources on the earth and is expensive, so that the inert gas needs to be collected and recycled, otherwise, the inert gas related production process is difficult to implement.
The inert gas is introduced with impurity gases such as water, nitrogen, oxygen, carbon dioxide, hydrogen, hydrocarbon and the like after being used in the production process, the impurity gases need to be removed to improve the purity of the inert gas, otherwise, the inert gas with low purity can seriously affect the quality of a semiconductor device, a complex gas purifying device is mainly adopted in the prior art, a plurality of multi-step procedures are used for removing various impurity gases one by one, the inert gas purifying process is quite complex, the cost is high, and therefore, the improvement room is left.
Disclosure of Invention
In order to simplify the inert gas purification process and reduce the cost, the application provides an inert gas purification material and a preparation method thereof.
In a first aspect, the present application provides an inert gas purification material, which adopts the following technical scheme:
an inert gas purification material comprises the following components in parts by mass:
100 parts of deionized water;
30-40 parts of sodium hydroxide;
15-20 parts of sodium peroxyacetate;
10-15 parts of barium carbonate;
2-3 parts of a catalyst;
15-20 parts of a thickening agent;
the catalyst is a compound of a cobalt catalyst, an iridium catalyst and a platinum catalyst.
According to the technical scheme, sodium peroxyacetate is used as an oxidant, under the action of a catalyst formed by compounding a cobalt catalyst, an iridium catalyst and a platinum catalyst, hydrocarbon in the inert gas can be rapidly oxidized after the inert gas is introduced into a purification material, so that carbon dioxide and water are formed, the carbon dioxide can form sodium carbonate to be dissolved in the purification material under the action of a sodium hydroxide solution, so that the hydrocarbon and the carbon dioxide are removed, nitrogen is adsorbed by the action of barium carbonate, the nitrogen is removed, and the oxygen and the hydrogen generate water under the action of the catalyst to be removed, so that the inert gas can achieve a good purification effect by introducing the inert gas into the purification material, multiple complex process steps are not needed, the preparation of the purification material is very convenient, the complexity of an inert gas purification process is effectively reduced, and the effect of reducing the cost is well achieved.
Through adding the thickening agent, the purification material has higher consistency, the inert gas can stay in the purification material for a longer time when being introduced into the purification material, and the inert gas can form bubbles with smaller diameters only by adding and stirring when being introduced into the inert gas, so that the impurity gas in the inert gas can fully react or be adsorbed, and the inert gas can have good purification effect only by once introducing the inert gas into the purification material when the inlet of the inert gas is introduced into the purification material and the height of the liquid level of the purification material is more than 1m, so that the purification efficiency is higher.
Preferably, the cobalt catalyst, iridium catalyst and platinum catalyst are all water-soluble substances.
By adopting the technical scheme, the cobalt catalyst, the iridium catalyst and the platinum catalyst are all water-soluble substances, so that the catalyst can be dissolved in water, the catalytic effect is better, the sodium peroxyacetate can rapidly oxidize hydrocarbon with complex components, and the gas purification effect is better.
Preferably, the cobalt catalyst is cobalt acetate, the iridium catalyst is iridium trichloride, and the platinum catalyst is chloroplatinic acid.
By adopting the technical scheme, the cobalt acetate, the iridium trichloride and the chloroplatinic acid are specifically selected to be compounded into the catalyst, so that the catalytic oxidation effect is better, complex hydrocarbon is better and rapidly oxidized, the efficiency of inert gas purification is higher, and the purification effect is better.
Preferably, the mass ratio of the cobalt acetate to the iridium trichloride to the chloroplatinic acid is 3-4:1-2:6-7.
By adopting the technical scheme, the cobalt acetate, the iridium trichloride and the chloroplatinic acid are matched with each other by specifically selecting the mass ratio of the cobalt acetate, the iridium trichloride and the chloroplatinic acid, so that the catalytic oxidation effect is better, the inert gas purification effect is further improved, and the purity of the purified inert gas is higher.
Preferably, the thickener is a compound of nano silicon dioxide and polyethylene glycol.
Through adopting above-mentioned technical scheme, through specifically selecting nano silica, polyethylene glycol to compound, the thickening effect is better, and nano silica surface has a large amount of micropores moreover, can also play fine physical adsorption effect when playing the thickening effect, and polyethylene glycol has fine hygroscopicity moreover for the steam is difficult for following inert gas and discharges, thereby makes purifying effect better, and purity after the inert gas purification is higher.
Preferably, the mass ratio of the nano silicon dioxide to the polyethylene glycol is 2:1-3.
By adopting the technical scheme, the thickening effect is better and the purification effect of inert gas is better by specifically selecting the mass ratio of the nano silicon dioxide to the polyethylene glycol.
Preferably, the molecular weight of the polyethylene glycol is more than or equal to 4000.
By adopting the technical scheme, the thickening effect is better by specifically selecting the molecular weight of polyethylene glycol, and the inert gas can be better purified in the purification material, so that the purity after purification is higher.
In a second aspect, the present application provides a method for preparing an inert gas purification material, which adopts the following technical scheme:
the preparation method of the inert gas purification material comprises the following steps:
step 1), mixing deionized water and sodium hydroxide to obtain a premix;
and 2) cooling to room temperature, adding sodium peroxyacetate, barium carbonate, a catalyst and a thickening agent into the premix, and uniformly stirring to obtain the inert gas purification material.
By adopting the technical scheme, the prepared purification material can deeply purify the inert gas, so that the inert gas can have a good purification effect after being introduced into the purification material, the purity of the purified inert gas is higher, the preparation of the purification material is simple, the process steps for purifying the inert gas are simpler and more convenient, complex large-scale equipment is not needed to be matched, the difficulty and cost of an inert gas purification process are effectively reduced, and the application value is higher.
In summary, the application has the following beneficial effects:
1. according to the application, sodium peroxyacetate is used as an oxidant, under the action of a catalyst formed by compounding a cobalt catalyst, an iridium catalyst and a platinum catalyst, hydrocarbon in the inert gas can be rapidly oxidized after the inert gas is introduced into a purification material, so that carbon dioxide and water are formed, and under the action of a sodium hydroxide solution, the carbon dioxide can form sodium carbonate to be dissolved in the purification material, so that the hydrocarbon and the carbon dioxide are removed, and then nitrogen is adsorbed by the action of barium carbonate, and then the nitrogen and the oxygen are removed under the action of the catalyst to generate water, so that the inert gas can realize good purification effect by introducing the inert gas into the purification material, multiple complex process steps are not needed, the preparation of the purification material is very convenient, the complexity of an inert gas purification process is effectively reduced, and the effect of reducing the cost is well realized.
2. According to the application, the thickening agent is preferably added, so that the purification material has higher consistency, the inert gas can stay in the purification material for a longer time when being introduced into the purification material, and the inert gas can form bubbles with smaller diameters only by adding and stirring while being introduced into the inert gas, so that the impurity gas in the inert gas can fully react or be adsorbed, and therefore, when the height of an inlet of the inert gas when being introduced into the purification material and the liquid level of the purification material is more than 1m, the inert gas can have a good purification effect only by being introduced into the purification material once, and the purification efficiency is higher.
3. In the application, the cobalt catalyst, the iridium catalyst and the platinum catalyst are water-soluble substances, so that the catalyst can be dissolved in water, the catalytic effect is better, the sodium peroxyacetate can rapidly oxidize hydrocarbon with complex components, and the gas purification effect is better.
Detailed Description
The present application will be described in further detail with reference to examples.
Example 1
An inert gas purification material, consisting of the following components:
deionized water, sodium hydroxide, sodium peroxyacetate, barium carbonate, a catalyst and a thickener.
Wherein, the sodium hydroxide is from commercial market, and CAS number is: 1310-73-2.
Wherein, the sodium peroxyacetate is from commercial market, and the CAS number is: 64057-57-4.
Wherein, barium carbonate comes from commercial market, CAS number is: 513-77-9.
Wherein the catalyst is a compound of cobalt catalyst, iridium catalyst and platinum catalyst.
Cobalt catalyst is cobalt acetate which is commercially available and has the CAS number of: 71-48-7.
The iridium catalyst is iridium trichloride which is commercially available, and the CAS number is: 14996-61-3.
The platinum catalyst is chloroplatinic acid from commercial sources, CAS number: 16941-12-1.
The catalyst was prepared by stirring 3kg of cobalt acetate, 1kg of iridium trichloride, and 6kg of chloroplatinic acid at 120r/min for 10 min.
Wherein the thickener is the compounding of nano silicon dioxide and polyethylene glycol.
The nano silicon dioxide is purchased from Lingshu county Maozuo building materials limited company, 1250 mesh.
Polyethylene glycol is polyethylene glycol-4000 purchased and placed in Jiangsu province sea-safe petrochemical plants.
The thickener is prepared by stirring 20kg of nano silicon dioxide, 10kg of polyethylene glycol-4000 at 120r/min for 10 min.
The preparation method of the inert gas purification material comprises the following steps:
step 1), 100kg of deionized water and 30kg of sodium hydroxide are weighed and put into a stirring kettle, and the stirring is carried out at the rotating speed of 35r/min until the deionized water and the 30kg of sodium hydroxide are completely dissolved, so as to obtain a premix.
And 2) naturally cooling the premix to room temperature, and then adding 15kg of sodium peroxyacetate, 10kg of barium carbonate, 2kg of catalyst and 15kg of thickener into the premix, stirring for 15min at the rotating speed of 120r/min, and uniformly stirring to obtain the inert gas purification material.
Example 2
An inert gas purification material, consisting of the following components:
deionized water, sodium hydroxide, sodium peroxyacetate, barium carbonate, a catalyst and a thickener.
Wherein, the sodium hydroxide is from commercial market, and CAS number is: 1310-73-2.
Wherein, the sodium peroxyacetate is from commercial market, and the CAS number is: 64057-57-4.
Wherein, barium carbonate comes from commercial market, CAS number is: 513-77-9.
Wherein the catalyst is a compound of cobalt catalyst, iridium catalyst and platinum catalyst.
Cobalt catalyst is cobalt acetate which is commercially available and has the CAS number of: 71-48-7.
The iridium catalyst is iridium trichloride which is commercially available, and the CAS number is: 14996-61-3.
The platinum catalyst is chloroplatinic acid from commercial sources, CAS number: 16941-12-1.
The catalyst was prepared from 3.5kg of cobalt acetate, 1.5kg of iridium trichloride and 6.5kg of chloroplatinic acid by stirring at 120r/min for 10 min.
Wherein the thickener is the compounding of nano silicon dioxide and polyethylene glycol.
The nano silicon dioxide is purchased from Lingshu county Maozuo building materials limited company, 1250 mesh.
Polyethylene glycol is polyethylene glycol-4000 purchased and placed in Jiangsu province sea-safe petrochemical plants.
The thickener is prepared by stirring 20kg of nano silicon dioxide and 20kg of polyethylene glycol-4000 at 120r/min for 10 min.
The preparation method of the inert gas purification material comprises the following steps:
step 1), 100kg of deionized water and 35kg of sodium hydroxide are weighed and put into a stirring kettle, and the stirring is carried out at the rotating speed of 35r/min until the deionized water and the 35kg of sodium hydroxide are completely dissolved, so as to obtain a premix.
And 2) naturally cooling the premix to room temperature, and then adding 18kg of sodium peroxyacetate, 13kg of barium carbonate, 2.5kg of catalyst and 18kg of thickener into the premix, stirring for 15min at the rotating speed of 120r/min, and uniformly stirring to obtain the inert gas purification material.
Example 3
An inert gas purification material, consisting of the following components:
deionized water, sodium hydroxide, sodium peroxyacetate, barium carbonate, a catalyst and a thickener.
Wherein, the sodium hydroxide is from commercial market, and CAS number is: 1310-73-2.
Wherein, the sodium peroxyacetate is from commercial market, and the CAS number is: 64057-57-4.
Wherein, barium carbonate comes from commercial market, CAS number is: 513-77-9.
Wherein the catalyst is a compound of cobalt catalyst, iridium catalyst and platinum catalyst.
Cobalt catalyst is cobalt acetate which is commercially available and has the CAS number of: 71-48-7.
The iridium catalyst is iridium trichloride which is commercially available, and the CAS number is: 14996-61-3.
The platinum catalyst is chloroplatinic acid from commercial sources, CAS number: 16941-12-1.
The catalyst was prepared from 4kg of cobalt acetate, 2kg of iridium trichloride and 7kg of chloroplatinic acid by stirring at 120r/min for 10 min.
Wherein the thickener is the compounding of nano silicon dioxide and polyethylene glycol.
The nano silicon dioxide is purchased from Lingshu county Maozuo building materials limited company, 1250 mesh.
Polyethylene glycol is polyethylene glycol-6000 purchased and placed in Jiangsu province sea-safe petrochemical plants.
The thickener is prepared by stirring 20kg of nano silicon dioxide and 30kg of polyethylene glycol-4000 at 120r/min for 10 min.
The preparation method of the inert gas purification material comprises the following steps:
step 1), 100kg of deionized water and 40kg of sodium hydroxide are weighed and put into a stirring kettle, and the stirring is carried out at the rotating speed of 35r/min until the deionized water and the 40kg of sodium hydroxide are completely dissolved, so as to obtain a premix.
And 2) naturally cooling the premix to room temperature, and then adding 20kg of sodium peroxyacetate, 15kg of barium carbonate, 3kg of catalyst and 20kg of thickener into the premix, stirring for 15min at the rotating speed of 120r/min, and uniformly stirring to obtain the inert gas purification material.
Example 4
An inert gas purification material, consisting of the following components:
deionized water, sodium hydroxide, sodium peroxyacetate, barium carbonate, a catalyst and a thickener.
Wherein, the sodium hydroxide is from commercial market, and CAS number is: 1310-73-2.
Wherein, the sodium peroxyacetate is from commercial market, and the CAS number is: 64057-57-4.
Wherein, barium carbonate comes from commercial market, CAS number is: 513-77-9.
Wherein the catalyst is a compound of cobalt catalyst, iridium catalyst and platinum catalyst.
Cobalt catalyst is cobalt nitrate from commercial sources, CAS number: 10141-05-6.
The iridium catalyst is iridium tetrachloride which is commercially available and has the CAS number of: 10025-97-5.
The platinum catalyst was platinum chloride, commercially available with CAS number: 13454-96-1.
The catalyst was prepared from 3.5kg of cobalt nitrate, 1.5kg of iridium tetrachloride and 6.5kg of platinum chloride by stirring at 120r/min for 10 min.
Wherein the thickener is the compounding of nano silicon dioxide and polyethylene glycol.
The nano silicon dioxide is purchased from Lingshu county Maozuo building materials limited company, 1250 mesh.
Polyethylene glycol is polyethylene glycol-4000 purchased and placed in Jiangsu province sea-safe petrochemical plants.
The thickener is prepared by stirring 20kg of nano silicon dioxide and 20kg of polyethylene glycol-4000 at 120r/min for 10 min.
The preparation method of the inert gas purification material comprises the following steps:
step 1), 100kg of deionized water and 35kg of sodium hydroxide are weighed and put into a stirring kettle, and the stirring is carried out at the rotating speed of 35r/min until the deionized water and the 35kg of sodium hydroxide are completely dissolved, so as to obtain a premix.
And 2) naturally cooling the premix to room temperature, and then adding 18kg of sodium peroxyacetate, 13kg of barium carbonate, 2.5kg of catalyst and 18kg of thickener into the premix, stirring for 15min at the rotating speed of 120r/min, and uniformly stirring to obtain the inert gas purification material.
Example 5
An inert gas purification material, consisting of the following components:
deionized water, sodium hydroxide, sodium peroxyacetate, barium carbonate, a catalyst and a thickener.
Wherein, the sodium hydroxide is from commercial market, and CAS number is: 1310-73-2.
Wherein, the sodium peroxyacetate is from commercial market, and the CAS number is: 64057-57-4.
Wherein, barium carbonate comes from commercial market, CAS number is: 513-77-9.
Wherein the catalyst is a compound of cobalt catalyst, iridium catalyst and platinum catalyst.
Cobalt catalyst is cobalt iso-octoate from commercial sources, CAS number: 136-52-7.
The iridium catalyst is chloroiridic acid which is commercially available and has the CAS number of: 16941-92-7.
The platinum catalyst is sodium chloroplatinate and is commercially available, and CAS number is: 19583-77-8.
The catalyst was prepared from 3.5kg cobalt iso-octoate, 1.5kg chloroiridium acid, 6.5kg sodium chloroplatinate with stirring at 120r/min for 10 min.
Wherein the thickener is the compounding of nano silicon dioxide and polyethylene glycol.
The nano silicon dioxide is purchased from Lingshu county Maozuo building materials limited company, 1250 mesh.
Polyethylene glycol is polyethylene glycol-4000 purchased and placed in Jiangsu province sea-safe petrochemical plants.
The thickener is prepared by stirring 20kg of nano silicon dioxide and 20kg of polyethylene glycol-4000 at 120r/min for 10 min.
The preparation method of the inert gas purification material comprises the following steps:
step 1), 100kg of deionized water and 35kg of sodium hydroxide are weighed and put into a stirring kettle, and the stirring is carried out at the rotating speed of 35r/min until the deionized water and the 35kg of sodium hydroxide are completely dissolved, so as to obtain a premix.
And 2) naturally cooling the premix to room temperature, and then adding 18kg of sodium peroxyacetate, 13kg of barium carbonate, 2.5kg of catalyst and 18kg of thickener into the premix, stirring for 15min at the rotating speed of 120r/min, and uniformly stirring to obtain the inert gas purification material.
Example 6
An inert gas purification material, consisting of the following components:
deionized water, sodium hydroxide, sodium peroxyacetate, barium carbonate, a catalyst and a thickener.
Wherein, the sodium hydroxide is from commercial market, and CAS number is: 1310-73-2.
Wherein, the sodium peroxyacetate is from commercial market, and the CAS number is: 64057-57-4.
Wherein, barium carbonate comes from commercial market, CAS number is: 513-77-9.
Wherein the catalyst is a compound of cobalt catalyst, iridium catalyst and platinum catalyst.
Cobalt catalyst is cobalt carbonate from commercial sources, CAS number: 513-79-1.
The iridium catalyst is iridium oxide and is commercially available, and the CAS number is: 12030-49-8.
The platinum catalyst is platinum oxide and is commercially available, and the CAS number is: 1314-15-4.
The catalyst was prepared from 3.5kg of cobalt carbonate, 1.5kg of iridium oxide, and 6.5kg of platinum oxide by stirring at 120r/min for 10 min.
Wherein the thickener is the compounding of nano silicon dioxide and polyethylene glycol.
The nano silicon dioxide is purchased from Lingshu county Maozuo building materials limited company, 1250 mesh.
Polyethylene glycol is polyethylene glycol-4000 purchased and placed in Jiangsu province sea-safe petrochemical plants.
The thickener is prepared by stirring 20kg of nano silicon dioxide and 20kg of polyethylene glycol-4000 at 120r/min for 10 min.
The preparation method of the inert gas purification material comprises the following steps:
step 1), 100kg of deionized water and 35kg of sodium hydroxide are weighed and put into a stirring kettle, and the stirring is carried out at the rotating speed of 35r/min until the deionized water and the 35kg of sodium hydroxide are completely dissolved, so as to obtain a premix.
And 2) naturally cooling the premix to room temperature, and then adding 18kg of sodium peroxyacetate, 13kg of barium carbonate, 2.5kg of catalyst and 18kg of thickener into the premix, stirring for 15min at the rotating speed of 120r/min, and uniformly stirring to obtain the inert gas purification material.
Comparative example 1
An inert gas purification material, consisting of the following components:
deionized water, sodium hydroxide, sodium peroxyacetate, barium carbonate, a catalyst and a thickener.
Wherein, the sodium hydroxide is from commercial market, and CAS number is: 1310-73-2.
Wherein, the sodium peroxyacetate is from commercial market, and the CAS number is: 64057-57-4.
Wherein, barium carbonate comes from commercial market, CAS number is: 513-77-9.
Wherein the catalyst is a manganese catalyst, an iridium catalyst and a platinum catalyst.
The manganese catalyst is manganese acetate which is commercially available and has the CAS number of: 19513-05-4.
The iridium catalyst is iridium trichloride which is commercially available, and the CAS number is: 14996-61-3.
The platinum catalyst is chloroplatinic acid from commercial sources, CAS number: 16941-12-1.
The catalyst was prepared from 3.5kg manganese acetate, 1.5kg iridium trichloride, 6.5kg chloroplatinic acid at 120r/min with stirring for 10 min.
Wherein the thickener is the compounding of nano silicon dioxide and polyethylene glycol.
The nano silicon dioxide is purchased from Lingshu county Maozuo building materials limited company, 1250 mesh.
Polyethylene glycol is polyethylene glycol-4000 purchased and placed in Jiangsu province sea-safe petrochemical plants.
The thickener is prepared by stirring 20kg of nano silicon dioxide and 20kg of polyethylene glycol-4000 at 120r/min for 10 min.
The preparation method of the inert gas purification material comprises the following steps:
step 1), 100kg of deionized water and 35kg of sodium hydroxide are weighed and put into a stirring kettle, and the stirring is carried out at the rotating speed of 35r/min until the deionized water and the 35kg of sodium hydroxide are completely dissolved, so as to obtain a premix.
And 2) naturally cooling the premix to room temperature, and then adding 18kg of sodium peroxyacetate, 13kg of barium carbonate, 2.5kg of catalyst and 18kg of thickener into the premix, stirring for 15min at the rotating speed of 120r/min, and uniformly stirring to obtain the inert gas purification material.
Comparative example 2
An inert gas purification material, consisting of the following components:
deionized water, sodium hydroxide, sodium peroxyacetate, barium carbonate, a catalyst and a thickener.
Wherein, the sodium hydroxide is from commercial market, and CAS number is: 1310-73-2.
Wherein, the sodium peroxyacetate is from commercial market, and the CAS number is: 64057-57-4.
Wherein, barium carbonate comes from commercial market, CAS number is: 513-77-9.
Wherein the catalyst is a compound of cobalt catalyst, tin catalyst and platinum catalyst.
Cobalt catalyst is cobalt acetate which is commercially available and has the CAS number of: 71-48-7.
The tin catalyst is dimethyl tin dichloride which is commercially available and has the CAS number of: 753-73-1.
The platinum catalyst is chloroplatinic acid from commercial sources, CAS number: 16941-12-1.
The catalyst was prepared from 3.5kg of cobalt acetate, 1.5kg of dimethyl tin dichloride and 6.5kg of chloroplatinic acid by stirring at 120r/min for 10 min.
Wherein the thickener is the compounding of nano silicon dioxide and polyethylene glycol.
The nano silicon dioxide is purchased from Lingshu county Maozuo building materials limited company, 1250 mesh.
Polyethylene glycol is polyethylene glycol-4000 purchased and placed in Jiangsu province sea-safe petrochemical plants.
The thickener is prepared by stirring 20kg of nano silicon dioxide and 20kg of polyethylene glycol-4000 at 120r/min for 10 min.
The preparation method of the inert gas purification material comprises the following steps:
step 1), 100kg of deionized water and 35kg of sodium hydroxide are weighed and put into a stirring kettle, and the stirring is carried out at the rotating speed of 35r/min until the deionized water and the 35kg of sodium hydroxide are completely dissolved, so as to obtain a premix.
And 2) naturally cooling the premix to room temperature, and then adding 18kg of sodium peroxyacetate, 13kg of barium carbonate, 2.5kg of catalyst and 18kg of thickener into the premix, stirring for 15min at the rotating speed of 120r/min, and uniformly stirring to obtain the inert gas purification material.
Comparative example 3
An inert gas purification material, consisting of the following components:
deionized water, sodium hydroxide, sodium peroxyacetate, barium carbonate, a catalyst and a thickener.
Wherein, the sodium hydroxide is from commercial market, and CAS number is: 1310-73-2.
Wherein, the sodium peroxyacetate is from commercial market, and the CAS number is: 64057-57-4.
Wherein, barium carbonate comes from commercial market, CAS number is: 513-77-9.
Wherein the catalyst is a compound of cobalt catalyst, iridium catalyst and zinc catalyst.
Cobalt catalyst is cobalt acetate which is commercially available and has the CAS number of: 71-48-7.
The iridium catalyst is iridium trichloride which is commercially available, and the CAS number is: 14996-61-3.
The zinc catalyst is zinc chloride which is commercially available and has the CAS number of: 7646-85-7.
The catalyst was prepared from 3.5kg of cobalt acetate, 1.5kg of iridium trichloride, 6.5kg of zinc chloride, and stirring at 120r/min for 10 min.
Wherein the thickener is the compounding of nano silicon dioxide and polyethylene glycol.
The nano silicon dioxide is purchased from Lingshu county Maozuo building materials limited company, 1250 mesh.
Polyethylene glycol is polyethylene glycol-4000 purchased and placed in Jiangsu province sea-safe petrochemical plants.
The thickener is prepared by stirring 20kg of nano silicon dioxide and 20kg of polyethylene glycol-4000 at 120r/min for 10 min.
The preparation method of the inert gas purification material comprises the following steps:
step 1), 100kg of deionized water and 35kg of sodium hydroxide are weighed and put into a stirring kettle, and the stirring is carried out at the rotating speed of 35r/min until the deionized water and the 35kg of sodium hydroxide are completely dissolved, so as to obtain a premix.
And 2) naturally cooling the premix to room temperature, and then adding 18kg of sodium peroxyacetate, 13kg of barium carbonate, 2.5kg of catalyst and 18kg of thickener into the premix, stirring for 15min at the rotating speed of 120r/min, and uniformly stirring to obtain the inert gas purification material.
Comparative example 4
An inert gas purification material, consisting of the following components:
deionized water, sodium hydroxide, sodium peroxyacetate, barium carbonate, a catalyst and a thickener.
Wherein, the sodium hydroxide is from commercial market, and CAS number is: 1310-73-2.
Wherein, the sodium peroxyacetate is from commercial market, and the CAS number is: 64057-57-4.
Wherein, barium carbonate comes from commercial market, CAS number is: 513-77-9.
Wherein the catalyst is a manganese catalyst, a tin catalyst and a zinc catalyst.
The manganese catalyst is manganese acetate which is commercially available and has the CAS number of: 19513-05-4.
The tin catalyst is dimethyl tin dichloride which is commercially available and has the CAS number of: 753-73-1.
The zinc catalyst is zinc chloride which is commercially available and has the CAS number of: 7646-85-7.
The catalyst was prepared by stirring 3.5kg of manganese acetate, 1.5kg of dimethyl tin dichloride and 6.5kg of zinc chloride at 120r/min for 10 min.
Wherein the thickener is the compounding of nano silicon dioxide and polyethylene glycol.
The nano silicon dioxide is purchased from Lingshu county Maozuo building materials limited company, 1250 mesh.
Polyethylene glycol is polyethylene glycol-4000 purchased and placed in Jiangsu province sea-safe petrochemical plants.
The thickener is prepared by stirring 20kg of nano silicon dioxide and 20kg of polyethylene glycol-4000 at 120r/min for 10 min.
The preparation method of the inert gas purification material comprises the following steps:
step 1), 100kg of deionized water and 35kg of sodium hydroxide are weighed and put into a stirring kettle, and the stirring is carried out at the rotating speed of 35r/min until the deionized water and the 35kg of sodium hydroxide are completely dissolved, so as to obtain a premix.
And 2) naturally cooling the premix to room temperature, and then adding 18kg of sodium peroxyacetate, 13kg of barium carbonate, 2.5kg of catalyst and 18kg of thickener into the premix, stirring for 15min at the rotating speed of 120r/min, and uniformly stirring to obtain the inert gas purification material.
Comparative example 5
An inert gas purification material, consisting of the following components:
deionized water, sodium hydroxide, copper oxide, barium carbonate, a catalyst and a thickener.
Wherein, the sodium hydroxide is from commercial market, and CAS number is: 1310-73-2.
Wherein, copper oxide is from commercial market, CAS number: 1317-38-0.
Wherein, barium carbonate comes from commercial market, CAS number is: 513-77-9.
Wherein the catalyst is a compound of cobalt catalyst, iridium catalyst and platinum catalyst.
Cobalt catalyst is cobalt acetate which is commercially available and has the CAS number of: 71-48-7.
The iridium catalyst is iridium trichloride which is commercially available, and the CAS number is: 14996-61-3.
The platinum catalyst is chloroplatinic acid from commercial sources, CAS number: 16941-12-1.
The catalyst was prepared from 3.5kg of cobalt acetate, 1.5kg of iridium trichloride and 6.5kg of chloroplatinic acid by stirring at 120r/min for 10 min.
Wherein the thickener is the compounding of nano silicon dioxide and polyethylene glycol.
The nano silicon dioxide is purchased from Lingshu county Maozuo building materials limited company, 1250 mesh.
Polyethylene glycol is polyethylene glycol-4000 purchased and placed in Jiangsu province sea-safe petrochemical plants.
The thickener is prepared by stirring 20kg of nano silicon dioxide and 20kg of polyethylene glycol-4000 at 120r/min for 10 min.
The preparation method of the inert gas purification material comprises the following steps:
step 1), 100kg of deionized water and 35kg of sodium hydroxide are weighed and put into a stirring kettle, and the stirring is carried out at the rotating speed of 35r/min until the deionized water and the 35kg of sodium hydroxide are completely dissolved, so as to obtain a premix.
And 2) naturally cooling the premix to room temperature, and then adding 18kg of copper oxide, 13kg of barium carbonate, 2.5kg of catalyst and 18kg of thickener into the premix, stirring for 15min at the rotating speed of 120r/min, and uniformly stirring to obtain the inert gas purification material.
Comparative example 6
An inert gas purification material, consisting of the following components:
deionized water, sodium hydroxide, magnesium oxide, barium carbonate, a catalyst and a thickener.
Wherein, the sodium hydroxide is from commercial market, and CAS number is: 1310-73-2.
Wherein, the magnesia is from commercial market, and the CAS number is: 1309-48-4.
Wherein, barium carbonate comes from commercial market, CAS number is: 513-77-9.
Wherein the catalyst is a compound of cobalt catalyst, iridium catalyst and platinum catalyst.
Cobalt catalyst is cobalt acetate which is commercially available and has the CAS number of: 71-48-7.
The iridium catalyst is iridium trichloride which is commercially available, and the CAS number is: 14996-61-3.
The platinum catalyst is chloroplatinic acid from commercial sources, CAS number: 16941-12-1.
The catalyst was prepared from 3.5kg of cobalt acetate, 1.5kg of iridium trichloride and 6.5kg of chloroplatinic acid by stirring at 120r/min for 10 min.
Wherein the thickener is the compounding of nano silicon dioxide and polyethylene glycol.
The nano silicon dioxide is purchased from Lingshu county Maozuo building materials limited company, 1250 mesh.
Polyethylene glycol is polyethylene glycol-4000 purchased and placed in Jiangsu province sea-safe petrochemical plants.
The thickener is prepared by stirring 20kg of nano silicon dioxide and 20kg of polyethylene glycol-4000 at 120r/min for 10 min.
The preparation method of the inert gas purification material comprises the following steps:
step 1), 100kg of deionized water and 35kg of sodium hydroxide are weighed and put into a stirring kettle, and the stirring is carried out at the rotating speed of 35r/min until the deionized water and the 35kg of sodium hydroxide are completely dissolved, so as to obtain a premix.
And 2) naturally cooling the premix to room temperature, and then adding 18kg of magnesium oxide, 13kg of barium carbonate, 2.5kg of catalyst and 18kg of thickener into the premix, stirring for 15min at the rotating speed of 120r/min, and uniformly stirring to obtain the inert gas purification material.
Comparative example 7
An inert gas purification material, consisting of the following components:
deionized water, sodium hydroxide, sodium peroxyacetate, barium carbonate and a catalyst.
Wherein, the sodium hydroxide is from commercial market, and CAS number is: 1310-73-2.
Wherein, the sodium peroxyacetate is from commercial market, and the CAS number is: 64057-57-4.
Wherein, barium carbonate comes from commercial market, CAS number is: 513-77-9.
Wherein the catalyst is a compound of cobalt catalyst, iridium catalyst and platinum catalyst.
Cobalt catalyst is cobalt acetate which is commercially available and has the CAS number of: 71-48-7.
The iridium catalyst is iridium trichloride which is commercially available, and the CAS number is: 14996-61-3.
The platinum catalyst is chloroplatinic acid from commercial sources, CAS number: 16941-12-1.
The catalyst was prepared from 3.5kg of cobalt acetate, 1.5kg of iridium trichloride and 6.5kg of chloroplatinic acid by stirring at 120r/min for 10 min.
The preparation method of the inert gas purification material comprises the following steps:
step 1), 118kg of deionized water and 35kg of sodium hydroxide are weighed and put into a stirring kettle, and the stirring is carried out at the rotating speed of 35r/min until the deionized water and the 35kg of sodium hydroxide are completely dissolved, so as to obtain a premix.
And 2) naturally cooling the premix to room temperature, and then adding 18kg of sodium peroxyacetate, 13kg of barium carbonate and 2.5kg of catalyst into the premix, stirring for 15min at a rotating speed of 120r/min, and uniformly stirring to obtain the inert gas purification material.
Experiment 1
The purity of the inert gas before and after purification by the inert gas purification material of each example and comparative example was measured.
The inert gas is three-stage helium, and the impurity gas comprises water, nitrogen, oxygen, carbon dioxide, hydrogen and hydrocarbon.
The purity of helium gas before purification was 99.563% by helium gas purity measuring instrument, and helium gas used in experiments of each example and comparative example was the same tank helium gas, and the purity was the same.
Helium purity measuring instrument is purchased from Beijing Tiandi head and technology development limited company, model: TD600-SH-He.
The specific experimental process is as follows:
the inert gas purification materials prepared in each embodiment or each comparative example are injected into a purification device, the purification device is a round barrel with two closed ends, the inner diameter is 10cm, the length is 2m, the purification device is placed in a mode that the axis of the purification device is perpendicular to the ground, the top end of the purification device is penetrated with an exhaust hole, the exhaust hole is in sealing connection with an exhaust valve, the exhaust hole can be closed through the exhaust valve or the inside of the purification device is communicated with the outside, the bottom of the purification device is penetrated with an air inlet hole, the air inlet hole is in sealing connection with an air inlet valve, and the exhaust hole can be closed through the air inlet valve or the inside of the purification device is communicated with the outside.
When the inert gas purification material is injected into the purification device, the inert gas purification material is connected with the air inlet valve through a pipeline, the air outlet valve is opened, the inert gas purification material is injected into the purification device from the air inlet valve, and the liquid level of the inert gas purification material is kept at a distance of 10cm from the air outlet valve.
After the injection of the inert gas purification material is completed, the air inlet valve and the air outlet valve are closed, and then the inert gas purification experiment can be prepared.
When inert gas purification experiments are carried out, the air inlet valve is connected through the pipeline, the air outlet valve is opened firstly, then the air inlet valve is opened, the air inlet pressure is controlled to be 0.1MPa, and the air inlet flow is controlled to be 0.1m 3 /h, inlet 3After 0min, the purity of the purified helium gas exiting the vent valve was measured.
The purity of helium after purification by the inert gas purification material of each example or each comparative example is detailed in table 1.
TABLE 1
According to the comparison of the data of each example and the data of the comparative example in the table 1, when the catalyst compounded by adopting the cobalt catalyst, the iridium catalyst and the platinum catalyst is matched with sodium peroxyacetate, the catalytic oxidation effect on impurity gas is better, the impurity gas can be well removed, so that the inert gas with higher purity can be obtained by one-time purification, the purification process is very simple and convenient, and the cost is lower.
Among them, in examples 1 to 5, the helium obtained after primary purification reaches the primary helium standard due to the adoption of the water-soluble catalyst, and the quality is better.
In example 6, the helium obtained after primary purification reaches the standard of secondary helium by adopting the water-insoluble catalyst, but compared with examples 1-5, the purification efficiency is reduced, if further purification is needed, the purified gas is collected and then is led into an inert gas purification material again for further purification, and the efficiency is reduced.
Comparative examples 1 to 4 have significantly reduced sodium peroxyacetate catalysis due to the change of the catalyst system, and although some purification effect can be achieved, the effect is significantly reduced compared with each example.
The comparison examples 5-6 have the advantages that the oxidizing agent is changed, so that the effect of the oxidizing agent and the catalyst is more general, and the purifying effect on helium is still obviously reduced compared with the examples even under the action of the catalyst compounded by the special cobalt catalyst, the iridium catalyst and the platinum catalyst.
Comparative example 7 eliminates the thickener, so that the movement speed of bubbles in the inert gas purification material is increased, resulting in a shortened reaction time, and thus, a certain reduction in purification effect.
The present embodiment is only for explanation of the present application and is not to be construed as limiting the present application, and modifications to the present embodiment, which may not creatively contribute to the present application as required by those skilled in the art after reading the present specification, are all protected by patent laws within the scope of claims of the present application.

Claims (8)

1. An inert gas purification material characterized by: comprises the following components in parts by mass:
100 parts of deionized water;
30-40 parts of sodium hydroxide;
15-20 parts of sodium peroxyacetate;
10-15 parts of barium carbonate;
2-3 parts of a catalyst;
15-20 parts of a thickening agent;
the catalyst is a compound of a cobalt catalyst, an iridium catalyst and a platinum catalyst.
2. An inert gas purification material according to claim 1, wherein: the cobalt catalyst, the iridium catalyst and the platinum catalyst are all water-soluble substances.
3. An inert gas purification material according to claim 2, characterized in that: the cobalt catalyst is cobalt acetate, the iridium catalyst is iridium trichloride, and the platinum catalyst is chloroplatinic acid.
4. An inert gas purification material according to claim 3, wherein: the mass ratio of the cobalt acetate to the iridium trichloride to the chloroplatinic acid is 3-4:1-2:6-7.
5. An inert gas purification material according to claim 1, wherein: the thickener is a compound of nano silicon dioxide and polyethylene glycol.
6. An inert gas purification material according to claim 5, wherein: the mass ratio of the nano silicon dioxide to the polyethylene glycol is 2:1-3.
7. An inert gas purification material according to claim 6, wherein: the molecular weight of the polyethylene glycol is more than or equal to 4000.
8. A process for preparing an inert gas purification material according to any one of claims 1 to 7, characterized in that: the method comprises the following steps:
step 1), mixing deionized water and sodium hydroxide to obtain a premix;
and 2) cooling to room temperature, adding sodium peroxyacetate, barium carbonate, a catalyst and a thickening agent into the premix, and uniformly stirring to obtain the inert gas purification material.
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