CN103071488B - High-purity hydrogen catalytic agent prepared by hydrogen catalytic deoxidation, as well as preparation method and application thereof - Google Patents
High-purity hydrogen catalytic agent prepared by hydrogen catalytic deoxidation, as well as preparation method and application thereof Download PDFInfo
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- CN103071488B CN103071488B CN201310008180.3A CN201310008180A CN103071488B CN 103071488 B CN103071488 B CN 103071488B CN 201310008180 A CN201310008180 A CN 201310008180A CN 103071488 B CN103071488 B CN 103071488B
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Abstract
The invention relates to a high-purity hydrogen catalytic agent prepared by hydrogen catalytic deoxidation, as well as a preparation method and application thereof. The catalytic agent takes palladium or platinum as a main catalyst active component, at the same time, a small amount of a rare earth element and transition metals are added and taken as cocatalyst components, and the components and a catalytic agent carrier are soaked, dried and calcinated, so that the high-purity hydrogen catalytic agent is obtained. Compared with the prior art, the catalytic agent has the advantages that raw materials can be obtained easily, the agent can be prepared simply, the cost is low, and the agent can be transported and stored safely. The catalytic agent is used for hydrogen purification, the operation temperature is low, the gas pressure range is wide, and the gas purity of the obtained product is high and can reach 99.99995%.
Description
Technical field
The present invention relates to a kind of hydrogen purification Catalysts and its preparation method, especially relate to a kind of hydrogen catalytic deoxidation and prepare High Purity Hydrogen Catalysts and its preparation method.
Background technology
The energy is the important substance basis of human survival and development, and along with the high speed development of industrial and agricultural production and the raising of human living standard, energy-output ratio increases day by day.The fossil energy that the earth stores is limited, and due to a large amount of exploitation, reserves reduce rapidly, and fossil energy is petered out.At present, energy crisis becomes the problem that countries in the world are paid close attention to, and taps a new source of energy and becomes the great state basic policy of every country.
Hydrogen Energy wide material sources, and colourless, nontoxic, tasteless, be convenient to store and transport, environmentally safe, is described as the new forms of energy of " clean ", is following generally acknowledged except electricity, a kind of important second energy carrier.
High Purity Hydrogen typically refers to the hydrogen of purity more than 99.999%.Can be widely used in the industrial departments such as chemistry, electronics, the energy, metallurgy, electric power, as the emphasis of future-oriented strategy development, High Purity Hydrogen will be the emphasis of future studies.
Industrial conventional hydrogen purification method mainly contains following several:
1) absorption deoxidation is the method by the various gaseous impurity of the selective removing of suitable adsorbent, is divided into again low-temperature adsorption and pressure swing adsorption method.This method hydrogen recovery rate is low, complicated operation, and adsorption bed needs regeneration, and technique is loaded down with trivial details.
2) chemical absorbing deoxidation, the active component namely in deoxidier and oxygen react produces oxide, and oxygen is absorbed, and then logical hydrogen makes deoxidier regenerate.Conventional active component has the base metal deoxidiers such as iron, copper, manganese, nickel.The advantage of the method is that the base metal deoxidier deoxidation degree of depth is good, low price, but deoxidier needs periodic regeneration, easily causes loss of active component, affects hydrogen purity.
3) catalyst deoxidation, namely chooses suitable catalyst and makes a small amount of oxygen in hydrogen and hydrogen reaction generate the effect that water reaches deoxidation.The active component of this kind of catalyst mostly is the noble metal such as palladium, platinum.This kind of catalyst efficiency is high, and the advantage such as it is wide to have operating temperature region, and technique is simple.But because catalyst activity component is mainly precious metal element, therefore cost is high, most patent report hydrogen purification catalyst activity constituent content is higher, is unfavorable for promoting.
Summary of the invention
Object of the present invention be exactly in order to overcome above-mentioned prior art exist defect and provide a kind of hydrogen catalytic deoxidation to prepare High Purity Hydrogen Catalysts and its preparation method and application.
Object of the present invention can be achieved through the following technical solutions: high-purity catalyst for hydrogen is prepared in a kind of hydrogen catalytic deoxidation, it is characterized in that, this catalyst be a kind of by many metal components as active constituent loading at supported catalyst, described active component is by main active component and help active component in molar ratio 1: (0.01 ~ 1) forms, and described active component content is 0.1 ~ 15% of vehicle weight.
Described main active component is metal platinum or Metal Palladium or both mixtures; Described help active component be transition metal or rare earth element one or more.
Described transition metal is one or more of iron, cobalt, molybdenum, nickel or manganese, and described rare earth element is one or more of lanthanum, cerium, scandium or neodymium.
Described transition metal is one or both of nickel or molybdenum; Described rare earth element be lanthanum, cerium one or both.
Described carrier is one or more in silica, aluminium oxide, titanium oxide, imvite, kaolin.
The preparation method of high-purity catalyst for hydrogen is prepared in a kind of hydrogen catalytic deoxidation, it is characterized in that, the presoma of active constituent is mixed with maceration extract in proportion, by carrier impregnation 1 ~ 48h in maceration extract, through 100 ~ 150 DEG C of drying 6 ~ 10h, 300 ~ 800 DEG C of roasting 4 ~ 6h, then pass into hydrogen and obtain catalyst at 300 ~ 500 DEG C of activation 10 ~ 16h.
The presoma of described active constituent is any one in nitrate, acetate or chloride.
The time of described carrier impregnation in maceration extract is 6-24h, and dry temperature is 120 ~ 150 DEG C, and the temperature of roasting is 300 ~ 600 DEG C.
An application for high-purity catalyst for hydrogen is prepared in hydrogen catalytic deoxidation, it is characterized in that, described catalyst is used for hydrogen catalytic deoxidation and prepares High Purity Hydrogen, and described hydrogen is general hydrogen, and the operating temperature in preparation process is 100 ~ 200 DEG C, operating pressure 0 ~ 2MPa.
Described hydrogen be brine electrolysis prepare obtain general hydrogen, described operating temperature is 120 ~ 180 DEG C, and described operating pressure is 0 ~ 0.6MPa.
Compared with prior art, the present invention has the following advantages:
(1) catalyst of the present invention is owing to employing transition metal or rare earth element as helping active component, so noble metal use amount is lower, and noble metal and transition metal or rare earth element interworking activity higher;
(2) catalyst preparation materials of the present invention is easy to get, and preparation is simple, with low cost, shipping storage safety;
(3) catalyst of the present invention is used as hydrogen purification, and operating temperature is low, and gas pressure range is wide, and products obtained therefrom gas purity is high, can reach more than 99.99995%;
(4) economy of the present invention and use value well, have good promotion prospect.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in detail.
Embodiment 1
Get 8g Pd (NH
3)
4cl
2, 3g (NH
4)
6mo
7o
244H
2o is dissolved in deionized water, obtain activity component impregnation liquid, 40g aluminium oxide is joined in maceration extract, stir, dipping 12h, after dipping at 130 DEG C dry 6h, roasting 5h at 500 DEG C, logical hydrogen is at 400 DEG C of activation process 12h afterwards, namely obtains many metal components loaded catalyst of the present invention.
Wherein, main active constituent with help the mol ratio of active constituent to be 1: 0.52; Catalyst activity component content is 12.75% of vehicle weight.
The general hydrogen that brine electrolysis obtains is 150 DEG C through temperature, after pressure is 0.4MPa purification process, obtains hydrogen purity and reach 99.9999%.
Embodiment 2
Get 5g Pd (NH
3)
4cl
2, 2gNi (NO
3)
26H
2o, 2gLa (NO
3)
36H
2o is dissolved in deionized water, obtain activity component impregnation liquid, 40g aluminium oxide is joined in maceration extract, stir, dipping 12h, after dipping at 130 DEG C dry 6h, roasting 4h at 500 DEG C, logical hydrogen is at 400 DEG C of activation process 12h afterwards, namely obtains many metal components loaded catalyst of the present invention.
Wherein, main active constituent with help the mol ratio of active constituent to be 1: 0.56; Catalyst activity component content is 8.03% of vehicle weight.
The general hydrogen that brine electrolysis obtains through temperature be 160 DEG C, after pressure is 0.4MPa purification process, obtaining hydrogen purity is 99.999%.
Embodiment 3
Get 4gPd (NH
3)
4cl
2, 2gH
2ptCl
66H
2o, 2g Ni (NO
3)
26H
2o, 1g (NH
4)
6mo
7o
244H
2o is dissolved in 20g deionized water, obtain activity component impregnation liquid, 50g titanium dioxide is joined in maceration extract, stir, dipping 15h, after dipping at 130 DEG C dry 8h, roasting 6h at 500 DEG C, logical hydrogen is at 400 DEG C of activation process 12h afterwards, namely obtains many metal components loaded catalyst of the present invention.
Wherein, main active constituent with help the mol ratio of active constituent to be 1: 0.67; Catalyst activity component content is 7.83% of vehicle weight.
The general hydrogen that brine electrolysis obtains is 160 DEG C through temperature, after pressure is 0.3MPa purification process, obtains hydrogen purity and reach 99.9995%.
Embodiment 4
Get 3g Pd (NH
3)
4cl
2, 3g H
2ptCl
66H
2o, 4g Ni (NO
3)
26H
2o is dissolved in 20g deionized water, obtain activity component impregnation liquid, 40g silica is joined in maceration extract, stir, dipping 12h, after dipping at 130 DEG C dry 8h, roasting 6h at 500 DEG C, logical hydrogen is at 400 DEG C of activation process 12h afterwards, namely obtains many metal components loaded catalyst of the present invention.
Wherein, main active constituent with help the mol ratio of active constituent to be 1: 0.88; Catalyst activity component content is 6.94% of vehicle weight.
The general hydrogen that brine electrolysis obtains through temperature be 180 DEG C, after pressure is 0.4MPa purification process, obtaining hydrogen purity is 99.9999%.
Embodiment 5
Get 2gPd (NH
3)
4cl
2, 2gH
2ptCl
66H
2o, 1gNi (NO
3)
26H
2o, 0.5g (NH
4)
6mo
7o
244H
2o, 0.5gLa (NO
3)
36H
2o, 0.5gCe (NO
3)
36H
2o is dissolved in 20g deionized water, obtain activity component impregnation liquid, 40g silica is joined in maceration extract, stir, dipping 18h, after dipping at 130 DEG C dry 10h, roasting 6h at 500 DEG C, logical hydrogen is at 400 DEG C of activation process 12h afterwards, namely obtains many metal components loaded catalyst of the present invention.
Wherein, main active constituent with help the mol ratio of active constituent to be 1: 0.87; Catalyst activity component content is 6.97% of vehicle weight.
The general hydrogen that brine electrolysis obtains through temperature be 180 DEG C, after pressure is 0.6MPa purification process, obtaining hydrogen purity can reach 99.99995%.
Embodiment 6
Get 2gPd (NH
3)
4cl
2, 1g (NH
4)
6mo
7o
244H
2o, 0.5gLa (NO
3)
36H
2o, 0.5gCe (NO3)
36H
2o is dissolved in 20g deionized water, obtain activity component impregnation liquid, 40g silica is joined in maceration extract, stir, dipping 15h, after dipping at 130 DEG C dry 10h, roasting 6h at 500 DEG C, logical hydrogen is at 400 DEG C of activation process 12h afterwards, namely obtains many metal components loaded catalyst of the present invention.
Wherein, main active constituent with help the mol ratio of active constituent to be 1: 0.69; Catalyst activity component content is 5.35% of vehicle weight.
The general hydrogen that brine electrolysis obtains through temperature be 180 DEG C, after pressure is 0.1MPa purification process, obtaining hydrogen purity is 99.99993%.
Embodiment 7
High-purity catalyst for hydrogen is prepared in a kind of hydrogen catalytic deoxidation, this catalyst be a kind of by many metal components as the catalyst of active constituent loading in carrier imvite, described active component is by main active component Pt and help active component iron to form at 1: 0.01 in molar ratio, and described active component content is 0.1% of imvite weight.
Above-mentioned catalyst obtains by the following method: by Pt (NO
3)
2, Fe (NO
3)
3be mixed with maceration extract, imvite be immersed in 1h in maceration extract, through 100 DEG C of dry 10h, 300 DEG C of roasting 6h, then pass into hydrogen and obtain catalyst at 300 DEG C of activation 16h.
The general hydrogen that brine electrolysis obtains through temperature be 100 DEG C, after pressure is 2MPa purification process, obtaining hydrogen purity is 99.9999%.
Embodiment 8
High-purity catalyst for hydrogen is prepared in a kind of hydrogen catalytic deoxidation, this catalyst be a kind of by many metal components as the catalyst of active constituent loading on carrier kaolin, described active component is by main active component Pd and help active component Co to form at 1: 1 in molar ratio, and described active component content is 15% of kaolin weight.
Above-mentioned catalyst obtains by the following method: by Pd (OAc)
2, Co (OAc)
2be mixed with maceration extract, kaolin be immersed in 48h in maceration extract, through 150 DEG C of dry 6h, 800 DEG C of roasting 4h, then pass into hydrogen and obtain catalyst at 500 DEG C of activation 10h.
The general hydrogen that brine electrolysis obtains through temperature be 200 DEG C, after pressure is 0MPa (normal pressure) purification process, obtaining hydrogen purity is 99.99999%.
Claims (7)
1. high-purity catalyst for hydrogen is prepared in a hydrogen catalytic deoxidation, it is characterized in that, this catalyst be a kind of by many metal components as active constituent loading at supported catalyst, described active component is by main active component and help active component 1:(0.01 ~ 1 in molar ratio) form, described active component content is 0.1 ~ 15% of vehicle weight;
Described main active component is metal platinum or Metal Palladium or both mixtures; Described help active component be transition metal or rare earth element one or more;
Described transition metal is one or both of nickel or molybdenum; Described rare earth element be lanthanum, cerium one or both.
2. high-purity catalyst for hydrogen is prepared in a kind of hydrogen catalytic deoxidation according to claim 1, and it is characterized in that, described carrier is one or more in silica, aluminium oxide, titanium oxide, imvite, kaolin.
3. the preparation method of high-purity catalyst for hydrogen is prepared in a hydrogen catalytic deoxidation as claimed in claim 1, it is characterized in that, the presoma of active constituent is mixed with maceration extract in proportion, by carrier impregnation 1 ~ 48h in maceration extract, through 100 ~ 150 DEG C of drying 6 ~ 10h, 300 ~ 800 DEG C of roasting 4 ~ 6h, then pass into hydrogen and obtain catalyst at 300 ~ 500 DEG C of activation 10 ~ 16h.
4. the preparation method of high-purity catalyst for hydrogen is prepared in a kind of hydrogen catalytic deoxidation according to claim 3, it is characterized in that, the presoma of described active constituent is any one in nitrate, acetate or chloride.
5. the preparation method of high-purity catalyst for hydrogen is prepared in a kind of hydrogen catalytic deoxidation according to claim 3, it is characterized in that, the time of described carrier impregnation in maceration extract is 6-24h, and dry temperature is 120 ~ 150 DEG C, and the temperature of roasting is 300 ~ 600 DEG C.
6. the application of high-purity catalyst for hydrogen is prepared in a hydrogen catalytic deoxidation as claimed in claim 1, it is characterized in that, described catalyst is used for hydrogen catalytic deoxidation and prepares High Purity Hydrogen, and described hydrogen is general hydrogen, operating temperature in preparation process is 100 ~ 200 DEG C, operating pressure 0 ~ 2MPa.
7. the application of high-purity catalyst for hydrogen is prepared in a kind of hydrogen catalytic deoxidation according to claim 6, it is characterized in that, described hydrogen be brine electrolysis prepare obtain general hydrogen, described operating temperature is 120 ~ 180 DEG C, and described operating pressure is 0 ~ 0.6MPa.
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| CN106582712A (en) * | 2016-12-16 | 2017-04-26 | 碳能科技（北京）有限公司 | Catalyst for hydrogen production through water electrolysis and preparation method thereof |
| CN110152659A (en) * | 2019-05-20 | 2019-08-23 | 安徽元琛环保科技股份有限公司 | Denitration takes off VOC catalyst, preparation method, regeneration method |
| CN111185167B (en) * | 2020-03-19 | 2021-06-08 | 中国科学院过程工程研究所 | Pt-based catalyst for CO purification and preparation method and application thereof |
| CN111905729A (en) * | 2020-07-30 | 2020-11-10 | 成都龙飞科技有限公司 | Organic hydrocarbon deoxidation catalyst and preparation method thereof |
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| JPS5826004A (en) * | 1981-08-10 | 1983-02-16 | Kansai Coke & Chem Co Ltd | Removing method for oxygen from gas containing oxygen consisting essentially of hydrogen |
| CN85102710A (en) * | 1985-04-01 | 1986-09-17 | 中国科学院大连化学物理研究所 | Platinum, Pd/TiO 2 deoxygenationcatalyst |
| CN1724114A (en) * | 2005-06-20 | 2006-01-25 | 天津化工研究设计院 | Double functional deoxidation agent and production process thereof |
| CN101142019A (en) * | 2005-03-18 | 2008-03-12 | 株式会社日本触媒 | Catalyst for removing oxygen and method for removing oxygen using the catalyst |
| CN101693199A (en) * | 2009-10-13 | 2010-04-14 | 上海化工研究院 | Catalyst for purifying hydrogen as well as preparation method and applications thereof |
-
2013
- 2013-01-09 CN CN201310008180.3A patent/CN103071488B/en active Active
Patent Citations (5)
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|---|---|---|---|---|
| JPS5826004A (en) * | 1981-08-10 | 1983-02-16 | Kansai Coke & Chem Co Ltd | Removing method for oxygen from gas containing oxygen consisting essentially of hydrogen |
| CN85102710A (en) * | 1985-04-01 | 1986-09-17 | 中国科学院大连化学物理研究所 | Platinum, Pd/TiO 2 deoxygenationcatalyst |
| CN101142019A (en) * | 2005-03-18 | 2008-03-12 | 株式会社日本触媒 | Catalyst for removing oxygen and method for removing oxygen using the catalyst |
| CN1724114A (en) * | 2005-06-20 | 2006-01-25 | 天津化工研究设计院 | Double functional deoxidation agent and production process thereof |
| CN101693199A (en) * | 2009-10-13 | 2010-04-14 | 上海化工研究院 | Catalyst for purifying hydrogen as well as preparation method and applications thereof |
Non-Patent Citations (1)
| Title |
|---|
| 氢气中氧气的钯催化去除;曾力丁等;《华南理工大学学报(自然科学版)》;20081130;第36卷(第11期);第22-26页 * |
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Address after: 200062 Shanghai city Putuo District Yunling Road No. 345 Co-patentee after: QINGLEI SPECIAL GAS Co.,Ltd. SHANGHAI RESEARCH INSTITUTE OF CHEMICAL INDUSTRY Patentee after: SHANGHAI RESEARCH INSTITUTE OF CHEMICAL INDUSTRY Co.,Ltd. Address before: 200062 Shanghai city Putuo District Yunling Road No. 345 Co-patentee before: QINGLEI SPECIAL GAS Co.,Ltd. SHANGHAI RESEARCH INSTITUTE OF CHEMICAL INDUSTRY Patentee before: Shanghai Research Institute of Chemical Industry |
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Effective date of registration: 20171130 Address after: 200062 Shanghai city Putuo District Yunling Road No. 345 Patentee after: SHANGHAI RESEARCH INSTITUTE OF CHEMICAL INDUSTRY Co.,Ltd. Address before: 200062 Shanghai city Putuo District Yunling Road No. 345 Co-patentee before: QINGLEI SPECIAL GAS Co.,Ltd. SHANGHAI RESEARCH INSTITUTE OF CHEMICAL INDUSTRY Patentee before: SHANGHAI RESEARCH INSTITUTE OF CHEMICAL INDUSTRY Co.,Ltd. |