CN104646027A - Preparation technology for methanol steam reforming and hydrogen production catalyst - Google Patents
Preparation technology for methanol steam reforming and hydrogen production catalyst Download PDFInfo
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- CN104646027A CN104646027A CN201510075655.XA CN201510075655A CN104646027A CN 104646027 A CN104646027 A CN 104646027A CN 201510075655 A CN201510075655 A CN 201510075655A CN 104646027 A CN104646027 A CN 104646027A
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Abstract
The invention discloses a preparation technology for a methanol steam reforming and hydrogen production catalyst. The methanol steam reforming and hydrogen production catalyst is a noble metal catalyst; the noble metal catalyst is prepared from the following substances in parts by mass: 2-20 parts of CuO, 2-20 parts of ZnO, 0.1-5 parts of ZrO, 40-95 parts of Al2O3, 0-5 parts of CeO2, 0-5 parts of La2O3 and 0-5 parts of noble metal, wherein the noble metal is one or more of Pb, Pt, Ir, Rh and Ru; a honeycomb ceramic carrier coated with an aluminum oxide coating layer is immersed into a solution for preparing the noble metal catalyst and is used for carrying the noble metal catalyst. According to the preparation technology for the methanol steam reforming and hydrogen production catalyst, the problems that the production process for the methanol steam reforming and hydrogen production catalyst by using a depositing method is complicated and the stacking density is large can be solved.
Description
Technical field
The invention belongs to steam reformation of methanol to produce hydrogen technical field, relate to a kind of preparation technology of catalyst, particularly relate to a kind of preparation technology of catalyst for steam reformation of methanol to produce hydrogen.
Background technology
In recent years, along with the development of Proton Exchange Membrane Fuel Cells, particularly it is applied to automobile and distributed power generation, in the urgent need to the mobile hydrogen making system of small-sized efficient, efficient, dispersion to supply feed hydrogen.So there is hydrogen generating system miscellaneous, also there is hydrogen production process miscellaneous simultaneously.
A kind of hydrogen production from methanol-steam reforming equipment that such as Chinese patent CN202519022U discloses, described equipment comprises liquid container, heat exchanger, vaporizer, reformer chamber, separation chamber.Described equipment comprises one or more heating unit, for hydrogen producer needs temperature controlled parts to carry out temperature control; The residual air that heating unit is exported by separation chamber is or/and obtained hydrogen heating.Transfer pipe between reformer chamber and separation chamber is through a preheating temperature control mechanism, and this preheating temperature control mechanism is in order to the gas of heating from reformer chamber output; Described preheating temperature control mechanism, as the buffering between reformer chamber and separation chamber, makes the temperature of the gas exported from reformer chamber identical with the temperature of separation chamber or close.
The and for example hydrogen production process that provides of China Patent Publication No. CN101033059, this hydrogen production process does not need outside heat supply due to it, and easy realization scene heats, so receive vast concern.Adopt off-gas to carry out heating system in the method, the result of generation is that each position of system is heated uneven, the most directly, is also that what to affect most is the catalytic activity of catalyst.
Current catalyst for steam reformation of methanol to produce hydrogen is mainly copper-based catalysts.Copper-based catalysts adopts precipitation method preparation, and its production process is complicated, wayward, and the product bulk density of production is large, is unfavorable for small-sized movable hydrogen generating system.
In view of this, nowadays in the urgent need to designing a kind of new catalyst for steam reformation of methanol to produce hydrogen, to overcome the above-mentioned defect of existing catalyst.
Summary of the invention
Technical problem to be solved by this invention is: the preparation technology providing a kind of catalyst for steam reformation of methanol to produce hydrogen, uses under being more conducive to being greater than the condition of work of 300 DEG C.
For solving the problems of the technologies described above, the present invention adopts following technical scheme:
A preparation technology for catalyst for steam reformation of methanol to produce hydrogen, described preparation technology comprises the steps:
Step S1, configuration Alumina gel solution, the solid content of Alumina gel is 50%;
Step S2, honeycomb ceramic carrier is immersed in the obtained solution of step S1;
The honeycomb ceramic carrier at room temperature dried in the air after step S3, dry dipping; Baking temperature is set as 120 DEG C, and drying time is 2 hours;
Step S4, calcination is carried out to dried material; Calcination temperature is 500 DEG C, and calcination time is 5 hours;
Step S5, be cooled to room temperature;
The honeycomb ceramic carrier that step S6, continuation obtain through step S5 by the solution impregnation that step S1 configures; The drying of step S3, the calcination of step S4, the cooling of step S5 is then utilized to obtain being coated with aluminum oxide coating layer honeycomb ceramic carrier;
Step S7, preparation nitrate, the one-tenth assignment system of the noble metal catalyst that the composition of nitrate finally generates through calcination according to it, adopts the nitrate of respective substance and mass fraction thereof to obtain noble metal catalyst; Described noble metal catalyst comprises material and mass fraction is: the CuO of 2-20 part, the ZrO of the ZnO of 2-20 part, 0.1-5 part, the Al of 40-95 part
2o
3, the CeO of 0-5 part
2, the La of 0-5 part
2o
3, the noble metal of 0-5 part; Noble metal is one or more in Pb, Pt, Ir, Rh, Ru;
Step S8, nitrate corresponding in S7 is mixed with solution;
Step S9, the honeycomb ceramic carrier obtained by step S6 are immersed in the obtained solution of step S8;
The honeycomb ceramic carrier at room temperature dried in the air after step S10, dry dipping; Baking temperature is set as 120 DEG C, and drying time is 2 hours;
Step S11, calcination is carried out to dried material; Calcination temperature is 500 DEG C, and calcination time is 5 hours;
Step S12, be cooled to room temperature;
The honeycomb ceramic carrier that the solution impregnation that step S13, continuation step S8 obtain obtains through step S12; Then utilize the drying of step S10, the noble metal catalyst of honeycomb ceramic carrier as carrier that the calcination of step S11, the cooling of step S12 obtain being coated with aluminum oxide coating layer.
A preparation technology for catalyst for steam reformation of methanol to produce hydrogen, catalyst for steam reformation of methanol to produce hydrogen is noble metal catalyst;
Described noble metal catalyst comprises material and mass fraction is: the CuO of 2-20 part, the ZrO of the ZnO of 2-20 part, 0.1-5 part, the Al of 40-95 part
2o
3, the CeO of 0-5 part
2, the La of 0-5 part
2o
3, the noble metal of 0-5 part; Noble metal is one or more in Pb, Pt, Ir, Rh, Ru;
The honeycomb ceramic carrier being coated with aluminum oxide coating layer is immersed in the solution of noble metal catalyst preparation, utilizes the honeycomb ceramic carrier carrying noble metal catalyst being coated with aluminum oxide coating layer.
As a preferred embodiment of the present invention, described preparation technology comprises the steps:
Step S1, configuration Alumina gel solution, the solid content of Alumina gel is 40%-60%;
Step S2, honeycomb ceramic carrier is immersed in the obtained solution of step S1;
The honeycomb ceramic carrier at room temperature dried in the air after step S3, dry dipping; Baking temperature is set as 80 DEG C-150 DEG C, and drying time is 0.5-10 hour;
Step S4, calcination is carried out to dried material; Calcination temperature is 450 DEG C-650 DEG C, and calcination time is 1-20 hour;
Step S5, be cooled to room temperature;
The honeycomb ceramic carrier that step S6, continuation obtain through step S5 by the solution impregnation that step S1 configures; The drying of step S3, the calcination of step S4, the cooling of step S5 is then utilized to obtain being coated with aluminum oxide coating layer honeycomb ceramic carrier;
Step S7, preparation nitrate, the one-tenth assignment system of the noble metal catalyst that the composition of nitrate finally generates through calcination according to it, adopts the nitrate of respective substance and mass fraction thereof to obtain noble metal catalyst; Described noble metal catalyst comprises material and mass fraction is: the CuO of 2-20 part, the ZrO of the ZnO of 2-20 part, 0.1-5 part, the Al of 40-95 part
2o
3, the CeO of 0-5 part
2, the La of 0-5 part
2o
3, the noble metal of 0-5 part; Noble metal is one or more in Pb, Pt, Ir, Rh, Ru;
Step S8, nitrate corresponding in S7 is mixed with solution;
Step S9, the honeycomb ceramic carrier obtained by step S6 are immersed in the obtained solution of step S8;
The honeycomb ceramic carrier at room temperature dried in the air after step S10, dry dipping; Baking temperature is set as 80 DEG C-150 DEG C, and drying time is 0.5-10 hour;
Step S11, calcination is carried out to dried material; Calcination temperature is 450 DEG C-650 DEG C, and calcination time is 1-20 hour;
Step S12, cooling step.
As a preferred embodiment of the present invention, the honeycomb ceramic carrier that the solution impregnation that described preparation technology comprises step S13 further, continuation step S8 obtains obtains through step S12; Then utilize the drying of step S10, the noble metal catalyst of honeycomb ceramic carrier as carrier that the calcination of step S11, the cooling of step S12 obtain being coated with aluminum oxide coating layer.
Beneficial effect of the present invention is: the preparation technology of the catalyst for steam reformation of methanol to produce hydrogen that the present invention proposes, can overcome the problem that existing employing intermediate processing methanol steam reformation noble metal catalyst production process is complicated and bulk density is large; Noble metal catalyst uses under being more conducive to being greater than the condition of work of 300 DEG C.
Accompanying drawing explanation
Fig. 1 is the flow chart of the preparation technology of catalyst for steam reformation of methanol to produce hydrogen of the present invention.
Detailed description of the invention
The preferred embodiments of the present invention are described in detail below in conjunction with accompanying drawing.
Embodiment one
Refer to Fig. 1, present invention is disclosed a kind of preparation technology of catalyst for steam reformation of methanol to produce hydrogen, described preparation technology comprises the steps:
Step S1, configuration Alumina gel solution, the solid content of Alumina gel is 50%;
Step S2, honeycomb ceramic carrier is immersed in the obtained solution of step S1;
The honeycomb ceramic carrier at room temperature dried in the air after step S3, dry dipping; Baking temperature is set as 120 DEG C, and drying time is 2 hours;
Step S4, calcination is carried out to dried material; Calcination temperature is 500 DEG C, and calcination time is 5 hours;
Step S5, be cooled to room temperature;
The honeycomb ceramic carrier that step S6, continuation obtain through step S5 by the solution impregnation that step S1 configures; The drying of step S3, the calcination of step S4, the cooling of step S5 is then utilized to obtain being coated with aluminum oxide coating layer honeycomb ceramic carrier;
Step S7, preparation nitrate, the one-tenth assignment system (as copper nitrate, zinc nitrate, aluminum nitrate, zirconium nitrate, cerous nitrate, lanthanum nitrate, platinum nitrate, palladium nitrate etc.) of the noble metal catalyst that the composition of nitrate finally generates through calcination according to it, adopts the nitrate of respective substance and mass fraction thereof to obtain noble metal catalyst; Described noble metal catalyst comprises material and mass fraction is: the CuO of 2-20 part, the ZrO of the ZnO of 2-20 part, 0.1-5 part, the Al of 40-95 part
2o
3, the CeO of 0-5 part
2, the La of 0-5 part
2o
3, the noble metal of 0-5 part; Noble metal is one or more in Pb, Pt, Ir, Rh, Ru;
Step S8, nitrate corresponding in S7 is mixed with solution;
Step S9, the honeycomb ceramic carrier obtained by step S6 are immersed in the obtained solution of step S8;
The honeycomb ceramic carrier at room temperature dried in the air after step S10, dry dipping; Baking temperature is set as 120 DEG C, and drying time is 2 hours;
Step S11, calcination is carried out to dried material; Calcination temperature is 500 DEG C, and calcination time is 5 hours;
Step S12, be cooled to room temperature;
The honeycomb ceramic carrier that the solution impregnation that step S13, continuation step S8 obtain obtains through step S12; Then utilize the drying of step S10, the noble metal catalyst of honeycomb ceramic carrier as carrier that the calcination of step S11, the cooling of step S12 obtain being coated with aluminum oxide coating layer.
Embodiment two
A preparation technology for catalyst for steam reformation of methanol to produce hydrogen, catalyst for steam reformation of methanol to produce hydrogen is noble metal catalyst;
Described noble metal catalyst comprises material and mass fraction is: the CuO of 2-20 part, the ZrO of the ZnO of 2-20 part, 0.1-5 part, the Al of 40-95 part
2o
3, the CeO of 0-5 part
2, the La of 0-5 part
2o
3, the noble metal of 0-5 part; Noble metal is one or more in Pb, Pt, Ir, Rh, Ru;
The honeycomb ceramic carrier being coated with aluminum oxide coating layer is immersed in the solution of noble metal catalyst preparation, utilizes the honeycomb ceramic carrier carrying noble metal catalyst being coated with aluminum oxide coating layer.
Described preparation technology comprises the steps:
Step S1, configuration Alumina gel solution, the solid content of Alumina gel is 40%-60%;
Step S2, honeycomb ceramic carrier is immersed in the obtained solution of step S1;
The honeycomb ceramic carrier at room temperature dried in the air after step S3, dry dipping; Baking temperature is set as 80 DEG C-150 DEG C, and drying time is 0.5-10 hour;
Step S4, calcination is carried out to dried material; Calcination temperature is 450 DEG C-650 DEG C, and calcination time is 1-20 hour;
Step S5, be cooled to room temperature;
The honeycomb ceramic carrier that step S6, continuation obtain through step S5 by the solution impregnation that step S1 configures; The drying of step S3, the calcination of step S4, the cooling of step S5 is then utilized to obtain being coated with aluminum oxide coating layer honeycomb ceramic carrier;
Step S7, preparation nitrate, the one-tenth assignment system of the noble metal catalyst that the composition of nitrate finally generates through calcination according to it, adopts the nitrate of respective substance and mass fraction thereof to obtain noble metal catalyst; Described noble metal catalyst comprises material and mass fraction is: the CuO of 2-20 part, the ZrO of the ZnO of 2-20 part, 0.1-5 part, the Al of 40-95 part
2o
3, the CeO of 0-5 part
2, the La of 0-5 part
2o
3, the noble metal of 0-5 part; Noble metal is one or more in Pb, Pt, Ir, Rh, Ru;
Step S8, nitrate corresponding in S7 is mixed with solution;
Step S9, the honeycomb ceramic carrier obtained by step S6 are immersed in the obtained solution of step S8;
The honeycomb ceramic carrier at room temperature dried in the air after step S10, dry dipping; Baking temperature is set as 80 DEG C-150 DEG C, and drying time is 0.5-10 hour;
Step S11, calcination is carried out to dried material; Calcination temperature is 450 DEG C-650 DEG C, and calcination time is 1-20 hour;
Step S12, cooling step.
The honeycomb ceramic carrier that the solution impregnation that step S13, continuation step S8 obtain obtains through step S12; Then utilize the drying of step S10, the noble metal catalyst of honeycomb ceramic carrier as carrier that the calcination of step S11, the cooling of step S12 obtain being coated with aluminum oxide coating layer.
In sum, the preparation technology of the catalyst for steam reformation of methanol to produce hydrogen that the present invention proposes, can overcome the problem that existing employing intermediate processing methanol steam reformation noble metal catalyst production process is complicated and bulk density is large; Noble metal catalyst uses under being more conducive to being greater than the condition of work of 300 DEG C.
Here description of the invention and application is illustrative, not wants by scope restriction of the present invention in the above-described embodiments.Distortion and the change of embodiment disclosed are here possible, are known for the replacement of embodiment those those of ordinary skill in the art and the various parts of equivalence.Those skilled in the art are noted that when not departing from spirit of the present invention or substantive characteristics, the present invention can in other forms, structure, layout, ratio, and to realize with other assembly, material and parts.When not departing from the scope of the invention and spirit, can other distortion be carried out here to disclosed embodiment and change.
Claims (4)
1. a preparation technology for catalyst for steam reformation of methanol to produce hydrogen, is characterized in that, described preparation technology comprises the steps:
Step S1, configuration Alumina gel solution, the solid content of Alumina gel is 50%;
Step S2, honeycomb ceramic carrier is immersed in the obtained solution of step S1;
The honeycomb ceramic carrier at room temperature dried in the air after step S3, dry dipping; Baking temperature is set as 120 DEG C, and drying time is 2 hours;
Step S4, calcination is carried out to dried material; Calcination temperature is 500 DEG C, and calcination time is 5 hours;
Step S5, be cooled to room temperature;
The honeycomb ceramic carrier that step S6, continuation obtain through step S5 by the solution impregnation that step S1 configures; The drying of step S3, the calcination of step S4, the cooling of step S5 is then utilized to obtain being coated with aluminum oxide coating layer honeycomb ceramic carrier;
Step S7, preparation nitrate, the one-tenth assignment system of the noble metal catalyst that the composition of nitrate finally generates through calcination according to it, adopts the nitrate of respective substance and mass fraction thereof to obtain noble metal catalyst; Described noble metal catalyst comprises material and mass fraction is: the CuO of 2-20 part, the ZrO of the ZnO of 2-20 part, 0.1-5 part, the Al of 40-95 part
2o
3, the CeO of 0-5 part
2, the La of 0-5 part
2o
3, the noble metal of 0-5 part; Noble metal catalyst is one or more in Pb, Pt, Ir, Rh, Ru;
Step S8, nitrate corresponding in S7 is mixed with solution;
Step S9, the honeycomb ceramic carrier obtained by step S6 are immersed in the obtained solution of step S8;
The honeycomb ceramic carrier at room temperature dried in the air after step S10, dry dipping; Baking temperature is set as 120 DEG C, and drying time is 2 hours;
Step S11, calcination is carried out to dried material; Calcination temperature is 500 DEG C, and calcination time is 5 hours;
Step S12, be cooled to room temperature;
The honeycomb ceramic carrier that the solution impregnation that step S13, continuation step S8 obtain obtains through step S12; Then utilize the drying of step S10, the noble metal catalyst of honeycomb ceramic carrier as carrier that the calcination of step S11, the cooling of step S12 obtain being coated with aluminum oxide coating layer.
2. a preparation technology for catalyst for steam reformation of methanol to produce hydrogen, is characterized in that, catalyst for steam reformation of methanol to produce hydrogen is noble metal catalyst;
Described noble metal catalyst comprises material and mass fraction is: the CuO of 2-20 part, the ZrO of the ZnO of 2-20 part, 0.1-5 part, the Al of 40-95 part
2o
3, the CeO of 0-5 part
2, the La of 0-5 part
2o
3, the noble metal of 0-5 part; Noble metal is one or more in Pb, Pt, Ir, Rh, Ru;
The honeycomb ceramic carrier being coated with aluminum oxide coating layer is immersed in the solution of noble metal catalyst preparation, utilizes the honeycomb ceramic carrier carrying noble metal catalyst being coated with aluminum oxide coating layer.
3. the preparation technology of catalyst for steam reformation of methanol to produce hydrogen according to claim 2, is characterized in that:
Described preparation technology comprises the steps:
Step S1, configuration Alumina gel solution, the solid content of Alumina gel is 40%-60%;
Step S2, honeycomb ceramic carrier is immersed in the obtained solution of step S1;
The honeycomb ceramic carrier at room temperature dried in the air after step S3, dry dipping; Baking temperature is set as 80 DEG C-150 DEG C, and drying time is 0.5-10 hour;
Step S4, calcination is carried out to dried material; Calcination temperature is 450 DEG C-650 DEG C, and calcination time is 1-20 hour;
Step S5, be cooled to room temperature;
The honeycomb ceramic carrier that step S6, continuation obtain through step S5 by the solution impregnation that step S1 configures; The drying of step S3, the calcination of step S4, the cooling of step S5 is then utilized to obtain being coated with aluminum oxide coating layer honeycomb ceramic carrier;
Step S7, preparation nitrate, the one-tenth assignment system of the noble metal catalyst that the composition of nitrate finally generates through calcination according to it, adopts the nitrate of respective substance and mass fraction thereof to obtain noble metal catalyst; Described noble metal catalyst comprises material and mass fraction is: the CuO of 2-20 part, the ZrO of the ZnO of 2-20 part, 0.1-5 part, the Al of 40-95 part
2o
3, the CeO of 0-5 part
2, the La of 0-5 part
2o
3, the noble metal of 0-5 part; Noble metal is one or more in Pb, Pt, Ir, Rh, Ru;
Step S8, nitrate corresponding in S7 is mixed with solution;
Step S9, the honeycomb ceramic carrier obtained by step S6 are immersed in the obtained solution of step S8;
The honeycomb ceramic carrier at room temperature dried in the air after step S10, dry dipping; Baking temperature is set as 80 DEG C-150 DEG C, and drying time is 0.5-10 hour;
Step S11, calcination is carried out to dried material; Calcination temperature is 450 DEG C-650 DEG C, and calcination time is 1-20 hour;
Step S12, cooling step.
4. the preparation technology of catalyst for steam reformation of methanol to produce hydrogen according to claim 3, is characterized in that:
The honeycomb ceramic carrier that the solution impregnation that described preparation technology comprises step S13 further, continuation step S8 obtains obtains through step S12; Then utilize the drying of step S10, the noble metal catalyst of honeycomb ceramic carrier as carrier that the calcination of step S11, the cooling of step S12 obtain being coated with aluminum oxide coating layer.
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| CN201510075655.XA CN104646027A (en) | 2015-02-12 | 2015-02-12 | Preparation technology for methanol steam reforming and hydrogen production catalyst |
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Application publication date: 20150527 |