CN106031870B - A kind of Hydrogen Ignition catalyst and its preparation method and application - Google Patents
A kind of Hydrogen Ignition catalyst and its preparation method and application Download PDFInfo
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- CN106031870B CN106031870B CN201610015625.4A CN201610015625A CN106031870B CN 106031870 B CN106031870 B CN 106031870B CN 201610015625 A CN201610015625 A CN 201610015625A CN 106031870 B CN106031870 B CN 106031870B
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/56—Platinum group metals
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
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Abstract
The present invention provides a kind of preparation methods of Hydrogen Ignition catalyst, which comprises the steps of: (1) precious metal salt is dissolved in deionized water and obtains the first solution;(2) lanthanum salt is dissolved in the first solution again, obtains the second solution;(3) aluminum oxide colloidal sol is dispersed in deionized water, obtains third solution;(4) third solution and the second solution are mixed, uniformly mixed solution is the 4th solution;(5) the 4th solution is coated on carrier, obtains Intermediate Catalyst;(6) required Hydrogen Ignition catalyst will be obtained after the activation cooling of Intermediate Catalyst drying and roasting;Noble metal in the step (1) is platinum or palladium;The content for making noble metal by the coating number of regulating step (5) is 0.1wt%-10wt%.Method of the invention is convenient for large-scale production and preparation, while the catalyst life of this method preparation is long.
Description
Technical field
It is technical in preparing hydrogen by reforming methanol that the present invention relates to a kind of preparation methods of igniter catalyst and igniter catalyst
Using in particular to a kind of igniter catalyst and its preparation method and application of hydrogen quick catalysis igniting.
Background technique
Currently, there are many fuel gas sparking mode in industrial application, aerospace applications and life production application,
It is mostly based on the mode of electric ignition (electrically heated rod or electricity sparking) formula or precious metal catalyst igniting.Electric sparking mode technology maturation,
And reliability is higher, but needs to configure electric energy of the corresponding power supply for starting ignition, service life and number are limited.Noble metal
Catalytic ignition mode initially starts from platinum filament, and development later is platinum powder, and development was noble metal composite later, and noble metal is adhered to
On catalyst carrier (such as aluminium oxide, silica etc.), used as igniter catalyst.The mode of electric ignition has electrically heated rod
(heater igniter) and electricity sparking (spark igniter) two ways;In addition, an if maintenance flare (pilot
Flame), without electricity sparking.Certainly maintaining flare, igniting still needs electric ignition for the first time.
Under normal circumstances, hydrogen and oxygen react required temperature at 500 DEG C or more, and hydrogen molecule is due in height at this time
The intermolecular probability for occurring freely to collide is increased under the conditions of temperature, shows higher-energy state, so as to which oxygen occurs with oxygen
Change reaction.But in the presence of a catalyst, the activation energy of hydrogen oxygen composite reaction reduces, so that hydrogen molecule is in lower energy
Also recombination reaction can occur with oxygen under state.When i.e. hydrogen is by adsorption of metal ions, hydrogen atom is activated, and is adsorbed on gold
Hydrogen atom or hydrogen ion on category ion further react with oxygen under the conditions of relatively mild.Based on principles above, urge
Change igniting to be widely used.
Usual carried noble metal igniter catalyst technology of preparing uses infusion process, coating process and chemical deposition, colloid
The technologies such as method, however the technologies such as chemical deposition, colloid method preparation process is complicated, is not easy to mass production, is relatively suitable for real
Room is tested, coating process is suitable for doing film class, and infusion process is suitable for various situations, and by a relatively simple, is suitable for batch production.
The invention patent based on the above reasons and the optimization of our company's independent research preparing hydrogen by reforming methanol technology, devises one
Kind is using the method for simply preparing igniter catalyst.This method is prepared for a kind of efficient hydrogen by allotment bullion content
Igniter catalyst, and it is technical that the catalyst is used for preparing hydrogen by reforming methanol.
Summary of the invention
Present invention aim to address subproblems present in existing Hydrogen Ignition catalysis technique, provide a kind of hydrogen point
Fiery catalyst and its preparation method and application.
The purpose of the present invention is what is be achieved through the following technical solutions:
A kind of preparation method of Hydrogen Ignition catalyst, includes the following steps:
(1) precious metal salt is dissolved in deionized water and obtains the first solution;
(2) lanthanum salt is dissolved in the first solution again, obtains the second solution;
(3) aluminum oxide colloidal sol is dispersed in deionized water, obtains third solution;
(4) third solution and the second solution are mixed, uniformly mixed solution is the 4th solution;
(5) the 4th solution is coated on carrier, obtains Intermediate Catalyst;
(6) required Hydrogen Ignition catalyst will be obtained after the activation cooling of Intermediate Catalyst drying and roasting;
The content for making noble metal by the coating number of regulating step (5) is 0.1wt%-10wt%.
Preferably, step (1)-(4) dissolution or mixing accelerated by way of heating, ultrasound or stirring dissolution or
Mixing.
Preferably, the carrier of the step (5) is porous honeycomb, spherical, netted refractory ceramics or aluminium alloy.
Preferably, the coating of the step (5) is using one of infusion process, spray coating method and drop-coating.
Preferably, the drying and roasting activation cooling of the step (6) is by Intermediate Catalyst in being placed at room temperature for 30-50min
Afterwards, it is placed in insulating box, insulating box initial temperature is set as 80-150 DEG C, dries 1-2 hour, then set calorstat temperature to
It 250-350 DEG C, is cooled to room temperature after activating 3-5 hour to get required Hydrogen Ignition catalyst is arrived.
Preferably, the drying and roasting activation cooling of the step (6) is to be put into Intermediate Catalyst in air dry oven first
At 80-150 DEG C, dry 1-2 hour, then 250-350 DEG C is set by calorstat temperature, it is cooled to after activating 3-5 hour
Room temperature to get arrive required Hydrogen Ignition catalyst.
Preferably, by the coating number of regulating step (5) make noble metal content be 0.1wt%-0.5wt% or
0.5wt%-1wt%.
Preferably, the noble metal in the step (1) is platinum or palladium.
Another aspect of the present invention, the catalyst include active component, combustion adjuvant, dispersing agent and carrier;The activity
Group is divided into the salting liquid or salt powder of platinum or palladium;The combustion adjuvant is lanthanum salt;The dispersing agent is aluminum oxide colloid;It is described
Carrier is porous honeycomb, spherical, netted refractory ceramics or aluminium alloy;The content of platinum or palladium is in the active component
0.1wt%-10wt%.
Another aspect of the present invention, the catalyst are suitable for various hydrogen catalytics igniting scene;In gas combustion process
The catalyst self-temperature is no more than 500 DEG C.
Beneficial effects of the present invention: the preparation method preparation igniter catalyst, compared with platinum powder or platinum filament, cost compared with
It is low, it is only necessary to which that carrier surface is uniformly distributed and a small amount of platinum;For speed of ignition, the higher speed of ignition of noble-metal-supported amount is more
Fastly, but load capacity is higher to mean that cost is higher, so in the case where guaranteeing certain speed of ignition, reduce as far as possible at
This, thus section selected by the application (0.5%-0.1%) be can quick firing critical section, but other sections are also this
The protection main points of application.Compared with the preparation methods such as sol method, chemical deposition, coating process, preparation method is simple, is convenient for scale
Metaplasia produces preparation;And igniter catalyst igniting is lasted a long time compared with electric ignition, for active component noble metal itself, is urged
Agent is placed on above combustion furnace, is only done igniting and is used;Burning after igniting carries out below catalyst, catalyst own temperature
500 DEG C are not exceeded, no life span;Drying can quickly slough Intermediate Catalyst surface free water at 80-150 DEG C, intermediate
Catalytic inner moisture is also migrated from inner aperture to macropore, is finally migrated to surface, is sloughed, while internal active component also can
With water translocation to Intermediate Catalyst surface.The reason of roasting at 250-350 DEG C, selecting this temperature section is: 1) roasting removes
H2O.Al2O3Volatilizable component NH in middle combination water and ammonium salt3;2) roasting can be such that active component has at this temperature
Stable catalytic activity simultaneously maintains certain crystal particle size;If 3) maturing temperature is excessively high, active group distribution may result in
Raw sintering phenomenon causes catalyst inactivation or catalytic performance to decline.The selection reason of calcining time is following two points: 1) roasting
Time is short: water and volatilizable component NH are combined in catalyst3Remove insufficient, active component is unstable, and catalyst performance is unstable
It is fixed;2) appropriate calcining time to combine water and volatilizable component NH in catalyst3Sufficiently, catalyst activity component reaches for removal
Stable state, catalyst performance stabilised.
Detailed description of the invention
Fig. 1 is igniter catalyst preparation process schematic diagram;
Fig. 2 is that Hydrogen Ignition catalyst places different location in burning furnace cavity;
Fig. 3 is that different platinum salt proportions (embodiment 1-3) prepare igniter catalyst igniting time delay comparison diagram;
Fig. 4 is hydrogen catalytic ignition process temperature changing curve diagram.
Specific embodiment
In order to better illustrate the present invention, with reference to the attached drawing in the embodiment of the present invention, in the embodiment of the present invention
Technical solution is clearly and completely described.
A kind of preparation method of Hydrogen Ignition catalyst includes the following steps: that precious metal salt is dissolved in deionized water and obtained by (1)
To the first solution;(2) lanthanum salt is dissolved in the first solution again, obtains the second solution;(3) aluminum oxide colloidal sol is evenly dispersed
In deionized water, third solution is obtained;(4) third solution and the second solution are mixed, uniformly mixed solution is the 4th molten
Liquid;(5) the 4th solution is coated on carrier, obtains Intermediate Catalyst;It (6) will be after the activation cooling of Intermediate Catalyst drying and roasting
Obtain required Hydrogen Ignition catalyst;Noble metal in the step (1) is platinum or palladium;Pass through the coating time of regulating step (5)
Number is so that the content of noble metal is 0.1wt%-10wt%.The dissolutions of step (1)-(4) or mixing by heating, ultrasound or
The mode of stirring accelerates to dissolve or mix.The carrier of the step (5) is porous honeycomb, spherical, netted refractory ceramics
Or aluminium alloy.The coating of the step (5) is using one of infusion process, spray coating method and drop-coating.The drying of the step (6)
Calcination activation cooling is placed in insulating box by Intermediate Catalyst after being placed at room temperature for 30-50min, and insulating box initial temperature is set
It is 80-150 DEG C, dry 1-2 hour, then 250-350 DEG C is set by calorstat temperature, it is cooled to after activating 3-5 hour
Room temperature to get arrive required Hydrogen Ignition catalyst.The drying and roasting activation cooling of the step (6) is to be put into Intermediate Catalyst
First at 80-150 DEG C in air dry oven, dry 1-2 hour, then 250-350 DEG C is set by calorstat temperature, activate 3-5
It is cooled to room temperature after a hour to get required Hydrogen Ignition catalyst is arrived.Your gold made by the coating number of regulating step (5)
The content of category is a section in 0.1wt%-0.5wt%, 0.5wt%-1wt%, 1wt%-5wt%, 5wt%-10wt%.
It include active component, combustion adjuvant, dispersing agent and carrier by Hydrogen Ignition catalyst prepared by the above method;It is described
Active component is the salting liquid or salt powder of platinum or palladium;The combustion adjuvant is lanthanum salt;The dispersing agent is aluminum oxide colloid;
The carrier is porous honeycomb, spherical, netted refractory ceramics or aluminium alloy;The content of platinum or palladium in the active component
Respectively in the section 0.1wt%-10wt%.The catalyst is suitable for various hydrogen catalytics igniting scene;In gas combustion process
The catalyst self-temperature is no more than 500 DEG C.
The present invention is by the content of active component platinum salt or palladium salt in allotment catalyst formulation, so that Hydrogen Ignition catalyst
The content of middle platinum or palladium is respectively in the area 0.1wt%-0.5wt%, 0.5wt%-1wt%, 1wt%-5wt%, 5wt%-10wt%
Between, as shown in embodiment 1-6.The preparation method is simple, convenient for operation and convenient for large-scale production.Whole process is mainly divided following
Three steps, as shown in Figure 1, the preparation of i.e. platinum salt or palladium salt solution, carrier impregnation is in catalyst solution, calcination activation catalyst.
Hydrogen Ignition catalyst prepared by the above different ratio is used for 201510707749.4 institute of our company's patent of invention
It states in hydrogen from methyl alcohol machine system, does hydrogen catalytic fire trial, by the way that temperature sensor is fixed on Hydrogen Ignition catalyst,
For monitoring the temperature change of the catalyst, to monitor the igniting time delay of the catalyst.Its principle is when hydrogen is initially by platinum
Or when palladium absorption, accelerate oxidation rate, it is a sections as shown in Figure 4, it monitors that the catalyst temperature increases rapidly, it is normal to reach hydrogen
Firing temperature point A point (500 DEG C or more);Later, into b sections, hydrogen-oxygen enters normal oxidation reduction reaction, if hydrogen and oxygen are held
It is continuous, uninterrupted to supply seasonable, rapid drop in temperature to certain temperature to stable state.It verifies in this way, by Hydrogen Ignition
Catalyst is placed in above combustion furnace, is only done igniting and is used, and the burning after igniting carries out below the catalyst, above four kinds of proportions
The Hydrogen Ignition catalyst of preparation can light a fire successfully, while the catalyst own temperature does not exceed 500 DEG C, no life span
Limitation.
Hydrogen Ignition catalyst is done into catalytic ignition test in methanol recapitalization combustion furnace different location, as shown in Fig. 2, three
Different location, can successful ignition.
Embodiment 1
Experiment condition: using internal diameter Φ 90mm, height 450mm burning furnace cavity, as shown in Fig. 2, by bottom fuel inlet
It is passed through the mixed gas of 70L/min flow, hydrogen molar content 42%, Hydrogen Ignition catalyst is placed in position 1 in Fig. 2.Wherein
Hydrogen Ignition catalyst is that platinum content is 5wt%-10wt% when preparing, which is 100% (each sample
Igniting ten times), consistency is higher (each sampling five, without loss of ignition phenomenon).Firing temperature and time delay when simultaneously to test
It is monitored, the catalytic ignition time delay is shorter, as shown in " temperature 1 " in Fig. 3, under the conditions of 163 DEG C of initial temperature, simultaneously
It is passed through hydrogen and air, 40 second ignitions success in about 2 minutes, and firing temperature curve can measure.
Embodiment 2
Experiment condition: using internal diameter Φ 90mm, height 450mm burning furnace cavity, as shown in Fig. 2, by bottom fuel inlet
It is passed through the mixed gas of 70L/min flow, hydrogen molar content 42%, Hydrogen Ignition catalyst is placed in position 1 in Fig. 2.Wherein
The catalyst is that platinum content is 5wt%-1wt% when preparing, which is 100% (each sample igniting ten
It is secondary), consistency is higher (each sampling five, without loss of ignition phenomenon).Firing temperature and time delay carry out when simultaneously to test
Monitoring, the catalytic ignition time delay is shorter, as shown in " temperature 2 " in Fig. 3, under the conditions of 163 DEG C of initial temperature, while being passed through hydrogen
Gas and air, 18 second ignitions success in about 3 minutes, and firing temperature curve can measure.
Embodiment 3
Experiment condition: using internal diameter Φ 90mm, height 450mm burning furnace cavity, as shown in Fig. 2, by bottom fuel inlet
It is passed through the mixed gas of 70L/min flow, hydrogen molar content 42%, Hydrogen Ignition catalyst is placed in position 1 in Fig. 2.Wherein
The catalyst is that platinum content is 0.5wt%-1wt% when preparing, which is 100% (each sample igniting
Ten times), consistency is higher (each sampling five, without loss of ignition phenomenon).Firing temperature and time delay carry out when simultaneously to test
Monitoring, the catalytic ignition time delay is shorter, as shown in " temperature 3 " in Fig. 3, under the conditions of 210 DEG C of initial temperature, be passed through simultaneously
Hydrogen and air, 48 second ignitions success in about 3 minutes, and firing temperature curve can measure.
Embodiment 4
Experiment condition: using internal diameter Φ 90mm, height 450mm burning furnace cavity, as shown in Fig. 2, by bottom fuel inlet
It is passed through the mixed gas of 70L/min flow, hydrogen molar content 42%, Hydrogen Ignition catalyst is placed in position 1 in Fig. 2.Wherein
The catalyst is that platinum content is 0.1wt%-0.5wt% when preparing, which is 80% (each sample igniting
Ten times), consistency is slightly lower (sampling five, a failure).Firing temperature and time delay are monitored when simultaneously to test, this is urged
Agent igniting time delay is longer, and about 5 minutes (stopwatch monitoring time delay), and firing temperature curve does not detect.
Above embodiments 1-4 experimental conditions can be compared by the following table 1, have a clear understanding of result.
The Hydrogen Ignition catalytic ignition situation comparison of the different platinum content preparations of table 1.
Embodiment 5
The present embodiment use with embodiment 1 to embodiment 4 similarity condition, only platinum in embodiment 1 to embodiment 4 is exchanged with
Palladium, experimental conditions are compared with platinum prepares catalyst, and under same Proportion of the active componend, igniting time delay is slightly longer than platinum preparation catalysis
Agent, other indistinctions.
Embodiment 6
The present embodiment by the way that the fuel gas mixing hydrogen and air of sufficient amount to be passed through to burning furnace cavity as shown in Figure 2,
Hydrogen Ignition catalyst is respectively placed in position 1, position 2 and the position of position 3 three, carries out igniting test respectively.When test
High temperature resisting thermocouple is fixed on Hydrogen Ignition catalyst, electric thermo-couple temperature variation extends to steady when detecting catalyst igniting
It is qualitative, three positions energy successful ignition, and time delay of lighting a fire is essentially identical.From to the long-term of Hydrogen Ignition catalyst reasonable employment
From the point of view of performance, position 1 and position 2 are chronically at a kind of condition of high temperature, are easier to make the noble metal in Hydrogen Ignition catalyst to send out
Raw burn knot, to influence its performance, therefore position 3 is optimal placed location.
The Hydrogen Ignition catalyst of preparation method preparation, compared with platinum powder or platinum filament, cost is relatively low, it is only necessary to carrier table
Face is uniformly distributed and a small amount of platinum;Compared with the preparation methods such as sol method, chemical deposition, coating process, preparation method is simple, just
In large-scale production and preparation;And Hydrogen Ignition catalytic ignition lasts a long time compared with electric ignition, with regard to active component noble metal sheet
For body, the Hydrogen Ignition catalyst of the application is placed on above combustion furnace, is only done igniting and is used;Burning after igniting is urged at this
It is carried out below agent, catalyst own temperature does not exceed 500 DEG C, no life span limitation.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Within the technical scope of the present disclosure, any changes or substitutions that can be easily thought of by anyone skilled in the art,
It should all be included within the scope of the present invention.Therefore, protection scope of the present invention should be with the protection of claims
Subject to range.
Claims (7)
1. a kind of preparation method of Hydrogen Ignition catalyst, which comprises the steps of:
(1) precious metal salt is dissolved in deionized water and obtains the first solution;
(2) lanthanum salt is dissolved in the first solution again, obtains the second solution;
(3) aluminum oxide colloidal sol is dispersed in deionized water, obtains third solution;
(4) third solution and the second solution are mixed, uniformly mixed solution is the 4th solution;
(5) the 4th solution is coated on carrier, obtains Intermediate Catalyst;
(6) required Hydrogen Ignition catalyst will be obtained after the activation cooling of Intermediate Catalyst drying and roasting;
The content for making noble metal by the coating number of regulating step (5) is 0.1wt%-10wt%;
The noble metal is platinum or palladium;
The drying and roasting activation cooling of the step (6) is obtained by two methods: one is Intermediate Catalyst is put in room temperature
It after setting 30-50min, is placed in insulating box, insulating box initial temperature is set as 80-150 DEG C, dry 1-2 hour, then by insulating box
Temperature setting is 250-350 DEG C, is cooled to room temperature after activating 3-5 hour to get required Hydrogen Ignition catalyst is arrived;The second is
Intermediate Catalyst is put into air dry oven first at 80-150 DEG C, dry 1-2 hour, then sets calorstat temperature to
250-350 DEG C, calcination activation was cooled to room temperature to arrive required Hydrogen Ignition catalyst after 3-5 hour.
2. preparation method according to claim 1, which is characterized in that the dissolution or mixing of step (1)-(4) pass through
The mode of heating, ultrasound or stirring accelerates to dissolve or mix.
3. preparation method according to claim 1, which is characterized in that the carrier of the step (5) is porous honeycomb, ball
Shape, netted refractory ceramics or aluminium alloy.
4. preparation method according to claim 1, which is characterized in that the coating of the step (5) is using infusion process, spraying
One of method and drop-coating.
5. preparation method according to claim 1, which is characterized in that made by the coating number of regulating step (5) expensive
The content of metal is 0.1wt%-0.5wt% or 0.5wt%-1wt%.
6. a kind of Hydrogen Ignition catalyst of -5 any the method preparations according to claim 1, which is characterized in that the hydrogen
Igniter catalyst includes active component, combustion adjuvant, dispersing agent and carrier;The active component is the salting liquid or salt fines of platinum or palladium
End;The combustion adjuvant is lanthanum salt;The dispersing agent is aluminum oxide colloid;The carrier is porous honeycomb, spherical, netted
Refractory ceramics or aluminium alloy;The content of platinum or palladium is in the section 0.1wt%-10wt% in the active component.
7. the purposes of Hydrogen Ignition catalyst according to claim 6, which is characterized in that the Hydrogen Ignition catalyst is suitable for
Various hydrogen catalytics igniting scenes;The catalyst self-temperature described in gas combustion process is no more than 500 DEG C.
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CN102049312A (en) * | 2009-10-27 | 2011-05-11 | 中国石油化工股份有限公司 | Preparation method of catalytic combustion catalyst |
CN102427878A (en) * | 2009-05-20 | 2012-04-25 | 巴斯夫欧洲公司 | Monolith catalyst and use thereof |
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CN102427878A (en) * | 2009-05-20 | 2012-04-25 | 巴斯夫欧洲公司 | Monolith catalyst and use thereof |
CN102049312A (en) * | 2009-10-27 | 2011-05-11 | 中国石油化工股份有限公司 | Preparation method of catalytic combustion catalyst |
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