CN109621963A - A kind of preparation method and application of the three-way catalyst for reverse water-gas-shift reaction - Google Patents
A kind of preparation method and application of the three-way catalyst for reverse water-gas-shift reaction Download PDFInfo
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- CN109621963A CN109621963A CN201811539419.9A CN201811539419A CN109621963A CN 109621963 A CN109621963 A CN 109621963A CN 201811539419 A CN201811539419 A CN 201811539419A CN 109621963 A CN109621963 A CN 109621963A
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/78—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with alkali- or alkaline earth metals
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- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
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Abstract
The present invention provides a kind of ternary Cu/MgO/Al2O3The preparation method of catalyst and its application in reverse water-gas-shift reaction belong to material preparation and catalysis technical field.Using CuMgAl-LDH as presoma, Cu/MgO/Al is prepared for through high temperature reduction2O3, preparation-obtained Cu/MgO/Al2O3The active high feature of Ni metal dispersion degree, under normal pressure can efficient catalytic against the progress of water gas reaction, catalyst performance is high, and long-time catalytic reaction activity is without significant change.The method for preparing catalyst is simple, is conducive to large-scale industrial production, has significant economic and social benefit.
Description
Technical field
The invention belongs to material preparation and catalysis technical fields, and in particular to pass through to a kind of by presoma of CuMgAl-LDH
The ternary Cu/MgO/Al of high temperature reduction preparation2O3Catalyst and its application in reverse water-gas-shift reaction.
Background technique
CO2It is a kind of greenhouse gases.Although on a large scale using fossil resource to human society since twoth century of past
The CO for bringing unprecedented prosperity, but largely discharging2Lead to global warming and the deterioration of environment.If there is the estimated ground of research
Ball temperature rises 3 DEG C again, then the trend of global warming will be thoroughly out of control, and again inability is intervened temperature of the earth by the mankind
Variation, the earth will suffer from extinction.According to statistics, combustion of the whole world due to various fossil fuel (coal, petroleum, natural gas) at present
Burn the CO in be discharged into atmosphere2Amount has reached 185 ~ 24,200,000,000 tons/year, however it is utilized still less than 100,000,000 tons/year.Therefore
CO2Emission reduction and recycle arrive very urgent rank break.Make CO2Fix and be converted to low-carbon alcohols, lower carbon number hydrocarbons and organic acid etc.
Other carbon source forms store, and on the one hand can alleviate greenhouse effects, and important chemical industry on the other hand can also be provided for the mankind
Raw material, therefore current CO2Fixation and conversion by countries in the world it is unprecedented concern and pay attention to.
Related CO at present2Emission reduction, recycle research be concentrated mainly on find fossil energy substitute, exploitation save
It can new technology and new process, CO2It seals up for safekeeping, CO2Recycle four aspects.Solar energy, water energy, wind energy, nuclear energy and biomass energy etc. are new
The energy is current most study instead of the energy.On the other hand, it eliminates and falls behind technique, develop power-saving technology and new process, mention
High fossil fuel utilization efficiency, can also reduce CO indirectly2Discharge. CO2Geological storage (Geological can be divided by sealing up for safekeeping
Storage) and ocean seals (Ocean Storage) two classes up for safekeeping.But CO2It seals research up for safekeeping and is merely observed that greenhouse effects heat up to the earth
Influence, and ignore other influences on earth ecology.
As things go, compared with sealing up for safekeeping, by CO2The fuel and large chemicals for being converted to high added value can be with
It plays storage simultaneously, utilize CO2With the effect of renewable energy, there is important strategic importance.Because can not only create in this way
Considerable economic benefit, also increases " service life " of carbon to a certain extent, while can further realize the circulation benefit of carbon
With.The exhaustion of the energy is the exhaustion of fuel after all.In numerous CO2Chemical activator in, CO2Catalytic hydrogenation is by people
Favor.This is not just merely because catalytic hydrogenation can be CO2Emission reduction contribute, it is often more important that this mode can will be seen
Like useless CO2The various fuel that can directly utilize are converted into, wherein reverse water-gas-shift reaction (CO2+H2=CO+H2O)
It is considered as one of the reaction for most having application prospect, so exploitation has high activity, high stability and highly selective coal against the current
Gas catalyst for water-gas shift reaction is to CO2Utilization and the production of the energy be of great significance.Coal gas reacting condition is one against the current
Reversible reaction, under normal circumstances, the catalyst suitable for water gas shift reaction are also applied for coal gas reacting condition against the current, this kind of
Catalyst is based on copper-based catalysts.But reverse water-gas-shift reaction belongs to the endothermic reaction, high temperature is conducive to CO2Conversion and
The formation of CO.CN103230799A patent discloses a kind of Cu-Zn base catalyst for reverse water-gas-shift reaction, passes through
One or more of Zn and transition metal, alkali metal, alkaline-earth metal or rare earth element are added in copper-based catalysts, obtains
There is the catalyst compared with high reaction activity and higher CO selectivity under low temperature, but at high temperature, copper-based catalysts easy-sintering.It opens
One kind catalysts of coal gas against the current resistant to high temperature are sent out to have great importance.
Summary of the invention
The purpose of the present invention is to provide one kind to prepare ternary Cu/MgO/ through high temperature reduction using CuMgAl-LDH as presoma
Al2O3Catalyst method simultaneously is applied to it to realize reverse water-gas-shift reaction under normal pressure.Intend to solve that current Reversed Water-gas Shift is urged
The problems such as reaction condition of high temperature and pressure generally required for agent.Cu/MgO/Al prepared by the present invention2O3Active gold
The features such as metal nano-particle dispersion degree is high, reactivity is good.Raw material of the present invention is cheap and easy to get, and preparation method is simple, is conducive to big
The industrial production of scale has significant economic and social benefit.
To achieve the above object, the present invention adopts the following technical scheme:
A kind of ternary Cu/MgO/Al of efficient catalytic against water gas reaction2O3Catalyst is passed through by presoma of CuMgAl-LDH
It, being capable of preferably adsorption reaction gas CO with stronger alkalinity made from high temperature reduction2, catalyst stability is high, Neng Gouchang
Time uses.
Cu/MgO/Al of the efficient catalytic against water gas reaction2O3It is to be synthesized by high temperature reduction CuMgAl-LDH
's.Its synthesis step are as follows: the Cu (NO for being respectively 0.3:1.7:1 by molar ratio3)2·3H2O 、Mg(NO3)2·6H2O 、Al
(NO3)3·9H2O is add to deionized water, and urea is added into mixed solution, wherein urea and Al (NO3)3·9H2O's rubs
You are than being 20:1.120 ~ 140 DEG C of 24 h of ageing in polytetrafluoroethylene (PTFE) water heating kettle are transferred to after ultrasonic disperse is uniform.It is centrifuged, washed
It washs, dry and obtain CuMgAl-LDH presoma.CuMgAl-LDH presoma is in 400 DEG C of H2(10% H2/ Ar, 60 mL/min)
5 h are restored in atmosphere obtains Cu/MgO/Al2O3。
Remarkable advantage of the invention is:
(1) present invention prepares Cu/MgO/Al through high temperature reduction using CuMgAl-LDH as presoma for the first time2O3, and be applied to against the current
In gas shift reaction.
(2) Cu/MgO/Al of the invention2O3For reverse water-gas-shift reaction, active high, the good, stability of selectivity
Well, the features such as reaction condition mild (can carry out under normal pressure).
(3) preparation method is simple for catalyst in the present invention, is conducive to promote on a large scale.
Detailed description of the invention
Fig. 1 is the X-ray diffraction (XRD) figure of catalyst precursor CuMgAl-LDH of the invention.
Fig. 2 is ternary Cu/MgO/Al of the invention2O3The X-ray diffraction (XRD) figure of catalyst.
Fig. 3 is ternary Cu/MgO/Al of the invention2O3Catalyst is used for the active testing figure of reverse water-gas-shift reaction.Figure
3-1 indicates reactivity figure when reaction temperature is 250 DEG C；Fig. 3-2 indicates reactivity when reaction temperature is 300 DEG C
Figure；Fig. 3-3 indicates reactivity figure when reaction temperature is 350 DEG C.
Fig. 4 is the catalyst of the invention catalyst stability test figure in 350 DEG C of reactions.
Specific embodiment
It is several embodiments of the present invention below, further illustrates the present invention, but the present invention is not limited only to this.
Embodiment 1
Cu/MgO/Al2O3Preparation
Weigh the Cu (NO that molar ratio is 0.3:1.7:13)2·3H2O、Mg(NO3)2·6H2O、Al(NO3)3·9H2O and suitable
Deionized water ultrasonic disperse is added in urea in beaker, wherein C[Al 3+ ]=0.05 mol/L, C[urea]=1 mol/L.By ultrasound point
Solution after dissipating uniformly is transferred to 120 ~ 140 DEG C of 24 h of heating in 100 ml polytetrafluoroethylene (PTFE) water heating kettles.It is washed with deionized water
Until washing, be centrifuged the pH until cleaning solution=7.Sample after washing is transferred in 60 DEG C of vacuum drying ovens dry one the whole night,
Sample after drying is polished to obtain nattier blue CuMgAl-LDH presoma.By gained CuMgAl-LDH presoma in H2
(10% H2/ Ar, flow velocity=60 ml/min) 400 DEG C are warming up to the heating rate of 2 DEG C/min in atmosphere, in 400 DEG C of items
5 h are restored under part obtains ternary Cu/MgO/Al2O3。
Fig. 1 illustrates the X-ray diffraction (XRD) figure of CuMgAl-LDH presoma of the invention, as can be seen from the figure makes
Standby CuMgAl-LDH is pure phase.Fig. 2 illustrates the Cu/MgO/Al prepared as presoma through high temperature reduction using CuMgAl-LDH2O3
XRD diagram.The diffraction maximum of Cu and MgO as we can see from the figure, does not see Al in XRD diagram2O3Diffraction maximum, this is because
Al2O3It is amorphous.
Embodiment 2
Cu/MgO/Al2O3It is catalyzed reverse water-gas-shift reaction
By the Cu/MgO/Al of preparation2O3For being catalyzed reverse water-gas-shift reaction.Concrete operations be weigh 200 mg catalyst and
0.8 g quartz sand, which is put into sample cell, to be inserted after mixing in flat threeway quartz reactor, is interleave in the reactor
Enter K-type thermocouple for detection reaction temperature.It is CO in gaseous mixture ratio2 : H2 : N2=15:60:25, gaseous mixture flow velocity:
20 ml/min (GHSV = 6000 mlh-1g-1) T=250, investigate its catalytic performance under conditions of 300,350 DEG C.Using
Panna A91 chromatography on-line period is detected, CO2Measurement separated using Porapark Q packed column, examined into TCD
Device detection is surveyed, hydrocarbon uses SH-RtⓇ- Q-BOND capillary column is separated, and is detected into fid detector.The CO of generation
CH is converted into nickel reburner4After enter back into fid detector and detected.Fig. 4 is that catalyst is stablized in 350 DEG C of 20 h of reaction
Property test chart.The conversion ratio of reactant and the selectivity of product are calculated using area correction normalization method.
The foregoing is merely presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with
Modification, is all covered by the present invention.
Claims (3)
1. a kind of ternary Cu/MgO/Al2O3The preparation method of catalyst, it is characterised in that: using CuMgAl-LDH be presoma through height
Temperature reduction is prepared for Cu/MgO/Al2O3, under normal pressure can efficient catalytic reverse water-gas-shift reaction.
2. ternary Cu/MgO/Al according to claim 12O3The preparation method of catalyst, it is characterised in that: respectively by Cu
(NO3)2·3H2O 、Mg(NO3)2·6H2O、Al(NO3)3·9H2O is (0.3 ~ 0.7) in molar ratio: (1.7 ~ 1.3): 1 is added to
In deionized water, urea is then added into mixed solution, wherein the concentration of urea is 18 ~ 20 times of aluminum nitrate concentration, warp
Be transferred to after ultrasonic disperse is uniform in polytetrafluoroethylene (PTFE) water heating kettle in 120 ~ 140 DEG C of 24 h of heating, product through centrifugation, washing,
Drying obtains CuMgAl-LDH presoma, by obtained CuMgAl-LDH presoma in 400 DEG C of H24 ~ 5 h are restored in atmosphere
Obtain ternary Cu/MgO/Al2O3。
3. a kind of ternary Cu/MgO/Al of method preparation as described in claim 12O3Catalyst is in reverse water-gas-shift reaction
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Cited By (1)
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| CN115155581A (en) * | 2022-08-02 | 2022-10-11 | 北京航空航天大学 | Copper-based composite catalyst and preparation method and application thereof |
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Application publication date: 20190416 |