CN109745991A - The preparation method and application of O composite metallic oxide catalyst for coal gasification - Google Patents
The preparation method and application of O composite metallic oxide catalyst for coal gasification Download PDFInfo
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- Y02P20/00—Technologies relating to chemical industry
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
The invention discloses a kind of preparation method and application of O composite metallic oxide catalyst for coal gasification, lanthanum nitrate, nitric acid metal salt A, ferric nitrate and nitric acid metal salt B are added to the water uniformly mixed, metal nitrate saline solution by this method；Then EDTA and citric acid are mixed, adjusts pH value 7~9, is placed in water bath with thermostatic control and stirs evenly, be configured to precursor solution；Metal nitrate saline solution is added in above-mentioned precursor solution, continues stirring until forming wet gel；Dry, calcining cooling obtains O composite metallic oxide catalyst.Catalyst of the invention can not only effectively improve the rate of gasification of coal, and conversion ratio is up to 90%；Original structure and catalytic activity can also be still kept after the reaction, and then can be recycled to achieve the purpose that recycling.
Description
Technical field
The present invention relates to metal oxide catalysts, in particular to a kind of composite metal oxide catalyst for coal gasification
The preparation method and application of agent.
Background technique
Coal gasification is increasingly valued by people as one of the important means of coal machining and transform.This is because
Coal gasification can provide synthesis gas and substitute natural gas.If can be gasified using colms such as dirty coal, fine coal, to protection ring
It is significant that border reduces cost.As a kind of mild gasification technology, the catalytic gasification of coal is always that people quite feel and interesting must grind
Study carefully the selection that project key therein is catalyst.
Numerous studies confirmation, coal and gasifying agent (such as vapor, CO2、H2、O2) between the most effective catalysis of gasification reaction
Agent is mainly alkali metal class[1], alkaline-earth metal class[2](AAEM), transition metal-type[3].The price of catalyst and recycling and generation
Secondary pollution problems restrict always the process of industrialization of catalytic coal gasifaction[4].Studies have shown that the industrialization of composite catalyst
Prospect is preferable, but it is the key that its economic production that catalyst, which recycles and reuses,.
Therefore, it develops recoverable and the high new catalyst of catalytic activity has the industrialization of Coal Gasification Technology
Important meaning.
[1] Tang J, Wang J.Fuel Process.Technol., 2016,142:34.
[2] Freek K, Hans P, Moulijn J A.AlChE J., 1986,32 (4): 691.
[3] Popa T, Fan M, Argyle M D, Dyar M D, Gao Y, Tang J, Speicher E A, Kammen
D M.Appl Catal A-Gen., 2013, s464/
465(6):207.
[4] Mei Y G, Wang Z Q, Fang H B, Wang Y W, Huang J J, Fang
Y T.Energy Fuels, 2017,31 (2): 1235.
Summary of the invention
The present invention is for the price height of existing catalyst and recycling and generates secondary pollution problems, and restricts coal
The defect of the process of industrialization of catalytic gasification provides a kind of preparation side of O composite metallic oxide catalyst for coal gasification
Method and application.
To achieve the above object, the preparation of a kind of O composite metallic oxide catalyst for coal gasification provided by the invention
Method, comprising the following steps:
1) x: 1-x: y: 1-y lanthanum nitrate, nitric acid metal salt A, ferric nitrate and nitric acid metal salt B are weighed respectively in molar ratio,
And x=0~1, y=0~1, wherein metal ion A is any one in Sr, Ba and Ca, nitric acid metal salt in nitric acid metal salt A
Metal ion B is any one in Co, Cu, Mn, Ni and Zn in B；
2) lanthanum nitrate, nitric acid metal salt A, ferric nitrate and nitric acid metal salt B are added to the water uniformly mixed, metal nitrate
Aqueous solution；
3) by the molar ratio 1: 1 of EDTA, citric acid and the metal ion total mole number in above-mentioned metal nitrate saline solution
Weigh EDTA, citric acid and metal nitrate saline solution at~2: 1；
4) EDTA and citric acid are mixed, adjusts pH value 7~9, is placed in water bath with thermostatic control and stirs evenly, be configured to forerunner
Liquid solution；
5) metal nitrate saline solution is added in above-mentioned precursor solution, continues stirring until forming wet gel；
6) wet gel is dry until forming xerogel；
7) by above-mentioned xerogel, the first stage calcines 0.5~1h under the conditions of temperature is 400~500 DEG C；Again by its
Second stage calcines 8~10h under the conditions of temperature is 800~900 DEG C；
8) it takes out, is ground after cooling and obtain black powder, as O composite metallic oxide catalyst LaxA1-xFeyB1-yO3-δ；
Wherein, A is Sr or Ba or Ca；B is Co or Cu or Mn or Ni or Zn；X=0~1, y=0~1.
Further, in the step 1), x=0.1~0.3, y=0.1~0.3, wherein metal in nitric acid metal salt A
Ion A is Sr or Ba, and metal ion B is Co or Ni in nitric acid metal salt B.
Still further, described x=0.1, y=0.2, wherein metal ion A is Sr, nitric acid metal in nitric acid metal salt A
Metal ion B is Co in salt B.
Still further, the metal ion in the step 3), in EDTA, citric acid and above-mentioned metal nitrate saline solution
The molar ratio 1: 1.2: 1 of total mole number.
Still further, the temperature of water bath with thermostatic control is 70~85 DEG C in the step 4).
Still further, drying temperature is 100~110 DEG C in the step 6).
Still further, first stage calcining: the first stage forges under the conditions of temperature is 400~450 DEG C in the step 7)
Burn 0.5~0.8h；By it, second stage calcines 8~10h under the conditions of temperature is 830~870 DEG C again.
Still further, first stage calcining: the first stage calcines under the conditions of temperature is 400 DEG C in the step 7)
0.5h；By it, second stage calcines 10h under the conditions of temperature is 850 DEG C again.
Above-mentioned O composite metallic oxide catalyst answering in coal gasification course is prepared the present invention also provides a kind of
With.
Preferably, the application method (dry pigmentation mixing):
A. the coal and catalyst for weighing drying by weight 1: 1~8, are put into agate mortar, and grinding finishes collection and puts
The baking oven entered toasts 10~20min, obtains mixture,
B. hydrogen, vapor reaction are passed through into mixture, filtration drying obtains methane.
The principle of the present invention:
1) catalytic gasification of coal be improve coal gasification efficiency important channel, catalytic gasification can be substantially reduced reaction temperature,
Improve efficiency of carbon con version, investment reduction cost.The either gasification of pure atmosphere or mixed atmosphere gasification of vapor or hydrogen, alkali gold
Belong to and alkali earth metal is the good catalyst of effect, but its loss and clogging problems in use are difficult to solve,
It is difficult to be easy distillation loss recycling, assembles and corrode the piping installation in downstream.
2) perovskite catalyst of the invention at an appropriate reaction temperature in there is no be sintered and loss phenomenon, rely on
Dry-mixed mixed method is obtained with preferable catalytic effect.Method by being calcined in simple air simultaneously, it will be able to
Restore its perovskite structure, the ability with round-robin.It is a kind of very promising catalysis that can be used as catalytic coal gasifaction
Agent.
The beneficial effects of the present invention are:
1. the rate of gasification of coal can not only be effectively improved, conversion ratio is up to 90%；Catalyst still keeps former after the reaction
There are structure and catalytic activity, and then can recycle to achieve the purpose that recycling.
2. catalyst has stronger automatic recovery ability, by calcining in simple air, knot in furnace is not only solved
Slag problem, and reduce the cost recovery of catalyst.
Detailed description of the invention
Fig. 1 is XRD comparison diagram: after the fresh O composite metallic oxide catalyst and gasification reaction of synthesis in air again
Calcine the comparison of the catalyst formed；
Fig. 2 is influence diagram of the catalyst to the efficiency of carbon con version of coal gasification reaction of different loads amount.
Specific embodiment
In order to better explain the present invention, below in conjunction with the specific embodiment main contents that the present invention is furture elucidated, but
The contents of the present invention are not limited solely to following embodiment.
Embodiment 1
O composite metallic oxide catalyst La for coal gasification0.5Sr0.5Fe0.2Co0.8O3-δPreparation:
1) 0.5: 0.5: 0.2: 0.8 (5:5:2:8) weighs lanthanum nitrate, strontium nitrate, ferric nitrate, nitric acid respectively in molar ratio
Cobalt；
2) by lanthanum nitrate, strontium nitrate, ferric nitrate, cobalt nitrate is added to the water uniformly mixed, metal nitrate saline solution；
3) by the molar ratio 1: 1 of EDTA, citric acid and the metal ion total mole number in above-mentioned metal nitrate saline solution:
1 weighs EDTA, citric acid and metal nitrate saline solution；
4) EDTA and citric acid are mixed, adjust pH value 8, be placed in the water bath with thermostatic control that temperature is 75 DEG C and stir evenly,
It is configured to precursor solution；
5) metal nitrate saline solution is added in above-mentioned precursor solution, continues stirring until forming wet gel；
6) wet gel is dry under the conditions of temperature is 105 DEG C until forming xerogel；
7) by above-mentioned xerogel, the first stage calcines 0.5h under the conditions of temperature is 400 DEG C；It is again 870 in temperature by it
Second stage calcines 10h under the conditions of DEG C；
8) it takes out, is ground after cooling and obtain black powder, as O composite metallic oxide catalyst
La0.5Sr0.5Fe0.5Co0.5O3-δ。
Embodiment 2
O composite metallic oxide catalyst La0.1Sr0.9Co0.8Fe0.2O3-δPreparation:
1) lanthanum nitrate strontium nitrate, cobalt nitrate, ferric nitrate are respectively weighed at 0.1: 0.9:0.8: 0.2 in molar ratio；
2) lanthanum nitrate, strontium nitrate, cobalt nitrate and ferric nitrate are added in distilled water and are mixed evenly to form metal nitrate
Saline solution；
3) by the molar ratio 1 of EDTA, citric acid and the metal ion total mole number in above-mentioned metal nitrate saline solution:
Weigh EDTA, citric acid and metal nitrate saline solution at 1.2: 1；
4) EDTA and citric acid are mixed, adjust pH value 8, be placed in the water bath with thermostatic control that temperature is 75 DEG C and stir evenly,
It is configured to precursor solution；
5) metal nitrate saline solution is added in above-mentioned precursor solution, continues stirring until forming wet gel；
6) wet gel is dry under the conditions of temperature is 110 DEG C until forming xerogel；
7) by above-mentioned xerogel, the first stage calcines 0.5h under the conditions of temperature is 400 DEG C；It is again 850 in temperature by it
Second stage calcines 10h under the conditions of DEG C；
8) it takes out, is ground after cooling and obtain black powder, as O composite metallic oxide catalyst
La0.1Sr0.9Co0.8Fe0.2O3-δ。
Embodiment 3
O composite metallic oxide catalyst La0.1Ba0.9Fe0.1Co0.9O3-δPreparation:
1) 0.1: 0.9:0.1: 0.9 (1: 9: 1: 9) weigh lanthanum nitrate, barium nitrate, ferric nitrate, nitric acid respectively in molar ratio
Manganese；
2) by lanthanum nitrate, barium nitrate, ferric nitrate, manganese nitrate is added to the water uniformly mixed, forms metal nitrate saline solution；
3) by the molar ratio 1 of EDTA, citric acid and the metal ion total mole number in above-mentioned metal nitrate saline solution:
Weigh EDTA, citric acid and metal nitrate saline solution at 1.2: 1；
4) EDTA and citric acid are mixed, adjust pH value 8, be placed in the water bath with thermostatic control that temperature is 80 DEG C and stir evenly,
It is configured to precursor solution；
5) metal nitrate saline solution is added in above-mentioned precursor solution, continues stirring until forming wet gel；
6) wet gel is dry under the conditions of temperature is 110 DEG C until forming xerogel；
7) by above-mentioned xerogel, the first stage calcines 0.5h under the conditions of temperature is 400 DEG C；It is again 850 in temperature by it
Second stage calcines 8h under the conditions of DEG C；
8) it takes out, is ground after cooling and obtain black powder, as O composite metallic oxide catalyst
La0.1Ba0.9Fe0.1Co0.9O3-δ。
Embodiment 4
O composite metallic oxide catalyst La0.5Sr0.5Co0.8Fe0.2O3-δPreparation:
1) lanthanum nitrate strontium nitrate, cobalt nitrate, ferric nitrate are respectively weighed at 0.5: 0.5:0.8: 0.2 in molar ratio；
2) lanthanum nitrate, strontium nitrate, cobalt nitrate and ferric nitrate are added in distilled water and are mixed evenly to form metal nitrate
Saline solution；
3) by the molar ratio 1 of EDTA, citric acid and the metal ion total mole number in above-mentioned metal nitrate saline solution:
Weigh EDTA, citric acid and metal nitrate saline solution at 1.5: 1；
4) EDTA and citric acid are mixed, adjust pH value 8, be placed in the water bath with thermostatic control that temperature is 80 DEG C and stir evenly,
It is configured to precursor solution；
5) metal nitrate saline solution is added in above-mentioned precursor solution, continues stirring until forming wet gel；
6) wet gel is dry under the conditions of temperature is 110 DEG C until forming xerogel；
7) by above-mentioned xerogel, the first stage calcines 0.5h under the conditions of temperature is 400 DEG C；It is again 850 in temperature by it
Second stage calcines 5h under the conditions of DEG C；
8) it takes out, is ground after cooling and obtain black powder, as O composite metallic oxide catalyst
La0.5Sr0.5Co0.8Fe0.2O3-δ。
O composite metallic oxide catalyst prepared by above-described embodiment 1~4 carries out coal gasification with following methods:
Coal gasification application method (dry pigmentation mixing):
A. the coal and catalyst for weighing drying by weight 4: 1, are put into agate mortar, and grinding finishes what collection was put into
Temperature is that 120 DEG C of baking ovens toast 10~20min, obtains mixture,
B. it is passed through hydrogen and vapor into mixture, is reacted under the conditions of temperature is 850 DEG C, collects gasification product.
C. after gasification reaction, N2 scavenging pipeline is switched to, the air of 500ml/min is subsequently passed, is cooled to room temperature
After collect sample.
It is as shown in Figure 1 the XRD diagram of perovskite catalyst reaction front and back.Catalyst is after gasification reaction again in air gas
After being calcined under atmosphere, carbon residue can be completely removed and restore the perovskite structure of itself.With traditional coal gasification catalyst ratio, this hair
The catalyst of bright preparation has good renewable ability.The performance of catalyst is as shown in Fig. 2, in catalyst
When the load capacity of La0.1Sr0.9Co0.8Fe0.2O3- δ is 20%, the effect of the efficiency of carbon con version of coal gasification preferably reaches
80~90%, therefore, composite catalyst of the invention is a kind of very promising catalyst that can be used as coal gasification.
Other unspecified parts are the prior art.Although above-described embodiment is made that the present invention and retouches in detail
State, but it is only a part of the embodiment of the present invention, rather than whole embodiments, people can also according to the present embodiment without
Other embodiments are obtained under the premise of creativeness, these embodiments belong to the scope of the present invention.
Claims (10)
1. a kind of preparation method of the O composite metallic oxide catalyst for coal gasification, it is characterised in that: the following steps are included:
1) x: 1-x: y: 1-y lanthanum nitrate, nitric acid metal salt A, ferric nitrate and nitric acid metal salt B, and x=are weighed respectively in molar ratio
0~1, y=0~1, wherein metal ion A is any one in Sr, Ba and Ca in nitric acid metal salt A, golden in nitric acid metal salt B
Belonging to ion B is any one in Co, Cu, Mn, Ni and Zn；
2) lanthanum nitrate, nitric acid metal salt A, ferric nitrate and nitric acid metal salt B are added to the water uniformly mixed, metal nitrate is water-soluble
Liquid；
3) by the molar ratio 1: 1~2: 1 of EDTA, citric acid and the metal ion total mole number in above-mentioned metal nitrate saline solution
Weigh EDTA, citric acid and metal nitrate saline solution；
4) EDTA and citric acid are mixed, adjusts pH value 7~9, is placed in water bath with thermostatic control and stirs evenly, it is molten to be configured to presoma
Liquid；
5) metal nitrate saline solution is added in above-mentioned precursor solution, continues stirring until forming wet gel；
6) wet gel is dry until forming xerogel；
7) by above-mentioned xerogel, the first stage calcines 0.5~1h under the conditions of temperature is 400~500 DEG C；Again by it in temperature
Second stage calcines 8~10h under the conditions of being 800~900 DEG C；
8) it takes out, is ground after cooling and obtain black powder, as O composite metallic oxide catalyst LaxA1-xFeyB1-yO3-δ；Its
In, A is Sr or Ba or Ca；B is Co or Cu or Mn or Ni or Zn；X=0~1, y=0~1.
2. the preparation method for the O composite metallic oxide catalyst of coal gasification according to claim 1, it is characterised in that:
In the step 1), x=0.1~0.3, y=0.1~0.3, wherein metal ion A is Sr or Ba, nitric acid in nitric acid metal salt A
Metal ion B is Co or Ni in metal salt B.
3. the preparation method for the O composite metallic oxide catalyst of coal gasification according to claim 2, it is characterised in that:
Described x=0.1, y=0.2, wherein metal ion A is Sr in nitric acid metal salt A, and metal ion B is Co in nitric acid metal salt B.
4. the preparation method of the O composite metallic oxide catalyst according to claim 1 or claim 2 for coal gasification, feature exist
In: in the step 3), the molar ratio of EDTA, citric acid and the metal ion total mole number in above-mentioned metal nitrate saline solution
1∶1.2∶1。
5. the preparation method of the O composite metallic oxide catalyst according to claim 1 or claim 2 for coal gasification, feature exist
In: in the step 4), the temperature of water bath with thermostatic control is 70~85 DEG C.
6. the preparation method of the O composite metallic oxide catalyst according to claim 1 or claim 2 for coal gasification, feature exist
In: in the step 6), drying temperature is 100~110 DEG C.
7. the preparation method of the O composite metallic oxide catalyst according to claim 1 or claim 2 for coal gasification, feature exist
In: in the step 7), first stage calcining: the first stage calcines 0.5~0.8h under the conditions of temperature is 400~450 DEG C；Again will
Its second stage under the conditions of temperature is 830~870 DEG C calcines 8~10h.
8. the preparation method for the O composite metallic oxide catalyst of coal gasification according to claim 7, it is characterised in that:
In the step 7), first stage calcining: the first stage calcines 0.5h under the conditions of temperature is 400 DEG C；It is again 850 in temperature by it
Second stage calcines 10h under the conditions of DEG C.
9. application of the O composite metallic oxide catalyst in coal gasification course is prepared in a kind of claim 1.
10. application according to claim 9, it is characterised in that: the application method:
A. the coal and catalyst for weighing drying by weight 1: 1~8, are put into agate mortar, and grinding finishes what collection was put into
Baking oven toasts 10~20min, obtains mixture,
B. hydrogen, vapor reaction are passed through into mixture, filtration drying obtains methane.
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| CN112058272A (en) * | 2020-08-20 | 2020-12-11 | 天津大学 | Perovskite type catalyst prepared by sol-gel weak oxidation calcination method and method |
| CN113578332A (en) * | 2021-08-23 | 2021-11-02 | 深圳明讯新材料科技有限公司 | Preparation method of catalyst for preparing new energy methane gas |
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