CN103484170A - Cerium lanthanum-based desulfurizing agent and preparation method thereof - Google Patents
Cerium lanthanum-based desulfurizing agent and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a cerium lanthanum-based desulfurizing agent and a preparation method thereof. The cerium lanthanum-based desulfurizing agent is prepared by the following steps: mixing cerium oxide, lanthanum oxide, a pore-forming agent and an adhesive firstly with a dry mixing method to obtain a powder mixture; mixing the obtained powder mixture by a planetary ball mill; drying the ball-milled powder in a vacuum-drying box for 2 hours by controlling the temperature to be 150 DEG C, and performing extrusion molding; and placing the material into a muffle furnace, heating to 600 to 1,000 DEG C by controlling the speed to be 10 DEG C/min, sintering at a constant temperature for 4 hours, and naturally cooling to obtain the cerium lanthanum-based desulfurizing agent, wherein the using amounts of the cerium oxide, the lanthanum oxide, the pore-forming agent and the adhesive is calculated according to the mass ratio, namely the mass ratio of the cerium oxide, the lanthanum oxide, the pore-forming agent and the adhesive is 15:(4.5-6.5):(1-1.5):1. The cerium lanthanum-based desulfurizing agent has desulfurization efficiency, simple preparation scheme, wide application prospect and high social and economic values.
Description
Technical field
The present invention relates to a kind of cerium lanthanum base desulfurizer and preparation method thereof.
Background technology
Except CO, H, CH and other gaseous hydrocarbons, also have COS, H in common coal gas
2the impurity such as S, dust, halogenide, basic metal and tar steam, these impurity can, to particularly internal combustion turbine generation corrosion and wearing and tearing of follow-up system, also can produce harm to environment.
Integrated gasification combined cycle plants (IGCC) power generation system is a kind of high-level efficiency, oligosaprobic novel clean generation technology, and in the IGCC power generation system, the purification of raw gas is a key link, this link mainly comprises dedusting and desulfurization, common desulfurization method has low-temp desulfurization and two kinds of modes of high temperature desulfurizing at present, two kinds of modes have all obtained application in related occasion, wherein high temperature desulfurizing can be raised the efficiency because of it, simplify technique and reduce costs and there is obvious advantage, yet the key of high temperature desulfurizing is again the development of sweetening agent, the sweetening agent that the cerium oxide of take is the master is subject to numerous investigators' extensive concern in recent years, the cerium oxide base sweetening agent also is described as s-generation desulfurizing agent for high-temp gas, for removing more efficiently the pollutent in coal gas, the development effect is more obvious, the sweetening agent that desulfuration efficiency is higher is the key of high temperature desulfurizing, and efficient oxidation thing desulphurizer mixing utilizes advantage separately, it will be a good research direction.
For the IGCC unit normally being moved and reaching higher reliability, must, before coal gas enters internal combustion turbine, to it, carry out the desulfurizing and purifying processing.In the high temperature desulfurizing mode that the desulfurization of IGCC power generation system is taked, sweetening agent is crucial, and current disclosed patent has:
1. Yujiang County of Shenyang Institute of Aeronautical Engineering dragon, Xie Wei, Chang Liping, the inventions such as Xie Kechang, Wang Dehai take desulfurizing agent for high-temp gas and the desulfurizer thereof that flyash is carrier, the patent No.: 200710158238.7;
2. coal gas of high temperature desulfurizing agent and preparation method in the zinc oxide that the Zheng Xianrong of Institutes Of Technology Of Taiyuan, Chang Liping, Wang Jiancheng, Bao Weiren, Xie Kechang, Jin Qingmai etc. invent, the patent No.: 200910175382.0;
3. the Guo Shuqiang of Shanghai University, Li Deqi, Ding Weizhong, Pan Jinbo, Li Yulong etc. invent manganese lanthanum desulfurizing agent for high-temp gas and preparation method, the patent No.: 201010616929.9;
4. Ferrocerium oxide high-temperature coal gas desulfurization agent and the preparation of the inventions such as the Guo Bo of Institutes Of Technology Of Taiyuan, Chang Liping, Miao Maoqian, Zhang Zhi orchid, the patent No.: 200710139672.0;
5. a kind of improved high temperature desulfuration agent that the Liu Yuzhen of Beijing Sanju New Environmental Protection Materials Co., Ltd, Li Jingbin etc. invent and preparation method thereof, the patent No.: 200810113632.3.
Above-mentioned sweetening agent patent concentrates on zinc oxide, cerium oxide etc., and its desulfuration efficiency is generally the 80%-90% left and right, fails to bring into play various metals and mixes mutually to improve the advantage of desulfuration efficiency.The present invention is mixed with cerium oxide and lanthanum trioxide according to a certain percentage and obtains sweetening agent, has the easily advantages such as synthetic, low cost, high-level efficiency, has proposed a kind of preparation method and application thereof of new high temperature desulfuration agent.
Summary of the invention
One of purpose of the present invention is to provide a kind of cerium lanthanum base desulfurizer, this cerium lanthanum base desulfurizer have easily synthetic, production cost is low, the desulfuration efficiency advantages of higher.
Purpose of the present invention and the preparation method of a kind of cerium lanthanum base desulfurizer of being to provide above-mentioned.
Technical scheme of the present invention
A kind of cerium lanthanum base desulfurizer is prepared by a method comprising the following steps:
At first, adopt dry mix, cerium oxide, lanthanum trioxide and pore-forming material, caking agent are mixed to get to powder mixture;
Then, adopt planetary ball mill to be mixed the powder mixture of gained, it is dry 2h extruded moulding under 150 ℃ that the ball milling powder of gained is controlled temperature in vacuum drying oven, then it is positioned over to the speed of controlling 10 ℃/min in retort furnace and is warming up to 600-1000 ℃, be preferably 800 ℃ of lower constant temperature sintering 4h, obtain cerium lanthanum base desulfurizer after naturally cooling, take out close drying and preserve;
Described pore-forming material is that molecular weight is 1 * 10
5-2 * 10
5the analytical pure amylose starch;
Described caking agent is chemical pure kaolin, and preferred molecular weight is 258.09
;
The consumption of described cerium oxide, lanthanum trioxide, pore-forming material and caking agent, calculate in mass ratio, i.e. cerium oxide: lanthanum trioxide: pore-forming material: caking agent is 15:4.5-6.5:1-1.5:1.
Above-mentioned a kind of cerium lanthanum base desulfurizer can be widely applied in the purification of IGCC coal gas desulfurization, also may be used on many industrial occasions, and emission control to environmental pollutants will demonstrate good effect, have very high promotional value and application prospect.
Beneficial effect of the present invention
A kind of cerium lanthanum base desulfurizer of the present invention, owing to containing lanthanum trioxide and cerium oxide, lanthanum trioxide is a kind of good structural promoter, makes final prepared cerium lanthanum base desulfurizer have good thermostability, can meet higher calcining temperature requirement.Simultaneously, cerium oxide and lanthanum trioxide have formed CeO
2-La
2o
3mixture, impel crystal by bulk to spherical transformation, the crystal volume increases, and makes final prepared cerium lanthanum base desulfurizer have higher desulfuration efficiency.
Final prepared cerium lanthanum base desulfurizer of the present invention, because it has good thermostability and high desulfuration efficiency, therefore can be widely applied in the purification of IGCC coal gas desulfurization, also may be used on many industrial occasions, emission control to environmental pollutants demonstrates good effect, has very high promotional value and application prospect.
In sum, cerium lanthanum base desulfurizer of the present invention is a kind of NEW TYPE OF COMPOSITE metal oxide desulfurizer, the main ingredient cerium oxide is described as s-generation high temperature desulfuration agent, by mixing a certain amount of lanthanum trioxide, it is carried out to modification, and the cerium lanthanum base desulfurizer be prepared from has higher desulfuration efficiency.Along with people's improving constantly for environmental quality requirement, the standard of pollutant emission also improves, cerium lanthanum base desulfurizer of the present invention can be good at being on active service in the high temperature desulfurizing system, there is good effect for power plant and relevant gas industry flue gas desulfurization, have very high social economic value, market outlook are wide.
The accompanying drawing explanation
Fig. 1, cerium lanthanum base desulfurizer evaluation system schematic diagram;
The A1-700 sample SEM figure of Fig. 2, embodiment 1 gained;
The A1-800 sample SEM figure of Fig. 3, embodiment 2 gained;
The A1-700 sample of Fig. 4, embodiment 1,2 gained, A1-800 sample at the differential responses temperature on the impact of desulfuration efficiency;
The B1 sample SEM figure of Fig. 5, embodiment 3 gained;
The B2 sample SEM figure of Fig. 6, embodiment 4 gained;
The B1 of Fig. 7, embodiment 3,4 gained, B2 sample at the differential responses temperature on the impact of desulfuration efficiency.
Embodiment
Also by reference to the accompanying drawings the present invention is further set forth below by specific embodiment, but do not limit the present invention.
The present invention's cerium lanthanum base desulfurizer evaluation system schematic diagram used as shown in Figure 1, comprise mixed gas bottle 1, valve 2, T-valve 3, fixed-bed reactor 4, process furnace 5, heat sink 6, hydrogen sulfide detector 7 and vent gas treatment groove 8,4 minutes inside diameter D=14mm of fixed-bed reactor wherein, length l=450mm, adopt thermopair to control the fixed bed interior reaction temperature;
Its working process is as follows:
At first open process furnace 5, it carried out to preheating, be heated to temperature required, containing H
2the Simulation with I GCC raw gas of S enters fixed-bed reactor 4 and reactive desulfurizing agent from bottom to top, then flow into heat sink 6 and reduce gas temperature, between gaseous fraction, do not react, in exit gas, concentration of hydrogen sulfide adopts hydrogen sulfide detector 7 to detect online, and reacted mixed gas enters the vent gas treatment groove.
Desulfuration efficiency is calculated according to (1) formula:
In formula, η means desulfuration efficiency, C
inmean fixed-bed reactor air inlet concentration of hydrogen sulfide, C
outmean the fixed-bed reactor concentration of hydrogen sulfide of giving vent to anger.
While with cerium lanthanum base desulfurizer evaluation system, cerium lanthanum base desulfurizer being estimated in various embodiments of the present invention, gaseous fraction used is as shown in table 1.
the composition of table 1 mixed gas
| Gas | CO | H 2 | H 2O | CO 2 | H 2S | N2 |
| Content | 36.35% | 27.38% | 15.10% | 12.48% | 2000pm | Balanced gas |
In various embodiments of the present invention, agents useful for same manufacturer and specification are as follows:
Cerium oxide: Shanghai is moistened prompt chemical reagent company limited and is produced, and specification is 3.5N, molecular weight 172.11;
Lanthanum trioxide: Shanghai is moistened prompt chemical reagent company limited and is produced, and specification is 4N, molecular weight 325.84;
Starch: dust those chemical reagent company limiteds in Shanghai produce, and specification is AR, straight chain, molecular weight 1 * 10
5-2 * 10
5;
Kaolin: Shanghai fuzz Chemical Manufacture, specification CP, molecular weight is 258.09.
embodiment 1
A kind of cerium lanthanum base desulfurizer is prepared by a method comprising the following steps:
At first, adopt dry mix, 30g cerium oxide, 12g lanthanum trioxide and 3g pore-forming material, 2g caking agent are mixed to get to powder mixture;
Then, adopt planetary ball mill to be mixed the powder mixture of gained, it is dry 2h extruded moulding under 150 ℃ that the ball milling powder of gained is controlled temperature in vacuum drying oven, then it is positioned over to the speed of controlling 10 ℃/min in retort furnace and is warming up to 700 ℃ of lower constant temperature sintering 4h, obtain cerium lanthanum base desulfurizer A1-700 after naturally cooling, take out close drying and preserve;
Described pore-forming material is that molecular weight is 1 * 10
5-2 * 10
5the analytical pure amylose starch;
Described caking agent is the chemical pure kaolin that molecular weight is 258.09
;
The consumption of described cerium oxide, lanthanum trioxide, pore-forming material and caking agent, calculate in mass ratio, i.e. cerium oxide: lanthanum trioxide: pore-forming material: caking agent is 15:6:1.5:1.
embodiment 2
A kind of cerium lanthanum base desulfurizer is prepared by a method comprising the following steps:
At first, adopt dry mix, 30g cerium oxide, 12g lanthanum trioxide and 3g pore-forming material, 2g caking agent are mixed to get to powder mixture;
Then, adopt planetary ball mill to be mixed the powder mixture of gained, it is dry 2h extruded moulding under 150 ℃ that the ball milling powder of gained is controlled temperature in vacuum drying oven, then it is positioned over to the speed of controlling 10 ℃/min in retort furnace and is warming up to 800 ℃ of lower constant temperature sintering 4h, obtain cerium lanthanum base desulfurizer A1-800 after naturally cooling, take out close drying and preserve;
Described pore-forming material is that molecular weight is 1 * 10
5-2 * 10
5the analytical pure amylose starch;
Described caking agent is the chemical pure kaolin that molecular weight is 258.09;
The consumption of described cerium oxide, lanthanum trioxide, pore-forming material and caking agent, calculate in mass ratio, i.e. cerium oxide: lanthanum trioxide: pore-forming material: caking agent is 15:6:1.5:1.
By embodiment 1, the cerium lanthanum base desulfurizer A1-700 of 2 gained, cerium lanthanum base desulfurizer A1-800 is scanned by the JSM-6390LV of Jeol Ltd. tungsten filament scanning electron microscope, the SEM figure of gained is as Fig. 2, shown in Fig. 3, as can be seen from Figure 2 A1-700 sample sunk part is more, as can be seen from Figure 3 A1-800 sample particle distribution range is less and even, A1-700 sample enhancing in the relative Fig. 2 in clear zone illustrates that plane of crystal is outstanding more, thereby specific surface area also can increase, pore volume increases, and crystal also has the tendency from bulk to granular transformation, show thus that within the specific limits rising along with sintering temperature is conducive to cerium lanthanum base desulfurizer pore volume and increases and crystal transition.
By embodiment 1, the cerium lanthanum base desulfurizer A1-700 of 2 gained, cerium lanthanum base desulfurizer A1-800 is in cerium lanthanum base desulfurizer evaluation system, controlling respectively the fixed-bed reactor temperature of reaction is 600 ℃, 700 ℃, 800 ℃, 900 ℃, 1000 ℃ are carried out desulphurization reaction, its sweetening effectiveness is estimated, its sweetening effectiveness as shown in Figure 4, cerium lanthanum base desulfurizer prepared by the relative 700 ℃ of sintering temperatures of cerium lanthanum base desulfurizer that as can be seen from Figure 4 prepared by 800 ℃ of sintering temperatures has better sweetening effectiveness, and the rising along with temperature of reaction, sweetening effectiveness improves gradually, sweetening effectiveness the best under 800 ℃ of temperature of reaction, but the further raising along with temperature of reaction, sweetening effectiveness reduces on the contrary.
Shown that thus in cerium lanthanum base desulfurizer preparation process of the present invention, 800 ℃ of sintering temperatures are relatively better, higher temperature of reaction is conducive to sweetening effectiveness and improves, but the too high sweetening effectiveness that may cause because of the coking of cerium lanthanum base desulfurizer of temperature of reaction descends.
embodiment 3
A kind of cerium lanthanum base desulfurizer is prepared by a method comprising the following steps:
At first, adopt dry mix, 30g cerium oxide, 13g lanthanum trioxide and 2g pore-forming material, 2g caking agent are mixed to get to powder mixture;
Then, adopt planetary ball mill to be mixed the powder mixture of gained, it is dry 2h extruded moulding under 150 ℃ that the ball milling powder of gained is controlled temperature in vacuum drying oven, then it is positioned over to the speed of controlling 10 ℃/min in retort furnace and is warming up to 800 ℃ of lower constant temperature sintering 4h, obtain cerium lanthanum base desulfurizer B1 after naturally cooling, take out close drying and preserve;
Described pore-forming material is that molecular weight is 1 * 10
5-2 * 10
5the analytical pure amylose starch;
Described caking agent is the chemical pure kaolin that molecular weight is 258.09
;
The consumption of described cerium oxide, lanthanum trioxide, pore-forming material and caking agent, calculate in mass ratio, i.e. cerium oxide: lanthanum trioxide: pore-forming material: caking agent is 15:6.5:1:1.
embodiment 4
A kind of cerium lanthanum base desulfurizer is prepared by a method comprising the following steps:
At first, adopt dry mix, 30g cerium oxide, 9g lanthanum trioxide and 2g pore-forming material, 2g caking agent are mixed to get to powder mixture;
Then, adopt planetary ball mill to be mixed the powder mixture of gained, it is dry 2h extruded moulding under 150 ℃ that the ball milling powder of gained is controlled temperature in vacuum drying oven, then it is positioned over to the speed of controlling 10 ℃/min in retort furnace and is warming up to 800 ℃ of lower constant temperature sintering 4h, obtain cerium lanthanum base desulfurizer B2 after naturally cooling, take out close drying and preserve;
Described pore-forming material is that molecular weight is 1 * 10
5-2 * 10
5the analytical pure amylose starch;
Described caking agent is the chemical pure kaolin that molecular weight is 258.09
;
The consumption of described cerium oxide, lanthanum trioxide, pore-forming material and caking agent, calculate in mass ratio, i.e. cerium oxide: lanthanum trioxide: pore-forming material: caking agent is 15:4.5:1:1.
The cerium lanthanum base desulfurizer B1 of embodiment 3,4 gained, cerium lanthanum base desulfurizer B2 are scanned by the JSM-6390LV of Jeol Ltd. tungsten filament scanning electron microscope, the SEM figure of gained as shown in Figure 5, Figure 6, can find out that from the contrast of Fig. 5, Fig. 6 the macrobead spherulite has appearred in cerium lanthanum base desulfurizer B1, and the crystal volume in spherulite volume ratio cerium lanthanum base desulfurizer B2 is large, further compacter between the relative cerium lanthanum of cerium lanthanum base desulfurizer B1 base desulfurizer B2 crystal and crystal.This may be that cerium oxide and lanthanum trioxide have formed CeO
2-La
2o
3mixture impel crystal by bulk to the ball shape crystalline transformation, and the crystal volume increases.Shown that thus increasing of lanthanum trioxide component concentration is conducive to the sweetening agent crystal and changes to spherulite, the crystal volume increases.
By embodiment 3, the cerium lanthanum base desulfurizer B1 of 4 gained, cerium lanthanum base desulfurizer B2 is in cerium lanthanum base desulfurizer evaluation system, controlling respectively the fixed-bed reactor temperature of reaction is 600 ℃, 700 ℃, 800 ℃, 900 ℃, 1000 ℃ are carried out desulphurization reaction, its sweetening effectiveness is estimated, its sweetening effectiveness as shown in Figure 7, as can be seen from Figure 7 prepared sweetening agent B1 has higher desulfuration efficiency, and also the temperature of reaction of 800 ℃, be issued to the highest sweetening effectiveness, shown that thus suitable increase lanthanum trioxide incorporation is conducive to improve the sweetening agent desulfuration efficiency, this may be to change to spherulite because increasing of lanthanum trioxide group component is conducive to cerium lanthanum base desulfurizer crystal, the crystal volume increases.
In sum, of the present invention under 800 ℃ of sintering temperatures resulting a kind of cerium lanthanum base desulfurizer, carry out desulphurization reaction and there is higher activity and reaction effect under 800 ℃, and within the specific limits, the increase of the incorporation of lanthanum trioxide is conducive to the raising of sweetening agent sweetening effectiveness.
The above is only giving an example of embodiments of the present invention; it should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the technology of the present invention principle; can also make some improvement and modification, these improve and modification all should be considered as protection scope of the present invention.
Claims (6)
1. a cerium lanthanum base desulfurizer is characterized in that the method preparation as follows of described cerium lanthanum base desulfurizer and obtains:
At first adopt dry mix, cerium oxide, lanthanum trioxide and pore-forming material, caking agent are mixed to get to powder mixture;
Then, adopt planetary ball mill to be mixed the powder mixture of gained, it is dry 2h extruded moulding under 150 ℃ that the ball milling powder of gained is controlled temperature in vacuum drying oven, then it is positioned in retort furnace, the speed of controlling 10 ℃/min is warming up to 600-1000 ℃ of lower constant temperature sintering 4h, obtains cerium lanthanum base desulfurizer after naturally cooling;
Described pore-forming material is that molecular weight is 1 * 10
5-2 * 10
5the analytical pure amylose starch;
Described caking agent is chemical pure kaolin
;
The consumption of described cerium oxide, lanthanum trioxide, pore-forming material and caking agent, calculate in mass ratio, i.e. cerium oxide: lanthanum trioxide: pore-forming material: caking agent is 15:4.5-6.5:1-1.5:1.
2. a kind of cerium lanthanum base desulfurizer as claimed in claim 1, is characterized in that describedly in retort furnace, and the speed of controlling 10 ℃/min is warming up to 800 ℃ of lower constant temperature sintering 4h, obtains cerium lanthanum base desulfurizer after naturally cooling.
3. a kind of cerium lanthanum base desulfurizer as claimed in claim 2, is characterized in that the consumption of described cerium oxide, lanthanum trioxide, pore-forming material and caking agent, and calculate in mass ratio, i.e. cerium oxide: lanthanum trioxide: pore-forming material: caking agent is 15:4.5:1:1.
4. a kind of cerium lanthanum base desulfurizer as claimed in claim 2, is characterized in that the consumption of described cerium oxide, lanthanum trioxide, pore-forming material and caking agent, and calculate in mass ratio, i.e. cerium oxide: lanthanum trioxide: pore-forming material: caking agent is 15:6:1.5:1.
5. a kind of cerium lanthanum base desulfurizer as claimed in claim 2, is characterized in that the consumption of described cerium oxide, lanthanum trioxide, pore-forming material and caking agent, and calculate in mass ratio, i.e. cerium oxide: lanthanum trioxide: pore-forming material: caking agent is 15:6.5:1:1.
6. as claim 3,4 or 5 described a kind of cerium lanthanum base desulfurizers, it is characterized in that described caking agent is the chemical pure kaolin that molecular weight is 258.09.
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| US20040031730A1 (en) * | 2002-08-13 | 2004-02-19 | Gislason Jason J. | Desulfurization and novel composistions for same |
| CN1519297A (en) * | 2003-01-24 | 2004-08-11 | 中国石油化工股份有限公司 | Adsorbent for desulfurizing fuel oil and preparation method |
| CN101235324A (en) * | 2007-11-13 | 2008-08-06 | 沈阳航空工业学院 | High-temperature coal gas desulfurizer using coal ash as carrier and desulfurization device thereof |
| CN102021047A (en) * | 2010-12-31 | 2011-04-20 | 上海大学 | Manganese lanthanum high-temperature gas desulfurizer and preparation method thereof |
-
2013
- 2013-10-08 CN CN201310460874.0A patent/CN103484170A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040031730A1 (en) * | 2002-08-13 | 2004-02-19 | Gislason Jason J. | Desulfurization and novel composistions for same |
| CN1519297A (en) * | 2003-01-24 | 2004-08-11 | 中国石油化工股份有限公司 | Adsorbent for desulfurizing fuel oil and preparation method |
| CN101235324A (en) * | 2007-11-13 | 2008-08-06 | 沈阳航空工业学院 | High-temperature coal gas desulfurizer using coal ash as carrier and desulfurization device thereof |
| CN102021047A (en) * | 2010-12-31 | 2011-04-20 | 上海大学 | Manganese lanthanum high-temperature gas desulfurizer and preparation method thereof |
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Application publication date: 20140101 |