CN102416349A - Preparation method for monolithic catalyst sample - Google Patents
Preparation method for monolithic catalyst sample Download PDFInfo
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- CN102416349A CN102416349A CN2011103899330A CN201110389933A CN102416349A CN 102416349 A CN102416349 A CN 102416349A CN 2011103899330 A CN2011103899330 A CN 2011103899330A CN 201110389933 A CN201110389933 A CN 201110389933A CN 102416349 A CN102416349 A CN 102416349A
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Abstract
The invention provides a preparation method for a monolithic catalyst sample. The method mainly comprises the following steps of: preparing small-volume honeycomb ceramic; and loading catalyst active ingredients onto a carrier. The coating of the integral catalyst sample prepared with the method uniform, and the surface property, pore canal structure and the like are extremely approximate to those of a large monolithic catalyst; and when the monolithic catalyst sample is used for evaluating a fixed-bed micro-reactor, the catalytic performance and structural representation result of the monolithic catalyst sample can be associated with the large monolithic catalyst, and the aims of truly lowering the research and development cost and shortening the research and development period are fulfilled.
Description
Technical field
The present invention relates to a kind of preparation method of integral catalyzer sample, the another one aspect that the present invention relates to is the preparation method of small size honeycomb ceramic carrier.
Background technology
Integral catalyzer is the integrated catalyst by many narrow parallel channels proper alignment.Because the cross section of the ceramic-substrate catalyst of early development is alveolate texture, so be referred to as honeycombed catalyst again.Its fundamental characteristics is to have limited radially mixing in the passage, and general no any effect of mass transmitting between adjacency channel.Catalytic active component is made into coating (10-50 μ m) as thin as a wafer, and the gas of reaction or fluid are through these ducts and react.With respect to traditional beaded catalyst bed, integral catalyzer has low pressure drop, is applicable to the reaction of high-speed; Its active component all is attached to the surface in duct, and its utilization rate is higher; Catalyst has higher mechanical strength.The excellent characteristics that integral catalyzer had make it in high-speed, the reaction of high temperature automotive tail gas clean-up, obtain using widely.Honeycomb ceramic integral formula catalyst is the main body of car tail-gas catalytic purifier, is that the pottery of principal crystalline phase has lower hot expansibility with the cordierite, is the preferred material of carrier for ceramic honeycomb catalyst always.
Need carry out sample performance evaluation, test stand performance evaluation and vehicle performance evaluation in the development process of tai-gas clean-up catalyst.Test stand performance evaluation and vehicle performance evaluation be the evaluate catalysts performance more truly, but its cost is higher, consuming time longer, so carry out effective sample performance evaluation, can reduce the catalyst development cost significantly, shorten the R&D cycle.
The catalyst sample can be divided powdered and two types of integral body again.The fine catalyst sample can be the powder that only contains active component and auxiliary agent, also can be that active component and auxiliary agent are coated to the powder that back compressing tablet screening obtains on the carrier.Yet the composition of these two kinds of fine catalyst samples, shape or structure all there are differences with the integral catalyzer of practice, thereby the catalytic performance result of its evaluation and relevance are all poor.But because existing assessment technique and development cost limit, fine catalyst is mostly adopted in catalyst sample evaluation at present.
The volume that is used for the integral catalyzer sample of catalyst sample performance evaluation generally is 0.5-10.0mL, but all the big integral catalyzer with practice is identical owing to its composition, shape or structure, so its catalytic performance result is near truth.The integral catalyzer volume is bigger, can not directly be used for catalyst sample performance evaluation.Therefore seeking suitable method, to prepare the integral catalyzer sample extremely important.Directly integral catalyzer is prepared into the catalyst sample except lacking corresponding techniques at present; Another aspect is that the honeycomb ceramic carrier volume sold on the market is all greater than 100 mL; Can't directly be used to prepare the integral catalyzer sample; And also lack corresponding techniques with the integral catalyzer of honeycomb ceramic carrier preparation, it is prepared into the integral catalyzer sample.Therefore, select suitable method for use, prepare the integral catalyzer sample that is applicable to fixed-bed micro-reactor from the ceramic honey comb of integral catalyzer or big volume particularly important for saving R&D costs, shortening R&D cycle.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of integral catalyzer sample, and the integral catalyzer sample of processing is used for catalyst sample performance evaluation; Another object of the present invention provides a kind of preparation method of small size honeycomb ceramic carrier.
The integral catalyzer volume is generally all greater than 100mL.The integral catalyzer sample is that active component and auxiliary agent are coated on the small size carrier that volume is 0.5-10mL, and its composition, shape or the structure all integral catalyzer with practice are identical, so its catalytic performance result is more near truth.
A kind of preparation method of integral catalyzer sample comprises the steps: that (1) calculate diameter, the length of required integral catalyzer sample according to real reaction condition and reactor diameter; (2) preparation small size ceramic honey comb: drill bit is installed on the industrial bench drill of working stability; Again ceramic honey comb is placed on the bench drill platform, ceramic honey comb is drilled through certain depth and small cylinder as much as possible with drill bit; On cutting machine, adjust to the Len req that calculates then, and it is rinsed well with deionized water; It is smooth to pick out bottom surface, and the side does not have the ceramic honey comb of big breakage, is dried, can obtains the small size honeycomb ceramic carrier after the roasting; (3) supported catalyst active component: the small size ceramic honey comb after the roasting is weighed; After weighing it is dipped in the catalyst-coated liquid, takes out behind the 5-8min, dry up raffinate, aging, roasting dry to catalyst after 7-10 hour can obtain the integral catalyzer sample under the room temperature; Integral catalyzer sample to after the roasting is weighed once more.
Described preparation method, the drying condition described in step (2), (3) is meant that temperature is 100-120 ℃, the time is 3-5 hour; Roasting condition described in step (2), (3) is meant that temperature is 500-600 ℃, and the time is 3-5 hour.
Described preparation method, the drying condition described in step (2), (3) is meant that temperature is 100-120 ℃, the time is 3-5 hour; Roasting condition described in step (2), (3) is meant that temperature is 540-560 ℃, and the time is 3-5 hour.
Among the described preparation method, step (2), (3) during roasting used equipment be heating furnace; Heating furnace was with the temperature programming of 2-5 ℃/min when carrier or catalyst were put into the heating furnace roasting.
Described heating furnace is a Muffle furnace.
Described preparation method, the drill bit described in the step (2) is the thin-walled hollow diamond bit, its internal diameter and length can be chosen by reactor diameter and real reaction condition.
The described certain depth that ceramic honey comb is drilled through is to decide according to the real reaction condition, and its numerical value is greater than the 2-5mm that calculates Len got.
Described preparation method, available integral catalyzer replaces the ceramic honey comb in the step (2), directly obtains the integral catalyzer sample according to the method in step (1), (2).
Described integral catalyzer sample is meant the integral catalyzer of volume at 0.5mL-10.0mL.
Beneficial effect of the present invention:
(1) preparation method is easy, flexible; Can directly prepare the integral catalyzer sample of different size from integral catalyzer; The small size honeycomb ceramic carrier that also can prepare different size according to actual needs; And the carrier profile that obtains destruction is little, size Control is accurate, is suitable for preparing the integral catalyzer sample;
(2) the integral catalyzer sample coating prepared of the present invention is even; Surface nature and pore passage structure etc. are all very approaching with integral catalyzer; And composition, the shape all integral catalyzer with practice are identical; Use it for fixed-bed micro-reactor and carry out catalyst sample performance evaluation; Its catalytic performance result is very near truth, thus can be effectively carry out its catalytic performance and structural characterization result and integral catalyzer related, to reach real reduction R&D costs, to shorten the purpose of R&D cycle.
Description of drawings
Fig. 1 drills through the sketch map of small size honeycomb ceramic carrier from honeycomb ceramic carrier for the present invention.
The integral catalyzer sample that Fig. 2 prepares for the present invention is loaded into the sketch map of quartz ampoule.
The specific embodiment
Embodiment 1:
The reacting gas total flow is 300 mL/min, requires control air speed 15000 h
-1So the honeycomb ceramic carrier volume that needs is 1.2 mL.The fixed bed reactors internal diameter is 7mm, and the diameter and the length that draw honeycomb ceramic carrier are respectively 7mm and 31mm.Therefore choose the diamond bit that internal diameter and length are respectively 7mm and 35mm.The cylinder cordierite honeycomb ceramic of buying is of a size of φ 101.91*123.26mm.On this cordierite honeycomb ceramic, drill through the small cylinder of some, use the cutting machine intercepted length to be 31mm then, at last it is rinsed well with deionized water, 110 ℃ of following oven dry 4 h, again in Muffle furnace with 2 ℃/min temperature programming to 550 ℃ roasting, 2 h.The process that drills through the small size honeycomb ceramic carrier from honeycomb ceramic carrier is as shown in Figure 1, and 1 among Fig. 1 is honeycomb ceramic carrier, and 2 is the small size honeycomb ceramic carrier.
Small size honeycomb ceramic carrier after the above-mentioned roasting is weighed; It is dipped in the catalyst-coated liquid, slowly takes out behind the 5min, dry up raffinate with ear washing bulb, aging 8 h under the room temperature, 110 ℃ of drying 4 h, then in Muffle furnace with 2 ℃/min temperature programming to 550 ℃ roasting, 2 h; Integral catalyzer sample to after the roasting is weighed once more.
Fig. 2 has illustrated the integral catalyzer sample is loaded in the quartz ampoule.The silica wool of certain-length in the correct position filling of quartz ampoule is to play the support effect.Again integral catalyzer sample to be evaluated is filled in quartz ampoule one end that keeps flat lentamente, gradually quartz ampoule is become vertically, and rap quartz ampoule, let the integral catalyzer sample arrive on the silica wool gradually.Among Fig. 23 is quartz ampoule, and 4 is the integral catalyzer sample.
Embodiment 2:
The reacting gas total flow is 300 mL/min, requires control air speed 15000 h
-1So the honeycomb ceramic carrier volume that needs is 1.2 mL.The fixed bed reactors internal diameter is 9mm, and the diameter and the length that draw honeycomb ceramic carrier are respectively 9mm and 19mm.Therefore choose the diamond bit that internal diameter and length are respectively 9mm and 35mm.The cylinder cordierite honeycomb ceramic of buying is of a size of φ 117.39*151.25mm.On this cordierite honeycomb ceramic, drill through the small cylinder of some, use the cutting machine intercepted length to be 19mm then, at last it is rinsed well with deionized water, 110 ℃ of following oven dry 4 h, again in Muffle furnace with 2 ℃/min temperature programming to 550 ℃ roasting, 2 h.
Small size honeycomb ceramic carrier after the above-mentioned roasting is weighed; It is dipped in the catalyst-coated liquid, slowly takes out behind the 5min, dry up raffinate with ear washing bulb, aging 8 h under the room temperature, 110 ℃ of drying 4 h, then in Muffle furnace with 2 ℃/min temperature programming to 550 ℃ roasting, 2 h; Integral catalyzer sample to after the roasting is weighed once more.
The prepared integral catalyzer sample of the present invention is mainly used in the evaluation of exhaust gas from diesel vehicle denitration reaction; But the present invention is not limited only to this; The exhaust gas from diesel vehicle denitration is merely a kind of probe reaction, and the present invention is applicable to that all relate to the preparation of small size honeycomb ceramic carrier and integral catalyzer sample.
According to the announcement and the instruction of above-mentioned specification, those skilled in the art in the invention can also change and revise above-mentioned embodiment.Therefore, the specific embodiment that discloses and describe above the present invention is not limited to also should fall in the protection domain of claim of the present invention modifications more of the present invention and change.In addition, although used some specific terms in this specification, these terms are explanation for ease just, the present invention is not constituted any restriction.
Claims (9)
1. the preparation method of an integral catalyzer sample is characterized in that, comprises the steps:
(1) calculates diameter, the length of required integral catalyzer sample according to real reaction condition and reactor diameter;
(2) preparation small size honeycomb ceramic carrier: drill bit is installed on the industrial bench drill of working stability; Again ceramic honey comb is placed on the bench drill platform, ceramic honey comb is drilled through certain depth and small cylinder as much as possible with drill bit; On cutting machine, adjust to the length that calculates in the step (1) then, and it is rinsed well with deionized water; It is smooth to pick out bottom surface, and the side does not have the ceramic honey comb of big breakage, is dried, can obtains the small size honeycomb ceramic carrier after the roasting;
(3) supported catalyst active component: the small size ceramic honey comb after the roasting is weighed; After weighing it is dipped in the catalyst-coated liquid, takes out behind the 5-8min, dry up raffinate, aging, roasting dry to catalyst after 7-10 hour can obtain the integral catalyzer sample under the room temperature; Integral catalyzer sample to after the roasting is weighed once more.
2. preparation method according to claim 1 is characterized in that: the drying condition described in step (2), (3) is meant that temperature is 100-120 ℃, and the time is 3-5 hour; Roasting condition described in step (2), (3) is meant that temperature is 500-600 ℃, and the time is 3-5 hour.
3. preparation method according to claim 2 is characterized in that: the drying condition described in step (2), (3) is meant that temperature is 100-120 ℃, and the time is 3-5 hour; Roasting condition described in step (2), (3) is meant that temperature is 540-560 ℃, and the time is 3-5 hour.
4. preparation method according to claim 1 is characterized in that: in the step (2), (3) during roasting used equipment be heating furnace; Heating furnace was with the temperature programming of 2-5 ℃/min when carrier or catalyst were put into the heating furnace roasting.
5. preparation method according to claim 4 is characterized in that: described heating furnace is a Muffle furnace.
6. preparation method according to claim 1 is characterized in that: the drill bit described in the step (2) is the thin-walled hollow diamond bit, and its internal diameter and length can be chosen by reactor diameter and real reaction condition.
7. preparation method according to claim 1 is characterized in that: the certain depth that ceramic honey comb is drilled through described in the step (2) is to decide according to the real reaction condition, and its numerical value is greater than the 2-5mm that calculates Len got.
8. preparation method according to claim 1 is characterized in that: available integral catalyzer replaces the ceramic honey comb in the step (2), directly obtains the integral catalyzer sample according to the method in step (1) and the step (2).
9. the described integral catalyzer sample of the arbitrary claim of above claim 1 to 8 is meant the integral catalyzer of volume at 0.5mL-10.0mL.
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| CN 201110389933 CN102416349B (en) | 2011-11-30 | 2011-11-30 | Preparation method for monolithic catalyst sample |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104634807A (en) * | 2015-01-11 | 2015-05-20 | 浙江大学 | Honeycomb-shaped SCR catalyst rapid aging experimental device |
| CN112058192A (en) * | 2020-09-04 | 2020-12-11 | 湖南大学 | Continuous flow micro-reactor, manufacturing method and application |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101787331A (en) * | 2010-03-05 | 2010-07-28 | 山东省科学院能源研究所 | Application of monolithic catalyst in biodiesel synthesis and method for synthesizing biodiesel |
| CN102085489A (en) * | 2009-12-07 | 2011-06-08 | 山西潞安矿业(集团)有限责任公司 | Method for preparing cordierite honeycomb ceramic catalyst carrier from coal gangues |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102085489A (en) * | 2009-12-07 | 2011-06-08 | 山西潞安矿业(集团)有限责任公司 | Method for preparing cordierite honeycomb ceramic catalyst carrier from coal gangues |
| CN101787331A (en) * | 2010-03-05 | 2010-07-28 | 山东省科学院能源研究所 | Application of monolithic catalyst in biodiesel synthesis and method for synthesizing biodiesel |
Non-Patent Citations (1)
| Title |
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| 田建民等: "载体预处理对CuO-CeO2/堇青石催化剂性能的影响", 《内蒙古工业大学学报》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104634807A (en) * | 2015-01-11 | 2015-05-20 | 浙江大学 | Honeycomb-shaped SCR catalyst rapid aging experimental device |
| CN104634807B (en) * | 2015-01-11 | 2018-02-16 | 浙江大学 | A kind of honeycomb-shaped SCR catalyst quick aging experimental provision |
| CN112058192A (en) * | 2020-09-04 | 2020-12-11 | 湖南大学 | Continuous flow micro-reactor, manufacturing method and application |
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Address after: Lotus Road 511441 Guangdong city of Guangzhou province Panyu District town No. 368 block stone Patentee after: Waygreen Technologies, Inc. Address before: 510006 Guangdong city of Guangzhou province Panyu District Xiaoguwei Street Outer Ring Road No. 232 Building 5 floor B District 13 Patentee before: Waygreen Technologies, Inc. |
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