CN101450311A - Microwave treatment method capable of increasing copper base catalyst performance - Google Patents
Microwave treatment method capable of increasing copper base catalyst performance Download PDFInfo
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- CN101450311A CN101450311A CNA2007101909083A CN200710190908A CN101450311A CN 101450311 A CN101450311 A CN 101450311A CN A2007101909083 A CNA2007101909083 A CN A2007101909083A CN 200710190908 A CN200710190908 A CN 200710190908A CN 101450311 A CN101450311 A CN 101450311A
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- microwave
- catalyst
- handling method
- drying
- copper base
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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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
Abstract
The invention belongs to the technical field of catalysis and relates to a microwave treatment method for improving the performance of a copper-based catalyst, namely a copper-zinc matrix is loaded on an alumina carrier, and the catalyst prepared and formed by washing, filtration, drying, roasting and tabletting is subjected to microwave heat treatment for 1 to 5 hours at a temperature of between 60 and 200 DEG C. The catalyst prepared by the method has low bulk density and tablet shrinkage rate, high tablet strength, and improved catalytic activity and thermal stability.
Description
Technical field: the present invention relates to a kind of microwave handling method that improves copper base catalyst performance, the metal catalyst technical field.
Background technology: methyl alcohol is one of the most basic Organic Chemicals.In recent years, methyl alcohol demand and production capacity sustainable growth, the purposes of methyl alcohol also has new development.Plant-scale methyl alcohol generally is with containing H
2, CO, CO
2The synthesis gas method production of under certain pressure and temperature and the condition that has catalyst to exist, reacting.Methanol synthesis catalyst is one of key technology of synthesizing methanol industrial technology level height, along with the maximization of the fast development of methanol industry, particularly methanol device, the research and development of methanol synthesis catalyst is had higher requirement.
Methanol synthesis catalyst mainly is made up of oxides such as copper, zinc and aluminium at present.Common method for preparing catalyst is to prepare copper zinc parent earlier, and it is loaded on the alumina support, through washing, filter, and oven dry, operations such as roasting and moulding make catalyst.Methanol synthesis catalyst with the method preparation can meet the needs of production substantially, but apart from requirements at the higher level distance is arranged still.
Summary of the invention: the objective of the invention is to propose a kind of new microwave handling method that can further improve copper base catalyst performance.
The present invention is achieved like this: it mainly may further comprise the steps, copper zinc parent is loaded on the alumina support, through washing, filter, oven dry, roasting prepares moulding after beating sheet, is characterized in that the catalyst that will prepare moulding carries out 1~5 hour microwave thermal processing between 60 ℃~200 ℃, promptly make catalyst of the present invention.
Microwave be wavelength between 1mm~1m, frequency is 3.0 * 10
2~3.0 * 10
5MHz has a kind of electromagnetic wave of penetrability.No matter be the mode of heating of conduction, convection current, radiation, thermal source all is outside, the rising of temperature of charge is by in outer the reaching, to be transmitted to inside again after the heating of surface, this will be subjected to the restriction of Fourier's law, usually being heated material is the non-conductor of heat, and very big thermal resistance is arranged, and heat time heating time is very long naturally.The heating using microwave heat is being heated the inner generation of material, and the inside and outside is hot together like this, and not only temperature is very even, and can not bring half-cooked phenomenon.During conventional the heating, the temperature surface is high, and inner low, this Temperature Distribution is unfavorable for that moisture evaporates rapidly.And the heating using microwave inside and outside is hot together, simultaneously because the surface is easier to heat radiation, internal temperature is higher than the outside often, the direction of the thermograde direction and the gradation of moisture is identical, it is consistent with the mass transfer direction to conduct heat, and impels internal moisture to evaporate rapidly, forms the internal pressure gradient, make moisture be diffused into the surface very soon and vapor away, this just makes shorten dramatically drying time.
Microwave drying has following advantage: 1) heating using microwave can improve thermal diffusion and matter diffusivity; 2) form the pressure inside gradient and improve rate of drying; 3) improve rate of drying and do not improve material surface temperature and internal temperature; 4) the selectivity heating is distributed according to need energy in material; 5) has better product quality.
Catalyst for methanol with the inventive method preparation is compared with the catalyst of conventional method preparation, can reduce the tablet shrinkage factor, improves tablet strength, reduces bulk density, improves catalytic activity and heat endurance, can satisfy higher needs.
The specific embodiment: following embodiment is in order to further specify content of the present invention:
Embodiment 1: prepare copper zinc parent earlier, it is loaded on the alumina support, through aging, washing is filtered, drying, and operations such as roasting and moulding make catalyst sample.
Embodiment 2: the catalyst sample that example 1 is made carries out 1~5 hour heat treatment with baking oven between 60 ℃~200 ℃.
Embodiment 3: preparation process is with example 2, but changes heat treatment method into microwave heating treatment.
Embodiment 4: preparation process is handled but change heat treatment method into infra-red heat with example 2.
Embodiment 5: preparation process is with example 2, but changes heat treatment method into baking oven and Microwave Hybrid heat treatment.
The Cu-series catalyst for synthesizing methanol sample that the foregoing description is made carries out performance test.
The catalyst activity testing conditions is as follows:
Catalyst sample: granularity is 0.425mm~1.180mm
The sample activation: sample is before detection of active, with reducing gases (H
2: N
2=3:97) at 210 ℃ of reduction 16h.
The active detection: the sample after the reduction, feeding contains finite concentration CO and CO
2Synthesis gas, at pressure 5.0MPa, under uniform temperature and the air speed condition, measure initial activity (to generate the space-time yield gml of methyl alcohol
-1H
-1Or the CO conversion ratio is represented).Sample stands 350 ℃, the heat-resisting processing of 20h then, returns under the above-mentioned identical conditions again, measures the activity after heat-resisting, to characterize the height of sample heat endurance.
Adopt the full-automatic specific surface area analysis instrument of the U.S. Nova 2200e of Quantachrome company type pore structure analyzer and CHEMBET-3000 type to measure catalyst surface area, pore volume and pore-size distribution.
Adopt Japanese Dmax IIIA type x-ray diffractometer of science, sweep limits 2 θ=10 °~60 °, voltage 40kV, electric current 30mA, the Cu target is measured catalyst thing phase, calculates grain size with the broadening method.
Adopt the big connection intelligent testing machine ZQJ-II of factory type intelligence granule strength testing machine to measure radially anti-crushing power of catalyst granules.
The performance test results is listed in table 1-3.Wherein sample 3 is the catalyst with the inventive method preparation, and sample 1 is the reference catalyst with the conventional method preparation, and sample 2,4 is respectively the catalyst after oven drying, the infra-red drying processing.
Table 1 bulk density, intensity, tablet shrinkage factor, anti-crushing power tables of data radially
Table 2 activity data table
Table 3 sample specific surface, pore volume tables of data
Can find out by test result, the bulk density and the tablet shrinkage factor of the catalyst 3 of employing the inventive method preparation are low, the tablet strength height, catalytic activity and heat endurance are apparently higher than the reference sample, show that the present invention has compared tangible progress with existing method, promptly higher methyl alcohol synthesizing activity can satisfy higher needs.
The inventive method preparation catalyst, be applicable to contain CO, CO
2And H
2Synthesis gas make methyl alcohol, be particularly useful for low-temp low-pressure synthesizing methanol device.
Claims (6)
1. a microwave handling method that improves copper base catalyst performance loads on copper zinc parent on the alumina support, through washing, filter, oven dry, roasting prepares moulding after beating sheet, it is characterized in that the catalyst that will prepare moulding carries out 1~5 hour microwave thermal processing between 60-200 ℃ of temperature.
2. the microwave handling method of catalyst as claimed in claim 1 is characterized in that microwave thermal is treated to microwave drying.
3. the microwave handling method of catalyst as claimed in claim 1 is characterized in that microwave thermal is treated to baking oven and Microwave Hybrid drying.
4. the microwave handling method of catalyst as claimed in claim 1 is characterized in that microwave thermal is treated to infrared and the Microwave Hybrid drying.
5. the microwave handling method of catalyst as claimed in claim 1, the catalyst after it is characterized in that handling is applicable to contain CO, CO
2And H
2Synthesis gas make the device of methyl alcohol.
6. the microwave handling method of catalyst as claimed in claim 5, the catalyst after it is characterized in that handling is applicable to low-temp low-pressure synthesizing methanol device.
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CNA2007101909083A CN101450311A (en) | 2007-11-29 | 2007-11-29 | Microwave treatment method capable of increasing copper base catalyst performance |
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CNA2007101909083A CN101450311A (en) | 2007-11-29 | 2007-11-29 | Microwave treatment method capable of increasing copper base catalyst performance |
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102240552A (en) * | 2011-05-16 | 2011-11-16 | 中国石油化工集团公司 | Method for preparing high-performance methanol synthesis catalyst |
CN102580787A (en) * | 2012-02-27 | 2012-07-18 | 翁希明 | Drying technology of nanoscale coating material for automobile tail gas catalyst |
CN102614942A (en) * | 2012-02-27 | 2012-08-01 | 翁希明 | Automobile tail gas three-way catalyst drying technology |
CN103506170A (en) * | 2012-06-30 | 2014-01-15 | 中国石油化工股份有限公司 | Preparation method of low-sodium copper-based dehydrogenation catalyst |
-
2007
- 2007-11-29 CN CNA2007101909083A patent/CN101450311A/en active Pending
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102240552A (en) * | 2011-05-16 | 2011-11-16 | 中国石油化工集团公司 | Method for preparing high-performance methanol synthesis catalyst |
CN102580787A (en) * | 2012-02-27 | 2012-07-18 | 翁希明 | Drying technology of nanoscale coating material for automobile tail gas catalyst |
CN102614942A (en) * | 2012-02-27 | 2012-08-01 | 翁希明 | Automobile tail gas three-way catalyst drying technology |
CN103506170A (en) * | 2012-06-30 | 2014-01-15 | 中国石油化工股份有限公司 | Preparation method of low-sodium copper-based dehydrogenation catalyst |
CN103506170B (en) * | 2012-06-30 | 2015-07-01 | 中国石油化工股份有限公司 | Preparation method of low-sodium copper-based dehydrogenation catalyst |
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Open date: 20090610 |