CN105688882A - Rare earth catalyst and powder-metallurgy preparing method thereof - Google Patents
Rare earth catalyst and powder-metallurgy preparing method thereof Download PDFInfo
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- CN105688882A CN105688882A CN201610110955.1A CN201610110955A CN105688882A CN 105688882 A CN105688882 A CN 105688882A CN 201610110955 A CN201610110955 A CN 201610110955A CN 105688882 A CN105688882 A CN 105688882A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- 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
- B01J23/10—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of rare earths
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/92—Chemical or biological purification of waste gases of engine exhaust gases
- B01D53/94—Chemical or biological purification of waste gases of engine exhaust gases by catalytic processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2258/00—Sources of waste gases
- B01D2258/01—Engine exhaust gases
Abstract
The invention discloses a rare earth catalyst and a powder-metallurgy preparing method thereof. The rare earth catalyst comprises, by weight, 18-36 parts of platinum, 13-30 parts of lithium, 15-32 parts of ruthenium, 11-25 parts of graphite, 8-24 parts of calcium oxalate, 13-26 parts of sodium nitrate, 8-22 parts of calcium silicate, 25-40 parts of acetic acid and 22-44 parts of absolute ethyl alcohol. According to the rare earth catalyst and the method, rare earth elements and graphite are combined, and the rare earth catalyst prepared through the powdering process, the acid pickling process, the high-temperature calcination process and the like has the advantages of being good in high temperature resistance, even in active-ingredient distribution, long in catalysis life and the like.
Description
Technical field
The present invention relates to catalyst material, particularly relate to a kind of rare earth catalyst and method for preparing powder metallurgy thereof。
Background technology
Catalyst stability represented typically by " life-span ", and it refers to the time that catalyst experiences to not reusable degree from the activity decrease begun to use to it, and this so-called " degree " depends on the technical specification used。Catalyst stability includes the heat-resistant stability to pyrocaloric effect, to friction, the mechanical stability impacted and the antitoxin stability to poisoning effect。
Cause catalyst efficiency decay and shorten the reason in its life-span a lot, mainly have: the poisoning effect (being again catalyst poisoning) of impurity in raw material；Heat effect during high temperature makes the crystal grain of active component in catalyst increase, thus causing that specific surface area reduces, or causes catalyst degeneration；Dust in reaction raw materials or the carbon deposits generated in course of reaction cover catalyst surface, thus reducing the activity of catalyst；Effective ingredient in catalyst runs off in course of reaction；Strong thermal shock or pressure fluctuations make catalyst granules crush；Washing away of reaction-ure fluid makes catalyst efflorescence blow mistake etc.。
Rare earth element is up to 17 kinds, and the feature of its electronic structure is outermost layer is 4f1+n5d0～1s2, under normal condition, the 5d track of most of rare earth elements is empty, and unoccupied orbital can be used as catalytic action electron transfer station, and outer electronic structure, as the central atom of complex, has the various ligancies from 6～12。The transmutability of this ligancy of rare earth element determines them and has remaining " atomicity "。
In car combustion engine, dyestuff in combustion, because its incomplete combustion causes that the composition of its discharge has carbon dioxide, steam, carbon monoxide, Hydrocarbon, oxynitride, lead compound, sulphur compound etc.。Wherein carbon monoxide, Hydrocarbon, oxynitride, lead compound, sulphur compound are the major pollutants causing environmental pollution。Rare earth element made the cleaning catalyst of motor-vehicle tail-gas by prior art, but due in the catalyst for preparing active component skewness cause that catalytic effect is not good, thus causing harmful substance in tail gas higher。Additionally, the rare earth catalyst life-span that traditional method for preparing catalyst prepares is shorter, and high-temperature resistant result is poor。
Summary of the invention
Solve the technical problem that:
Being evenly distributed to obtain a kind of active component, the life-span is long, and has the rare earth catalyst of good resistance to elevated temperatures, the invention provides a kind of rare earth catalyst and method for preparing powder metallurgy thereof。
Technical scheme:
A kind of rare earth catalyst, is made up of following components proportioning by weight: 18～36 parts of platinum, lithium 13～30 parts, ruthenium 15～32 parts, 11～25 parts of graphite, calcium oxalate 8～24 parts, sodium nitrate 13～26 parts, calcium silicates 8～22 parts, acetic acid 25～40 parts, dehydrated alcohol 22～44 parts。
Preferably, described rare earth catalyst is made up of following components proportioning by weight: 32 parts of platinum, lithium 26 parts, ruthenium 24 parts, 18 parts of graphite, calcium oxalate 18 parts, sodium nitrate 21 parts, calcium silicates 15 parts, acetic acid 34 parts, dehydrated alcohol 40 parts。
The method for preparing powder metallurgy of a kind of rare earth catalyst, comprises the steps of
(1) being simultaneously introduced in ball mill by platinum, lithium, ruthenium, graphite, calcium oxalate, sodium nitrate and calcium silicates, grind 1～2.5 hour, powder diameter is 200～400 orders；
(2) mixture step (1) obtained adds in acetic acid, under 4～12 DEG C of conditions, stirring reaction 15～40 minutes, filters and removes filtrate, it is thus achieved that filtering residue；
(3) mass ratio of the filtering residue obtained with deionized water cleaning step (2), filtering residue and deionized water is 1:1～1.2, cleans twice；
(4) in the filtering residue after step (3) is cleaned, add dehydrated alcohol, stirring reaction 5～15 minutes, absorb water twice；Filter after removing dehydrated alcohol, filtering residue is placed under 56～78 DEG C of conditions and dries, it is thus achieved that mixture of powders；
(5) being placed in mixing device by mixture of powders, above-mentioned powder is blown afloat by the gases at high pressure utilizing pressure to be 1.78～2.85MPa, stops passing into gases at high pressure after 6～10 minutes, the co-deposited also Homogeneous phase mixing of each powder；
(6) powder after above-mentioned Homogeneous phase mixing is placed in electric furnace; the mode adopting the intensification of 3 stages in the protection atmosphere of helium is sintered; the temperature in 3 stages respectively 320 DEG C, 460 DEG C, 630 DEG C; per stage sintering time is 1～4.5 hour, can obtain rare earth catalyst after having sintered。
Preferably, platinum, lithium, ruthenium, graphite, calcium oxalate, sodium nitrate and calcium silicates are simultaneously introduced in ball mill in (1) by step, grind 2 hours, and powder diameter is 300 orders。
Preferably, mixture step (1) obtained in step (2) adds in acetic acid, under 6 DEG C of conditions, stirring reaction 20 minutes, filters and removes filtrate, it is thus achieved that filtering residue。
Preferably, the filtering residue obtained with deionized water cleaning step (2) in step (3), the mass ratio of filtering residue and deionized water is 1:1.1, cleans twice。
Preferably, step (4) adds dehydrated alcohol, stirring reaction 12 minutes in the filtering residue after step (3) is cleaned, absorbs water twice；Filter after removing dehydrated alcohol, filtering residue is placed under 65 DEG C of conditions and dries, it is thus achieved that mixture of powders。
Preferably, mixture of powders is placed in mixing device in (5) by step, utilizes the gases at high pressure that pressure is 2.25MPa to be blown afloat by above-mentioned powder, stops passing into gases at high pressure after 8 minutes, the co-deposited also Homogeneous phase mixing of each powder。
Preferably; powder after above-mentioned Homogeneous phase mixing is placed in electric furnace by step (6); the mode adopting the intensification of 3 stages in the protection atmosphere of helium is sintered; the temperature in 3 stages respectively 320 DEG C, 460 DEG C, 630 DEG C; per stage sintering time is 3 hours, can obtain rare earth catalyst after having sintered。
Beneficial effect:
Rare earth element is combined by the present invention with graphite, and the rare earth catalyst prepared through processes such as powdered, pickling, high-temperature calcinations has good resistance to elevated temperatures, and the advantage such as active component is evenly distributed, long catalytic life。
Detailed description of the invention
Embodiment 1
A kind of rare earth catalyst, is made up of following components proportioning by weight: 18 parts of platinum, lithium 13 parts, ruthenium 15 parts, 11 parts of graphite, calcium oxalate 8 parts, sodium nitrate 13 parts, calcium silicates 8 parts, acetic acid 25 parts, dehydrated alcohol 22 parts。
The method for preparing powder metallurgy of a kind of rare earth catalyst, comprises the steps of
(1) being simultaneously introduced in ball mill by platinum, lithium, ruthenium, graphite, calcium oxalate, sodium nitrate and calcium silicates, grind 1 hour, powder diameter is 200 orders；
(2) mixture step (1) obtained adds in acetic acid, under 4 DEG C of conditions, stirring reaction 15 minutes, filters and removes filtrate, it is thus achieved that filtering residue；
(3) mass ratio of the filtering residue obtained with deionized water cleaning step (2), filtering residue and deionized water is 1:1, cleans twice；
(4) in the filtering residue after step (3) is cleaned, add dehydrated alcohol, stirring reaction 5 minutes, absorb water twice；Filter after removing dehydrated alcohol, filtering residue is placed under 56 DEG C of conditions and dries, it is thus achieved that mixture of powders；
(5) mixture of powders is placed in mixing device, utilizes the gases at high pressure that pressure is 1.78MPa to be blown afloat by above-mentioned powder, stop after 6 minutes passing into gases at high pressure, the co-deposited also Homogeneous phase mixing of each powder；
(6) powder after above-mentioned Homogeneous phase mixing is placed in electric furnace; the mode adopting the intensification of 3 stages in the protection atmosphere of helium is sintered; the temperature in 3 stages respectively 320 DEG C, 460 DEG C, 630 DEG C, per stage sintering time is 1 hour, can obtain rare earth catalyst after having sintered。
Embodiment 2
A kind of rare earth catalyst, is made up of following components proportioning by weight: 32 parts of platinum, lithium 26 parts, ruthenium 24 parts, 18 parts of graphite, calcium oxalate 18 parts, sodium nitrate 21 parts, calcium silicates 15 parts, acetic acid 34 parts, dehydrated alcohol 40 parts。
The method for preparing powder metallurgy of a kind of rare earth catalyst, comprises the steps of
(1) being simultaneously introduced in ball mill by platinum, lithium, ruthenium, graphite, calcium oxalate, sodium nitrate and calcium silicates, grind 2 hours, powder diameter is 300 orders；
(2) mixture step (1) obtained adds in acetic acid, under 6 DEG C of conditions, stirring reaction 20 minutes, filters and removes filtrate, it is thus achieved that filtering residue；
(3) mass ratio of the filtering residue obtained with deionized water cleaning step (2), filtering residue and deionized water is 1:1.1, cleans twice；
(4) in the filtering residue after step (3) is cleaned, add dehydrated alcohol, stirring reaction 12 minutes, absorb water twice；Filter after removing dehydrated alcohol, filtering residue is placed under 65 DEG C of conditions and dries, it is thus achieved that mixture of powders；
(5) mixture of powders is placed in mixing device, utilizes the gases at high pressure that pressure is 2.25MPa to be blown afloat by above-mentioned powder, stop after 8 minutes passing into gases at high pressure, the co-deposited also Homogeneous phase mixing of each powder；
(6) powder after above-mentioned Homogeneous phase mixing is placed in electric furnace; the mode adopting the intensification of 3 stages in the protection atmosphere of helium is sintered; the temperature in 3 stages respectively 320 DEG C, 460 DEG C, 630 DEG C, per stage sintering time is 3 hours, can obtain rare earth catalyst after having sintered。
Embodiment 3
A kind of rare earth catalyst, is made up of following components proportioning by weight: 36 parts of platinum, lithium 30 parts, ruthenium 32 parts, 25 parts of graphite, calcium oxalate 24 parts, sodium nitrate 26 parts, calcium silicates 22 parts, acetic acid 40 parts, dehydrated alcohol 44 parts。
The method for preparing powder metallurgy of a kind of rare earth catalyst, comprises the steps of
(1) being simultaneously introduced in ball mill by platinum, lithium, ruthenium, graphite, calcium oxalate, sodium nitrate and calcium silicates, grind 2.5 hours, powder diameter is 400 orders；
(2) mixture step (1) obtained adds in acetic acid, under 12 DEG C of conditions, stirring reaction 40 minutes, filters and removes filtrate, it is thus achieved that filtering residue；
(3) mass ratio of the filtering residue obtained with deionized water cleaning step (2), filtering residue and deionized water is 1:1.2, cleans twice；
(4) in the filtering residue after step (3) is cleaned, add dehydrated alcohol, stirring reaction 15 minutes, absorb water twice；Filter after removing dehydrated alcohol, filtering residue is placed under 78 DEG C of conditions and dries, it is thus achieved that mixture of powders；
(5) mixture of powders is placed in mixing device, utilizes the gases at high pressure that pressure is 2.85MPa to be blown afloat by above-mentioned powder, stop after 10 minutes passing into gases at high pressure, the co-deposited also Homogeneous phase mixing of each powder；
(6) powder after above-mentioned Homogeneous phase mixing is placed in electric furnace; the mode adopting the intensification of 3 stages in the protection atmosphere of helium is sintered; the temperature in 3 stages respectively 320 DEG C, 460 DEG C, 630 DEG C, per stage sintering time is 4.5 hours, can obtain rare earth catalyst after having sintered。
The rare earth catalyst that embodiment 1～3 prepares is used for the purification of vehicle exhaust, and result is as shown in the table:
The rare earth catalyst the performance test results that table 1 embodiment 1～3 prepares
| Life-span | Applicable temperature | Density | Yield | |
| Embodiment 1 | 16 days | 13～165 DEG C | 8.79g/cm3 | 86% |
| Embodiment 2 | 25 days | 19～266 DEG C | 8.47g/cm3 | 94% |
| Embodiment 3 | 19 days | 17～234 DEG C | 9.12g/cm3 | 91% |
Claims (9)
1. a rare earth catalyst, it is characterized in that, be made up of following components proportioning by weight: 18～36 parts of platinum, lithium 13～30 parts, ruthenium 15～32 parts, 11～25 parts of graphite, calcium oxalate 8～24 parts, sodium nitrate 13～26 parts, calcium silicates 8～22 parts, acetic acid 25～40 parts, dehydrated alcohol 22～44 parts。
2. a kind of rare earth catalyst according to claim 1, it is characterized in that, be made up of following components proportioning by weight: 32 parts of platinum, lithium 26 parts, ruthenium 24 parts, 18 parts of graphite, calcium oxalate 18 parts, sodium nitrate 21 parts, calcium silicates 15 parts, acetic acid 34 parts, dehydrated alcohol 40 parts。
3. the method for preparing powder metallurgy of a kind of rare earth catalyst described in claim 1, it is characterised in that comprise the steps of
(1) being simultaneously introduced in ball mill by platinum, lithium, ruthenium, graphite, calcium oxalate, sodium nitrate and calcium silicates, grind 1～2.5 hour, powder diameter is 200～400 orders；
(2) mixture step (1) obtained adds in acetic acid, under 4～12 DEG C of conditions, stirring reaction 15～40 minutes, filters and removes filtrate, it is thus achieved that filtering residue；
(3) mass ratio of the filtering residue obtained with deionized water cleaning step (2), filtering residue and deionized water is 1:1～1.2, cleans twice；
(4) in the filtering residue after step (3) is cleaned, add dehydrated alcohol, stirring reaction 5～15 minutes, absorb water twice；Filter after removing dehydrated alcohol, filtering residue is placed under 56～78 DEG C of conditions and dries, it is thus achieved that mixture of powders；
(5) being placed in mixing device by mixture of powders, above-mentioned powder is blown afloat by the gases at high pressure utilizing pressure to be 1.78～2.85MPa, stops passing into gases at high pressure after 6～10 minutes, the co-deposited also Homogeneous phase mixing of each powder；
(6) powder after above-mentioned Homogeneous phase mixing is placed in electric furnace; the mode adopting the intensification of 3 stages in the protection atmosphere of helium is sintered; the temperature in 3 stages respectively 320 DEG C, 460 DEG C, 630 DEG C; per stage sintering time is 1～4.5 hour, can obtain rare earth catalyst after having sintered。
4. the method for preparing powder metallurgy of a kind of rare earth catalyst according to claim 3, it is characterized in that, platinum, lithium, ruthenium, graphite, calcium oxalate, sodium nitrate and calcium silicates are simultaneously introduced in ball mill in (1) by step, grind 2 hours, and powder diameter is 300 orders。
5. the method for preparing powder metallurgy of a kind of rare earth catalyst according to claim 3, it is characterised in that mixture step (1) obtained in step (2) adds in acetic acid, under 6 DEG C of conditions, stirring reaction 20 minutes, filters and removes filtrate, it is thus achieved that filtering residue。
6. the method for preparing powder metallurgy of a kind of rare earth catalyst according to claim 3, it is characterized in that, the mass ratio of the filtering residue obtained with deionized water cleaning step (2) in step (3), filtering residue and deionized water is 1:1.1, cleans twice。
7. the method for preparing powder metallurgy of a kind of rare earth catalyst according to claim 3, it is characterised in that add dehydrated alcohol, stirring reaction 12 minutes in the filtering residue after step (3) is cleaned in step (4), absorb water twice；Filter after removing dehydrated alcohol, filtering residue is placed under 65 DEG C of conditions and dries, it is thus achieved that mixture of powders。
8. the method for preparing powder metallurgy of a kind of rare earth catalyst according to claim 3, it is characterized in that, mixture of powders is placed in mixing device in (5) by step, the gases at high pressure that pressure is 2.25MPa are utilized to be blown afloat by above-mentioned powder, stop after 8 minutes passing into gases at high pressure, the co-deposited also Homogeneous phase mixing of each powder。
9. the method for preparing powder metallurgy of a kind of rare earth catalyst according to claim 3; it is characterized in that; powder after above-mentioned Homogeneous phase mixing is placed in electric furnace by step (6); the mode adopting the intensification of 3 stages in the protection atmosphere of helium is sintered; the temperature in 3 stages respectively 320 DEG C, 460 DEG C, 630 DEG C; per stage sintering time is 3 hours, can obtain rare earth catalyst after having sintered。
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| CN101491778A (en) * | 2008-01-23 | 2009-07-29 | 中国石油化工股份有限公司 | Preparation method of thin shell shaped noble metal catalyst |
| CN101857221A (en) * | 2010-05-21 | 2010-10-13 | 哈尔滨工业大学 | Method for preparing graphene compounds and graphene oxide compounds with high efficiency |
| CN102149662A (en) * | 2008-07-31 | 2011-08-10 | 国际人造丝公司 | Ethanol production from acetic acid utillizing a cobalt catalyst |
| CN102149661A (en) * | 2008-07-31 | 2011-08-10 | 国际人造丝公司 | Direct and selective production of ethanol from acetic acid utilizing a platinum/tin catalyst |
| CN102658165A (en) * | 2012-04-06 | 2012-09-12 | 华东理工大学 | Catalyst for preparing ethanol by acetic acid gas phase hydrogenation and preparation method thereof |
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2016
- 2016-02-29 CN CN201610110955.1A patent/CN105688882A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101491778A (en) * | 2008-01-23 | 2009-07-29 | 中国石油化工股份有限公司 | Preparation method of thin shell shaped noble metal catalyst |
| CN102149662A (en) * | 2008-07-31 | 2011-08-10 | 国际人造丝公司 | Ethanol production from acetic acid utillizing a cobalt catalyst |
| CN102149661A (en) * | 2008-07-31 | 2011-08-10 | 国际人造丝公司 | Direct and selective production of ethanol from acetic acid utilizing a platinum/tin catalyst |
| CN101857221A (en) * | 2010-05-21 | 2010-10-13 | 哈尔滨工业大学 | Method for preparing graphene compounds and graphene oxide compounds with high efficiency |
| CN102658165A (en) * | 2012-04-06 | 2012-09-12 | 华东理工大学 | Catalyst for preparing ethanol by acetic acid gas phase hydrogenation and preparation method thereof |
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