CN101518739A - Integral type catalyst with heat storage function as well as preparation method and application thereof - Google Patents
Integral type catalyst with heat storage function as well as preparation method and application thereof Download PDFInfo
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- CN101518739A CN101518739A CN200910038326A CN200910038326A CN101518739A CN 101518739 A CN101518739 A CN 101518739A CN 200910038326 A CN200910038326 A CN 200910038326A CN 200910038326 A CN200910038326 A CN 200910038326A CN 101518739 A CN101518739 A CN 101518739A
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- integral catalyzer
- catalyst
- recuperation layer
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- activated alumina
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- 239000003054 catalyst Substances 0.000 title claims abstract description 102
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 238000005338 heat storage Methods 0.000 title abstract description 16
- 239000006255 coating slurry Substances 0.000 claims abstract description 55
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 31
- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 claims abstract description 27
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 claims abstract description 27
- 229910052863 mullite Inorganic materials 0.000 claims abstract description 27
- 239000007789 gas Substances 0.000 claims abstract description 24
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 22
- 239000010431 corundum Substances 0.000 claims abstract description 22
- 238000007084 catalytic combustion reaction Methods 0.000 claims abstract description 15
- 239000000356 contaminant Substances 0.000 claims abstract description 3
- 239000010815 organic waste Substances 0.000 claims abstract description 3
- 230000001413 cellular effect Effects 0.000 claims description 52
- 238000005303 weighing Methods 0.000 claims description 47
- 230000000694 effects Effects 0.000 claims description 42
- 238000009825 accumulation Methods 0.000 claims description 34
- 229910052878 cordierite Inorganic materials 0.000 claims description 26
- 239000003292 glue Substances 0.000 claims description 22
- 239000012153 distilled water Substances 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- 238000002156 mixing Methods 0.000 claims description 12
- 239000000243 solution Substances 0.000 claims description 12
- 229910001593 boehmite Inorganic materials 0.000 claims description 11
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 claims description 11
- 230000003197 catalytic effect Effects 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 7
- 241001466460 Alveolata Species 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 6
- 229910000510 noble metal Inorganic materials 0.000 claims description 5
- 239000008246 gaseous mixture Substances 0.000 claims description 3
- 229910002651 NO3 Inorganic materials 0.000 claims description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 238000005470 impregnation Methods 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 239000000203 mixture Substances 0.000 abstract description 12
- 239000004480 active ingredient Substances 0.000 abstract 3
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 abstract 2
- QPLDLSVMHZLSFG-UHFFFAOYSA-N CuO Inorganic materials [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 abstract 1
- 210000003850 cellular structure Anatomy 0.000 abstract 1
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(II) oxide Inorganic materials [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 abstract 1
- GNMQOUGYKPVJRR-UHFFFAOYSA-N nickel(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Ni+3].[Ni+3] GNMQOUGYKPVJRR-UHFFFAOYSA-N 0.000 abstract 1
- PZFKDUMHDHEBLD-UHFFFAOYSA-N oxo(oxonickeliooxy)nickel Chemical compound O=[Ni]O[Ni]=O PZFKDUMHDHEBLD-UHFFFAOYSA-N 0.000 abstract 1
- 238000000746 purification Methods 0.000 abstract 1
- 238000002791 soaking Methods 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 description 14
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 9
- 238000004090 dissolution Methods 0.000 description 9
- 238000003760 magnetic stirring Methods 0.000 description 9
- 238000000465 moulding Methods 0.000 description 9
- 238000002485 combustion reaction Methods 0.000 description 7
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- 238000006555 catalytic reaction Methods 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 4
- 239000012496 blank sample Substances 0.000 description 4
- 238000009826 distribution Methods 0.000 description 4
- 229910003465 moissanite Inorganic materials 0.000 description 4
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 4
- 229910010271 silicon carbide Inorganic materials 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 230000000737 periodic effect Effects 0.000 description 3
- 238000012546 transfer Methods 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000003795 desorption Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 230000001172 regenerating effect Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 239000002912 waste gas Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000005474 detonation Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
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- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005496 tempering Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
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Abstract
The invention discloses an integral type catalyst with heat storage function as well as a preparation method and application thereof. The integral type catalyst is loaded with an activated alumina and catalyst active ingredients on the surface of a heat storage layer, and has an integral porous cellular structure; the heat storage layer consists of at least one of SiC and corundum, dichroite and mullite; the catalyst active ingredients mainly comprise CuO, CoO, Ni2O3 and MnO2, and can be added with Pt, Pd or mixture of the both; and the activated alumina accounts for 2 to 20 percent of the mass of the integral type catalyst. The preparation method comprises the following steps: firstly, preparing the activated alumina and the catalyst active ingredients into coating slurry; and then soaking the heat storage layer into the coating slurry to prepare the integral type catalyst with the heat storage function. The catalyst has the thermal efficiency reaching 96 percent, and can realize high-efficiency purification on industrial organic waste gases after integrating with a reverse flow reactor for catalytic combustion of contaminants under non-steady operation conditions.
Description
Technical field
The present invention relates to the organic exhaust gas catalyst, particularly relate to a kind of integral catalyzer that is used for purifying big air quantity organic exhaust gas and preparation method thereof and application in the flow-reversal system with heat accumulation function.
Background technology
Production process such as chemical industry, petrochemical industry and enamel-covered wire spray paint etc. in the operation, all can discharge the waste gas of various volatile organisms (VOCs) such as containing benzene, VOCs, two VOCs, produce primary pollution but also may cause secondary pollution such as photochemical fog.The processing method that these organic exhaust gas are adopted has absorption process, absorption method, thermal incineration method and Production by Catalytic Combustion Process at present.Production by Catalytic Combustion Process efficient height wherein, energy consumption is low; The equipment needed thereby volume is little, and price is low; Therefore obtained using widely.
Tradition stationary state catalytic combustion technology requires reactant concentration to surpass a critical value, need makeup energy always, and the frequent fluctuation of exhaust gas concentration, temperature and flow etc. may cause instrument to be difficult to even running.And flow-reversal catalytic reaction technology is a kind of dynamic operation technology (US 2007/02211255), it is by forcing the input parameter of periodic variation system, make system be in unstable state, improved the time equal operating characteristics of reactor, remedied the deficiency of conventional art.This catalytic reactor integrated level height is the accelerator of reaction, is again heat regenerator, has made full use of high active surface and big thermal capacity and the outer surface of catalytic bed of catalyst.The flow-reversal catalytic combustion reactor mainly is made up of gas generating unit, thin-wall stainless steel pipe reactor, gaseous mixture flow control system and organic matter detection system, test data also directly is stored in the hard disc of computer with the excel format record behind software collection, directly is presented on the computer screen simultaneously.
At present, flow-reversal catalytic reaction technology generally is to load expensive noble metal catalyst by the stage casing, and the high heat capacity inert filler is filled at two ends, carries out integrated with reactor, reach stage casing catalysis, the purpose of heat release is held at two ends, and at strengthening research that catalyst itself holds exothermicity seldom.In this system, because axial heat conduction is one of key factor of device performance, heat storage capacity and heat-transfer effect that the improvement of catalyst hot property will intensifying device integral body reach better energy-saving and emission-reduction purpose; In addition, catalyst combustion reaction is just carried out in the device stage casing, scope is narrower, thereby sufficient the contact may be lacked between waste gas and the catalyst in the short time and to cause reaction to be carried out not thorough, airflow-reversing moment, absorption and the desorption instability that also can cause gas vent concentration of organic pollution on inert material.
The improvement of catalyst hot property depends primarily on the raising that catalyst carrier is held exothermicity, and in the preparation and the application facet of relevant heat storage, on April 23rd, 2003, the open disclosed heat storage of Chinese invention patent (publication number is CN1412518) can be widely used in novel Regenerative Combustion System, can significantly improve the temperature efficiency and the thermal efficiency of Regenerative Combustion System; Chinese invention patent application (CN1164001) then provides a kind of heat-accumulation combustion still can purify NO under high temperature, corrosive atmosphere
x, harmful exhaust gas composition such as CO, HC and improve the heat storage of reliability.Patent CN201072125 discloses a kind of heating power explosion-proof type catalytic thermal storage body, utilize adiabatic high temperature resistant firestopping piece to prevent heating power tempering detonation, thereby the assurance safe combustion mainly is applicable to heating plant, does not relate to the concrete application in the flow-reversal catalytic combustion reactor.
This shows, at selecting the suitable heat storage catalyst carrier of holding concurrently for use, and then synthetic integral catalyzer, and carry out highly integrated achievement in research, temporarily do not appear in the newspapers with Periodic Flow Reversal Reactors with heat accumulation function.
Summary of the invention
The object of the present invention is to provide a kind of inexpensively and have the integral catalyzer of heat accumulation function, solve single catalyst and can not satisfy practical application condition and cost height, problem that resource utilization is low.
Another purpose of the present invention is to provide the preparation method of the integral catalyzer with heat accumulation function.
The present invention also has a purpose to be this integral catalyzer with heat accumulation function is applied in the flow-reversal catalytic combustion reactor, removes industrial organic exhaust gas.
The object of the invention is achieved through the following technical solutions:
A kind of integral catalyzer with heat accumulation function, described integral catalyzer are at the recuperation layer area load activated alumina and catalyst activity component to be arranged, and are the alveolate texture that whole porous forms, and this hole evenly distributes, as gas channel;
Described recuperation layer is made up of at least a and cordierite and mullite in SiC and the corundum, the quality of recuperation layer accounts for the 70-93% of whole integral catalyzer quality, by quality ratio, cordierite: mullite: SiC: corundum=0.5-2.0:0.7-3.0:0-0.5:0-0.6;
Described catalyst activity component comprises CuO, CoO, Ni
2O
3And MnO
2, catalytic active component accounts for the 5-10% of whole integral catalyzer quality, with molar ratio computing, and CuO:CoO:Ni
2O
3: MnO
2=2-4:0.5-1.5:1-3:1-3;
Described activated alumina accounts for the 2-20% of integral catalyzer quality.
The porosity of the alveolate texture that described porous forms be the 8-47 hole/centimetre
2
Described the recuperation layer area load have activated alumina and catalyst activity component be by the equivalent impregnation method with activated alumina and catalyst activity component attached to recuperation layer on, make after the drying roasting.
Described catalyst activity component also comprises Pt and/or Pd; By quality ratio, CuO:Pt:Pd=2-4:0-0.08:0-0.15.
Preparation method with integral catalyzer of heat accumulation function: comprise the steps:
(1) with the dissolved in distilled water boehmite of 6-10 times of quality, magnetic stirrer 2-4h; According to catalyst activity component CuO:CoO:Ni
2O
3: MnO
2: the mol ratio of Pt:Pd is 2-4:0.5-1.5:1-3:1-3:0-0.08:0-0.15, prepares corresponding presoma nitrate of each component or muriatic mixed solution; Two solution mixings obtain the coating slurries;
(2) at least a and cordierite and the mullite in difference weighing recuperation layer SiC and the corundum, cordierite: mullite: SiC: the mass ratio=0.5-2.0:0.7-3.0:0-0.5:0-0.6 of corundum; Be alveolate texture after the high-temperature roasting, then it be soaked in the described coating slurries of step (1), take out behind the placement 0.5-1.5h, blow unnecessary glue in the hole off with compressed air, oven dry 1-3h then in 400-500 ℃ of following roasting 3-5h, obtains applying cellular recuperation layer under 100-200 ℃;
(3) will apply cellular recuperation layer and be soaked in the described coating slurries of step (1) again, and take out behind the placement 0.5-1.5h, and blow unnecessary glue in the hole off with compressed air, oven dry 1-3h under 100-200 ℃ is then in 400-500 ℃ of following roasting 3-5h;
(4) repeating step (3) is impregnated fully until the coating slurries, makes the integer catalyzer with heat accumulation function.
Application with integral catalyzer of heat accumulation function: integral catalyzer is applied to the flow-reversal catalytic combustion reactor, substitutes wherein noble metal catalyst and inert material, is 5000-80000h in air speed
-1, operating temperature 150-850 ℃, volatile organic contaminant concentration 50-10000ppm in the gaseous mixture, purifying industrial organic waste gas under the airflow-reversing cycle 1-360min condition.
With respect to prior art, the present invention has following advantage and beneficial effect:
1. based on high specific heat capacity and the thermal conductivity factor and the cellular overall structure of recuperation layer, the active oxidation aluminized coating can increase specific area and the catalyst activity component is uniformly dispersed, the catalyst activity component is embedded in the activated alumina, integral catalyzer specific area and thermal capacity with heat accumulation function are bigger, good heat conductivity, can accomplish efficiently to hold heat release, more help axial heat conduction, the heat storage capacity of intensifying device integral body and heat-transfer effect.
2. the integral catalyzer that has heat accumulation function integrates catalysis and accumulation of heat, the noble metal catalyst and the inert material that load in the alternative flow-reversal combustion reactor, widen the catalytic combustion segment limit, make rational use of resources, reach save material, the multipurpose of conserve space, energy-saving and emission-reduction.
3. the integral catalyzer mechanical strength height that has heat accumulation function, Heat stability is good, safe and reliable, long service life can be applicable in the multiple catalytic combustion reactor, more having superiority aspect the organic exhaust gas of handling big air quantity, has high using value.
The present invention is further illustrated below in conjunction with the drawings and specific embodiments, but protection scope of the present invention is not limited to the scope of embodiment statement.
Description of drawings
Fig. 1 is the amount of stored heat in cellular heat storage of heat accumulating sections and the corresponding catalyst 1.5h;
Fig. 2 is that the heat release section cold air is preheated temperature over time;
Fig. 3 is the temperature efficiency before and after three kinds of catalyst cupport active components;
Fig. 4 is the catalytic activity of three kinds of catalyst;
Fig. 5 is the influence of commutation cycle to reactor bed axial temperature distribution curve;
Fig. 6 is the influence of concentration to reactor bed axial temperature distribution curve;
Wherein the corresponding VOCs concentration of Figure 4 and 5 is 1000ppm (about 4000mg/Nm
3), Fig. 5 and 6 corresponding air speeds are 50000h
-1
The specific embodiment
(1) coating slurries preparation: take by weighing purity and be 60% boehmite (Al
2O
33H
2O) 30g places a clean beaker, adds the distilled water (300g) of its 10 times of quality, utilizes magnetic stirring apparatus accelerate dissolution 2h; According to CuO:CoO:Ni
2O
3: MnO
2: mol ratio=2.3:1.0:1.5:2.0:0.03 of Pt, weighing Cu (NO
3)
23H
2O 18.05g, Co (NO
3)
26H
2O 10.63g, Ni (NO
3)
26H
2O 21.95g, Mn (NO
3)
226.30g, H
2PtCl
66H
2O 0.31g puts into another clean beaker, adds 200g distilled water and heating for dissolving 0.5h; Last two solution mix and are mixed with the coating slurries.Wherein, the active oxidation aluminized coating mainly plays and increases specific area and with the finely dispersed effect of catalyst activity component, the catalyst activity component is to be embedded in the activated alumina.
(2) cellular recuperation layer is selected: cordierite, mullite, SiC and the corundum of weighing recuperation layer and mixing respectively, cordierite: mullite: SiC: the mol ratio of corundum is=2.0:3.0:0.4:0.6, be cellular cylinder after 1400 ℃ of roasting moulding, specifically be of a size of 30 millimeters 50 millimeters of (diameter) * (highly), the porosity specification be 32 holes/centimetre
2, it is carried out weighing and writes down exact mass;
(3) Preparation of Catalyst: cellular recuperation layer is soaked in the coating slurries, takes out after leaving standstill 1.0h, blow unnecessary glue in the hole off with compressed air, in 120 ℃ of oven dry 2h down, move in the Muffle furnace, 500 ℃ of roasting 4h obtain applying cellular recuperation layer;
(4) will apply cellular recuperation layer and be soaked in the described coating slurries of step (1) again, and take out behind the placement 1h, and blow unnecessary glue in the hole off with compressed air, oven dry 2h under 120 ℃ is then in 500 ℃ of following roasting 4h;
(5) repeat whole steps, the coating slurries are impregnated fully, must have the integral catalyzer of heat accumulation function (4) twice, and note is made the 1# catalyst.
The 1# catalyst is carried out accurate weighing, activated alumina and catalyst activity component actual negative carrying capacity are to account for 11.8% of integral catalyzer quality, wherein activated alumina is to account for 6.1% of integral catalyzer quality, the catalyst activity component is to account for 5.7% of integral catalyzer quality, and recuperation layer is to account for 88.2% of whole integral catalyzer quality.
(1) coating slurries preparation: take by weighing purity and be 60% boehmite (Al
2O
33H
2O) 30g places a clean beaker, adds the distilled water (300g) of its 10 times of quality, utilizes magnetic stirring apparatus accelerate dissolution 2h; According to CuO:CoO:Ni
2O
3: MnO
2: mol ratio=2.3:1.0:1.5:2.0:0.03 of Pt, weighing Cu (NO
3)
23H
2O 18.05g, Co (NO
3)
26H
2O 10.63g, Ni (NO
3)
26H
2O 21.95g, Mn (NO
3)
226.30g, H
2PtCl
66H
2O 0.31g puts into another clean beaker, adds 200g distilled water and heating for dissolving 0.5h; Last two solution mix and are mixed with the coating slurries.
(2) cellular recuperation layer is selected: cordierite, mullite and the SiC of weighing recuperation layer and mixing respectively, the mol ratio of cordierite: mullite: SiC is=2.0:2.5:0.5, be cellular cylinder after 1450 ℃ of roasting moulding, specifically be of a size of 30 millimeters 50 millimeters of (diameter) * (highly), the porosity specification be 32 holes/centimetre
2, it is carried out weighing and writes down exact mass;
(3) Preparation of Catalyst: cellular heat storage is soaked in the coating slurries, takes out after leaving standstill 1.0h, blow unnecessary glue in the hole off with compressed air, in 120 ℃ of oven dry 2h down, move in the Muffle furnace, 500 ℃ of roasting 4h obtain applying cellular recuperation layer;
(4) will apply cellular recuperation layer and be soaked in the described coating slurries of step (1) again, and take out behind the placement 1h, and blow unnecessary glue in the hole off with compressed air, oven dry 2h under 120 ℃ is then in 500 ℃ of following roasting 4h;
(5) repeat whole steps, the coating slurries are impregnated fully, must have the integral catalyzer of heat accumulation function (4) twice, and note is made the 2# catalyst.
The 2# catalyst is carried out accurate weighing, activated alumina and catalyst activity component actual negative carrying capacity are to account for 11.5% of integral catalyzer quality, wherein activated alumina is to account for 6.0% of integral catalyzer quality, the catalyst activity component is to account for 5.5% of integral catalyzer quality, and recuperation layer is to account for 88.5% of whole integral catalyzer quality.
(1) coating slurries preparation: take by weighing purity and be 60% boehmite (Al
2O
33H
2O) 30g places a clean beaker, adds the distilled water (300g) of its 10 times of quality, utilizes magnetic stirring apparatus accelerate dissolution 2h; According to CuO:CoO:Ni
2O
3: MnO
2: mol ratio=2.3:1.0:1.5:2.0:0.03 of Pt, weighing Cu (NO
3)
23H
2O 18.05g, Co (NO
3)
26H
2O 10.63g, Ni (NO
3)
26H
2O 21.95g, Mn (NO
3)
226.30g, H
2PtCl
66H
2O 0.31g puts into another clean beaker, adds 200g distilled water and heating for dissolving 0.5h; Last two solution mix and are mixed with the coating slurries.
(2) cellular recuperation layer is selected: cordierite, mullite and the corundum of weighing recuperation layer and mixing respectively, cordierite: mullite: the mol ratio of corundum is=2.0:2.5:0.6, be cellular cylinder after 1350 ℃ of roasting moulding, specifically be of a size of 30 millimeters 50 millimeters of (diameter) * (highly), the porosity specification be 32 holes/centimetre
2, it is carried out weighing and writes down exact mass;
(3) Preparation of Catalyst: cellular recuperation layer is soaked in the coating slurries, takes out after leaving standstill 1.0h, blow unnecessary glue in the hole off with compressed air, in 120 ℃ of oven dry 2h down, move in the Muffle furnace, 500 ℃ of roasting 4h obtain applying cellular recuperation layer;
(4) will apply cellular recuperation layer and be soaked in the described coating slurries of step (1) again, and take out behind the placement 1h, and blow unnecessary glue in the hole off with compressed air, oven dry 2h under 120 ℃ is then in 500 ℃ of following roasting 4h;
(5) repeat whole steps, the coating slurries are impregnated fully, must have the integral catalyzer of heat accumulation function (4) twice, and note is made the 3# catalyst.
The 3# catalyst is carried out accurate weighing, activated alumina and catalyst activity component actual negative carrying capacity are to account for 11.6% of integral catalyzer quality, wherein activated alumina is to account for 6.2% of integral catalyzer quality, the catalyst activity component is to account for 5.4% of integral catalyzer quality, and recuperation layer is to account for 88.4% of whole integral catalyzer quality.
Embodiment 4
(1) coating slurries preparation: take by weighing purity and be 60% boehmite (Al
2O
33H
2O) 30g places a clean beaker, adds the distilled water (300g) of its 10 times of quality, utilizes magnetic stirring apparatus accelerate dissolution 2h; According to CuO:CoO:Ni
2O
3: MnO
2: mol ratio=2.3:1.0:1.5:2.0:0.03 of Pt, weighing Cu (NO
3)
23H
2O 18.05g, Co (NO
3)
26H
2O 10.63g, Ni (NO
3)
26H
2O 21.95g, Mn (NO
3)
226.30g, H
2PtCl
66H
2O 0.31g puts into another clean beaker, adds 200g distilled water and heating for dissolving 0.5h; Last two solution mix and are mixed with the coating slurries.
(2) cellular recuperation layer is selected: cordierite, mullite, SiC and the corundum of weighing recuperation layer and mixing respectively, cordierite: mullite: SiC: the mol ratio of corundum is=1.5:2.0:0.5:0.1, be cellular cylinder after 1500 ℃ of roasting moulding, specifically be of a size of 30 millimeters 50 millimeters of (diameter) * (highly), the porosity specification be 32 holes/centimetre
2, it is carried out weighing and writes down exact mass;
(3) Preparation of Catalyst: cellular recuperation layer is soaked in the coating slurries, takes out after leaving standstill 1.0h, blow unnecessary glue in the hole off with compressed air, in 120 ℃ of oven dry 2h down, move in the Muffle furnace, 500 ℃ of roasting 4h obtain applying cellular recuperation layer;
(4) will apply cellular recuperation layer and be soaked in the described coating slurries of step (1) again, and take out behind the placement 1h, and blow unnecessary glue in the hole off with compressed air, oven dry 2h under 120 ℃ is then in 500 ℃ of following roasting 4h;
(5) repeat whole steps, the coating slurries are impregnated fully, must have the integral catalyzer of heat accumulation function (4) twice, and note is made the 4# catalyst.
The 4# catalyst is carried out accurate weighing, activated alumina and catalyst activity component actual negative carrying capacity are to account for 11.8% of integral catalyzer quality, wherein activated alumina is to account for 6.5% of integral catalyzer quality, the catalyst activity component is to account for 5.3% of integral catalyzer quality, and recuperation layer is to account for 88.2% of whole integral catalyzer quality.
(1) coating slurries preparation: take by weighing purity and be 60% boehmite (Al
2O
33H
2O) 30g places a clean beaker, adds the distilled water (300g) of its 10 times of quality, utilizes magnetic stirring apparatus accelerate dissolution 2h; According to CuO:CoO:Ni
2O
3: MnO
2: mol ratio=2.3:1.0:1.5:2.0:0.03 of Pt, weighing Cu (NO
3)
23H
2O 18.05g, Co (NO
3)
26H
2O 10.63g, Ni (NO
3)
26H
2O
21.95g, Mn (NO
3)
226.30g, H
2PtCl
66H
2O 0.31g puts into another clean beaker, adds 200g distilled water and heating for dissolving 0.5h; Last two solution mix and are mixed with the coating slurries.
(2) cellular recuperation layer is selected: cordierite, mullite, SiC and the corundum of weighing recuperation layer and mixing respectively, cordierite: mullite: SiC: the mol ratio of corundum is=0.5:1.5:0.1:0.6, be cellular cylinder after 1420 ℃ of roasting moulding, specifically be of a size of 30 millimeters 50 millimeters of (diameter) * (highly), the porosity specification be 32 holes/centimetre
2, it is carried out weighing and writes down exact mass;
(3) Preparation of Catalyst: cellular recuperation layer is soaked in the coating slurries, takes out after leaving standstill 1.0h, blow unnecessary glue in the hole off with compressed air, in 120 ℃ of oven dry 2h down, move in the Muffle furnace, 500 ℃ of roasting 4h obtain applying cellular recuperation layer;
(4) will apply cellular recuperation layer and be soaked in the described coating slurries of step (1) again, and take out behind the placement 1h, and blow unnecessary glue in the hole off with compressed air, oven dry 2h under 120 ℃ is then in 500 ℃ of following roasting 4h;
(5) repeat whole steps, the coating slurries are impregnated fully, must have the integral catalyzer of heat accumulation function (4) twice, and note is made the 5# catalyst.
The 5# catalyst is carried out accurate weighing, activated alumina and catalyst activity component actual negative carrying capacity are to account for 11.9% of integral catalyzer quality, wherein activated alumina is to account for 6.4% of integral catalyzer quality, the catalyst activity component is to account for 5.5% of integral catalyzer quality, and recuperation layer is to account for 88.1% of whole integral catalyzer quality.
Embodiment 6
(1) coating slurries preparation: take by weighing purity and be 60% boehmite (Al
2O
33H
2O), place a clean beaker, add the distilled water (300g) of its 10 times of quality, utilize magnetic stirring apparatus accelerate dissolution 2h; According to CuO:CoO:Ni
2O
3: MnO
2: mol ratio=2.3:1.0:1.5:2.0:0.03 of Pt, weighing Cu (NO
3)
23H
2O 18.05g, Co (NO
3)
26H
2O10.63g, Ni (NO
3)
26H
2O 21.95g, Mn (NO
3)
226.30g, H
2PtCl
66H
2O 0.31g puts into another clean beaker, adds 200g distilled water and heating for dissolving 0.5h; Last two solution mix and are mixed with the coating slurries.
(2) cellular recuperation layer is selected: cordierite, mullite and the SiC of weighing recuperation layer and mixing respectively, the mol ratio of cordierite: mullite: SiC is=1.5:1.8:0.2, be cellular cylinder after 1370 ℃ of roasting moulding, specifically be of a size of 30 millimeters 50 millimeters of (diameter) * (highly), the porosity specification be 32 holes/centimetre
2, it is carried out weighing and writes down exact mass;
(3) Preparation of Catalyst: cellular recuperation layer is soaked in the coating slurries, takes out after leaving standstill 1.0h, blow unnecessary glue in the hole off with compressed air, in 120 ℃ of oven dry 2h down, move in the Muffle furnace, 500 ℃ of roasting 4h obtain applying cellular recuperation layer;
(4) will apply cellular recuperation layer and be soaked in the described coating slurries of step (1) again, and take out behind the placement 1h, and blow unnecessary glue in the hole off with compressed air, oven dry 2h under 120 ℃ is then in 500 ℃ of following roasting 4h;
(5) repeat whole steps, the coating slurries are impregnated fully, must have the integral catalyzer of heat accumulation function (4) twice, and note is made the 6# catalyst.
The 6# catalyst is carried out accurate weighing, activated alumina and catalyst activity component actual negative carrying capacity are to account for 12.0% of integral catalyzer quality, wherein activated alumina is to account for 6.7% of integral catalyzer quality, the catalyst activity component is to account for 5.3% of integral catalyzer quality, and recuperation layer is to account for 88.0% of whole integral catalyzer quality.
Embodiment 7
(1) coating slurries preparation: take by weighing purity and be 60% boehmite (Al
2O
33H
2O) 30g places a clean beaker, adds the distilled water (300g) of its 10 times of quality, utilizes magnetic stirring apparatus accelerate dissolution 2h; According to CuO:CoO:Ni
2O
3: MnO
2: mol ratio=2.3:1.0:1.5:2.0:0.03 of Pt, weighing Cu (NO
3)
23H
2O 18.05g, Co (NO
3)
26H
2O 10.63g, Ni (NO
3)
26H
2O 21.95g, Mn (NO
3)
226.30g, H
2PtCl
66H
2O 0.31g puts into another clean beaker, adds 200g distilled water and heating for dissolving 0.5h; Last two solution mix and are mixed with the coating slurries.
(2) cellular recuperation layer is selected: cordierite, mullite and the SiC corundum of weighing recuperation layer and mixing respectively, the mol ratio of cordierite: mullite: SiC is=0.5:1.0:0.1, be cellular cylinder after 1400 ℃ of roasting moulding, specifically be of a size of 30 millimeters 50 millimeters of (diameter) * (highly), the porosity specification be 32 holes/centimetre
2, it is carried out weighing and writes down exact mass.
(3) Preparation of Catalyst: cellular recuperation layer is soaked in the coating slurries, takes out after leaving standstill 1.0h, blow unnecessary glue in the hole off with compressed air, in 120 ℃ of oven dry 2h down, move in the Muffle furnace, 500 ℃ of roasting 4h obtain applying cellular recuperation layer;
(4) will apply cellular recuperation layer and be soaked in the described coating slurries of step (1) again, and take out behind the placement 1h, and blow unnecessary glue in the hole off with compressed air, oven dry 2h under 120 ℃ is then in 500 ℃ of following roasting 4h;
(5) repeat whole steps, the coating slurries are impregnated fully, must have the integral catalyzer of heat accumulation function (4) twice, and note is made the 7# catalyst.
The 7# catalyst is carried out accurate weighing, activated alumina and catalyst activity component actual negative carrying capacity are to account for 11.5% of integral catalyzer quality, wherein activated alumina is to account for 6.1% of integral catalyzer quality, the catalyst activity component is to account for 5.4% of integral catalyzer quality, and recuperation layer is to account for 88.5% of whole integral catalyzer quality.
Embodiment 8
(1) coating slurries preparation: take by weighing purity and be 60% boehmite (Al
2O
33H
2O) 30g places a clean beaker, adds the distilled water (300g) of its 10 times of quality, utilizes magnetic stirring apparatus accelerate dissolution 2h; According to CuO:CoO:Ni
2O
3: MnO
2: mol ratio=2.3:1.0:1.5:2.0:0.03 of Pt, weighing Cu (NO
3)
23H
2O 18.05g, Co (NO
3)
26H
2O 10.63g, Ni (NO
3)
26H
2O 21.95g, Mn (NO
3)
226.30g, H
2PtCl
66H
2O 0.31g puts into another clean beaker, adds 200g distilled water and heating for dissolving 0.5h; Last two solution mix and are mixed with the coating slurries.
(2) cellular recuperation layer is selected: cordierite, mullite, SiC and the corundum of weighing recuperation layer and mixing respectively, cordierite: mullite: the mol ratio of corundum is=1.5:1.8:0.3, be cellular cylinder after 1450 ℃ of roasting moulding, specifically be of a size of 30 millimeters 50 millimeters of (diameter) * (highly), the porosity specification be 32 holes/centimetre
2, it is carried out weighing and writes down exact mass;
(3) Preparation of Catalyst: cellular recuperation layer is soaked in the coating slurries, takes out after leaving standstill 1.0h, blow unnecessary glue in the hole off with compressed air, in 120 ℃ of oven dry 2h down, move in the Muffle furnace, 500 ℃ of roasting 4h obtain applying cellular recuperation layer;
(4) will apply cellular recuperation layer and be soaked in the described coating slurries of step (1) again, and take out behind the placement 1h, and blow unnecessary glue in the hole off with compressed air, oven dry 2h under 120 ℃ is then in 500 ℃ of following roasting 4h;
(5) repeat whole steps, the coating slurries are impregnated fully, must have the integral catalyzer of heat accumulation function (4) twice, and note is made the 8# catalyst.
The 8# catalyst is carried out accurate weighing, activated alumina and catalyst activity component actual negative carrying capacity are to account for 11.3% of integral catalyzer quality, wherein activated alumina is to account for 6.0% of integral catalyzer quality, the catalyst activity component is to account for 5.3% of integral catalyzer quality, and recuperation layer is to account for 88.7% of whole integral catalyzer quality.
Embodiment 9
(1) coating slurries preparation: take by weighing purity and be 60% boehmite (Al
2O
33H
2O) 30g places a clean beaker, adds the distilled water (300g) of its 10 times of quality, utilizes magnetic stirring apparatus accelerate dissolution 2h; According to CuO:CoO:Ni
2O
3: MnO
2: mol ratio=2.3:1.0:1.5:2.0:0.03 of Pt, weighing Cu (NO
3)
23H
2O 18.05g, Co (NO
3)
26H
2O 10.63g, Ni (NO
3)
26H
2O 21.95g, Mn (NO
3)
226.30g, H
2PtCl
66H
2O 0.31g puts into another clean beaker, adds 200g distilled water and heating for dissolving 0.5h; Last two solution mix and are mixed with the coating slurries.
(2) cellular recuperation layer is selected: cordierite, mullite and the corundum of weighing recuperation layer and mixing respectively, cordierite: mullite: the mol ratio of corundum is=0.5:1.0:0.1, be cellular cylinder after 1350 ℃ of roasting moulding, specifically be of a size of 30 millimeters 50 millimeters of (diameter) * (highly), the porosity specification be 32 holes/centimetre
2, it is carried out weighing and writes down exact mass;
(3) Preparation of Catalyst: cellular recuperation layer is soaked in the coating slurries, takes out after leaving standstill 1.0h, blow unnecessary glue in the hole off with compressed air, in 120 ℃ of oven dry 2h down, move in the Muffle furnace, 500 ℃ of roasting 4h obtain applying cellular recuperation layer;
(4) will apply cellular recuperation layer and be soaked in the described coating slurries of step (1) again, and take out behind the placement 1h, and blow unnecessary glue in the hole off with compressed air, oven dry 2h under 120 ℃ is then in 500 ℃ of following roasting 4h;
(5) repeat whole steps, the coating slurries are impregnated fully, must have the integral catalyzer of heat accumulation function (4) twice, and note is made the 9# catalyst.
The 9# catalyst is carried out accurate weighing, activated alumina and catalyst activity component actual negative carrying capacity are to account for 11.7% of integral catalyzer quality, wherein activated alumina is to account for 6.6% of integral catalyzer quality, the catalyst activity component is to account for 5.1% of integral catalyzer quality, and recuperation layer is to account for 88.3% of whole integral catalyzer quality.
The catalysis of embodiment catalyst and thermal storage effect test
Be primarily aimed at 1# corresponding in embodiment 1,2 and 3 below, 2#, the 3# integral catalyzer carries out performance test.
Respectively with 1#, 2#, 3# integral catalyzer and blank sample thereof (being cellular recuperation layer) are inserted in the reactor, at first the air through the heating furnace preheating enters from reactor one end, the integral catalyzer (/ corresponding blank sample) of flowing through, heat is absorbed and accumulates at this moment, 1.5h the back is heat under reversal valve control, cold airflow switches, cold air etc. mass flow flows into, in integral catalyzer (corresponding blank sample), obtain preheating, like this by heat, the cold airflow alternating current when reactor heat accumulating sections and heat release section savings with release energy different, thereby compared different composition integral catalyzers (/ corresponding blank sample) hold exothermicity, test result is seen Fig. 1,2, Fig. 1 is 300 ℃ of hot air intake temperature, and heat time heating time is during 1.5h, the amount of stored heat (kJ) before and after each integral catalyzer supported catalyst active component of heat accumulating sections.Can find out that by this figure under the same terms, comparing the accumulation of heat effect before 1# integral catalyzer and the load has tangible enhancing.Fig. 2 finds the prolongation along with the time for to be preheated temperature over time when 30 ℃ of cold airs of heat release section are flowed through catalyst, and the outlet temperature of air reduces gradually, and this is because the temperature of catalyst reduces the heat release ability drop gradually.Wherein the heat accumulated of 1# catalyst heat accumulating sections is maximum, and the mean temperature that is preheated after the cooling section cold air is flowed through is also the highest relatively, and the gas temperature downward trend is slow slightly.By the temperature efficiency (Fig. 3) before and after the catalyst cupport active component as can be known, 1#, 2# and 3# catalyst in use all have the temperature efficiency up to 96%.
At the normal pressure steady state operation is air speed 50000h
-1, operating temperature 150-850 ℃, benzene, toluene and dimethylbenzene mixed volatilization organic gas (VOCs) concentration 1000ppm (about 4000mg/Nm
3) under the condition, each catalyst all can reach higher removal effect when the clearance of organic exhaust gas be the results are shown in Figure 4,300 ℃.Air speed 50000h wherein
-1Be meant volume space velocity, be the ratio of volumetric flow of gas and integral catalyzer volume.
The comprehensive relatively accumulation of heat and the catalytic performance of catalyst are that example is introduced its concrete application in the flow-reversal catalytic combustion reactor with 1# integral catalyzer among the embodiment 1 below.
The application characteristic of 1# catalyst in the flow-reversal catalytic combustion reactor
The 1# catalyst of preparation is inserted in the flow-reversal catalytic combustion reactor, replace noble metal catalyst and inert material two parts, at normal pressure, air speed 5000-80000h
-1, operating temperature 150-850 ℃ under the gas flow conversion commutation cycle 1-360min operating condition, is that benzene, toluene and the dimethylbenzene mixed volatilization organic gas (VOCs) of 50-10000ppm carries out purified treatment to concentration.At normal pressure, air speed is 50000h
-1, gas flow is under the periodic transformation operating condition, and test result finds that catalyst all can reach 93.5% to the clearance of the organic exhaust gas of 1000ppm in the time of 300 ℃, the clearance in Fig. 4 during steady state operation.Commutation cycle 120min, air speed is respectively 10000h
-1, 50000h
-1, 80000h
-1The time, in bed, can form a two ends relatively flat, middle local precipitous instantaneous axis to Temperature Distribution and since device integral-filled prepared integral catalyzer, the bed heat storage capacity strengthens to some extent, so that the bed temperature level is higher, and raises with the increase of air speed; The VOCs removal effect is at air speed 50000h
-1The time best, reach 95% in the time of 300 ℃.
In the reactor dynamic operation, the commutation cycle increases when VOCs clearance more in short-term is all than stable state, and since heat-storage catalytic section long enough, the very low situation of conversion ratio in the back first few minutes that can not occur commutating.When commutation cycle during less than 5min, the VOCs clearance is not unalterable, but a trend that slowly increases is arranged, and this may be to be caused by a small amount of VOCs desorption that commutation moment is adsorbed on the catalyst.With the commutation cycle is that 5-20min is that example is tested, prolongation along with the commutation cycle, temperature peak and temperature levels (Fig. 5) though on a declining curve, but because the accumulation of heat effect of catalyst, the bulk temperature of bed distributes more even, all is higher than the light-off temperature of VOCs catalytic combustion, and bed temperature dull rising with the VOCs exothermic catalytic reaction in the steady state operation can not occur, therefore suppress the decline of reaction motive force, can keep high VOCs clearance.
At commutation cycle 10min, 300 ℃ of temperature, air speed 50000h
-1The time, by to concentration being the mixing organic exhaust gas test discovery of 200-1000ppm, the VOCs clearance is slight downward trend with the increase with concentration, and this may be that a small amount of VOCs molecule does not participate in reaction and just discharges reactor with air-flow because the time of molecular balance increases and elongated with concentration.Fig. 6 is the corresponding above-mentioned commutation cycle, when VOCs concentration is increased to 1000ppm by 200ppm, and commutate the from left to right axial temperature distribution curve of moment bed of gas flow.Because 1# integral catalyzer heat-transfer capability is strong, the reactive combustion liberated heat in time shifts to the port of export, can not cause " temperature runaway is out of control ", and bed temperature rises mild.
Claims (6)
1, a kind of integral catalyzer with heat accumulation function, it is characterized in that described integral catalyzer is at the recuperation layer area load activated alumina and catalyst activity component to be arranged, be the alveolate texture that whole porous forms, this hole evenly distributes, as gas channel;
Described recuperation layer is made up of at least a and cordierite and mullite in SiC and the corundum, the quality of recuperation layer accounts for the 70-93% of whole integral catalyzer quality, by quality ratio, cordierite: mullite: SiC: corundum=0.5-2.0:0.7-3.0:0-0.5:0-0.6;
Described catalyst activity component comprises CuO, CoO, Ni
2O
3And MnO
2, catalytic active component accounts for the 5-10% of whole integral catalyzer quality, with molar ratio computing, and CuO:CoO:Ni
2O
3: MnO
2=2-4:0.5-1.5:1-3:1-3;
Described activated alumina accounts for the 2-20% of integral catalyzer quality.
2, the integral catalyzer with heat accumulation function according to claim 1 is characterized in that: the porosity of the alveolate texture that described porous forms be the 8-47 hole/centimetre
2
3, the integral catalyzer with heat accumulation function according to claim 1, it is characterized in that: described the recuperation layer area load have activated alumina and catalyst activity component be by the equivalent impregnation method with activated alumina and catalyst activity component attached to recuperation layer on, make after the drying roasting.
4, the integral catalyzer with heat accumulation function according to claim 1 is characterized in that: described catalyst activity component also comprises Pt and/or Pd; By quality ratio, CuO:Pt:Pd=2-4:0-0.08:0-0.15.
5, the described preparation method of claim 1: it is characterized in that comprising the steps: with integral catalyzer of heat accumulation function
(1) with the dissolved in distilled water boehmite of 6-10 times of quality, magnetic stirrer 2-4h; According to catalyst activity component CuO:CoO:Ni
2O
3: MnO
2: the mol ratio of Pt:Pd is 2-4:0.5-1.5:1-3:1-3:0-0.08:0-0.15, prepares corresponding presoma nitrate of each component or muriatic mixed solution; Two solution mixings obtain the coating slurries;
(2) at least a and cordierite and the mullite in difference weighing recuperation layer SiC and the corundum, cordierite: mullite: SiC: the mass ratio=0.5-2.0:0.7-3.0:0-0.5:0-0.6 of corundum; Be alveolate texture after the high-temperature roasting, then it be soaked in the described coating slurries of step (1), take out behind the placement 0.5-1.5h, blow unnecessary glue in the hole off with compressed air, oven dry 1-3h then in 400-500 ℃ of following roasting 3-5h, obtains applying cellular recuperation layer under 100-200 ℃;
(3) will apply cellular recuperation layer and be soaked in the described coating slurries of step (1) again, and take out behind the placement 0.5-1.5h, and blow unnecessary glue in the hole off with compressed air, oven dry 1-3h under 100-200 ℃ is then in 400-500 ℃ of following roasting 3-5h;
(4) repeating step (3) is impregnated fully until the coating slurries, makes the integer catalyzer with heat accumulation function.
6, the described application with integral catalyzer of heat accumulation function of claim 1 is characterized in that integral catalyzer is applied to the flow-reversal catalytic combustion reactor, substitutes wherein noble metal catalyst and inert material, is 5000-80000h in air speed
-1, operating temperature 150-850 ℃, volatile organic contaminant concentration 50-10000ppm in the gaseous mixture, purifying industrial organic waste gas under the airflow-reversing cycle 1-360min condition.
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