CN104056623B - A kind of manufacture method of nitric acid production nonwoven catalyst - Google Patents
A kind of manufacture method of nitric acid production nonwoven catalyst Download PDFInfo
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- CN104056623B CN104056623B CN201410280368.8A CN201410280368A CN104056623B CN 104056623 B CN104056623 B CN 104056623B CN 201410280368 A CN201410280368 A CN 201410280368A CN 104056623 B CN104056623 B CN 104056623B
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Abstract
The preparation method that the present invention relates to a kind of preparing nitric acid by ammonia oxidation catalyst, this catalyst is different from conventional screen catalyst, is a kind of novel non-woven material.This Catalyst Production cost is low, and the process-cycle is short.Ammonia is after catalyst surface burns, and before and after gas reaction, pressure drop is little；Noble metal loading is few；Its non-geometric gap structure is conducive to the distribution of reacting gas, alternative current mesh catalyst.
Description
Technical field:
The present invention relates to the manufacture method of a kind of nitric acid production catalyst, described method application sintering technology, noble metal fiber sintering is become non-woven material.The method is different from currently used silk screen production processes.
Technical background:
It is the widely used method in the current world that application Ostwald legal system makes nitric acid.Main flow is as follows: ammonia obtains nitric oxide through air oxidation, is further oxidized to nitrogen dioxide, obtains nitric acid after absorption tower absorbs.The method uses platinum alloy mesh catalyst to promote the reaction of oxygen in ammonia and air to be performed continuously over.Andrussow method is used to prepare the process of hydrocyanic acid substantially similar with the above-mentioned process preparing nitric acid, so, the use scope of this invention contains the preparation of hydrocyanic acid.
Current ammoxidation catalyst mainly exists with netted form, main processing technology is: noble metal metallurgy ingot casting, via obtaining noble metal bar after cold rolling hot-rolled process, use monofilament drawing technique through rough, in the after annealing warping drawing and carefully draw, netting machine is woven into netted form.The wire surface that single wire drawing obtains is smooth, and cross section is rounded, is suitable on netting machine filamentation, the metal gauze smooth surface knitted.Use different netting machines, it is possible to obtain plain net, warp-knitting net, weft-knitting net.Recent decades, people have done substantial amounts of optimization at the braiding style of net type, and the composition of precious metal alloys has been carried out continuous trial, but knitting skill does not change, noble metal loss in the course of processing is big, and the process-cycle is long, and processing cost is difficult to be greatly reduced.
Bundle drawing method technology is the technology that a kind of low cost high-volume manufactures metal wire material, is the main method prepared of current micro-sized metal fiber through engineering approaches.It is tens wires even up to ten thousand to be wrapped in carry out drawing in pipe, it is achieved that multi-filament is decrement simultaneously, in time pulling to required fibre diameter, removes cage walls, fiber separation out.The tinsel fasciculation form that the method prepares, it is difficult to be separated into single, so netting machine braiding platinum guaze can not be used for the tinsel that the method prepares.
The present invention principle according to nitric acid oxidation, makes metallic fiber by noble metal by clustered drawing, cuts into high temperature sintering after chopped fiber, forms a kind of non-woven material.
The sintering process of non-woven material includes the preparation of metallic fiber, fiber lay down felt, sintering process.Sintering theory is, warm-up movement at high temperature occurs metallic atom, and fiber junction point melts, and eventually forms the non-woven material of entirety.By controlling sintering temperature, sintering time, the temperature lift-down curve of temperature, it is possible to control the intensity of sinter.
Summary of the invention:
The present invention relates to the manufacture method of a kind of nonwoven catalyst.Concrete grammar is, by drawing technique, obtains the metallic fiber of fasciculation, then lay after metallic fiber is cut into chopped fiber, sintering, make nonwoven catalyst.
A kind of nonwoven catalyst for nitric acid production, its preparation includes: by bundle drawing method technology, noble metal drawing is obtained metallic fiber, metallic fiber is cut into chopped fiber, and then chopped fiber is evenly laid out, and noble metal fiber is made non-woven material by the mode finally by sintering.
A kind of nonwoven catalyst for nitric acid production, its preparation includes: by bundle drawing method technology, noble metal drawing is obtained metallic fiber, metallic fiber cuts into chopped fiber, and chopped fiber is evenly laid out in sintering substrate, and noble metal fiber is made non-woven material by the mode finally by sintering.
Sintering of catalyst substrate is aluminium oxide.
By noble metal through melting, cold rolling, hot rolling and rough after, obtain the metal wire material that diameter is 0.9mm.By integrated a branch of for many noble metal wire rods, additional cladding material, then carry out drawing.The diameter range of the metallic fiber obtained is 0.040～0.090mm.
Main preparation technology is as follows: 1. 2. surface treatment encapsulates 3. compacting 4. bundle drawing method and 5. separate 6. rolling
Metallic fiber closes on winding barrel, and using fibre cutting machine that metallic fiber cuts into length is 5～10mm.Noble metal non-woven material:
Metallic fiber early stage made is transferred on the sieve that aperture is 5～8 orders, and metallic fiber falls on alumina substrates uniformly from sieve aperture.Alumina base floor space is that the metallic fiber weight per unit area being sieved is 1000～2000g/m by required sintering area2.The alumina substrate being placed with metallic fiber is put into high temperature sintering furnace sintering.Composition according to precious metal alloys is different, and sintering temperature is set to 1000 DEG C～1400 DEG C, and sintering time is 8～24h.After sintering, the junction point between metallic fiber is owing at high temperature occurring molecular thermalmotion to link together, and forms overall non-woven material.
The preparation of metallic fiber can adopt above-mentioned clustered drawing, it is possible to use molten takes out method or prepared by cutting method.The thickness of metallic fiber non-woven material is controlled, and specific surface area is big, and intensity is high.And special non-geometrically makes ammonia sky gaseous mixture at catalyst surface homogenous combustion.
Accompanying drawing explanation
Fig. 1 is nonwoven catalyst schematic diagram of the present invention
In figure: 1: nonwoven catalyst sample
Detailed description of the invention:
Embodiment 1
Melting binary PtRh10 material, obtains PtRh10 ingot.After passing it through cold rolling, hot rolling and being rough, obtain the metal wire material that diameter is 0.9mm.This metal wire rod, through surface treatment, encapsulation, compacting, bundle drawing method, separation, winding process, obtains the PtRh10 metallic fiber that diameter is 0.062mm fasciculation.By cutting machine, cellosilk is processed growth degree is the metallic fiber of 5mm.Metallic fiber early stage made is transferred on the sieve that aperture is 5 orders, and metallic fiber falls on alumina substrates uniformly from sieve aperture.Alumina base floor space is 1000mm × 1000mm, and the metallic fiber weight per unit area being sieved is 1500g/m2.The alumina substrate being placed with metallic fiber is put into high temperature sintering furnace sintering.Sintering temperature is 1350 DEG C, and sintering time is 12h.After sintering, the junction point between metallic fiber, owing at high temperature occurring molecular thermalmotion to link together, forms overall non-woven material.
It is 160mm that the non-woven material obtained cuts into diameter, loads test oxidation furnace.Pass into Hydrogen activation nonwoven catalyst, then pass into ammonia, air Mixture.Ammonia is in catalyst surface smooth combustion.
Embodiment 2
Melting binary PtRh7 material, obtains PtRh7 ingot.After passing it through cold rolling, hot rolling and being rough, obtain the metal wire material that diameter is 0.9mm.This metal wire rod, through surface treatment, encapsulation, compacting, bundle drawing method, separation, winding process, obtains the PtRh10 metallic fiber that diameter is 0.062mm fasciculation.By cutting machine, cellosilk is processed growth degree is the metallic fiber of 5mm.Metallic fiber early stage made is transferred on the sieve that aperture is 5 orders, and metallic fiber falls on alumina substrates uniformly from sieve aperture.Alumina base floor space is 1000mm × 1000mm, and the metallic fiber weight per unit area being sieved is 1500g/m2.The alumina substrate being placed with metallic fiber is put into high temperature sintering furnace sintering.Sintering temperature is 1250 DEG C, and sintering time is 12h.After sintering, the junction point between metallic fiber, owing at high temperature occurring molecular thermalmotion to link together, forms overall non-woven material.
It is 160mm that the non-woven material obtained cuts into diameter, loads test oxidation furnace.Pass into Hydrogen activation nonwoven catalyst, then pass into ammonia, air Mixture.Ammonia is in catalyst surface smooth combustion.
Embodiment 3
Melting binary PtRh5 material, obtains PtRh5 ingot.After passing it through cold rolling, hot rolling and being rough, obtain the metal wire material that diameter is 0.9mm.This metal wire rod, through surface treatment, encapsulation, compacting, bundle drawing method, separation, winding process, obtains the PtRh5 metallic fiber that diameter is 0.062mm fasciculation.By cutting machine, cellosilk is processed growth degree is the metallic fiber of 5mm.Metallic fiber early stage made is transferred on the sieve that aperture is 5 orders, and metallic fiber falls on alumina substrates uniformly from sieve aperture.Alumina base floor space is 1000mm × 1000mm, and the metallic fiber weight per unit area being sieved is 1500g/m2.The alumina substrate being placed with metallic fiber is put into high temperature sintering furnace sintering.Sintering temperature is 1200 DEG C, and sintering time is 12h.After sintering, the junction point between metallic fiber, owing at high temperature occurring molecular thermalmotion to link together, forms overall non-woven material.
It is 160mm that the non-woven material obtained cuts into diameter, loads test oxidation furnace.Pass into Hydrogen activation nonwoven catalyst, then pass into ammonia, air Mixture.Ammonia is in catalyst surface smooth combustion.
Embodiment 4
Melting ternary PtRh3.7Pd3.8 material, obtains ternary PtRh3.7Pd3.8 ingot.PtRh3.7Pd3.8 alloy mass score ratio is for, after passing it through cold rolling, hot rolling and being rough, obtaining the metal wire material that diameter is 0.9mm.This metal wire rod, through surface treatment, encapsulation, compacting, bundle drawing method, separation, winding process, obtains the PtRh3.7Pd3.8 metallic fiber that diameter is 0.062mm fasciculation.By cutting machine, cellosilk is processed growth degree is the metallic fiber of 5mm.Metallic fiber early stage made is transferred on the sieve that aperture is 5 orders, and metallic fiber falls on alumina substrates uniformly from sieve aperture.Alumina base floor space is 1000mm × 1000mm, and the metallic fiber weight per unit area being sieved is 1500g/m2.The alumina substrate being placed with metallic fiber is put into high temperature sintering furnace sintering.Sintering temperature is 1200 DEG C, and sintering time is 12h.After sintering, the junction point between metallic fiber, owing at high temperature occurring molecular thermalmotion to link together, forms overall non-woven material.
It is 160mm that the non-woven material obtained cuts into diameter, loads test oxidation furnace.Pass into Hydrogen activation nonwoven catalyst, then pass into ammonia, air Mixture.Ammonia is in catalyst surface smooth combustion.
Embodiment 5
Melting binary PtPd material, obtains PtPd ingot.After passing it through cold rolling, hot rolling and being rough, obtain the metal wire material that diameter is 0.9mm.This metal wire rod, through surface treatment, encapsulation, compacting, bundle drawing method, separation, winding process, obtains the PtPd metallic fiber that diameter is 0.062mm fasciculation.By cutting machine, cellosilk is processed growth degree is the metallic fiber of 5mm.Metallic fiber early stage made is transferred on the sieve that aperture is 5 orders, and metallic fiber falls on alumina substrates uniformly from sieve aperture.Alumina base floor space is 1000mm × 1000mm, and the metallic fiber weight per unit area being sieved is 1500g/m2.The alumina substrate being placed with metallic fiber is put into high temperature sintering furnace sintering.Sintering temperature is 1100 DEG C, and sintering time is 12h.After sintering, the junction point between metallic fiber, owing at high temperature occurring molecular thermalmotion to link together, forms overall non-woven material.
The part test operational factor of embodiment 1 to embodiment 4 is in Table 1.
Table 1
The above; it it is only presently preferred embodiments of the present invention; not the present invention is done any restriction, every any simple modification, change and equivalent structure change above example made according to inventive technique essence, all still falls within the protection domain of technical solution of the present invention.
Claims (5)
1. the nonwoven catalyst for nitric acid production, its preparation includes: by bundle drawing method technology, noble metal drawing is obtained metallic fiber, metallic fiber is cut into chopped fiber, chopped fiber is evenly laid out in sintering of catalyst substrate, noble metal fiber is made non-woven material by the mode finally by sintering, it is characterized in that noble metal is PtRh10, PtRh7, PtRh5, PtRh3.7Pd3.8 or PtPd, the diameter of metallic fiber is 0.040～0.090mm, the length of the chopped fiber that metallic fiber cutting obtains is 5～10mm, by chopped fiber by again chopped fiber being tiled after the sieve of 5-8 order.
2. nonwoven catalyst according to claim 1, wherein sintering of catalyst substrate is aluminium oxide.
3. nonwoven catalyst according to claim 1, wherein sintering temperature is 1000～1400 DEG C, and sintering time is 8～24 hours.
4. nonwoven catalyst according to claim 1, it is characterised in that before sintering, the evenly laid out weight per unit area of chopped fiber is 1000～2000g/m2。
5. nonwoven catalyst according to claim 1, it is characterised in that take out method or cutting method prepares metallic fiber also by molten.
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| CN101518745A (en) * | 2009-04-03 | 2009-09-02 | 西北有色金属研究院 | Method for preparing metal fiber carrier for automobile exhaust purifier |
| CN101554585B (en) * | 2009-05-08 | 2011-04-27 | 中国化工供销太原贵金属有限公司 | Dual-function knitted catalytic gauze used for nitric acid manufacture |
| CN103803514A (en) * | 2014-01-28 | 2014-05-21 | 中海油太原贵金属有限公司 | Method for producing nitric acid |
| CN103846086A (en) * | 2014-03-05 | 2014-06-11 | 四川大学 | Catalyst for preparing nitric oxides through catalytic ammonia oxidation |
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