CN104056623A - Preparation method of nonwoven catalyst for nitric acid production - Google Patents
Preparation method of nonwoven catalyst for nitric acid production Download PDFInfo
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- CN104056623A CN104056623A CN201410280368.8A CN201410280368A CN104056623A CN 104056623 A CN104056623 A CN 104056623A CN 201410280368 A CN201410280368 A CN 201410280368A CN 104056623 A CN104056623 A CN 104056623A
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Abstract
The invention relates to a preparation method of a catalyst for nitric acid production from ammoxidation. Different from a traditional silk screen catalyst, the catalyst is novel of nonwoven material. The catalyst has low production cost and short processing period. Ammonia gas combusts on the surface of the catalyst, and the gas pressure drop before and after the reaction is small; the filling quantity noble metal is small; and the non-geometric gap structure facilitates the distribution of reaction gas and can substitute the current silk screen catalyst.
Description
Technical field:
The manufacture method that the present invention relates to a kind of nitric acid production catalyst, described method application sintering technology, becomes non-woven material by noble metal fiber sintering.The method is different from the silk screen manufacture method of current use.
Technical background:
It is the widely used method in the current world that application Ostwald legal system is made nitric acid.Main flow process is as follows: ammonia obtains nitric oxide through air oxidation, is further oxidized to nitrogen dioxide, after absorption tower absorbs, obtains nitric acid.The method is used platinum alloy mesh catalyst to impel the reaction of oxygen in ammonia and air to continue to carry out.Use Andrussow legal system substantially similar for the process of hydrogen cyanide and the above-mentioned process of preparing nitric acid, so, the preparation that the scope of application of this invention has comprised hydrogen cyanide.
Ammoxidation catalyst mainly exists with netted form at present, main manufacture craft 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 warping of annealing after drawing and carefully drawing, on netting machine, be woven into netted form.The wire surface that single wire drawing obtains is smooth, and cross section is rounded, is suitable on netting machine becoming silk, knit woven wire smooth surface.Use different netting machines, can obtain plain net, warp-knitting net, weft-knitting net.Recent decades, people have done a large amount of optimization at the braiding style of net type, and the composition of precious metal alloys has been carried out to continuous trial, but knitting skill does not change, the loss of noble metal in process is large, and the process-cycle is long, and processing cost is difficult to significantly reduce.
Boundling drawing technique is the technology that a kind of low cost is manufactured metal wire material in enormous quantities, is main method prepared by current micron order metallic fiber through engineering approaches.It is that tens wires even up to ten thousand are wrapped in pipe and carry out drawing, has realized multi-filament decrement simultaneously, in the time pulling to required fibre diameter, removes cage walls, fiber separation out.The wire fasciculation form that the method makes, be difficult to be separated into single, so the wire that the method can not be made weaves platinum guaze for netting machine.
The present invention, according to the principle of nitric acid oxidation, makes metallic fiber by noble metal by clustered drawing, cuts into high temperature sintering after short fiber, forms a kind of non-woven material.
The sintering process of non-woven material comprises 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 tie point melts, and finally forms overall non-woven material.By controlling sintering temperature, sintering time, the temperature lift-down curve of temperature, can control the intensity of sinter.
Summary of the invention:
The present invention relates to a kind of preparation method of nonwoven catalyst.Concrete grammar is, by drawing technique, obtains the metallic fiber of fasciculation, then after metallic fiber is cut into short fiber, lay, sintering, make nonwoven catalyst.
A kind of nonwoven catalyst for nitric acid production, its preparation comprises: by boundling drawing technique, noble metal drawing is obtained to metallic fiber, metallic fiber is cut into short fiber, and then short fiber evenly tiles, and finally by the mode of sintering, noble metal fiber is made to non-woven material.
A kind of nonwoven catalyst for nitric acid production, its preparation comprises: by boundling drawing technique, noble metal drawing is obtained to metallic fiber, metallic fiber is cut into short fiber, and short fiber is evenly laid in sintering substrate, finally by the mode of sintering, noble metal fiber is made to non-woven material.
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 many noble metal wire rods, additional clad material, then carry out drawing.The diameter range of the metallic fiber obtaining is 0.040～0.090mm.
Main preparation technology is as follows: 1. surface treatment 2. encapsulate 3. compacting 4. boundling drawing 5. separate 6. rolling
Metallic fiber closes on winding barrel, and using fibre cutting machine that metallic fiber is cut into length is 5～10mm.Noble metal non-woven material:
It is that on 5～8 object sieves, metallic fiber drops on alumina substrate uniformly from sieve aperture that the metallic fiber of making early stage is transferred to aperture.Alumina base floor space is by required sintering area, and the metallic fiber weight per unit area being sieved is 1000～2000g/m
2.The alumina substrate that is placed with metallic fiber is put into high temperature sintering furnace sintering.According to the composition difference of precious metal alloys, sintering temperature is made as 1000 DEG C～1400 DEG C, and sintering time is 8～24h.Tie point after sintering between metallic fiber links together owing at high temperature there is molecular thermalmotion, forms overall non-woven material.
The preparation of metallic fiber can adopt above-mentioned clustered drawing, also can take out method or prepared by cutting method with molten.The thickness of metallic fiber non-woven material is controlled, and specific area is large, and intensity is high.And special non-geometry makes the empty gaseous mixture of ammonia evenly burn at catalyst surface.
Brief description of the drawings
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.By its through cold rolling, hot rolling and rough after, obtain the metal wire material that diameter is 0.9mm.This metal wire rod is through surface treatment, encapsulation, compacting, boundling drawing, separation, winding process, and obtaining diameter is the PtRh10 metallic fiber of 0.062mm fasciculation.Filament is processed to the metallic fiber that growth degree is 5mm by cutting machine.It is that on 5 object sieves, metallic fiber drops on alumina substrate uniformly from sieve aperture that the metallic fiber of making early stage is transferred to aperture.Alumina base floor space is 1000mm × 1000mm, and the metallic fiber weight per unit area being sieved is 1500g/m
2.The alumina substrate that is 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 tie point between metallic fiber links together owing at high temperature there is molecular thermalmotion, forms overall non-woven material.
It is 160mm that the non-woven material obtaining is cut into diameter, packs test oxidation furnace into.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.By its through cold rolling, hot rolling and rough after, obtain the metal wire material that diameter is 0.9mm.This metal wire rod is through surface treatment, encapsulation, compacting, boundling drawing, separation, winding process, and obtaining diameter is the PtRh10 metallic fiber of 0.062mm fasciculation.Filament is processed to the metallic fiber that growth degree is 5mm by cutting machine.It is that on 5 object sieves, metallic fiber drops on alumina substrate uniformly from sieve aperture that the metallic fiber of making early stage is transferred to aperture.Alumina base floor space is 1000mm × 1000mm, and the metallic fiber weight per unit area being sieved is 1500g/m
2.The alumina substrate that is 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 tie point between metallic fiber links together owing at high temperature there is molecular thermalmotion, forms overall non-woven material.
It is 160mm that the non-woven material obtaining is cut into diameter, packs test oxidation furnace into.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.By its through cold rolling, hot rolling and rough after, obtain the metal wire material that diameter is 0.9mm.This metal wire rod is through surface treatment, encapsulation, compacting, boundling drawing, separation, winding process, and obtaining diameter is the PtRh5 metallic fiber of 0.062mm fasciculation.Filament is processed to the metallic fiber that growth degree is 5mm by cutting machine.It is that on 5 object sieves, metallic fiber drops on alumina substrate uniformly from sieve aperture that the metallic fiber of making early stage is transferred to aperture.Alumina base floor space is 1000mm × 1000mm, and the metallic fiber weight per unit area being sieved is 1500g/m
2.The alumina substrate that is 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 tie point between metallic fiber links together owing at high temperature there is molecular thermalmotion, forms overall non-woven material.
It is 160mm that the non-woven material obtaining is cut into diameter, packs test oxidation furnace into.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 mark than for by its through cold rolling, hot rolling and rough after, obtain the metal wire material that diameter is 0.9mm.This metal wire rod is through surface treatment, encapsulation, compacting, boundling drawing, separation, winding process, and obtaining diameter is the PtRh3.7Pd3.8 metallic fiber of 0.062mm fasciculation.Filament is processed to the metallic fiber that growth degree is 5mm by cutting machine.It is that on 5 object sieves, metallic fiber drops on alumina substrate uniformly from sieve aperture that the metallic fiber of making early stage is transferred to aperture.Alumina base floor space is 1000mm × 1000mm, and the metallic fiber weight per unit area being sieved is 1500g/m
2.The alumina substrate that is 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 tie point between metallic fiber links together owing at high temperature there is molecular thermalmotion, forms overall non-woven material.
It is 160mm that the non-woven material obtaining is cut into diameter, packs test oxidation furnace into.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.By its through cold rolling, hot rolling and rough after, obtain the metal wire material that diameter is 0.9mm.This metal wire rod is through surface treatment, encapsulation, compacting, boundling drawing, separation, winding process, and obtaining diameter is the PtPd metallic fiber of 0.062mm fasciculation.Filament is processed to the metallic fiber that growth degree is 5mm by cutting machine.It is that on 5 object sieves, metallic fiber drops on alumina substrate uniformly from sieve aperture that the metallic fiber of making early stage is transferred to aperture.Alumina base floor space is 1000mm × 1000mm, and the metallic fiber weight per unit area being sieved is 1500g/m
2.The alumina substrate that is 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 tie point between metallic fiber links together owing at high temperature there is molecular thermalmotion, 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 is only preferred embodiment of the present invention; not the present invention is done to any restriction, every any simple modification of above embodiment being done according to invention technical spirit, change and equivalent structure change, and all still belong in the protection domain of technical solution of the present invention.
Claims (9)
1. the nonwoven catalyst for nitric acid production, its preparation comprises: by boundling drawing technique, noble metal drawing is obtained to metallic fiber, metallic fiber is cut into short fiber, and then short fiber evenly tiles, and finally by the mode of sintering, noble metal fiber is made to non-woven material.
2. the nonwoven catalyst for nitric acid production, its preparation comprises: by boundling drawing technique, noble metal drawing is obtained to metallic fiber, metallic fiber is cut into short fiber, short fiber is evenly laid in sintering of catalyst substrate, finally by the mode of sintering, noble metal fiber is made to non-woven material.
3. according to claim 1 or nonwoven catalyst claimed in claim 2, wherein sintering of catalyst substrate is aluminium oxide.
4. according to claim 1 or nonwoven catalyst claimed in claim 2, wherein sintering temperature is 1000～1400 DEG C, and sintering time is 8～24 hours.
5. according to claim 1 or nonwoven catalyst claimed in claim 2, it is characterized in that before sintering, the short fiber evenly weight per unit area of tiling is 1000～2000g/m
2.
6. according to claim 1 or nonwoven catalyst claimed in claim 2, it is characterized in that short fiber again short fiber to be tiled by after 5-8 object sieve.
7. according to claim 1 or nonwoven catalyst claimed in claim 2, also it is characterized in that taking out method or cutting method is prepared metallic fiber by molten.
8. according to claim 1 or nonwoven catalyst claimed in claim 2, it is characterized in that noble metal is RtRh10, RtRh7, RtRh5, RtRh3.7Pd3.8 or PtPd.
9. according to claim 1 or nonwoven catalyst claimed in claim 2, the diameter that it is characterized in that metallic fiber is 0.040～0.090mm, and the length of the short fiber that metallic fiber cutting obtains is 5～10mm.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN101554585A (en) * | 2009-05-08 | 2009-10-14 | 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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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN101554585A (en) * | 2009-05-08 | 2009-10-14 | 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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Address after: 030006 6th floor, No.12 Kaifa lane, Taiyuan Xuefu Park, Shanxi comprehensive reform demonstration zone, Taiyuan City, Shanxi Province Patentee after: CNOOC (Shanxi) precious metal Co., Ltd Address before: 030006, No. six, Lane 12, Taiyuan high tech Zone, Shanxi, China Patentee before: CNOOC TAIYUAN PRECIOUS METALS Co.,Ltd. |