CN106927514A - A kind of method for preparing nitrosyl nitric acid ruthenium - Google Patents
A kind of method for preparing nitrosyl nitric acid ruthenium Download PDFInfo
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- CN106927514A CN106927514A CN201710165689.7A CN201710165689A CN106927514A CN 106927514 A CN106927514 A CN 106927514A CN 201710165689 A CN201710165689 A CN 201710165689A CN 106927514 A CN106927514 A CN 106927514A
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- nitric acid
- ruthenium
- acid ruthenium
- metal
- nitrosyl nitric
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- YLPJWCDYYXQCIP-UHFFFAOYSA-N nitroso nitrate;ruthenium Chemical compound [Ru].[O-][N+](=O)ON=O YLPJWCDYYXQCIP-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims abstract description 21
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 51
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000007787 solid Substances 0.000 claims abstract description 17
- 238000010438 heat treatment Methods 0.000 claims abstract description 10
- 238000010992 reflux Methods 0.000 claims abstract description 10
- 229910001927 ruthenium tetroxide Inorganic materials 0.000 claims abstract description 6
- KEAYESYHFKHZAL-UHFFFAOYSA-N Sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000007788 liquid Substances 0.000 claims description 8
- 238000001354 calcination Methods 0.000 claims description 7
- 238000000605 extraction Methods 0.000 claims description 7
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 6
- 229910017604 nitric acid Inorganic materials 0.000 claims description 5
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Substances [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 claims description 5
- AZFNGPAYDKGCRB-XCPIVNJJSA-M [(1s,2s)-2-amino-1,2-diphenylethyl]-(4-methylphenyl)sulfonylazanide;chlororuthenium(1+);1-methyl-4-propan-2-ylbenzene Chemical compound [Ru+]Cl.CC(C)C1=CC=C(C)C=C1.C1=CC(C)=CC=C1S(=O)(=O)[N-][C@@H](C=1C=CC=CC=1)[C@@H](N)C1=CC=CC=C1 AZFNGPAYDKGCRB-XCPIVNJJSA-M 0.000 claims description 4
- 235000010289 potassium nitrite Nutrition 0.000 claims description 4
- 239000004304 potassium nitrite Substances 0.000 claims description 4
- GQPLMRYTRLFLPF-UHFFFAOYSA-N nitrous oxide Inorganic materials [O-][N+]#N GQPLMRYTRLFLPF-UHFFFAOYSA-N 0.000 claims description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 2
- 229910052708 sodium Inorganic materials 0.000 claims description 2
- 235000010288 sodium nitrite Nutrition 0.000 claims description 2
- 239000000843 powder Substances 0.000 abstract description 22
- 229910052751 metal Inorganic materials 0.000 abstract description 16
- 239000002184 metal Substances 0.000 abstract description 16
- 239000003054 catalyst Substances 0.000 abstract description 15
- 229910052573 porcelain Inorganic materials 0.000 abstract description 6
- 238000002360 preparation method Methods 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 4
- 229910052736 halogen Inorganic materials 0.000 abstract description 2
- 150000002367 halogens Chemical class 0.000 abstract description 2
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 30
- 229910052707 ruthenium Inorganic materials 0.000 description 30
- 239000002253 acid Substances 0.000 description 11
- 238000010521 absorption reaction Methods 0.000 description 10
- 239000007789 gas Substances 0.000 description 9
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical group O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 8
- 239000000463 material Substances 0.000 description 7
- 230000000694 effects Effects 0.000 description 5
- 230000008676 import Effects 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- 238000003786 synthesis reaction Methods 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- -1 nitryl nitric acid ruthenium Chemical compound 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 230000035484 reaction time Effects 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- 241000370738 Chlorion Species 0.000 description 2
- 229910019891 RuCl3 Inorganic materials 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000002329 infrared spectrum Methods 0.000 description 2
- 230000000977 initiatory effect Effects 0.000 description 2
- 231100000572 poisoning Toxicity 0.000 description 2
- 230000000607 poisoning effect Effects 0.000 description 2
- 238000012805 post-processing Methods 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- YBCAZPLXEGKKFM-UHFFFAOYSA-K ruthenium(iii) chloride Chemical compound [Cl-].[Cl-].[Cl-].[Ru+3] YBCAZPLXEGKKFM-UHFFFAOYSA-K 0.000 description 2
- 238000010189 synthetic method Methods 0.000 description 2
- 229910009112 xH2O Inorganic materials 0.000 description 2
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 239000012327 Ruthenium complex Substances 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- KFIKNZBXPKXFTA-UHFFFAOYSA-N dipotassium;dioxido(dioxo)ruthenium Chemical compound [K+].[K+].[O-][Ru]([O-])(=O)=O KFIKNZBXPKXFTA-UHFFFAOYSA-N 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000005672 electromagnetic field Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 231100001261 hazardous Toxicity 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 238000007567 mass-production technique Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 150000003304 ruthenium compounds Chemical class 0.000 description 1
- BIXNGBXQRRXPLM-UHFFFAOYSA-K ruthenium(3+);trichloride;hydrate Chemical compound O.Cl[Ru](Cl)Cl BIXNGBXQRRXPLM-UHFFFAOYSA-K 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G55/00—Compounds of ruthenium, rhodium, palladium, osmium, iridium, or platinum
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a kind of method for preparing nitrosyl nitric acid ruthenium.By metal Ru powder, vanadic anhydride (V2O5) be placed in porcelain crucible, it is then placed in micro-wave oven.First certain hour is calcined using 1000W power microwaves, then certain hour is calcined with 1400W ~ 1600W again, is passed through air and metal Ru powder is aoxidized, produce ruthenium tetroxide gas, collect gas and be passed into salpeter solution, then add natrium nitrosum heating and condensing reflux；By the prepared solution containing nitrosyl nitric acid ruthenium, add appropriate absolute ether to be extracted, then evaporate ether and obtain nitrosyl nitric acid ruthenium solid；The method raw material is easy to get, and product yield is high, simple to operate, is easy to treatment, and the solid nitrosyl nitric acid ruthenium for obtaining is free of halogen, and product purity is high, can be directly used for the preparation of catalyst.
Description
Technical field
The present invention relates to a kind of synthetic method of noble ruthenium catalyst, specifically one kind directly prepares Asia with metal Ru powder
The method of nitryl nitric acid ruthenium.
Background technology
Load ruthenium catalyst has good catalysis activity, in petrochemical industry, organic synthesis, environmental project, pharmacy work
The fields such as journey have a wide range of applications.Carrier, auxiliary agent and ruthenium activity presoma are influence load ruthenium catalyst catalytic performances
Principal element.The electronic structure of ruthenium is 4d75s1, there is most oxidation state in all elements in the periodic table of elements, it is each
Plant electronic structure has various geometries again, for the ruthenium complex for synthesizing various provides good basis.Supported ruthenium is catalyzed
Active component ruthenium is introduced by ruthenium precursor compound in agent.Up to the present, before for preparing load ruthenium catalyst
Driving body mainly has hydrate ruthenium trichloride (RuCl3·nH2O), ruthenium (Ru of ten dicarbapentaborane three3(CO)12), nitrosyl nitric acid ruthenium (Ru (NO)
(NO3)3), potassium ruthenate (K2RuO4) etc..In the various compounds of ruthenium, RuCl3·nH2O is most common ruthenium compound, its property
Matter stabilization, cheap, water-soluble and part organic solvent, is widely used in preparing load ruthenium catalyst.But due to this
Contain substantial amounts of chlorion in the active presoma of kind, the chlorion remained on catalyst in catalyst preparation process cannot be complete
Remove, there is certain inhibitory action to catalytic performance；Meanwhile, research finds not halogen-containing ruthenium precursor compound such as Ru
(NO)(NO3)3And Ru3(CO)12It is the preferable presoma for preparing load ruthenium catalyst, but the price of this kind of compound is higher,
Hinder application in the industry.
It is nitrosyl and it is the salpeter solution of nitrosyl nitric acid ruthenium that the nitrosyl nitric acid ruthenium of commercial type is most
Introduce incomplete, cause the nitrosyl nitric acid ruthenium of preparation unstable, only in acid condition could stable existence, be condensed into solid
The nitrosyl nitric acid ruthenium of part can resolve into metal Ru again after body.And this solution acidity is higher, it is unfavorable for that supported ruthenium is urged
The preparation of agent, while also influencing whether the catalysis activity of catalyst.So replacing nitrosyl with solid nitrosyl nitric acid ruthenium
Nitric acid ruthenium solution is used to prepare the active presoma of load ruthenium catalyst, increasingly attracts attention.Reason can be according to need
The concentration wanted prepares the dipping solution of the ruthenium of nitric acid containing nitrosyl, it is also possible to the pH values needed for preparing catalyst with nitric acid regulation, more
Be conducive to the preparation of load ruthenium catalyst.Therefore, for reduces cost, the mass production technique of solid nitrosyl nitric acid ruthenium
Research has important practical significance.
Microwave is the technology for growing up early 1920s, is that material exists different from general conventional heating mode
Cause " body heating " or " interior heating " in electromagnetic field by dielectric loss.Communication aspect is initially applied to, because it has very
Good penetrability and selectivity, firing rate is fast, and material mode of heating is heated for body, can solve traditional heating mode generation
" cold " center " problem, while the absorbable microwave energy of the material that is heated, the heating rate of each several part is identical in material, in the absence of temperature
Gradient, so material is heated than more uniform in decomposable process.Meanwhile, microwave calcination has operation and equipment simple, defends safely
It is raw, it is easy to control, technological process is short, small, efficient energy-saving is polluted, improve working conditions, the features such as save floor space, microwave adds
Thermal technology has been widely used for the industries such as food, light textile, medicine, agricultural.
The content of the invention
It is an object of the present invention to provide a kind of synthetic method that nitrosyl nitric acid ruthenium is directly prepared with metal Ru powder, the synthesis side
Method has relatively big difference with existing method；Because existing method is usually that ruthenium is obtained into RuCl by series of steps such as alkali fusions3·
xH2O or RuO4Then it is that the effect such as nitric acid obtains Ru (NO) (NO Deng intermediate3)3Salpeter solution so that synthetic reaction compared with
Complexity, post processing is cumbersome, not only needs temperature very high, in addition it is also necessary to which longer time is, it is necessary to purity oxygen or ozone conduct
Oxidant, operating environment is than relatively hazardous.Meanwhile, chloride can be also introduced, so as to cause to contain impurity chlorine in product, easily cause
Catalyst poisoning；And the present invention uses new method to use metal Ru powder for initiation material, Asia is directly prepared using microwave calcination method
Nitryl nitric acid ruthenium, not only avoid prolonged high temperature, flammable gas required during reaction, such as purity oxygen, bring
Danger, and synthesis step is simplified, reduce raw material dosage, hence it is evident that shorten the reaction time, improve reaction efficiency.
The method is raw material using metal Ru powder, prepares nitrosyl nitric acid ruthenium；Simplify synthesis step and post processing, hence it is evident that
The reaction time is shortened, reaction efficiency is improve.
The technical solution adopted by the present invention is：Metal Ru, vanadic anhydride are placed in crucible, are put into micro-wave oven, first
Microwave calcination is carried out under 1000W power, air is passed through, microwave calcination, air pair are then carried out under 1400W ~ 1600W power
Metal Ru is aoxidized, and produces ruthenium tetroxide gas, is collected gas and is passed into salpeter solution, then adds nitrous
Sour sodium or potassium nitrite heating and condensing reflux；By the prepared solution containing nitrosyl nitric acid ruthenium, absolute ether is added to be extracted
Take, collect ether extraction liquid, then obtain nitrosyl nitric acid ruthenium solid after ether is evaporated；Its chemical reaction route be：
The metal Ru is 6~8 with the mol ratio of vanadic anhydride:1, the flow velocity of air is 4000 ~ 5000 m3·h-1。
The metal Ru is 1 with the mol ratio of nitric acid:4~5, the mass concentration of salpeter solution is 45% ~ 60%.
The metal Ru is 1 with the mol ratio of natrium nitrosum or potassium nitrite:1.5 ~ 2, the time is heated to reflux for 6 ~ 8h.
The 1000W power microwaves calcine 15 ~ 20min, and 1400W ~ 1600W power microwaves calcine 60 ~ 100min.
Compared with prior art, the beneficial effects are mainly as follows：
Existing method is usually that ruthenium is obtained into RuCl by series of steps such as alkali fusions3·xH2O or RuO4Deng intermediate, Ran Hou
Ru (NO) (NO is obtained in the effect such as nitric acid3)3Salpeter solution so that synthetic reaction is more complicated, post-process it is cumbersome, not only need
Temperature very high, in addition it is also necessary to longer time.Meanwhile, chloride can be also introduced, so as to cause to contain impurity chlorine in product, hold
Easily cause catalyst poisoning；And the present invention directly prepares nitrous with metal Ru powder using the method for microwave calcination as initiation material
Acyl nitric acid ruthenium, not only avoid long-time high temperature, flammable gas required during reaction, such as purity oxygen, the danger for bringing,
And synthesis step is simplified, and reduce raw material dosage, hence it is evident that shorten the reaction time, improve reaction efficiency.
Specific embodiment
With reference to specific embodiment, the present invention is described further, but protection scope of the present invention is not limited in
This.
Embodiment 1：
Weigh the ruthenium powder of 5.0 g, the vanadic anhydride of 1.23g to be placed in porcelain crucible, be then placed in micro-wave oven；It is passed through air,
Holding air velocity is 4000m3·h-1, 15min is calcined under 1000W microwave powers, then calcined under 1400W microblogging power
100min, aoxidizes to metal Ru powder；The RuO that will be produced4It is 45% that gas imports 3 equipped with 27.7g mass concentrations successively
Salpeter solution absorption bottle in, and control the temperature of salpeter solution for 70 DEG C, obtain Ru (NO3)3Acid solution.
By Ru (NO obtained above3)3Acid solution be all placed in neck round bottom flask, be slowly added to 5.12g's
NaNO2Powder, stirs and heating and condensing reflux 6h under the conditions of 80 DEG C, and solution colour gradually becomes dark red black, cools down molten
Liquid, and be placed in separatory funnel, add the absolute ether of 83mL to extract 3 times, ether extraction liquid is collected, it is spin-dried for diethyl ether solution
Yellow-brown solid 15.0g is obtained, calculated yield is 95.6%.Using KBr compressing tablets, the infrared of solid nitrosyl nitric acid ruthenium is determined
Spectrogram.In 1917.18 cm-1There is the characteristic absorption peak of ruthenium and nitrosyl radical (Ru-NO) coordination in place, with Ru (NO) (NO3)3
Feature structure parameter matches.
Embodiment 2：
Weigh the ruthenium powder of 10.0 g, the vanadic anhydride of 2.4g to be placed in porcelain crucible, be then placed in micro-wave oven, be passed through air,
Holding air velocity is 4500m3·h-1, 17min is calcined under 1000W microwave powers, then calcined under 1500W microwave powers
80min, aoxidizes to metal Ru powder.The RuO that will be produced4It is 50% that gas imports 3 equipped with 56.0g mass concentrations successively
In the absorption bottle of salpeter solution, and control the temperature of salpeter solution for 70 DEG C, obtain Ru (NO3)3Acid solution.
By Ru (NO obtained above3)3Acid solution be all placed in neck round bottom flask, be slowly added to the KNO of 14.7g2
Powder, stirs and 7h is heated to reflux under the conditions of 80 DEG C, and solution colour gradually becomes dark red black, cools down solution, and put
In separatory funnel, add the absolute ether of 168mL to extract 4 times, collect ether extraction liquid, be spin-dried for diethyl ether solution and obtain brown color
Solid 30.20g, calculated yield is 96.3%.Using KBr compressing tablets, the infrared spectrogram of solid nitrosyl nitric acid ruthenium is determined.
1920.75 cm-1There is the characteristic absorption peak of ruthenium and nitrosyl radical (Ru-NO) coordination in place, with Ru (NO) (NO3)3Feature structure
Parameter matches.
Embodiment 3：
Weigh the ruthenium powder of 15.0 g, the vanadic anhydride of 3.86g to be placed in porcelain crucible, be then placed in micro-wave oven, be passed through air,
Holding air velocity is 5000m3·h-1, 19min is calcined under 1000W microwave powers, then calcined under 1600W microblogging power
60min, aoxidizes to metal Ru powder.The RuO that will be produced4It is 55% that gas imports 3 equipped with 85.1g mass concentrations successively
In the absorption bottle of salpeter solution, and control the temperature of salpeter solution for 70 DEG C, obtain Ru (NO3)3Acid solution.
By Ru (NO obtained above3)3Acid solution be all placed in neck round bottom flask, be slowly added to 20.5g's
NaNO2Powder, stirs and 8h is heated to reflux under the conditions of 80 DEG C, and solution colour gradually becomes dark red black, cools down solution, and will
It is placed in separatory funnel, adds the absolute ether of 255mL to extract 3 times, collects ether extraction liquid, is spin-dried for diethyl ether solution and is obtained palm fibre
Yellow solid 46.47g, calculated yield is 98.7%.Using KBr compressing tablets, the infrared spectrum of solid nitrosyl nitric acid ruthenium is determined
Figure.In 1915.33 cm-1There is the characteristic absorption peak of ruthenium and nitrosyl radical (Ru-NO) coordination in place, with Ru (NO) (NO3)3Feature
Structural parameters match.
Embodiment 4：
Weigh the ruthenium powder of 20.0 g, the vanadic anhydride of 6.0g to be placed in porcelain crucible, be then placed in micro-wave oven, be passed through air,
Holding air velocity is 5000m3·h-1, 20min is calcined under 1000W microwave powers, then calcined under 1600W microblogging power
60min, aoxidizes to metal Ru powder.The RuO that will be produced4It is 55% that gas imports 3 equipped with 102.1g mass concentrations successively
Salpeter solution absorption bottle in, and control the temperature of salpeter solution for 70 DEG C, obtain Ru (NO3)3Acid solution.
By Ru (NO obtained above3)3Acid solution be all placed in neck round bottom flask, be slowly added to 29.56g's
KNO2Powder, stirs and 8h is heated to reflux under the conditions of 80 DEG C, and solution colour gradually becomes dark red black, cools down solution, and will
It is placed in separatory funnel, adds the absolute ether of 306mL to extract 3 ~ 4 times, collects ether extraction liquid, is spin-dried for diethyl ether solution and is obtained
Yellow-brown solid 60.3g, calculated yield is 96.1%.Using KBr compressing tablets, the infrared spectrum of solid nitrosyl nitric acid ruthenium is determined
Figure.In 1914.86 cm-1There is the characteristic absorption peak of ruthenium and nitrosyl radical (Ru-NO) coordination in place, with Ru (NO) (NO3)3Feature
Structural parameters match.
Embodiment 5：
Weigh the ruthenium powder of 25.0 g, the vanadic anhydride of 7.51g to be placed in porcelain crucible, be then placed in micro-wave oven.It is passed through air,
Holding air velocity is 5000m3·h-1, 20min is calcined under 1000W microwave powers, then calcined under 1600W microblogging power
60min, aoxidizes to metal Ru powder.The RuO that will be produced4It is 60% that gas imports 3 equipped with 130.0g mass concentrations successively
Salpeter solution absorption bottle in, and control the temperature of salpeter solution for 70 DEG C, obtain Ru (NO3)3Acid solution.
By Ru (NO obtained above3)3Acid solution be all placed in neck round bottom flask, be slowly added to 34.16g's
NaNO2Powder, stirs and 8h is heated to reflux under the conditions of 80 DEG C, and solution colour gradually becomes dark red black, cools down solution, and will
It is placed in separatory funnel, adds the absolute ether of 390mL to extract 3 ~ 4 times, collects ether extraction liquid, is spin-dried for diethyl ether solution and is obtained
Yellow-brown solid 76.03g, calculated yield is 96.9%.Using KBr compressing tablets, the infrared light of solid nitrosyl nitric acid ruthenium is determined
Spectrogram.In 1918.81 cm-1There is the characteristic absorption peak of ruthenium and nitrosyl radical (Ru-NO) coordination in place, with Ru (NO) (NO3)3It is special
Structural parameters are levied to match.
Claims (5)
1. a kind of method for preparing nitrosyl nitric acid ruthenium, it is characterised in that：Metal Ru, vanadic anhydride are placed in crucible, first
Microwave calcination is carried out under 1000W power, air is passed through, microwave calcination, air pair are then carried out under 1400W ~ 1600W power
Metal Ru is aoxidized, and produces ruthenium tetroxide gas, is collected gas and is passed into salpeter solution, then adds nitrous
Sour sodium or potassium nitrite heating and condensing reflux；By the prepared solution containing nitrosyl nitric acid ruthenium, absolute ether is added to be extracted
Take, collect ether extraction liquid, then obtain nitrosyl nitric acid ruthenium solid after ether is evaporated.
2. the method for preparing nitrosyl nitric acid ruthenium according to claim 1, it is characterised in that：Metal Ru and vanadic anhydride
Mol ratio be 6~8:1, the flow velocity of air is 4000 ~ 5000m3·h-1。
3. the method for preparing nitrosyl nitric acid ruthenium according to claim 1, it is characterised in that：Metal Ru is rubbed with nitric acid
You are than being 1:4~5, the mass concentration of salpeter solution is 45% ~ 60%.
4. the method for preparing nitrosyl nitric acid ruthenium according to claim 1, it is characterised in that：Metal Ru and natrium nitrosum or
The mol ratio of potassium nitrite is 1:1.5 ~ 2, the time is heated to reflux for 6 ~ 8h.
5. the method for preparing nitrosyl nitric acid ruthenium according to claim 1, it is characterised in that：1000W power microwaves are calcined
15 ~ 20min, 1400W ~ 1600W power microwaves calcine 60 ~ 100min.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060245999A1 (en) * | 2005-04-29 | 2006-11-02 | Cabot Corporation | High surface area tetragonal zirconia and processes for synthesizing same |
| CN102616868A (en) * | 2012-03-05 | 2012-08-01 | 阳光凯迪新能源集团有限公司 | Method for preparing solid nitrosyl ruthenium nitrate by using dead catalyst containing ruthenium |
| CN104556250A (en) * | 2014-12-19 | 2015-04-29 | 昆明珀玺金属材料有限公司 | New method for preparing ruthenium nitrosyl nitrate solution or pure crystal |
-
2017
- 2017-03-20 CN CN201710165689.7A patent/CN106927514B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060245999A1 (en) * | 2005-04-29 | 2006-11-02 | Cabot Corporation | High surface area tetragonal zirconia and processes for synthesizing same |
| CN102616868A (en) * | 2012-03-05 | 2012-08-01 | 阳光凯迪新能源集团有限公司 | Method for preparing solid nitrosyl ruthenium nitrate by using dead catalyst containing ruthenium |
| CN104556250A (en) * | 2014-12-19 | 2015-04-29 | 昆明珀玺金属材料有限公司 | New method for preparing ruthenium nitrosyl nitrate solution or pure crystal |
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