NO157651B - PROCEDURE FOR CATALYTIC PREPARATION OF LOWER NITROALKANES. - Google Patents
PROCEDURE FOR CATALYTIC PREPARATION OF LOWER NITROALKANES. Download PDFInfo
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- NO157651B NO157651B NO833234A NO833234A NO157651B NO 157651 B NO157651 B NO 157651B NO 833234 A NO833234 A NO 833234A NO 833234 A NO833234 A NO 833234A NO 157651 B NO157651 B NO 157651B
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- Prior art keywords
- catalyst
- nitric acid
- methane
- alkane
- ethane
- Prior art date
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- 238000000034 method Methods 0.000 title claims description 15
- 230000003197 catalytic effect Effects 0.000 title 1
- 239000003054 catalyst Substances 0.000 claims description 23
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 20
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 13
- 229910017604 nitric acid Inorganic materials 0.000 claims description 13
- 150000001335 aliphatic alkanes Chemical class 0.000 claims description 12
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 claims description 8
- 238000006396 nitration reaction Methods 0.000 claims description 8
- 150000003839 salts Chemical class 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 229910052751 metal Inorganic materials 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 5
- 125000004971 nitroalkyl group Chemical group 0.000 claims description 5
- 239000012808 vapor phase Substances 0.000 claims description 5
- 238000010790 dilution Methods 0.000 claims description 3
- 239000012895 dilution Substances 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 3
- 230000000737 periodic effect Effects 0.000 claims description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 2
- 229910052791 calcium Inorganic materials 0.000 claims description 2
- 239000011575 calcium Substances 0.000 claims description 2
- 229910052712 strontium Inorganic materials 0.000 claims description 2
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- 239000007789 gas Substances 0.000 description 7
- LYGJENNIWJXYER-UHFFFAOYSA-N nitromethane Chemical compound C[N+]([O-])=O LYGJENNIWJXYER-UHFFFAOYSA-N 0.000 description 6
- 239000003085 diluting agent Substances 0.000 description 5
- MCSAJNNLRCFZED-UHFFFAOYSA-N nitroethane Chemical compound CC[N+]([O-])=O MCSAJNNLRCFZED-UHFFFAOYSA-N 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 239000007788 liquid Substances 0.000 description 3
- 150000002739 metals Chemical class 0.000 description 3
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 3
- UOCLXMDMGBRAIB-UHFFFAOYSA-N 1,1,1-trichloroethane Chemical compound CC(Cl)(Cl)Cl UOCLXMDMGBRAIB-UHFFFAOYSA-N 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical class [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 2
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 2
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- JSZOAYXJRCEYSX-UHFFFAOYSA-N 1-nitropropane Chemical compound CCC[N+]([O-])=O JSZOAYXJRCEYSX-UHFFFAOYSA-N 0.000 description 1
- FGLBSLMDCBOPQK-UHFFFAOYSA-N 2-nitropropane Chemical compound CC(C)[N+]([O-])=O FGLBSLMDCBOPQK-UHFFFAOYSA-N 0.000 description 1
- 229910000619 316 stainless steel Inorganic materials 0.000 description 1
- 101100534229 Caenorhabditis elegans src-2 gene Proteins 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- -1 SC^ Chemical class 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 150000001299 aldehydes Chemical class 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- CREMABGTGYGIQB-UHFFFAOYSA-N carbon carbon Chemical compound C.C CREMABGTGYGIQB-UHFFFAOYSA-N 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 229910002090 carbon oxide Inorganic materials 0.000 description 1
- 150000001805 chlorine compounds Chemical class 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000003776 cleavage reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- OMBRFUXPXNIUCZ-UHFFFAOYSA-N dioxidonitrogen(1+) Chemical compound O=[N+]=O OMBRFUXPXNIUCZ-UHFFFAOYSA-N 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 239000003701 inert diluent Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 239000001294 propane Substances 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 230000007017 scission Effects 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- DHEQXMRUPNDRPG-UHFFFAOYSA-N strontium nitrate Inorganic materials [Sr+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O DHEQXMRUPNDRPG-UHFFFAOYSA-N 0.000 description 1
- 150000003464 sulfur compounds Chemical class 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
Description
Nitroalkaner er en viktig stabiliserende ingrediens som anvendes i 1 ,1 ,1 -trikloretan når dette brukes til damp-avfetting og kald-rensing. Alle fabrikanter rundt om i verden tilsetter nitrometan og/eller nitroetan til deres kommersielle 1,1,1-trikloretan-baserte løsningsmidler. Vanligvis blir nitroalkaner fremstilt ved dampfase-nitrering av et alkan med enten salpetersyre eller NC^. Det blir dannet en blanding av produkter på Nitroalkanes are an important stabilizing ingredient used in 1,1,1-trichloroethane when this is used for steam degreasing and cold cleaning. All manufacturers around the world add nitromethane and/or nitroethane to their commercial 1,1,1-trichloroethane-based solvents. Usually, nitroalkanes are prepared by vapor phase nitration of an alkane with either nitric acid or NC^. A mixture of products is formed on
grunn av karbon-karbon-spalting. Når således for eksempel pro-pan blir nitrert, inkluderer produktene 1-nitropropan, 2-nitropropan, nitroetan og nitrometan. På grunn av de oksydative forhold blir det også dannet andre oksygenholdige forbindelser, f.eks. aldehyder, syrer og karbonoksyder. Patenter som åpen-barer en slik fremgangsmåte, er U.S.-patenskrifter 2.844.634 og 2.905.724. due to carbon-carbon cleavage. Thus, for example, when propane is nitrated, the products include 1-nitropropane, 2-nitropropane, nitroethane, and nitromethane. Due to the oxidative conditions, other oxygen-containing compounds are also formed, e.g. aldehydes, acids and carbon oxides. Patents disclosing such a method are U.S. Patents 2,844,634 and 2,905,724.
Det er foreslått forbedringer av disse dampfase-nitreringer ved å anvende salpetersyre eller nitrogenoksyder sammen med oksy-generte svovel-forbindelser, f.eks. SC^ , ^SO^ (U.S.-patentskrift 3.272.874), og ved å utføre nitreringen i nærvær av ozon (U.S.-patentskrift 3.113.975). Improvements to these vapor phase nitrations have been proposed by using nitric acid or nitrogen oxides together with oxygenated sulfur compounds, e.g. SC^ , ^SO^ (U.S. Patent 3,272,874), and by performing the nitration in the presence of ozone (U.S. Patent 3,113,975).
Andre fremgangsmåter involverer nitrering av alkaner med nitrogenperoksyd (NC^^ i nærvær av oksygen (luft) under trykk ved 150 - 330°C (U.S.-patentskrift 3.780.115), omsetning av et alkan med salpetersyre i nærvær av et lavere alifatisk monokar-boksylsyreanhydrid for å danne en nitroester, med etterfølgende redusering av denne med et alkaliborhydrid for å danne nitro-alkanet (U.S.-patentskrift 3.706.808), og omsetning av organiske aminer med ozon (U.S.-patenskrift 3.377.387). Other methods involve nitration of alkanes with nitrogen peroxide (NC^^ in the presence of oxygen (air) under pressure at 150 - 330°C (U.S. Patent 3,780,115), reaction of an alkane with nitric acid in the presence of a lower aliphatic monocar- carboxylic anhydride to form a nitroester, with subsequent reduction of this with an alkali borohydride to form the nitro-alkane (U.S. Patent 3,706,808), and reaction of organic amines with ozone (U.S. Patent 3,377,387).
Det er nå blitt oppdaget at et lavere alkan kan omsettes It has now been discovered that a lower alkane can be converted
med salpetersyre i dampfase over en katalysator som er et salt eller oksyd av et metall fra gruppe II, for å gi et nitroalkan. with nitric acid in the vapor phase over a catalyst which is a salt or oxide of a Group II metal to give a nitroalkane.
Denne forbedrede fremgangsmåte for nitrering av alkaner, spesielt metan og etan, i dampfase innebærer anvendelse av en inert fortynningsgass, f.eks. nitrogen, og en katalysator som er et salt eller et oksyd av et metall fra gruppe II i det periodiske system, f.eks. CaC^ eller SrfNO^^- Katalysatoren kan være båret på en inert bærer, f.eks. aluminiumoksyd med lavt over-flateareal. Salpetersyren blir tilmåtet som væske og fordampet på katalysatoren. Det henvises forøvrig til patentkravene. Fremgangsmåten blir fortrinnsvis utført ved anvendelse av lavere alkaner, spesielt-metan og etan. Disse gasser blir fortrinnsvis blandet med et inert fortynningsmiddel så som nitrogen, argon, karbonmonoksyd eller karbondioksyd og ført over katalysatoren sammen med flytende salpetersyre som dermed fordampes. This improved process for the nitration of alkanes, especially methane and ethane, in the vapor phase involves the use of an inert dilution gas, e.g. nitrogen, and a catalyst which is a salt or an oxide of a metal from group II of the periodic table, e.g. CaC^ or SrfNO^^- The catalyst can be supported on an inert carrier, e.g. aluminum oxide with low surface area. The nitric acid is added as a liquid and evaporated on the catalyst. Reference is also made to the patent requirements. The method is preferably carried out using lower alkanes, especially methane and ethane. These gases are preferably mixed with an inert diluent such as nitrogen, argon, carbon monoxide or carbon dioxide and passed over the catalyst together with liquid nitric acid which is thus evaporated.
Gassene, men ikke salpetersyren, blir fortrinnsvis forhåndsoppvarmet til en temperatur på fra 200 til 400°C i avhengighet av det alkan som anvendes. Katalysator-sjiktet blir fortrinnsvis holdt ved en temperatur på fra 325 til 390°C for etan, og 380 til 425°C for metan. Mol-forholdet for det anvendte alkan er ønskelig fra 0,5 til 2 mol pr. mol salpetersyre. Det fore-trukne forhold er 1 til 1 . The gases, but not the nitric acid, are preferably preheated to a temperature of from 200 to 400°C depending on the alkane used. The catalyst layer is preferably maintained at a temperature of from 325 to 390°C for ethane, and 380 to 425°C for methane. The molar ratio for the alkane used is preferably from 0.5 to 2 mol per moles of nitric acid. The preferred ratio is 1 to 1.
Katalysatoren er fortrinnsvis salter av metaller fra gruppe II i det periodiske system, nemlig magnesium, kalsium, strontium og barium. Salter av disse metaller, innbefattet kloridene, salfåtene og nitratene, kan anvendes. Oksydene av de samme metal-lene er også nyttige. The catalyst is preferably salts of metals from group II in the periodic table, namely magnesium, calcium, strontium and barium. Salts of these metals, including the chlorides, sulfates and nitrates, can be used. The oxides of the same metals are also useful.
Enten oksydene eller saltene kan legges på en inert bærer og anvendes på denne måte. Fremgangsmåter for fremstilling av bårne katalysatorer er velkjent på fagområdet. Bæreren kan for eksempel impregneres ved nedsenking i en saltløsning eller ved sprøy-ting av løsningen, eller oppslemmingen når det dreier seg om oksyder eller uløselige salter, på bæreren. Either the oxides or the salts can be placed on an inert support and used in this way. Methods for producing supported catalysts are well known in the art. The carrier can, for example, be impregnated by immersion in a salt solution or by spraying the solution, or the slurry in the case of oxides or insoluble salts, onto the carrier.
De trykk som anvendes ved fremgangsmåten er ønskelig fra 6,9 til 207 kPa målt, og fortrinnsvis fra 41,4 til 68,9 kPa målt. The pressures used in the method are desirably from 6.9 to 207 kPa measured, and preferably from 41.4 to 68.9 kPa measured.
På grunn av den eksoterme natur og den brann-risiko som er involvert i denne omsetning, er det meget ønskelig å anvende et fortynningsmiddel. Spesiell kjøling og brann-forebygging må inn-øves dersom det ikke anvendes noe fortynningsmiddel. Fortynnings-midlet blir vanligvis anvendt i en mengde på ca. 50-60% av det totale volum av gass-tilmating, d.v.s. alkanet og salpetersyren (som damp) pluss fortynningsmiddel. Det er foretrukket å anvende minst ca. 54% fortynningsmiddel for å komme utenfor brennbarhets-området. Due to the exothermic nature and the fire risk involved in this transaction, it is highly desirable to use a diluent. Special cooling and fire prevention must be practiced if no diluent is used. The diluent is usually used in an amount of approx. 50-60% of the total volume of gas feed, i.e. the alkane and the nitric acid (as vapor) plus diluent. It is preferred to use at least approx. 54% diluent to get outside the flammability range.
Anvendelsen av en katalysator gjør det mulig å utføre denne kjente nitrerings-reaksjon ved lavere temperaturer og med bedre omdannelser og utbytter enn det som er kjent på området. The use of a catalyst makes it possible to carry out this known nitration reaction at lower temperatures and with better conversions and yields than is known in the field.
Et eksempel på en fremgangsmåte for fremstilling av katalysatoren, er som følger: An example of a method for producing the catalyst is as follows:
Fremstilling Manufacturing
En mengde på 300 g av aluminiumoksyd (kuler på 4,7 mm med A quantity of 300 g of aluminum oxide (balls of 4.7 mm with
et overflate-areal på 0,02 - 0,2 m /g) av kommersiell kvalitet ble nedsenket i en løsning av 100 g SrfNO^^ i 250 ml vann. Overskudd av løsningsmiddel ble avdampet, og den fuktige bærer ble oppvarmet under omrøring i en panne ved ca. 100°C i én time, og deretter oppvarmet i en ovn ved 150°C i 2 timer for å tørke katalysatoren. Den endelige katalysator inneholdt 22,2 vekt% a surface area of 0.02 - 0.2 m /g) of commercial quality was immersed in a solution of 100 g of SrfNO^^ in 250 ml of water. Excess solvent was evaporated, and the moist carrier was heated with stirring in a pan at approx. 100°C for one hour, and then heated in an oven at 150°C for 2 hours to dry the catalyst. The final catalyst contained 22.2 wt%
med Sr(N03)2. with Sr(N03)2.
Anvendelse av katalysatoren Use of the catalyst
Eksempler 1- 4 Examples 1-4
En mengde på 150 cm<3> av den ovenfor fremstilte katalysator ble anbrakt i en 45,7 x 25,4 mm rør- (316 rustfritt stål) reaktor. Røret ble oppvarmet i et fluidisert sand-sjikt til en temperatur på 425°C, og en blanding av metan og nitrogen i et forhold på A 150 cm<3> amount of the above prepared catalyst was placed in a 45.7 x 25.4 mm tubular (316 stainless steel) reactor. The tube was heated in a fluidized sand bed to a temperature of 425°C, and a mixture of methane and nitrogen in a ratio of
1/2 ble forhåndsoppvarmet til ca. 250°C og ført gjennom røret ved et trykk på 48,3 kPa målt. Konsentrert flytende salpetersyre uten noen som helst forhåndsoppvarming ble matet inn i gass-strømmen like over katalysator-sjiktet. Strømnings-hastighetene var 3200 ml/min. for nitrogen, 0,0625 gmol/min. for metan og 0,0600 gmol/min. for HN03, og kontakt-tiden (K.T.) var 0,7 sekund. Utstrømnings-gassene ble matet til en avkjølt vann-gassvasker (10°C). Metan-omdannelsen var 8,2%, og selektiviteten (sel.) for nitrometan (NM) var 41,1%. Produktiviteten (prod.) ble beregnet til 1280 kg/dag/m3 katalysator. 1/2 was preheated to approx. 250°C and passed through the pipe at a pressure of 48.3 kPa measured. Concentrated liquid nitric acid without any preheating was fed into the gas stream just above the catalyst bed. The flow rates were 3200 ml/min. for nitrogen, 0.0625 gmol/min. for methane and 0.0600 gmol/min. for HN03, and the contact time (K.T.) was 0.7 second. The effluent gases were fed to a cooled water gas scrubber (10°C). The methane conversion was 8.2%, and the selectivity (sel.) for nitromethane (NM) was 41.1%. The productivity (prod.) was calculated at 1280 kg/day/m3 of catalyst.
Ved anvendelse av samme katalysator og reaktor, med samme reaktor- og foroppvarmings-temperaturer, ble det anvendt forskjellige tilmatingshastigheter og kontakt-tider. Disse resultater er vist i tabell I. When using the same catalyst and reactor, with the same reactor and preheating temperatures, different feed rates and contact times were used. These results are shown in Table I.
Eksempler 5- 8 Examples 5-8
En katalysator-baerer av samme aliminiumoksyd som ble anvendt i de foregående eksempler, ble belastet med 25,8% SrC^ på samme måte som ovenfor. Etan ble anvendt i tilmåtingen istedenfor metan, og tilmåtingen ble forhåndsoppvarmet til 195°C og omsatt ved 335°C. Både nitrometan (NM) og nitroetan (NE) ble oppnådd som produkter. Strømnings-hastigheter, kontakt-tider (K.T.) og resultater er vist i tabell II. A catalyst carrier of the same alumina used in the preceding examples was loaded with 25.8% SrC₂ in the same manner as above. Ethane was used in the reaction instead of methane, and the reaction was preheated to 195°C and reacted at 335°C. Both nitromethane (NM) and nitroethane (NE) were obtained as products. Flow rates, contact times (K.T.) and results are shown in Table II.
Eksempler 9- 11 Examples 9-11
På samme måte som ovenfor ble en katalysator av CaC^ på en kuleformet aluminiumoksyd-bærer (6,3 mm i diameter og et overflate-areal på 0,03 m 2/g) innført i 1219 mm x 19 mm rørformet reaktor av rustfritt stål. Foroppvarmingstemperaturen i eksemplene 9 og 10 var 200°C, og reaktor-temperaturene var henholdsvis 355 og 348°C. In the same manner as above, a catalyst of CaC^ on a spherical alumina support (6.3 mm in diameter and a surface area of 0.03 m 2 /g) was introduced into the 1219 mm x 19 mm stainless steel tubular reactor. . The preheating temperature in examples 9 and 10 was 200°C, and the reactor temperatures were 355 and 348°C, respectively.
I eksempel 11 ble det forhåndsoppvarmet til 230°C og omsatt ved 360°C. Etan ble tilmåtet i eksemplene 9 og 10, mens metan ble tilmåtet i eksempel 11. Tilmatings-hastigheter, kontakt-tider og oppnådde resultater er angitt i tabell III. In example 11, it was preheated to 230°C and reacted at 360°C. Ethane was allowed in Examples 9 and 10, while methane was allowed in Example 11. Feed rates, contact times and results obtained are indicated in Table III.
Eksempler 12- 14 Examples 12-14
I disse eksempler (ved anvendelse av samme reaktor som i eksemplene 9-11 ovenfor) ble det anvendt forskjellige forhold mellom etan og salpetersyre. En forhåndsoppvarmings-temperatur på 280°C ble anvendt i hvert eksempel, og reaktor-temperaturene var henholdsvis 385, 390 og 393°C for eksemplene 12, 13 og 14. Den anvendte katalysator var 150 ml av vannfritt CaC^» mesh nr. In these examples (using the same reactor as in examples 9-11 above) different ratios of ethane and nitric acid were used. A preheat temperature of 280°C was used in each example, and the reactor temperatures were 385, 390 and 393°C for Examples 12, 13 and 14, respectively. The catalyst used was 150 ml of anhydrous CaCl 2 mesh no.
5. Parametere or resultater er vist i tabell IV. 5. Parameters or results are shown in table IV.
Claims (8)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| NO833234A NO157651C (en) | 1983-09-09 | 1983-09-09 | PROCEDURE FOR CATALYTIC PREPARATION OF LOWER NITROALKANES. |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| NO833234A NO157651C (en) | 1983-09-09 | 1983-09-09 | PROCEDURE FOR CATALYTIC PREPARATION OF LOWER NITROALKANES. |
Publications (3)
| Publication Number | Publication Date |
|---|---|
| NO833234L NO833234L (en) | 1985-03-11 |
| NO157651B true NO157651B (en) | 1988-01-18 |
| NO157651C NO157651C (en) | 1988-04-27 |
Family
ID=19887226
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| NO833234A NO157651C (en) | 1983-09-09 | 1983-09-09 | PROCEDURE FOR CATALYTIC PREPARATION OF LOWER NITROALKANES. |
Country Status (1)
| Country | Link |
|---|---|
| NO (1) | NO157651C (en) |
-
1983
- 1983-09-09 NO NO833234A patent/NO157651C/en unknown
Also Published As
| Publication number | Publication date |
|---|---|
| NO157651C (en) | 1988-04-27 |
| NO833234L (en) | 1985-03-11 |
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