DE765305C - - Google Patents
Info
- Publication number
- DE765305C DE765305C DENDAT765305D DE765305DA DE765305C DE 765305 C DE765305 C DE 765305C DE NDAT765305 D DENDAT765305 D DE NDAT765305D DE 765305D A DE765305D A DE 765305DA DE 765305 C DE765305 C DE 765305C
- Authority
- DE
- Germany
- Prior art keywords
- slag
- catalyst
- catalysts
- dehydrogenation
- treated
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 239000003054 catalyst Substances 0.000 claims description 17
- 239000002893 slag Substances 0.000 claims description 12
- 238000006356 dehydrogenation reaction Methods 0.000 claims description 5
- 238000003776 cleavage reaction Methods 0.000 claims description 4
- 230000003197 catalytic Effects 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 2
- 229910052736 halogen Inorganic materials 0.000 claims description 2
- 150000002367 halogens Chemical class 0.000 claims description 2
- 150000002430 hydrocarbons Chemical class 0.000 claims description 2
- 229910000805 Pig iron Inorganic materials 0.000 claims 1
- 150000007513 acids Chemical class 0.000 claims 1
- 238000000034 method Methods 0.000 claims 1
- 229910000499 pig iron Inorganic materials 0.000 claims 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- 239000003921 oil Substances 0.000 description 5
- 150000001336 alkenes Chemical class 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 150000002739 metals Chemical class 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 230000002378 acidificating Effects 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminum Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 239000000460 chlorine Substances 0.000 description 3
- 229910052801 chlorine Inorganic materials 0.000 description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N HCl Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- IJDNQMDRQITEOD-UHFFFAOYSA-N butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 description 2
- 239000001273 butane Substances 0.000 description 2
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium monoxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- PWHULOQIROXLJO-UHFFFAOYSA-N manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 2
- 229910052748 manganese Inorganic materials 0.000 description 2
- 239000011572 manganese Substances 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 229910000640 Fe alloy Inorganic materials 0.000 description 1
- 229910000990 Ni alloy Inorganic materials 0.000 description 1
- TVMXDCGIABBOFY-UHFFFAOYSA-N Octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- HOWJQLVNDUGZBI-UHFFFAOYSA-N butane;propane Chemical compound CCC.CCCC HOWJQLVNDUGZBI-UHFFFAOYSA-N 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 150000001805 chlorine compounds Chemical class 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 229910052570 clay Inorganic materials 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 229910052803 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000004673 fluoride salts Chemical class 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000010687 lubricating oil Substances 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 239000003863 metallic catalyst Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 230000001376 precipitating Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 1
- 239000001294 propane Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- KEAYESYHFKHZAL-UHFFFAOYSA-N sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 235000015096 spirit Nutrition 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- -1 their oxides Chemical class 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/16—Clays or other mineral silicates
Landscapes
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Catalysts (AREA)
Description
g/089?. i2 4i. st κg / 089 ?. i2 4i. st κ
Katalysator zur katalytischem. Spaltung «* Dehydrierung vonj&hl enwasserstof fen.Catalyst for catalytic. Cleavage «* dehydration of hydrogen and hydrogen.
Für die katalytische Spaltung und Dehydrierung von Kohlenwasserstoffen werden in der Technik Katalysatoren angewandt, die vorzugsweise aus Metallen, deren Oxyde, Chloride, Fluoride oder Sulfide, z.B. von Aluminium, Chrom, Kobalt, Kupfer, Eisen, üangan, Molybdän, Nickel und Zink bestehen. Es wurden für die Spaltung und Dehydrierung alj Katalysatoren auch Legierungen von Nickel und Ciiroin oder,? und Aluminium vorgeschlagen. Eine Reihe von Katalysatoren werden durch Fällung aus den Lösungen der obengenannten Metalle unter gleichzeitigem Auftragen auf Träger, wie Kieselgur oder Ton, hergestellt. Die Herstellung metallischer Katalysatoren, sowie die entstehenden Verluste bei der Regenerierung u.dgl. machen die Verwendung dieser Katalysatoren durch Schmelzen der Metalle (Kischkatalysatoren) oder Fällen der Metalle aus ihren Salzlösungen nit darauffolgender: Trocknen, Formen und Reduzieren umstand— lieh und kostspielig. Lan hex zum ■j.xffiraffinhaltiger Kohlenwasserstoffe auch bereits vorgeschlagen, als katalysator Hochofenschlacke zu verwenden, wie sie normalerweise anfällt. Ein solcher Katalysator wird ohne besondere Behandlung in einen Korb gebracht und mit diesem in 2u Spaltende ü\ mrfc er$etaucht. Bas Ziel ist; For the catalytic cleavage and dehydrogenation of hydrocarbons, catalysts are used in technology, which preferably consist of metals, their oxides, chlorides, fluorides or sulfides, for example aluminum, chromium, cobalt, copper, iron, manganese, molybdenum, nickel and zinc. For the cleavage and dehydrogenation alj catalysts also alloys of nickel and Ciiroin or,? and aluminum are suggested. A number of catalysts are produced by precipitation from the solutions of the abovementioned metals with simultaneous application to supports such as kieselguhr or clay. The production of metallic catalysts, as well as the resulting losses during regeneration and the like, make the use of these catalysts by melting the metals (kisch catalysts) or precipitating the metals from their salt solutions with the following: drying, shaping and reducing complicated and expensive. Lan hex has also already proposed to use blast furnace slag as a catalyst, as is normally the case. Such a catalyst is brought without any special treatment in a basket and with this in 2u gap end u \ MRFC he $ etaucht. Bas goal is ;
einer niedrigen Ausbeute an Benzin in der Hauptsache Heizöl zu gewinnen, das eine geringere Viskosität gegenüber dem Ausgangsmaterial besitzt.a low yield of gasoline, mainly heating oil to win, which has a lower viscosity compared to the starting material.
Ein andere^* Vorschlag geht dahin, bei der Behandlung von rnnprtirni raum u.dgl. durch Hydrieren und erhöhte Menge von Gasöl und wertvollen Schmierölen, Katalysatoren aus einer Schlacke zu verwenden, die beim Raffinieren von Eisenlegierungen gewonnen wird. Die Schlacke firtfet ebenfalls ohne weitere Behandlung Anwendung, für die zur "Vergrößerung ihrer Oberfläche und aktiveren Wirkung ein unmittelbares Einführen aus dem Ofen in Wasser erfolgt.Another ^ * suggestion is in treatment of rnnprtirni space and the like by hydrogenation and increased amount of gas oil and valuable lubricating oils to use catalysts from a slag when refining is obtained from iron alloys. The slag firtfet likewise without further treatment, for which application to "enlarge their surface and more active effect, they are introduced directly from the furnace into water.
Es wurde nun gefunden, dai3 die Schlacken aus derIt has now been found that the slag from the
7af7af
1 des Hoheisens($'aie die Oxyde des Aluminiums, Mangans und Eisens neben den Oxyden des Kaliums, Natrinrs, Kalziums, Magnesiums und Siliziums, sowie eine geringe Lenge gebundenen Schwefels in fein verteiltem Zustande enthalten, in gekörnter Form als Katalysatoren zum Spalten und Dehydrieren von Kohlenwasserstoffen geeignet sind. Insbesondere gilt dies z.B. für die übersauren bis sauren Schlacken mit SiOp : CaO-Verhkltnis von etwa 1 : 0,4 bis 1 : 0,8. Erfindungsgemäß wild die gewonnene Schlacke mit anorganischen Säuren oder Halogenen behandelt und dann anschließend *be* Erhitze^^^wasaerdampf getrocknet. Eine ao behandelte Hochofenschlacke erfährt als Katalysator in ihrer Aktivität , "~' ni° erhebliche steigerung, ter selektiver 7/ir£.ung ist aα verstehen, daß.jA—4T§!ch' der Behandlungsart der ochlacke ^üj^ste-^STs Spaltkatalyaator^ 1 of high iron ( which contain the oxides of aluminum, manganese, and iron in addition to the oxides of potassium, sodium, calcium, magnesium, and silicon, as well as a small amount of bound sulfur in finely divided form, in granular form as catalysts for splitting and dehydration This applies in particular, for example, to the acidic to acidic slags with SiOp: CaO ratio of about 1: 0.4 to 1: 0.8. According to the invention, the slag obtained is treated with inorganic acids or halogens and then subsequently * be * heating ^^^ dried wasaerdampf. An ao treated blast furnace slag experiences as a catalyst in its activity, "~ ' n i ° considerable increase, the more selective 7 / ir £ .ung is aα understand that.jA-4T§! ch' the type of treatment of the ochlacke ^ üj ^ ste- ^ STs Spaltkatalyaator ^
oder Dehydrierungskatalysator ge-In diesen Anwendungsgebieten laßt sichor dehydrogenation catalyst can be used in these fields of application
durch die Art äer ßehandllung tmd die Zeitdauer derby the type of external treatment and the duration of the
!rung wiederum eine verschieden starke Aktivität des Katalysators erreichen. Es ist daher möglich, z.B. für die Dehydrierung eines im wesentlichen aus Butan bestehenden Gemisches einen besonders geeigneten Katalysator dadurch herzustellen, daß die Einwirkung des Chlors auf länger als 1 Stunde, vorzugsweise 2 bis 3 Stunden, ausgedehnt wird, während für ein Propan-ßutan-G-emiseh die Einwirkung des Chlors von 1 Stunde bereits eine befriedigende Ausbeute ergibt.In turn, the activity of the catalyst varies reach. It is therefore possible, for example, for the dehydrogenation of a substance consisting essentially of butane Mixture to produce a particularly suitable catalyst that the action of the chlorine for longer than 1 hour, preferably 2 to 3 hours, while for a propane-ßutane-G-emiseh the action of the Chlorine already gives a satisfactory yield from 1 hour.
Ausführungsbeispiele:Embodiments:
1. 1000 si übersaure Hochofenschlacke wurden mit 200 cnr konzentrierter Salzsäure von spez. Gewicht 1,14, der etwa 5 OhromyIchlorid beigemischt war, bei 50° j/ eine Stunde lang erwärmt, anschließend die so behandelte Schlacke abfiltriert, getrocknet und bei 450° ί mit Wasserdampf zwecks Entfernung der Säurereste behandelt.1. 1000 Si over- acidic blast furnace slag was mixed with 200 cnr concentrated hydrochloric acid of spec. Weight 1.14, to which about 5 ohromyl chloride was added, heated at 50 ° j / for one hour, then the slag treated in this way was filtered off, dried and treated with steam at 450 ° ί to remove the acid residues.
Ein G-asöl mit 0,865 spez. Gewicht siedend zwischen 195° und 360 k wurde bei 470 Qf und einem Druck von 2,5 kg/ cm in der Jkenge von 100 cm /min über 1000 gJ ι -e Katalysators geleitet. Es wurde eine Ausbeute von 75 Gew.^ Spaltbenzin zwischen 30 und 195yC siedend mit einer Oktanzahl von 73 erhalten. Der Kontakt wurde nach "überleiten von 310 1 G-asöl regeneriert.A gas oil with 0.865 spec. Boiling weight between 195 ° and 360 k was passed at 470 Qf and a pressure of 2.5 kg / cm in the Jkenge of 100 cm / min over 1000 gI -e catalyst. A yield of 75 wt. The contact was regenerated after 310 l of gas oil had been passed over it.
2. Das gleiche Gfasöl wurde bei einer Temperatur von 495°f und einem Druck von 2,5 kg/cm mit derselben Durchsatzgeschwindigkeit über 1C00 ßb unbehandelte Schlacke geleitet. In diesem Falle ging die Ausbeute an Spaltbenzin auf 65 Qew.fo zurück. Die Oktanzahl fiel auf 59· Die Kohlenstoffabscheidung auf der Schlacke machte die Unterbrechong des Ver-2. The same gas oil was passed at a temperature of 495 ° f and a pressure of 2.5 kg / cm at the same throughput rate over 1C00 pb.b of untreated slag. In this case, the yield of mineral spirits fell to 65 Qew.fo. The octane number fell to 59 The carbon deposition on the slag made the disruption of the
3. 1000 gr oschiaclce wurden eine Stunde lang bei etwa 100 Je im Ghlorstrom und anschließend bei 350 £ im Wasserdampf behandelt.3. 1000 gr oschiaclce were treated for one hour at about 100 pounds in a stream of chlorine and then at 350 pounds in steam.
Ein von Olefinen freies Gemisch, bestehend aus 45 0A Propan und 55 f» Butan wurde bei 45O0J^ mit einer Durchsatzgeschwindigkeit von 10 l/min über 500 gr des vorgenannten Katalysators geleitet. Nach einmaligem Durcnleiten wurdenA free of olefins mixture consisting of 45 0 A propane and 55 f »butane was passed at 45O 0 J ^ with a throughput rate of 10 l / min for 500 gr of the aforementioned catalyst. After a single run, were
32 $ Olefine erhalten. Nach Herausnahme von 20 $ der gebildeten Get $ 32 olefins. After taking out $ 20 of the educated
/Olefine durch Polymerisation wurden durch abermaliges überleiten des restigen Gemisches 60 i» de3 Propan-Butan-Gemisches in Olefine umgewandelt,-/ Olefins through polymerization were converted into olefins by passing the remaining mixture over again 60 i » de3 propane-butane mixture,
PatentanspruchClaim
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