DE946342C - Process for carrying out exothermic catalytic gas reactions under high pressure - Google Patents
Process for carrying out exothermic catalytic gas reactions under high pressureInfo
- Publication number
- DE946342C DE946342C DEM14992A DEM0014992A DE946342C DE 946342 C DE946342 C DE 946342C DE M14992 A DEM14992 A DE M14992A DE M0014992 A DEM0014992 A DE M0014992A DE 946342 C DE946342 C DE 946342C
- Authority
- DE
- Germany
- Prior art keywords
- synthesis
- steam
- pressure
- container
- cooling liquid
- 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.)
- Expired
Links
Classifications
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- 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
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/0005—Catalytic processes under superatmospheric pressure
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- 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
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
- B01J8/0285—Heating or cooling the reactor
-
- 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
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
- B01J8/04—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds the fluid passing successively through two or more beds
-
- 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
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
- B01J8/04—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds the fluid passing successively through two or more beds
- B01J8/0446—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds the fluid passing successively through two or more beds the flow within the beds being predominantly vertical
- B01J8/0449—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds the fluid passing successively through two or more beds the flow within the beds being predominantly vertical in two or more cylindrical beds
- B01J8/0453—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds the fluid passing successively through two or more beds the flow within the beds being predominantly vertical in two or more cylindrical beds the beds being superimposed one above the other
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/02—Preparation, purification or separation of ammonia
- C01C1/04—Preparation of ammonia by synthesis in the gas phase
- C01C1/0405—Preparation of ammonia by synthesis in the gas phase from N2 and H2 in presence of a catalyst
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/15—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by reduction of oxides of carbon exclusively
- C07C29/151—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by reduction of oxides of carbon exclusively with hydrogen or hydrogen-containing gases
- C07C29/152—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by reduction of oxides of carbon exclusively with hydrogen or hydrogen-containing gases characterised by the reactor used
-
- 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
- B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
- B01J2208/00008—Controlling the process
- B01J2208/00017—Controlling the temperature
- B01J2208/00106—Controlling the temperature by indirect heat exchange
- B01J2208/00115—Controlling the temperature by indirect heat exchange with heat exchange elements inside the bed of solid particles
- B01J2208/00141—Coils
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- 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
- B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
- B01J2208/00008—Controlling the process
- B01J2208/00017—Controlling the temperature
- B01J2208/00106—Controlling the temperature by indirect heat exchange
- B01J2208/00168—Controlling the temperature by indirect heat exchange with heat exchange elements outside the bed of solid particles
- B01J2208/00203—Coils
-
- 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
- B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
- B01J2208/00008—Controlling the process
- B01J2208/00017—Controlling the temperature
- B01J2208/00106—Controlling the temperature by indirect heat exchange
- B01J2208/00168—Controlling the temperature by indirect heat exchange with heat exchange elements outside the bed of solid particles
- B01J2208/00256—Controlling the temperature by indirect heat exchange with heat exchange elements outside the bed of solid particles in a heat exchanger for the heat exchange medium separate from the reactor
-
- 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
- B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
- B01J2208/00008—Controlling the process
- B01J2208/00017—Controlling the temperature
- B01J2208/00477—Controlling the temperature by thermal insulation means
- B01J2208/00495—Controlling the temperature by thermal insulation means using insulating materials or refractories
-
- 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
- B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
- B01J2208/00008—Controlling the process
- B01J2208/00539—Pressure
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Analytical Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
- Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Description
Verfahren zur Durchführung exothermer katalytischer Gas reaktionen unter hohem Druck Es ist bekannt, daß es, um eine hohe Ausbeute bei exothermen Hochdrucksynthesen zu erzielen, notwendig ist, die durch die Reaktion gebildete Wärme sogleich abzuführen, und zwar derart, daß sich die Temperatur des Katalysators innerhalb wohlbestimmter Grenzen hält. Wenn die Reaktionswärme nicht abgeführt wird, so erhöht sich die Temperatur des Gasgemisches und setzt die Reaktionsausbeute herab. Ferner bietet bei einigen Reaktionen, z. B. bei der Methanolsynthese aus Wasserstoff und Kohlenoxyd, ein zu starker Temperaturanstieg des Katalysators nicht nur den Nachteil, die Ausbeute an Reaktionsprodukt herabzusetzen, sondern auch den, die Reaktion auf die Entstehung unerwünschter Nebenprodukte, wie Methan und Kohleudioxyd, hin zu begünstigen.Process for carrying out exothermic catalytic gas reactions under high pressure It is known that it is necessary to obtain a high yield in exothermic high pressure syntheses it is necessary to dissipate the heat generated by the reaction immediately, in such a way that the temperature of the catalyst is within a well-determined Limits. If the heat of reaction is not dissipated, the temperature increases of the gas mixture and reduces the reaction yield. It also offers some Reactions, e.g. B. in the methanol synthesis from hydrogen and carbon oxide, a too sharp rise in temperature of the catalyst not only the disadvantage, the yield to reduce the reaction product, but also the, the reaction to the formation to favor undesirable by-products such as methane and carbon dioxide.
Da diese Reaktionen stärker exotherm sind als die zur Bildung von Methanol führende, so ergibt sich daraus eine Temperaturerhöhung, welche die Nebenreaktionen beschleunigt und die Katalysatormasse sowie auch den Katalyseofen schädigt.Since these reactions are more exothermic than those leading to the formation of Carrying methanol, this results in an increase in temperature, which causes the side reactions accelerates and damages the catalyst mass as well as the catalytic furnace.
Um bei exothermen Drucksynthesen die Reaktionswärme abzuführes, wurden bereits zalitreiche Arten von Wärmeaustausehern vorgeschlagen, die in der Katalysatormasse angeordnet sind, durch welche die kalten, zur Reaktion bestimmten Gase, ziehen. Mit solchen Anordnungen jedoch ist es schwierig, den gewünschten Temperaturgradienten zu erzielen; ferner geht die durch die Reaktion entwickelte Wärme verloren und wird durch die Kühler am Ausgang der Syntheseöfen abgeführt. In order to dissipate the heat of reaction in exothermic pressure syntheses, were already proposed numerous types of heat exchangers that in the catalyst mass are arranged, through which the cold, intended to react Gases, pull. With such arrangements, however, it is difficult to achieve the desired temperature gradient to achieve; furthermore, the heat developed by the reaction is lost and becomes discharged through the cooler at the exit of the synthesis furnace.
Eine bekannte Methode zum Abführen der Reaktionswärme unter Benutzung derselben zur Herstellung von Dampf besteht darin, daß die Katalysatormasse in verschiedene Schichten unterteilt wird und in die Zwischenräume Stahlrohrschlangen eingesetzt werden, durch welche Wasser gepumpt wird. Durch sinngemäßes Regeln der Wassereinspritzung in die verschiedenen Rohrschlangen ist es möglich, die Temperatur in den erforderlichen Grenzen zu halten, um eine hohe Umsetzungsausbeutel zu erzielen. Der Bau der Rthrschlangen, die bestimmt sind, im Innern von Synthesekolonnen bei einem Druck von mehreren Hunderten Atmosphären und bei Temperaturen zur arbeiten, die 600° erreichen können, bietet große Schwierigkei- -ten. Bei diesen Temperaturen verringert skh die mechanische Festigkeit der Stähle beträchtlich; selbst wenn man hochlegierte Ohromnickelstähle verwendet, müßte man übertrieben dicke Rohre einsetzen; daher wird der Bau solcher Apparaturen praktisch unmöglich, wenn der Betriebsdruck 250 bis 300 Atm. übersteigt. A known method of removing the heat of reaction using the same for the production of steam is that the catalyst mass in different Layers is subdivided and steel pipe coils are used in the spaces between them through which water is pumped. By regulating the water injection accordingly in the various coils it is possible to adjust the temperature in the required Keeping limits in order to achieve a high implementation bag. The construction of the Rthrschlangen, which are intended to be inside synthesis columns at a pressure of several hundreds Atmospheres and at temperatures to work that can reach 600 ° offers great difficulties. At these temperatures, skh reduces the mechanical The strength of the steels is considerable; even if you have high-alloy ear nickel steels used, one would have to use excessively thick pipes; hence the construction becomes such Apparatus practically impossible if the operating pressure is 250 to 300 Atm. exceeds.
Vorliegende Erfindung zeigt eine konstruktive Lösung, um die obenerwähnten Schwierigkeiten zu überwinden, indem sie gestattet, die Wandstärke der Rohre, in denen das zur Abfuhr der Reaktionswärme -bestimmte Wasser umläuft, auf ein Mi-ni-mum herabzusetzen, selbst wenn das Verfahren bei Drücken über I000 Atm. durchgeführt wird. Die Erfindung besteht darin, daß der Synthesekreislauf mit dem Kreislauf des zur Abfuhr der Reaktionswärme bestimmten Wassers derart in Verbindung gesetzt wird, daß praktisch in beiden derselbe Druck herrscht. Diese Verbindung wird mittels eines sinngemäß gekühlten Sammelbehälters in solcher Weise hergestellt, daß dem Wasserdampf ein Eindringen in den Syntheseraum verwehrt ist. The present invention shows a constructive solution to the above-mentioned Difficulties to be overcome by allowing the wall thickness of the pipes in to which the water intended to dissipate the heat of reaction circulates to a minumum decrease even when the procedure is performed at pressures above 1000 atm. carried out will. The invention consists in that the synthesis cycle with the cycle of the to dissipate the heat of reaction certain water is connected in such a way, that practically the same pressure prevails in both. This connection is made using a appropriately cooled collecting container produced in such a way that the water vapor penetration into the synthesis room is prevented.
Die beigefügte Zeichnung zeigt ein Ausführungsbeispiel der Erfindung in Anwendung auf die Ammoniaksynthese. Das von der Umlaufpumpe G kommende Stickstoff-Wasserstoff-Gemisch zieht durch den Wärmeaustauscher D, der im Unterteil der hochdruckfesten Säule A angeordnet ist, folgt dann dem durch Pfeile angedeuteten Weg und gelangt von oben in die Katalysekammer bei einer zum Einleiten der Reaktion hinreichenden Temperatur, nämlich bei etwa 400°. Die Katalysatormasse ist in verschiedene von geeigneten Rosten getragene Schichten unterteilt. Durch die Reaktion steigt die Temperatur schnell über 5000. Beim Ausgang der ersten Katalysatorschicht B1 kommt das Gas mit einer Kühlvorrichtung C1 inBerülhrung, die aus Stahlrohrschlangen besteht, und wird auf 4500 heruntergekühlt. Die Pumpe 0 sichert den Wasserumlauf in der Rohrschlange C1 und mittels -Schiebers H1 wird die Durchflußmenge des Wassers der Menge der durch die Reaktion entwickelten Wärme angepaßt. Sinngemäß wird die Temperatur des Gases in den nachfolgenden Schichten der Katalysatormasse geregelt, derart, daß derjenige thermische Gradient erzielt wird, der einer hohen Ausbeute an Reaktionsprodukt am günstigsten ist. The attached drawing shows an embodiment of the invention in application to ammonia synthesis. The nitrogen-hydrogen mixture coming from the circulation pump G. passes through the heat exchanger D, which is located in the lower part of the high-pressure-resistant column A is arranged, then follows the path indicated by arrows and arrives from above into the catalytic chamber at a temperature sufficient to initiate the reaction, namely at about 400 °. The catalyst mass is in various of suitable grids worn layers divided. The temperature rises rapidly as a result of the reaction over 5000. At the exit of the first catalyst layer B1, the gas comes with a Cooling device C1 in contact, which consists of steel pipe coils, and is on 4500 cooled down. The pump 0 ensures the water circulation in the coil C1 and by means of slide H1 the flow rate of the water becomes the amount of the through the reaction evolved heat adjusted accordingly. The temperature of the gas is analogous regulated in the subsequent layers of the catalyst mass, such that the one thermal gradient is achieved, which leads to a high yield of reaction product is cheapest.
Die katalysierten Gase werden, nachdem sie ihre Wärme im Austauscher abgegeben haben, im Kühler E gekühlt; das kondensierte Ammoniak scheidet im Behälter F aus und wird durch den Schieber T abgelassen, während die Gase, die nicht reagiert haben, mittels Pumpe G in die Synthesekolonne w4 zurückgeführt werden. The catalyzed gases are after their heat in the exchanger have given up, cooled in the cooler E; the condensed ammonia separates in the container F off and is vented through the slide T while the gases that do not react have to be returned to the synthesis column w4 by means of pump G.
Der in den Rohrschlangen C1, C2 und C3 unter Hochdruck erzeugte Dampf wird in den Dampfumspanner I gesandt, wo Dampf bei niedrigerem Druck erzeugt wird, und das Kondenswasser Wird im geschlossenen Kreislauf benutzt, um Verkrustungen im-Innern der Rohre zu vermeiden. Die Wasserumlaufpumpe 0 wird von einem vertikalachsigen ElektromotorN angetrieben, der im selben Behälter V untergebracht ist, der das Kondenswasser aufsammelt. Auf diese Weise erübrigt sich eine Hochdruckstopfbüchsendichtung. The high pressure steam generated in coils C1, C2 and C3 is sent to the steam transformer I, where steam is generated at lower pressure, and the condensation water is used in a closed circuit to remove incrustations to avoid inside the pipes. The water circulation pump 0 is of a vertical axis Electric motor N driven, which is housed in the same container V that the condensation water picks up. This eliminates the need for a high pressure stuffing box seal.
Der Motor ist vom darunter befindlichen Sammler durch zwei wärmeisolierende Trennwände getrennt, und in dem zwischuen diesen entstandenen Raum ist ein Kühler P angeordnet. Dieser Raum steht durch das Rohr Q mit dem Syntheseraum in Verbindung. The engine is from the collector below by two heat-insulating Separate partitions, and in the space created between these there is a cooler P arranged. This space is connected to the synthesis space through the pipe Q.
Claims (2)
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
IT307960X | 1951-08-27 |
Publications (1)
Publication Number | Publication Date |
---|---|
DE946342C true DE946342C (en) | 1956-08-02 |
Family
ID=11232098
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
DEM14992A Expired DE946342C (en) | 1951-08-27 | 1952-08-02 | Process for carrying out exothermic catalytic gas reactions under high pressure |
Country Status (6)
Country | Link |
---|---|
BE (1) | BE513737A (en) |
CH (1) | CH307960A (en) |
DE (1) | DE946342C (en) |
FR (1) | FR1060747A (en) |
GB (1) | GB722948A (en) |
NL (1) | NL85287C (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE1029350B (en) * | 1952-06-28 | 1958-05-08 | Basf Ag | Process for carrying out exothermic reactions |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
IT381315A (en) * | ||||
US2446925A (en) * | 1941-07-05 | 1948-08-10 | Standard Oil Dev Co | Cracking of hydrocarbons with suspended catalyst |
US2539415A (en) * | 1947-03-14 | 1951-01-30 | Hydrocarbon Research Inc | Process and apparatus for the synthesis of hydrocarbons |
-
0
- BE BE513737D patent/BE513737A/xx unknown
- NL NL85287D patent/NL85287C/xx active
-
1952
- 1952-08-02 DE DEM14992A patent/DE946342C/en not_active Expired
- 1952-08-04 FR FR1060747D patent/FR1060747A/en not_active Expired
- 1952-08-12 CH CH307960D patent/CH307960A/en unknown
- 1952-08-25 GB GB21321/52A patent/GB722948A/en not_active Expired
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
IT381315A (en) * | ||||
US2446925A (en) * | 1941-07-05 | 1948-08-10 | Standard Oil Dev Co | Cracking of hydrocarbons with suspended catalyst |
US2539415A (en) * | 1947-03-14 | 1951-01-30 | Hydrocarbon Research Inc | Process and apparatus for the synthesis of hydrocarbons |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE1029350B (en) * | 1952-06-28 | 1958-05-08 | Basf Ag | Process for carrying out exothermic reactions |
Also Published As
Publication number | Publication date |
---|---|
NL85287C (en) | |
BE513737A (en) | |
FR1060747A (en) | 1954-04-05 |
GB722948A (en) | 1955-02-02 |
CH307960A (en) | 1955-06-30 |
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