EP0155876B1 - Verfahren und Einrichtung zum Herstellen von Lösungen mit einem hohen Prozentgehalt an gelöstem Gas; derart erhaltene Lösungen - Google Patents

Verfahren und Einrichtung zum Herstellen von Lösungen mit einem hohen Prozentgehalt an gelöstem Gas; derart erhaltene Lösungen Download PDF

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Publication number
EP0155876B1
EP0155876B1 EP85400353A EP85400353A EP0155876B1 EP 0155876 B1 EP0155876 B1 EP 0155876B1 EP 85400353 A EP85400353 A EP 85400353A EP 85400353 A EP85400353 A EP 85400353A EP 0155876 B1 EP0155876 B1 EP 0155876B1
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EP
European Patent Office
Prior art keywords
temperature
dissolution
hydrocarbon
pressure
zone
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Expired
Application number
EP85400353A
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English (en)
French (fr)
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EP0155876A1 (de
Inventor
Jean-Louis Pean
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
Original Assignee
LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
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Application filed by LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude filed Critical LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
Priority to AT85400353T priority Critical patent/ATE29678T1/de
Publication of EP0155876A1 publication Critical patent/EP0155876A1/de
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/20—Mixing gases with liquids
    • B01F23/29—Mixing systems, i.e. flow charts or diagrams

Definitions

  • the present invention relates to a process for obtaining saturated solutions with a high content of dissolved carbon dioxide, an installation for use and the use of these solutions obtained.
  • the concentration of C0 2 solutions does not generally exceed fifteen percent.
  • a process has now been found of the type of dissolution of carbon dioxide by compression of this gas in a solvent of the chlorofluorocarbon type, in which the counter-current dissolution-saturation is carried out in a saturator device comprising a “high” zone and a “lower” zone, the chlorofluorinated hydrocarbon being pulverized in said saturator apparatus maintained under carbon dioxide pressure.
  • This process makes it possible to obtain regular production of a mixture of the chlorofluorinated hydrocarbon / solvent / carbon dioxide type which can reach high concentrations of 25 to 30% by weight, at a temperature in the region of 20 ° C. and at a pressure below the voltage. carbon dioxide vapor at the same temperature.
  • the chlorofluorinated hydrocarbon is compressed beforehand to pulverize it under a higher pressure of approximately 10 6 Pa (10 bar) than that prevailing in the high dissolution-saturation zone, and by sub-cooling it to a lower temperature of 10 to 20 ° C relative to the temperature of the saturated solution leaving the said dissolution-saturation zone, the first contact of carbon dioxide with the liquid hydrocarbon being carried out by boiling in the lower dissolution-saturation zone under a subcritical pressure of approximately 3 ⁇ 10 6 Pa (30 bar), the temperature being maintained throughout the phase of dissolution of carbon dioxide in the chlorofluorinated hydrocarbon, in subcritical form, preferably below ambient temperature, by through internal thermal regulation at least of the order of a degree, by means of a heat transfer fluid.
  • the upward boiling of carbon dioxide, carried out in the lower part of the saturation phase, is carried out under a subcritical pressure preferably close to the critical pressure.
  • chlorofluorocarbon mixture with a high concentration of carbon dioxide is compressed under high pressure for their subsequent use.
  • Spraying gives a very large liquid-gas surface for liquid / gas contact.
  • the compressed chlorofluorocarbon is sub-cooled relative to the surrounding pressure, well below the equilibrium temperature.
  • chlorofluorinated hydrocarbons which are suitable for carrying out the process are the products known under the trade mark "Freon", in particular “dichlorodifluoromethane CC1 2 F 2 ", designated under the mark "Freon 12".
  • the temperature is fixed between -10 + 20 ° C, preferably lower than ambient temperature, and maintained by means of a controlled thermal regulation.
  • the quality of the saturation of the chlorofluorinated hydrocarbon with carbon dioxide is a function of the precise regulation of the temperature during the dissolution phase; this regulation having to be at least of the order of the degree, and advantageously in the form of an internal regulation by means of a heat transfer fluid, circulating in a closed circuit, the flow rate of circulation of the heat transfer fluid inside the dissolution-saturation zone being regulated by the temperature of said zone.
  • Solutions with a very high concentration of carbon dioxide, from 25 to 30% by weight, are particularly appreciated in many fields of application, in particular in the so-called expansion of plastic foams, the manufacture of expanded plastics and foam rubber where they lead to excellent results; also in the technical field of aerosols, in the overpressurization of a low voltage liquid steam, and in the field of liquid-gas mixtures: carbonation, flotation etc.
  • the installation essentially comprises two cold exchangers: a cooling exchanger (5) upstream of the saturator and an exchanger-regulator (31) internal to the saturator.
  • the “Freon” is stored, in bulk at room temperature, in the storage tank (1), it passes through a pump (2) with relief valve under 1.5 ⁇ 10 6 Pa (15 bar), it is then taken up again. by the double-acting piston booster pump (3).
  • the compressed "Freon" is sub-cooled in the cold exchanger called the cooler exchanger (5) on the inlet pipe of the "Freon” (4).
  • the inlet temperature varies between -10 ° C and + 50 ° C, and the minimum outlet temperature is -10 ° C; the instantaneous flow being 500 kg / hour.
  • the cold exchanger on the pipe is bathed in a thermostatically controlled bath (6) of a refrigeration unit (7) which can lower the temperature down to -10 ° C.
  • the temperature of the thermostatically controlled bath is controlled and regulated by means of the temperature regulator (8).
  • the sub-cooled “Freon” circulates inside the insulated pipe (9), crosses the valve (10) controlled by the level regulator (11), liquid hydrocarbon in the dissolution zone, then always under insulated pipe is routed to the spray nozzle (12 A), located at the top of the saturator (13).
  • This spray nozzle can be of any suitable type, such as the swirl type with full cone and impact diameter of 15 to 50 cm, with a high flow rate of 500 kg / hour under a differential pressure of 10 bars.
  • the recycled “Freon” is recompressed in the recycling pump (14) giving a differential pressure of 10 bars and a flow rate of 500 kg / hour, then it is reassembled in the heat-insulated pipe (15) towards the spray nozzle (12 B ) of the same type as the spray nozzle (12 A) and also located at the upper part of the saturator body (13).
  • the saturator body (13), the volume of which depends on the desired flow rate, can be of cylindrical shape, for example 2 meters high and 200 millimeters in diameter, resistant to a test pressure of 50 bars.
  • the saturator is provided with pressure control means by means of the display manometer and low and high pressure alarm pressure switch (16) and the purge valve and safety valve (17), calibrated at 35 bars, located both at the top of the saturator (13). It is also provided with means for controlling the temperature of the liquid in the saturator, by means of the temperature probe (18); as well as means for controlling and regulating the level of the "Freon", in the saturator, by means of the level regulator (11).
  • the saturator is surrounded by thermal insulation (13a).
  • Carbon dioxide is stored in bulk in the high-pressure storage tank (19), maintained at a minimum of 4 ⁇ 10 6 Pa (40 bar). At 0 ° C the pressure is 4 x 10 6 Pa (40 bar), at -5 ° C it is 3 ⁇ 10 6 Pa (30 bar), it is therefore expected to heat up by negative temperature in winter, by through the heating pin (20).
  • the carbon dioxide delivered under a pressure of at least 4 ⁇ 10 6 Pa (40 bar) passes through the anti-icing heater (21) of the regulator C0 2 (22).
  • the carbon dioxide pressure upstream of the regulator is at least 4 x 10 6 Pa (40 bar) and downstream of 3x x 10 6 Pa ⁇ 0.5 Pa (30 bar ⁇ 0.5 bar), the regulator (22) operates at an instantaneous flow rate of 120 kg / hour (60 m 3 / hour).
  • Carbon dioxide circulates in the pipe (23), fitted with a non-return valve or a high anti-siphon point, shown in (24), the two means being able to be combined.
  • This pipe (24) penetrates the lower part of the saturator body (13) where it is extended by a perforated ramp (25) intended for the boiling under pressure of carbon dioxide in the liquid "Freon” (26).
  • the temperature of the “Freon” solution containing C0 2 is + 10 ° C.
  • This solution with a high concentration of dissolved C0 2 is drawn off through the heat-insulated pipe (27) at the bottom of the saturator (13).
  • a fraction of this solution saturated with C0 2 is withdrawn for recycling via the pump (14), and the other fraction intended for use is compressed by the two recovery pumps in parallel (28A) and (28B), having each a minimum flow rate of 150 kg / hour, under a high discharge pressure, adjusted according to the user's request, for example 15 ⁇ 10 6 Pa (150 bar), and on the operating line (30), conveying the mixing towards use maintaining the C0 2 in dissolved phase, an anti-water hammer accumulator (29) has been inserted.
  • the saturator is also equipped with an internal exchanger called an exchanger-regulator (31) in order to compensate for the exothermic reaction of dissolution of the C0 2 in the "Freon".
  • This internal exchanger being located for its lower part above the ramp for boiling the C0 2 (25) and for its upper part below the liquid level maintained by the regulator (11).
  • the heat exchange takes place via the heat transfer fluid constituting the thermostatically controlled bath (6), maintained at -10 ° C by the refrigeration unit (7).
  • the current of heat transfer fluid circulating in a closed circuit insulated between the refrigeration unit and the saturator leaves the thermostated bath through the insulated pipe (32) until it is connected to the lower part of the internal exchanger (31) located above of the C0 2 (25) debubbling ramp.
  • the heat transfer fluid after circulation in the pipe (33), passage in the valve-triple system (34) is restarted by the circulation pumps (35A) and (358) for recycling by the thermally insulated pipe (36) to the thermostatically controlled bath (6).
  • the circulation rate of the heat transfer fluid inside the internal exchanger (31) is regulated by the temperature of the liquid medium in the saturator, indicated by the temperature probe (18) and by means of the regulator (37).

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)

Claims (8)

1. Verfahren zur Herstellung von gesättigten Lösungen mit hohem Gehalt (= zwischen 25 und 30 Gew.-%) an gelöstem Kohlendioxid durch Komprimieren dieses Gases in einem Lösungsmittel vom chlorfluorierten Kohlenwasserstofftyp, bei dem man das Lösen-Sättigen im Gegenstrom in einer Sättigervorrichtung durchführt, die eine «obere» und eine «untere» Zone aufweist, wobei der chlorfluorierte Kohlenwasserstoff in dieser Sättigervorrichtung, die unter Kohlendioxiddruck gehalten wird, zerstäubt wird, dadurch gekennzeichnet, dass der chlorfluorierte Kohlenwasserstoff vorher komprimiert wird, um ihn unter einem Druck von etwa 106 Pa (10 bar) höher als den, der in der oberen Lösungs-Sättigungs-Zone herrscht, zu zerstäuben, und ihn auf eine Temperatur 10 bis 20°C geringer gegenüber der Temperatur der gesättigten Lösung am Ausgang dieser Lösungs-Sättigungs-Zone unterkühlt, wobei der erste Kontakt des Kohlendioxids mit dem flüssigen Kohlenwasserstoff durch Entgasung in der unteren Lösungs-Sättigungs-Zone unter einem unterkritischen Druck von etwa 3 x 106 Pa (30 bar) durchführt und die Temperatur während der gesamten Phase der Auflösung des Kohlendioxids in dem chlorfluorierten Kohlenwasserstoff unterkritisch, vorzugsweise unterhalb der Umgebungstemperatur, mittels einer inneren thermischen Steuerung wenigstens gradweise mit Hilfe eines Wärmeübertragungsfluids hält.
2. Verfahren zur Herstellung von Lösungen mit hohem Gehalt an gelöstem Gas nach Anspruch 1, dadurch gekennzeichnet, dass der chlorfluorierte Kohlenwasserstoff Dichlordifluormethan ist.
3. Verfahren zur Herstellung einer Lösung von hohem Gehalt an gelöstem Gas nach einem der Ansprüche 1 und 2, dadurch gekennzeichnet, dass eine Fraktion des Gemisches von Lösungsmittel und chlorfluoriertem Kohlenwasserstoff mit einem Gehalt an gelöstem Kohlendioxid nach einem Komprimieren rezykliert und zu der Zerstäubung unter identischen Bedingungen wie die Zerstäubung des chlorfluorierten Kohlenwasserstoffes zurückgeschickt wird.
4. Verfahren zur Herstellung von Lösungen mit einem hohen Gehalt an gelöstem Gas nach einem der Ansprüche 1 bis 3, dadurch gekennzeichnet, dass die Unterkühlung des chlorfluorierten Kohlenwasserstoffes und die Steuerung der Temperatur im Verlauf der Phase der Gasauflösung mit Hilfe desselben Wärmeübertragungsfluids durchgeführt werden, das in einem geschlossenen Kreislauf zirkuliert, wobei der Zirkulationsdurchsatz des Wärmeübertragungsfluids in dieser Zone gesteuert wird.
5. Verfahren zur Herstellung von Lösungen mit hohem Gehalt an gelöstem Gas nach einem der Ansprüche 1 bis 4, dadurch gekennzeichnet, dass das Verfahren kontinuierlich ist.
6. Vorrichtung zur Durchführung eines Verfahrens zur Herstellung von gesättigten Lösungen mit hohem Gehalt (= zwischen 25 und 30 Gew.-%) an Kohlendioxid durch Kompression dieses Gases in einem Lösungsmittel vom chlorfluorierten Kohlenwasserstofftyp, dadurch gekennzeichnet, dass sie eine Pumpe für Überdruck des chlorfluorierten Kohlenwasserstoffes (3), einen kalten Austauscher (5) an der Kohlenwasserstoffeintrittsleitung (4), eine wärmeisolierte Sättigungseinrichtung (13), die in ihrem oberen Teil mit Kohlenwasserstoffzerstäubungsdüsen (12A) (12B) versehen ist, Drucksteuerungsmittel (16) und Sicherheitseinrichtungen (17), Mittel zur Steuerung der Temperatur der flüssigen Phase der Auflösung (18) und deren Niveau (11), einen inneren Austauscher-Regler (31), dann in ihrem inneren Teil eine Kohlendioxidentgasungsrampe (25) und die Abzapfleitung (27) mit den Pumpen einer Wiederherstellung von Hochdruck (28A) (28B) zur Benutzung und die Rückführpumpe (14) zur Sprühdüse (12B) hin aufweist und dass sie ausserdem in geschlossenem Kreislauf der Wärmeübertragungsfluidzirkulation zwischen den mit Thermostat versehenen Bad (6), das mit einem Temperaturregler (8) versehen ist und in der kälteerzeugenden Gruppe (7) eingeschlossen ist, und den inneren Austauscher-Regler (31) aufweist, wobei dieser Kreislauf mit Mitteln zur Zirkulation (34) (35a) (35b) und zur Durchsatzsteuerung (37) versehen ist.
7. Verwendung von Lösungen, die nach einem der Ansprüche 1 bis 5 erhalten wurden, auf dem Gebiet der Kunststoffschaumstoffe, der expandierten Kunststoffe und von geschäumtem Kautschuk, auf dem technischen Gebiet der Aerosole (= auf Überdruck Bringen einer Flüssigkeit mit geringem Dampfdruck) und auf dem Gebiet der Flüssigkeits-Gas-Gemische (= Sättigung mit Kohlensäure, Flotation).
EP85400353A 1984-02-29 1985-02-26 Verfahren und Einrichtung zum Herstellen von Lösungen mit einem hohen Prozentgehalt an gelöstem Gas; derart erhaltene Lösungen Expired EP0155876B1 (de)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT85400353T ATE29678T1 (de) 1984-02-29 1985-02-26 Verfahren und einrichtung zum herstellen von loesungen mit einem hohen prozentgehalt an geloestem gas; derart erhaltene loesungen.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR8403130 1984-02-29
FR8403130A FR2560064A1 (fr) 1984-02-29 1984-02-29 Procede d'obtention de solutions a forte teneur en gaz dissous, solutions obtenues et installation de mise en oeuvre

Publications (2)

Publication Number Publication Date
EP0155876A1 EP0155876A1 (de) 1985-09-25
EP0155876B1 true EP0155876B1 (de) 1987-09-16

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EP85400353A Expired EP0155876B1 (de) 1984-02-29 1985-02-26 Verfahren und Einrichtung zum Herstellen von Lösungen mit einem hohen Prozentgehalt an gelöstem Gas; derart erhaltene Lösungen

Country Status (9)

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US (1) US4626376A (de)
EP (1) EP0155876B1 (de)
JP (1) JPS60210693A (de)
AT (1) ATE29678T1 (de)
AU (1) AU573490B2 (de)
CA (1) CA1270745A (de)
DE (1) DE3560616D1 (de)
ES (1) ES8604236A1 (de)
FR (1) FR2560064A1 (de)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE19754686A1 (de) * 1997-12-10 1999-06-17 Messer Griesheim Gmbh Verfahren und Vorrichtung zum Eintragen von Gas in eine Flüssigkeit

Families Citing this family (9)

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Publication number Priority date Publication date Assignee Title
JPH0611512B2 (ja) * 1986-06-19 1994-02-16 三井東圧化学株式会社 発泡シートの連続的製造方法及び製造装置
US5112525A (en) * 1987-12-10 1992-05-12 Colgate-Palmolive Company Method for making a post-foaming gel
FR2642986B1 (fr) * 1989-02-15 1991-11-29 Carboxyque Francaise Procede et installation d'elaboration d'un melange de " freon " et d'anhydride carbonique
FR2651151B1 (fr) * 1989-02-15 1992-04-30 Carboxyque Francaise Procede d'elaboration et de stockage d'un melange de freon et d'anhydride carbonique.
DE59501858D1 (de) * 1994-11-02 1998-05-14 Solvay Fluor & Derivate Flüssiges kohlendioxid enthaltende treibmittel
US6135433A (en) * 1998-02-27 2000-10-24 Air Liquide America Corporation Continuous gas saturation system and method
GB2541753A (en) * 2015-08-25 2017-03-01 Linde Ag A method of cryogenic chilling or cryogenic freezing of a product
CN112850973B (zh) * 2021-03-05 2024-08-20 郑州大学 一种模块化多级区矿化冶金系统及处理方法
CN117983027B (zh) * 2024-04-03 2024-06-11 潍坊欣泽希化工有限公司 一种溴化氢乙酸溶液生产的动态吸收装置及其控制方法

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US2070167A (en) * 1932-09-23 1937-02-09 Iddings Carl Method of making liquid sprays
US2242429A (en) * 1937-07-27 1941-05-20 California Packing Corp Plant treatment
US2514463A (en) * 1948-10-25 1950-07-11 Jr George W Bayers Liquid carbonator
US2668419A (en) * 1951-10-26 1954-02-09 Specialties Dev Corp Fluid carbon dioxide composition
US2964165A (en) * 1956-11-13 1960-12-13 Chempel Inc Corrosion resistant aerosol package containing hydrolyzable material
US3342672A (en) * 1964-05-07 1967-09-19 Air Reduction Combination propellant system using nitrous oxide
US3387425A (en) * 1964-12-08 1968-06-11 Allied Chem Process for preparing aerosol packages
FR2154959A5 (en) * 1971-10-01 1973-05-18 Air Liquide Aerosol propellant foam - contains nitrous oxide dissolved in polyalcohol solvent
FR2227896B2 (de) * 1972-05-26 1978-06-23 Anhydride Carbonique Ind
DE2366186A1 (de) * 1973-05-26 1978-08-24

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE19754686A1 (de) * 1997-12-10 1999-06-17 Messer Griesheim Gmbh Verfahren und Vorrichtung zum Eintragen von Gas in eine Flüssigkeit

Also Published As

Publication number Publication date
AU3908485A (en) 1985-09-05
ES540730A0 (es) 1986-01-16
ATE29678T1 (de) 1987-10-15
AU573490B2 (en) 1988-06-09
FR2560064A1 (fr) 1985-08-30
EP0155876A1 (de) 1985-09-25
DE3560616D1 (en) 1987-10-22
ES8604236A1 (es) 1986-01-16
JPS60210693A (ja) 1985-10-23
CA1270745A (fr) 1990-06-26
US4626376A (en) 1986-12-02

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