DE1078999B - Process for separating a releasable substance adsorbed by a granular adsorption mass - Google Patents

Process for separating a releasable substance adsorbed by a granular adsorption mass

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Publication number
DE1078999B
DE1078999B DEG25566A DEG0025566A DE1078999B DE 1078999 B DE1078999 B DE 1078999B DE G25566 A DEG25566 A DE G25566A DE G0025566 A DEG0025566 A DE G0025566A DE 1078999 B DE1078999 B DE 1078999B
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DE
Germany
Prior art keywords
solvent
containers
container
separating
row
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.)
Pending
Application number
DEG25566A
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German (de)
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.)
Adsorptionstechnik A G
CAMAG CHEMIE ERZEUGNISSE
Original Assignee
Adsorptionstechnik A G
CAMAG CHEMIE ERZEUGNISSE
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Adsorptionstechnik A G, CAMAG CHEMIE ERZEUGNISSE filed Critical Adsorptionstechnik A G
Publication of DE1078999B publication Critical patent/DE1078999B/en
Pending legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G25/00—Refining of hydrocarbon oils in the absence of hydrogen, with solid sorbents
    • C10G25/06—Refining of hydrocarbon oils in the absence of hydrogen, with solid sorbents with moving sorbents or sorbents dispersed in the oil
    • 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
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
    • B01J20/08—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04 comprising aluminium oxide or hydroxide; comprising bauxite
    • 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
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/34—Regenerating or reactivating
    • B01J20/3433—Regenerating or reactivating of sorbents or filter aids other than those covered by B01J20/3408 - B01J20/3425
    • 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
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/34—Regenerating or reactivating
    • B01J20/345—Regenerating or reactivating using a particular desorbing compound or mixture
    • B01J20/3475—Regenerating or reactivating using a particular desorbing compound or mixture in the liquid phase
    • 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
    • B01J47/00—Ion-exchange processes in general; Apparatus therefor
    • B01J47/02—Column or bed processes
    • B01J47/026—Column or bed processes using columns or beds of different ion exchange materials in series

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Dispersion Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Treatment Of Liquids With Adsorbents In General (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Description

DEUTSCHESGERMAN

Die zur Reinigung von Flüssigkeiten, z. B. zur Raffinierung von Ölen, verwendeten körnigen Adsorptionsmassen müssen in gewissen Abständen von den Verunreinigungen und den Resten der behandelten Flüssigkeit befreit und regeneriert werden. Man gibt dann der Masse ein Lösungsmittel für den adsorbierten Stoff zu.The cleaning of liquids such. B. for refining oils, granular adsorption materials used must be at a certain distance from the impurities and the remains of the treated Fluid can be freed and regenerated. You then give the mass a solvent for the adsorbed Fabric too.

Soll bei einem kontinuierlichen Verfahren die regenerierte Adsorptionsmasse außer einem zugelassenen Rest des adsorbierten Stoffs, z. B. in einer Menge von 3%, bezogen auf die trockene Masse, nur noch reines Lösungsmittel enthalten, während der abgetrennte Stoff lösungsmittelfrei anfallen und der Lösungsmittelverbrauch stark eingeschränkt werden soll, dann muß man bei Anwendung von übereinander angeordneten, die Adsorptionsmasse enthaltenden Siebbehältern, wobei dem obersten das Lösungsmittel zugeführt und nach einer gewissen Einwirkungszeit der oberste Behälter entfernt, die Behälterreihe angehoben und unten ein neuer, mit beladener Adsorptionsmasse gefüllter Behälter zugeführt wird, erfindungsgemäß in der Weise arbeiten, daß dem jeweils obersten Behälter durchschnittlich so viel Lösungsmittel zugeführt wird, wie vorher mit dem obersten Behälter entfernt wurde, und daß die Behälterzahl bzw. Schichthöhe der Adsorptionsmasse in den Behältern so bemessen werden, daß das Lösungsmittel nicht durch die Behälterreihe durchbricht.Should the regenerated adsorption mass be used in a continuous process other than an approved one Remainder of the adsorbed substance, e.g. B. in an amount of 3%, based on the dry mass, only Contain pure solvent, while the separated material is free of solvents and the Solvent consumption is to be severely restricted, then you have to use one on top of the other arranged, the adsorbent containing sieve containers, with the uppermost the solvent and after a certain exposure time the top container is removed and the row of containers is raised and at the bottom a new container filled with loaded adsorption material is fed in, according to the invention work in such a way that the respective top container on average as much solvent is supplied, as was previously removed with the top container, and that the container number or layer height of the adsorption mass in the containers are dimensioned so that the solvent does not break through the row of containers.

Die Länge der Behälterreihe, die erforderlich ist, um zu gewährleisten, daß bei bis auf den zugelassenen Rest völliger Abtrennung des lösbaren Stoffes aus dem obersten Behälter das Lösungsmittel, z. B. Benzin, noch nicht durch die Adsorptionsmasse des untersten Behälters durchbricht, ergibt sich aus der Länge der Mischzone. Diese »Mischzone« befindet sich zwisehen der obersten Schicht, die bis auf den zugelassenen Rest keinen lösbaren Stoff mehr enthält, und der Adsorptionsmassenschicht am unteren Ende der Behälterreihe, in die noch gerade kein Lösungsmittel eingedrungen ist. Innerhalb dieser Mischzone fällt von oben nach unten der Lösungsmittelgehalt, während der Gehalt an dem lösbaren Stoff in der gleichen Richtung ansteigt. Die Mischzone bleibt während des Betriebes stationär und ändert auch ihre Länge nicht. Die erforderliche Länge der Behälterreihe ist also etwas größer als die Länge der Mischzone.The length of the row of containers required to ensure that except for the permitted one Remaining complete separation of the soluble substance from the top container, the solvent, z. B. gasoline, does not yet break through the adsorption mass of the lowest container, results from the length the mixing zone. This "mixed zone" is located between the top layer, except for the permitted one The remainder no longer contains any soluble substance, and the adsorption mass layer at the lower end of the row of containers, in which no solvent has just penetrated. Falls within this mixed zone from top to bottom the solvent content, while the solute content in the same Direction increases. The mixing zone remains stationary during operation and does not change its length. The required length of the row of containers is therefore slightly greater than the length of the mixing zone.

Vorbedingung für einwandfreies Funktionieren des Verfahrens ist ausreichende Mischbarkeit zwischen dem Lösungsmittel und dem herauszulösenden Stoff. Eine solche Mischbarkeit muß zumindest bei der Temperatur bestehen, bei der die Anlage betrieben werden soll.A precondition for the proper functioning of the process is sufficient miscibility between the solvent and the substance to be extracted. Such miscibility must at least with the Temperature at which the system is to be operated.

Um die Durchsatzgeschwindigkeit bei dem Auswaschverfahren möglichst groß zu halten, ist es Verfahren zum Abtrennen eines lösbaren, von einer körnigen AdsorptionsmasseIn order to keep the throughput speed in the washout process as high as possible, it is Process for separating a detachable from a granular adsorption mass

adsorbierten Stoffsadsorbed substance

Anmelder:Applicant:

Camag Chemie-ErzeugnisseCamag chemical products

u. Adsorptionstedmik A. G.,and Adsorptionstedmik A. G.,

Muttenz (Schweiz)Muttenz (Switzerland)

Vertreter: Dipl.-Ing. E. PrinzRepresentative: Dipl.-Ing. E. Prince

und Dr. rer. nat. G. Hauser, Patentanwälte,and Dr. rer. nat. G. Hauser, patent attorneys,

München-Pasing, Bodenseestr. 3 aMunich-Pasing, Bodenseestr. 3 a

Beanspruchte Priorität:
Österreich, vom 22. Februar 1958Claimed priority:
Austria, February 22, 1958

wünschenswert, die Viskosität der flüssigen Phase möglichst klein zu halten. Andererseits ist es jedoch erforderlich, um die Mischzone und damit die Gesamthöhe der Anlage möglichst klein zu halten, für einen genügend großen Viskositätsunterschied zwischen lösbarem Stoff und Lösungsmittel zu sorgen. Die aus diesen Gründen zu fordernde Differenz der Viskositäten beträgt nach empirischen Ermittlungen etwa 2 bis 3 cSt als Minimalwert. Eine Abgrenzung der Viskosität nach oben ist von untergeordneter Bedeutung. Um die Durchflußgeschwindigkeit hinreichend groß zu halten, werden 20 cSt jedoch kaum überschritten werden.desirable to keep the viscosity of the liquid phase as low as possible. On the other hand, however, it is necessary to keep the mixing zone and thus the total height of the system as small as possible, for one to ensure a sufficiently large difference in viscosity between the soluble substance and the solvent. From According to empirical investigations, the difference in viscosities required for these reasons is approximately 2 to 3 cSt as the minimum value. The upper limit of the viscosity is of secondary importance. In order to keep the flow rate sufficiently high, however, 20 cSt are hardly exceeded will.

Die gewünschte Viskosität des lösbaren Stoffes und gleichzeitig damit die erforderliche Viskositätsdifferenz werden durch Wahl der Arbeitstemperatur der Anlage eingestellt. Der Temperaturwert kann aus den bekannten Viskositäts-Temperatur-Kurven leicht ermittelt werden.The desired viscosity of the soluble substance and, at the same time, the required viscosity difference are set by selecting the working temperature of the system. The temperature value can be taken from the known viscosity-temperature curves can easily be determined.

In der folgenden Tabelle 1 ist ein Betriebsbeispiel für das Auswaschen eines Mineralöles aus einem Adsorptionsmittel angegeben.In the following table 1 is an operating example for the washing out of a mineral oil from an adsorbent specified.

Tabelle 1Table 1

Lösbarer Stoff Mineralöl,Soluble substance mineral oil,

20 cSt (20° C)
6,5cSt(50°C)20 cSt (20 ° C)
6.5cSt (50 ° C)

909 769/344909 769/344

Tabelle 1 (Fortsetzung)Table 1 (continued)

Lösungsmittel Siedegrenzbenzin,Solvent special boiling point petrol,

Kp. 100 bis 125° CBp 100 to 125 ° C

Adsorptionsmittel Aluminiumoxyd,Adsorbent aluminum oxide,

Körnung 0,06 bis 0,2 mmGrain 0.06 to 0.2 mm

Temperatur der Waschvorrichtung 800CTemperature of the washing device 80 0 C

Viskosität des Öles in der Waschvorrichtung 3,0 cSt ίοViscosity of the oil in the washing device 3.0 cSt ίο

Viskositätsdifferenz Öl/Benzin ... 2,5 cStViscosity difference oil / petrol ... 2.5 cSt

Schichthöhe des AdsorptionsmittelsLayer height of the adsorbent

im Einzelbehälter 100 mmin a single container 100 mm

Anzahl der Behälter in der Wasch- lg Number of containers in the wash lg

vorrichtungcontraption

Durchsatzverhältnis kg Benzin zu kg Adsorptionsmittel (trocken) .. 66 :Throughput ratio kg gasoline to kg adsorbent (dry) .. 66:

Durchsatz des trockenen Adsorptionsmittels, kg/dm2/Stunde 10 aoDry adsorbent throughput, kg / dm 2 / hour 10 ao

Anfangsgehalt des Adsorptionsmittels an Öl in Gewichtsprozent, bezogen auf trockenes Adsorptionsmittel Initial oil content of the adsorbent in percent by weight, based on dry adsorbent

Endgehalt des Adsorptionsmittels an Öl in Gewichtsprozent, bezogen auf trockenes Adsorptionsmittel 3,2Final oil content of the adsorbent in percent by weight, based on on dry adsorbent 3.2

In der Tabelle 2 sind Lösungsmitteldurchsatz und erzielter Auswaschungsgrad unter sonst gleichen Bedingungen für einfaches, chargenweises Auswaschen gezeigt. Es wurden dabei auch die gleichen Siebbehälter benutzt wie bei dem Betriebsbeispiel 1. Die Vorteile des erfindungsgemäßen Verfahrens treten durch diese Gegenüberstellung deutlich zutage.Table 2 shows the solvent throughput and the degree of leaching achieved under otherwise identical conditions shown for easy, batch washing. There were also the same sieve containers used as in operating example 1. The advantages of the process according to the invention occur this comparison clearly shows.

Tabelle 2Table 2

Durdisatzverhältnis
kg Benzin zu kg Adsorptionsmittel (trocken)Duration ratio
kg gasoline to kg adsorbent (dry)

Erzielter Endölgehalt
GewichtsprozentAchieved final oil content
Weight percent

66: 100 12,066: 100 12.0

100: 100 4,3100: 100 4.3

140 : 100 2,9140: 100 2.9

Claims (2)

Patentansprüche:Patent claims: 1. λ''erfahren zum Abtrennen eines lösbaren, von einer körnigen Adsorptionsmasse adsorbierten Stoffes mittels eines Lösungsmittels in einer Reihe übereinander angeordneter, oben offener, das beladene Adsorptionsmittel enthaltender Siebbehälter, wobei dem obersten das Lösungsmittel zugeführt, dann der oberste Behälter entfernt, die Behälterreihe entsprechend gehoben und unten ein neuer Behälter mit beladener Adsorptionsmasse hinzugefügt wird, dadurch gekennzeichnet, daß dem jeweils obersten Behälter durchschnittlich so viel Lösungsmittel zugeführt wird, wie mit dem vorher obersten Behälter entfernt wurde, und daß die Behälteranzahl bzw. die Schichthöhe der Adsorptionsmasse in den Behältern so bemessen werden, daß das Lösungsmittel niemals durch die ganze Behälterreihe durchbricht.1. λ '' experience for separating a detachable, from a granular adsorption mass adsorbed substance by means of a solvent in a row stacked sieve containers, open at the top and containing the loaded adsorbent, the topmost container being supplied with the solvent, then the topmost container being removed Row of containers raised accordingly and below a new container with loaded adsorption mass is added, characterized in that the respective top container on average as much Solvent is supplied as was removed with the previously uppermost container, and that the The number of containers or the layer height of the adsorption compound in the containers are dimensioned in such a way that that the solvent never breaks through the entire row of containers. 2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß zwischen den Viskositäten eines abzutrennenden, bei der Arbeitstemperatur flüssigen Stoffes und des Lösungsmittels eine Mindestdifferenz von 2 cSt aufrechterhalten wird.2. The method according to claim 1, characterized in that between the viscosities of a to be separated, a minimum difference between the working temperature of the liquid and the solvent of 2 cSt is maintained. In Betracht gezogene Druckschriften:
Deutsche Patentschriften Nr. 405 673, 825 989.Considered publications:
German patent specifications No. 405 673, 825 989. .©909 769/344 5.60. © 909 769/344 5.60
DEG25566A 1958-02-22 1958-10-25 Process for separating a releasable substance adsorbed by a granular adsorption mass Pending DE1078999B (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
AT1222870X 1958-02-22

Publications (1)

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DE1078999B true DE1078999B (en) 1960-04-07

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Country Link
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FR (1) FR1222870A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1203227B (en) * 1961-03-07 1965-10-21 John Herbert Raymond Thornhill Device for extracting soluble components from plant material
US4934407A (en) * 1988-02-29 1990-06-19 Abb Stal Ab Manifold for gas from parallel-working gas cleaning units

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE405673C (en) * 1922-09-13 1924-11-07 Adolf Andziol Device for continuous leaching
DE825989C (en) * 1949-04-13 1951-12-27 Metallgesellschaft Ag Process for removing solid matter from solutions, especially sediment from miscelles

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE405673C (en) * 1922-09-13 1924-11-07 Adolf Andziol Device for continuous leaching
DE825989C (en) * 1949-04-13 1951-12-27 Metallgesellschaft Ag Process for removing solid matter from solutions, especially sediment from miscelles

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1203227B (en) * 1961-03-07 1965-10-21 John Herbert Raymond Thornhill Device for extracting soluble components from plant material
US4934407A (en) * 1988-02-29 1990-06-19 Abb Stal Ab Manifold for gas from parallel-working gas cleaning units

Also Published As

Publication number Publication date
FR1222870A (en) 1960-06-14

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