WO1998009712A1 - Procede de chimisorption de gaz reactifs ou actifs - Google Patents

Procede de chimisorption de gaz reactifs ou actifs Download PDF

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Publication number
WO1998009712A1
WO1998009712A1 PCT/IB1996/000904 IB9600904W WO9809712A1 WO 1998009712 A1 WO1998009712 A1 WO 1998009712A1 IB 9600904 W IB9600904 W IB 9600904W WO 9809712 A1 WO9809712 A1 WO 9809712A1
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WO
WIPO (PCT)
Prior art keywords
lithium
gases
distinguished
fact
paragraph
Prior art date
Application number
PCT/IB1996/000904
Other languages
English (en)
Inventor
Zinaida T. Dimitrieva
Original Assignee
Destiny Oil Anstalt
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 Destiny Oil Anstalt filed Critical Destiny Oil Anstalt
Priority to AU67518/96A priority Critical patent/AU6751896A/en
Priority to PCT/IB1996/000904 priority patent/WO1998009712A1/fr
Publication of WO1998009712A1 publication Critical patent/WO1998009712A1/fr

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2251/00—Reactants
    • B01D2251/30—Alkali metal compounds
    • B01D2251/302—Alkali metal compounds of lithium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/10—Single element gases other than halogens
    • B01D2257/104—Oxygen
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/20—Halogens or halogen compounds
    • B01D2257/204—Inorganic halogen compounds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/30—Sulfur compounds
    • B01D2257/304—Hydrogen sulfide
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/50—Carbon oxides
    • B01D2257/504—Carbon dioxide
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/70—Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
    • B01D2257/702—Hydrocarbons
    • 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
    • Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
    • Y02C20/00—Capture or disposal of greenhouse gases
    • Y02C20/40—Capture or disposal of greenhouse gases of CO2

Definitions

  • the invention relates to technology for the chemiso ⁇ tion of active gases: oxygen, carbon dioxide, hydrocarbons, ammonia, hydrogen sulphide and halogenides.
  • active gases oxygen, carbon dioxide, hydrocarbons, ammonia, hydrogen sulphide and halogenides.
  • the invention can therefore be used most successfully in the field of the thorough refining of inert and perfect gases (nitrogen, argon, helium, neon, xenon and krypton).
  • inert and perfect gases nitrogen, argon, helium, neon, xenon and krypton.
  • the obvious areas of application for the invention are in contemporary micro-electronics, the more advanced type of cryogenics and laser technology, particularly eximer lasers.
  • the process of refining the oxygen out of the inert or perfect gas consists of cooling the contaminated gas to 140K, to 87K, or to the boiling temperature of the gas, and then sending it through an A-type or 13X type synthetic zeolite, with molecular cell (pore) dimensions of between 2.8 and 4.2» , and with a spherical granule diameter of 2.5mm.
  • the temperature of the column filled with zeolite is lowered by stages, at a rate of 5 - 10° a minute, with periods of constant temperature lasting not less than 40 minutes.
  • the oxygen is absorbed on the zeolites at a pressure of between 1.47 and 29.41 bar.
  • the desorption (evacuation) of the oxygen from the zeolites is carried out using a carrier gas, with adjustable pulse heating of the column up to the ambient temperature.
  • the basic drawbacks of methods of extracting oxygen from gas mixtures by means of molecular screens (zeolites) stem from the complexity of synthesising highly selective, high-capacity zeolites, in relation to oxygen or to any other gas, and also to the absence of any possibility of adjusting (controlling) the efficiency of the process by which the oxygen is absorbed onto the zeolites.
  • the technology for -using zeolites in the refining of perfect gases is burdened with (complicated by) the extremely unfavourable gas temperature regime and gas pressure. The degree of refining of perfect gases achieved with the help of zeolites is unsatisfactory for contemporary laser technology.
  • 1 mol of activated metal (M) acquires from 1/2 to 1 mol of O 2 , and, under the best conditions, 1 mol of activated metal oxide acquires a maximum of 1/2 mol of O 2 .
  • the catalytic conversion of O 2 on the surface of the metals and their oxides corresponds to the following reactions: M + V2O 2 - ⁇ MO, MO + x £>z —> MO 2 , M + O 2 — > MO 2 .
  • the catalyst, containing the metal and/or metal oxide is prepared in the following manner.
  • An alkaline solution of a bivalent metal sa , MCO 3 or M(NO 3 ), or M(OH) 2 (M Cu, Ni, Mn, Fe, etc.) is applied to a surface SiO 2 or AI2O 3 , is dried out from the water and is set out to MO 2 at 700 - 800°.
  • the metal dioxide is then reduced to the metal (M) or to MO, in a hydrogen atmosphere, at 100 - 200°, under high pressure.
  • the activated metal can also be obtained by reducing the salts of metals in a hydrogen atmosphere at high pressure and at high temperature.
  • the catalysts are recuperated after the addition of O 2 in a hydrogen atmosphere.
  • the method of refining nitrogen out of a perfect gas consists of bringing a gas mixture into contact with titanium or barium heated to 400 - 800° (DE 2553554, cL B 01 D 53/14).
  • a method for the application of activated coal as an adsorbent of methane, in the process of extracting it from helium (DE 3716899, cL B 01 D 53/04).
  • this method is not suitable for refining carbon dioxide out of perfect gases.
  • the aim of the invention is to create a method for the selective and universal chemisorption of such reactive-active gases as oxygen, carbon dioxide, ammonia, hydrogen sulphide, boron and sulphur halogenides, ethylene, propylene, methane, ethane and propane, which are typical pollutants of perfect and inert gases. None of these active gases is a pollutant of atmospheric air.
  • the selective chemisorbents used, according to invention are lithium compounds from the following classes: lithium halogenides (LiF, LiCl) and/or lithium alkyl(a ⁇ yl) oxides (CH 3 OIi, t-QH OLi, HsOLi, HsCHzOLi) and/or lithium arylides (lithium naphtalinide, lithium triphenylmethylide), and/or lithium alkyl(aryl)borates ([B(OCH 3 ) 4 ]Li, [B(O-t-C4H 9 )4]Li, [BtO Hs ⁇ Li, [t-C ⁇ BfOC-sHsWU
  • Lithium chemisorbents are used both individually and in the form of a mixture of compounds, with any composition and with any mass ratio between the constituents.
  • the lithium chemisorbents In order to avoid (exclude) the destruction of the chemisorbents during their thermoregeneration, they take the form of lithium alcoxides, lithium alkylborates, and lithium alkylboron compounds, with exclusively isomeric structures.
  • the lithium chemisorbents can simultaneously adsorb all the reactive-active gases listed above. Contrary to the physical adsorption, the chemisorptbn method makes it possible to extract (remove) pollutants from gas mixtures in very small quantities.
  • thermodeso ⁇ tion The waste chemisorbents of active gases, according to invention, are regenerated by thermodeso ⁇ tion at 220 - 250° in a vaccuum, or in a current of dried nitrogen or argon.
  • Such parameters of the chemiso ⁇ tion method as the bulk speed of filtration of gas mixtures, the pressure (resistance) in the filter, and the efficiency of adso ⁇ tion of the gases are controlled with the assistance of a selection of fibre thicknesses, density of fibrous material, particle dimensions, poly-dispersability of the thinner material and number of filter sections (beds).
  • the degree of extraction of the pollutants from the gas mixture is monitored with the help of mass spectrometry, gas chromatography and gas analysers, with the use of high-sensitivity laser sensors.
  • Example 1 A sample of absolutely dry LiF weighing 0.13 g (0.005 mol) is preliminarily vacuum-treated (0.01
  • thermo-desorbed oxygen is 0.321 g (0.01 mol O 2 ).
  • a sample of regenerated LiBF 4 complex, weighing 0.47 g (0.005 mol) after chemiso ⁇ tion of oxygen (example 1) is vacuum-treated (0.01 Pa) and exposed in a CO 2 atmosphere at 1.5 atmospheres and at 20° for a period of 50 - 60 minutes.
  • the adsorbent sample is vacuum-treated to remove the gas phase and the physically adsorbed CO2, after which the mass of the adsorbent is determined.
  • the chemisorbed CO 2 is desorbed by gradual heating of the sample up to 245°.
  • C ⁇ HsOLi and QHsC ⁇ OLi adsorb all active gases. If the calculation is made on the basis of 1 mol of adsorbent, they adsorb (mol): O 2 : 2 - 2.5; CO 2 : 1.8 - 2.0; NH 3 : 1.7 - 2.0; H 2 S: 2.0; BF 3 (BCI 3 ):
  • chemosorbents listed simultaneously adsorb BF3 (BCI3) and any other gas (whatever) from the above list.
  • a sample of a complex [t-C H 9 B(CH2C 6 H 5 ) 3 ]Li, amounting to 0.696 g (0.002 mol) is preliminarily vacuum-treated (0.01 Pa), and then exposed in an oxygen atmosphere at 1.5 atmospheres and at 17° for a period of 50 - 60 minutes. After chemiso ⁇ tion of the molecular oxygen, the adsorbent sample is again vacuum-treated to remove the gas phase and the physically adsorbed O 2 . Once the molecular mass of the sample of oxidised adsorbent has been determined, it is exposed in a propane atmosphere at 1.5 atmospheres and at 17° for a period of 50 - 60 minutes.
  • thermodeso ⁇ tion products are quantitatively analysed using gravimetry and gas chrornatography.
  • the quantity of thermodesorbed oxygen amounts to: 0.16 g (0.005 mol O 2 ).
  • propane the figure is 0.528 g (0.012 mol C ⁇ h).
  • a sample of a complex [BfCHzC ⁇ Hs rtLi, amounting to 0.764 g (0.02 mol) is preliminarily vacuum-treated (0.01 Pa), and then exposed in an atmosphere which is a mixture of ammonium and ethane gases at 1.5 atmospheres and at 17° for a period of 70 - 80 minutes. Following the chemiso ⁇ tion of the gases, the complex sample is again vacuumed to remove the gas phase and the physically adsorbed NH 3 and C2H5. The mass of the complex sample comprising the chemosorbed gases is determined by means of gravimetry. The absorbed ammonia and ethane on the complex are thermodesorbed by gradually heating of the sample up to 240 - 250° in a vacuum (0.01 Pa) over
  • thermodesorbed gases determined by gravimetry and gas chromatography, amount to: 0.068 g (0.004 mol NH 3 ) and 0.24 g (0.008 mol C 2 H ⁇ ).
  • the thermo- regenerated complex sample is again exposed, under the same conditions as described above, in an atmosphere of ammonia and ethane.
  • the su ⁇ lus gases and the physically adsorbed gases are extracted by vacuum-treating the complex sample.
  • the quantities for the chemosorbed gases amount to: 0.065 g (0.0038 mol NH 3 ) and 0.27 g (0.009 mol C 2 H6).
  • a complex sample amounting to 0.422 g (0.001 mol) and a sample of ( Hs ⁇ CIi, amounting to 0.25 g (0.001 mol) are mixed, vacuum-treated (0.01 Pa) and exposed in an atmosphere of oxygen and propane at normal pressure and at a temperature of 18° for a period of 45 - 50 minutes. Then the samples are vacuum-treated again to extract the swplus and physically adsorbed gases. Following the determination of the sample mass, the chemosorbed gases are thermodesorbed at 235 - 240° by gradually increasing the temperature in a vacuum (0.01 Pa) over 1.5 hours.
  • the quantities for the chemosorbed and thermodesorbed gases amount to: 0.192 g (0.006 mol O 2 ) and 0.44 (0.01 mol C ⁇ ). If the lithium triphenyl-methalenide, ( H ⁇ CIi in the mixture of adsorbents is replaced by lithium naphthalenide, C ⁇ oH 7 Ii, in a quantity amounting to 0.001 mol (0.134 g), under the same conditions, the quantities for the chemosorbed and thermodesorbed gases amount to 0.224 g (0.007 mol O 2 ) and 0.704 g (0.016 mol C h).
  • a complex sample [B(C6H 5 )]4Li, amounting to 0.652 g (0.002 mol) and a complex sample [t-C4H 9 OB(OCH 2 C6H 5 ) 3 ] i, amounting to 0.412 g (0.001 mol) are mixed, vacuum-treated (0.01 Pa) and exposed in a CO 2 atmosphere at 1.2 atmospheres and at 18° for a period of 60 minutes.
  • the mixture of the samples is again vacuum-treated to extract the su ⁇ lus gases and the physically adsorbed gases.
  • the chemosorbed gases are thermodesorbed at 230° by gradually increasing the temperature in a vacuum (0.01 Pa) over 1.5 - 2.0 hours.
  • the quantities for the chemosorbed and thermodesorbed gases amount to 0.264 g (0.006 mol CO 2 ) and 0.224 g (0.008 mol C 2 H,).
  • a multi-section or multi-bed filter is prepared.
  • the first bed of the filter contains IiF or LiCI, mixed with any compound from the lithium alcoholate class (CH 3 OLi, t- and/or mixed with any compound from the Rli class (lithium naphthalenide, ( Hs CLi) and a fibrous material.
  • the mixture of these adsorbents is applied to the surface of a fibre made of carbon and/or basalt, and/or glass, and/or asbestos.
  • the second section (bed) of the filter contains the same fibre as the first bed, to the surface of which is applied any compound from the lithium alkylborate (arylborate) class: ([B(OCH 3 ) 4 ]Li, [B(O-t- CH ⁇ U [B(O H 5 ) 4 ] [t-C ⁇ OB OCfiHs i, [B(OCH 2 H 5 )4]U [t-
  • the third section (bed) of the filter consists of a mixture of compounds from all the classes listed, diluted (mixed) with a hard dispersed material, for example quartz sand or silica gel, or marble or granite or kaolin If necessary, the number of such sections (beds) in the filter can be doubled or tripled.
  • Refined argon is passed through a filter prepared in such a manner and preliminarily vacuum- treated, to displace the residue (traces) of air. Following this procedure, 5 m 3 of the argon are filtered, containing the following pollutants per m 3 : 0.5 -10g '2 O 2 , 1.8 • lOg "3 C 3 H 8 . 2.5 • lOg "2 CO 2 , 0.1 • lOg "3 BF 3 . The argon is filtered at a bulk rate of 500 L/hour at 17°. The degree of refining of the argon is checked using mass spectrometry and laser spectroscopy. For one cycle of gas mixture filtration, the pollutant content per m 3 of argon amounts to: 0.7 • lOg "4 O 2 , 1.5 • 10g '5 C3H8, 2 • lOg "
  • the pollutant content per m 3 of argon amounts to: 0.15 -lOg *7 O 2 , 0.32 • lOg "7 CO 2 .
  • no propane and trifluoric boron could be detected in the argon

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Analytical Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Separation Of Gases By Adsorption (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

Protection de l'environnement. Technologie de raffinage de gaz inertes, de gaz parfaits. Fabrication de dispositifs micro-electroniques, technologie laser et cryogénique. L'invention porte sur la chimisorption de O2, CO2, H2S, BF3, BCl3, SF6, SCl6, CH3, C2H6, C3H8, C2H4, et C3H6 à l'aide d'adsorbants multifonctionnels. On utilise à cet effet des chimisorbants des classes suivantes: halogénures de lithium, et/ou alkyl(aryl) oxydes de lithium, et/ou arylides de lithium, et/ou alkylborates (arylborates) de lithium, et/ou lithium alkylbores (arylbores), et/ou lithium tétrafluorobores (tétrachlorobores), soit individuellement, soit sous forme de mélanges de toute combinaison de ces composants et selon tout rapport de masse entre les constituants. La chimisorption s'effectue dans des conditions statiques ou dynamiques et sous une pression élevée ou normale.
PCT/IB1996/000904 1996-09-09 1996-09-09 Procede de chimisorption de gaz reactifs ou actifs WO1998009712A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
AU67518/96A AU6751896A (en) 1996-09-09 1996-09-09 Method of selective chemisorption of reactive-active gases
PCT/IB1996/000904 WO1998009712A1 (fr) 1996-09-09 1996-09-09 Procede de chimisorption de gaz reactifs ou actifs

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/IB1996/000904 WO1998009712A1 (fr) 1996-09-09 1996-09-09 Procede de chimisorption de gaz reactifs ou actifs

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WO1998009712A1 true WO1998009712A1 (fr) 1998-03-12

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6361765B1 (en) 1999-06-03 2002-03-26 Unilever Home & Personal Care Usa, Division Of Conopco, Inc. Cosmetic compositions
RU2533491C1 (ru) * 2013-08-08 2014-11-20 Федеральное государственное унитарное предприятие "Государственный ордена Трудового Красного Знамени научно-исследовательский институт химии и технологии элементоорганических соединений" (ФГУП "ГНИИХТЭОС") Способ получения хемосорбента для очистки инертных газов и газов-восстановителей от примесей
RU2784197C1 (ru) * 2022-09-20 2022-11-23 Федеральное государственное бюджетное учреждение науки Институт химии твердого тела Уральского отделения Российской академии наук Способ очистки газовых смесей от кислорода

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1952878A1 (de) * 1969-04-10 1970-10-22 Wolfen Filmfab Veb Fotopolymerisierbarer Lack mit erhoehter Lichtempfindlichkeit
DE2400492A1 (de) * 1973-01-08 1974-07-18 Air Prod & Chem Verfahren zum reinigen eines inerten gases
GB2254728A (en) * 1979-09-28 1992-10-14 Comp Generale Electricite Apparatus for absorbing exhaust gases from a chemical laser and method of manufacture

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1952878A1 (de) * 1969-04-10 1970-10-22 Wolfen Filmfab Veb Fotopolymerisierbarer Lack mit erhoehter Lichtempfindlichkeit
DE2400492A1 (de) * 1973-01-08 1974-07-18 Air Prod & Chem Verfahren zum reinigen eines inerten gases
GB2254728A (en) * 1979-09-28 1992-10-14 Comp Generale Electricite Apparatus for absorbing exhaust gases from a chemical laser and method of manufacture

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6361765B1 (en) 1999-06-03 2002-03-26 Unilever Home & Personal Care Usa, Division Of Conopco, Inc. Cosmetic compositions
RU2533491C1 (ru) * 2013-08-08 2014-11-20 Федеральное государственное унитарное предприятие "Государственный ордена Трудового Красного Знамени научно-исследовательский институт химии и технологии элементоорганических соединений" (ФГУП "ГНИИХТЭОС") Способ получения хемосорбента для очистки инертных газов и газов-восстановителей от примесей
RU2784197C1 (ru) * 2022-09-20 2022-11-23 Федеральное государственное бюджетное учреждение науки Институт химии твердого тела Уральского отделения Российской академии наук Способ очистки газовых смесей от кислорода

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Publication number Publication date
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