WO1994016800A1 - Perstraction effectuee au moyen d'une reaction chimique - Google Patents

Perstraction effectuee au moyen d'une reaction chimique Download PDF

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Publication number
WO1994016800A1
WO1994016800A1 PCT/AU1994/000038 AU9400038W WO9416800A1 WO 1994016800 A1 WO1994016800 A1 WO 1994016800A1 AU 9400038 W AU9400038 W AU 9400038W WO 9416800 A1 WO9416800 A1 WO 9416800A1
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WO
WIPO (PCT)
Prior art keywords
oxygen
fluid
membrane
process according
stripper
Prior art date
Application number
PCT/AU1994/000038
Other languages
English (en)
Inventor
Robert Arthur Johnson
Original Assignee
Tygola Pty. Ltd.
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 Tygola Pty. Ltd. filed Critical Tygola Pty. Ltd.
Priority to AU59663/94A priority Critical patent/AU692759B2/en
Publication of WO1994016800A1 publication Critical patent/WO1994016800A1/fr

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
    • B01D61/36—Pervaporation; Membrane distillation; Liquid permeation
    • B01D61/364—Membrane distillation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D19/00—Degasification of liquids
    • B01D19/0031—Degasification of liquids by filtration
    • 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
    • B01D53/22—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 diffusion
    • B01D53/229—Integrated processes (Diffusion and at least one other process, e.g. adsorption, absorption)
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor

Definitions

  • This invention relates to a membrane-moderated chemical process for the removal of dissolved oxygen from liquid or gas streams.
  • Boiler/turbine operation in power stations typically involves mechanical deaeration of water at two points; at the exhausted steam condenser using an extraction pump or steam jet ejector, and prior to entering the boiler using a spray or tray-type deaerator.
  • Mechanical deaeration typically reduces dissolved oxygen levels to less than lppm.
  • the preferred oxygen scavenger is sodium sulfite.
  • the current use of less effective and/or environmental unfriendly scavengers has resulted from the potential for thermal decomposition of sodium sulphite above 277°C to give hydrogen sulfide and sulfur dioxide.
  • the degree of decomposition depends on pressure, concentration, pH and temperature. In general, direct dosing of water by sodium sulfite is limited to applications where operating pressures do not exceed 10300kPa (1500 psig) and other conditions are suitable.
  • Yang and Cussler also employed a vacuum in place of the sweep gas with similar results.
  • This process involves purely the "mechanical" removal of oxygen from the feed stream by the use of a "sweep" gas. No chemical reaction takes place at the membrane/sweep gas interface between the oxygen which has diffused through the membrane and the sweep gas.
  • One disadvantage of this method is that oxygen, once having entered the stripper side of the membrane, must pass along the membrane face and thereby give a smaller oxygen partial pressure gradient than that which could be obtained if the oxygen was eliminated and accordingly the driving force of the oxygen removal is reduced.
  • the process is not applicable to oxygen removal since oxygen does not react with water upon dissolution and is otherwise unaffected by the presence of acid or base.
  • This invention is relevant to the removal of oxygen from boiler-feed and cooling stream water as treatment can take place in a low temperature, low pressure point in a Power Station such that decomposition products ( with a resulting lowering of pH ) are not formed. Further the invention is advantageous as the water stream does not make direct contact with the stripper so that reaction products eg SOA ⁇ ' do not contribute to the "total solids content" of the water and hence scaling problems are reduced.
  • the invention is also relevant to the production of ultrapure water for use in the semiconductor, pharmaceuticals and biotechnology industries since very low levels of oxygen can be achieved. This invention is thus applicable to any volatile solute which may be required to be removed from a solution or gas mixture such as the removal of oxygen from mixtures of gases. One such application is as a polishing step in the production of ultrapure nitrogen from air.
  • a process for removing a volatile component from a first fluid containing, the volatile component including the steps of:
  • Any gas-permeable hydrophobic membrane in any structural configuration (hollow fibre, flat sheet, spiral wound, tubular, fan shaped etc) may be utilised.
  • Examples include microporous polytetrafluoroethylene membranes such as those sold under the trade name Goretex, or polypropylene membranes such as those sold under the trade marks Celgard and Accurel.
  • Volatile components are those components which are capable of being oxidised or reduced by a redox reagent of the second fluid and include such components as oxygen, halogens and ozone which can be reduced; primary alcohols, aldehydes, ketones and alkenes which can be oxidised.
  • the first fluid is an aqueous feed stream containing oxygen and the second fluid is a stripping solution containing an appropriate reducing agent for oxygen.
  • the first fluid is a gaseous mixture containing oxygen.
  • This process is identical to that described for the deoxygenation of liquids except that the oxygen is already in the gaseous form and therefore does not desorb form a liquid feed stream. That is, elimination of molecular oxygen from the stripper by reaction with a reducing agent causes molecular oxygen at the membrane-stripper interface to dissolve in the stripper and react. This oxygen is in turn replaced by oxygen which leaves the gaseous feed stream and passes through the membrane.
  • the stripper solution When the stripper solution is recirculated back to a stripper supply tank the stripper becomes saturated with the other gases present in the mixture and, unless these gases react with the reducing agent, will then not be removed from the gas feed stream.
  • Oxygen scavengers which are in common use for boiler and cooling water treatment includes sodium sulfite (Na 2 SO 3 ), sodium metabisulphite (Na 2 S 2 O5), sodium bisulphite (NaHSO 3 ), hydrazine (N 2 H4.H 2 O), hydroxylamine (NH 2 OH) in the form of salts and alkyl derivatives, hydroquinone (CgH4(OH) 2 ) derivatives, and carbohydrazide (NH NHCONHNH 2 ).
  • the oxygen scavenging action of sodium sulfite is indicated as follows: 2Na SO 3 (aq) + O 2 (aq) 2Na 2 SO4(aq).
  • the oxygen scavenger is non-volatile and does not produce volatile reaction products. Volatility will cause contamination of the feed stream from which the oxygen is being removed.
  • the oxygen scavengers hydrazine and hydroxylamine and their homologs can be used in the process they are less effective than other reducing agents.
  • Other reducing agents which may be used include stannous chloride (SnCl 2 ), cuprous chloride (CuCl), sodium borohydride (NaBH4), tetramethylammonium borohydride ((CH )4NBH 4 ) and pyrogallol (CgHgOs).
  • Typically large concentrations of the oxygen scavenger may be utilised.
  • Na 2 SO 3 of 5-15 per cent w/v may be used so that the ratio of the volume of feed fluid to the volume of stripping solution is high.
  • 500L of stripping solution containing 15 per cent w/v of sodium sulfite (75 kg total) will be sufficient to treat one megalitre of feedwater in a thermal power station, assuming that the initial oxygen content is 8 ppm.
  • the volume ratio of the two streams is increased greatly; that is, the ratio of water volume to stripper volume is increased.
  • oxidants for volatile components which are capable of being oxidised include chromium trioxide, dichromate, chromic acid, permanganate, hydrogen peroxide, silver(I) oxide, Mn(VII) or Cr(VI).
  • the temperature of the stripping solution may be increased by a few degrees, for example between 3 and 5° C above the feed stream temperature. This may be desirable as water vapour pressure lowered by the downstream chemicals may otherwise cause dilution of the stripping solution by water vapour transport across the membrane.
  • the temperature range required for the effective removal of oxygen from liquids and gas mixtures using the membrane controlled process is limited by the temperature constraints of the membrane and reductants.
  • the preferred temperature for the operation of the process is, however, between 0°C and 50°C.
  • the direction of the flow of these streams may be co-current or counter current, depending on the inter-facial pressure gradient requirements dictated by the design of the membrane module.
  • the second fluid also initially includes oxygen the reducing agent completely depletes the stripping solution of oxygen so that the partial pressure of oxygen at the membrane-stripping solution interface is effectively maintained at zero.
  • Figure 1 is a schematic diagram of the process and equipment referred to in Example 1.
  • Figure 2 is a graph of oxygen mass transfer concentration (OMTC) or (Ko) verses feed flow rate for a stripper solution at three different flow rates.
  • Figure 3 is a graph of OMTC verses feed flowrate for three stripper solutions at constant stripper flow rate.
  • Figure 4 is a graph of OMTC verses feed flowrate for six stripper solutions at constant flow rate.
  • Figure 5 is a graph of OMTC verses feed Flowrate for an uncatalysed and catalysed stripper solutions at constant flow rates and at three different temperatures.
  • Figure 6 is a graph of Ko verses feed flow rate of the process described in Example 2.
  • the feed stream employed in this example was distilled water saturated with oxygen.
  • Oxygen-saturated feed was used to simulate the process by which oxygen would be extracted from feedwater for boilers dedicated to steam production for process use, that is where no prior mechanical deaeration is employed.
  • FIG. 1 A schematic diagram of the process and equipment is shown in Fig. 1.
  • the feedwater was pumped through the tube (lumen) side of the hollow fibers (shown as a single piece of membrane in cross-section in Fig. 1) before entering the base of a small cell where it immediately impinged on the membrane of a dissolved oxygen (DO) meter.
  • DO dissolved oxygen
  • the outlet stream was then discarded rather than being recirculated back to the feed reservoir in order that single-pass oxygen removal could be observed.
  • a single pass was all that was required in this example as the purpose was to characterise the process in terms of its various resistances to mass transfer rather than to reduce the dissolved oxygen level to zero.
  • the DO meter was regularly calibrated for zero ppm DO using the sulfite stripper in use at the time.
  • the overall mass transfer coefficient (K Q or OMTC), that is the, oxygen flux (removal) per unit driving force (oxygen concentration difference across the membrane) has four main components.
  • the method of this example was to determine which of the above resistances to mass transfer limits the process.
  • the approach taken was to study the effects of varying the operating conditions of the process as already indicated.
  • Figure 3 shows a plot of K Q versus feed flow rate for three different stripper concentrations (5,10 and 15% w/v) at a stripper flowrate of 200mL/m at 20°C.
  • the results show that K Q decreases with increasing stripper concentration over the range of concentrations studied.
  • Catalysts which can be used include inorganic salts of cobalt, cobalt complexes, manganous salts, manganous complexes, hydrogen peroxide, chlorite, a variety of transition metal ions (Co 2+ , Mn 2+ , Cu 2+ ) and light.
  • Membrane mass transfer In the absence of an independent measurement of the membrane mass transfer coefficient, the value has been estimated from theory.
  • the most applicable gas permeation theory is Knudsen diffusion.
  • the membrane mass transfer coefficient estimated from this theory is of the order of 10 ⁇ mg/m 2 h ppm, which is several orders of magnitude higher than the measured overall mass transfer coefficients. This strongly suggests that the membrane resistance is insignificant.
  • Example 1 serves to demonstrate the characteristics of the invention when used in conjunction with a Hoechst Celanese Contactor. These characteristics are summarised below.
  • Feed side mass transfer resistance is not limiting at low fluxes. Results obtained at elevated temperatures suggest that it may be limiting when the K Q increases to about 70 mg/m 2 h ppm in accordance with theoretical predictions.
  • Stripper side mass transfer is not limited by flowrate but is limited by high stripper concentration. However, the latter has an insignificant effect when the sulfite- oxygen reaction is catalysed. (3) The process is limited by the rate of the sulfite-oxygen reaction. However, K Q can be at least doubled by catalysis.
  • Example 2 This example was intended to confirm the best performance achieved in Example 1, namely a K Q of 70-75 mg/m 2 h ppm using catalysis at 40°C.
  • the feedwater DO content was adjusted to about 1 ppm by the addition of a small quantity of Na 2 SO 3 in order to stimulate a process in which prior mechanical deaeration had been effected, for example that in a thermal power station.
  • Example 1 A Hoechst Celanese contractor identical to that used in Example 1 and having no previous use was employed in this example.
  • the stripper solution used was 5% w/v Na 2 SO 3 . All other experimental details are as given in Example 1.
  • K Q shows a definite increase with increasing flowrate before appearing to level out at 80-85 mg/m 2 h ppm. This value is in reasonable agreement with that obtained in Example 1 and is accepted as confirmation of the former results. Indeed, the small discrepancy between the values may be attributed to the use of different modules with different membrane histories.
  • Example 1 K Q remained constant over the range of feed flowrates used and it was therefore concluded that feedside resistance is non-limiting, at least at lower fluxes. In this example however, feedside resistance is indeed limiting at even low fluxes. This observation is attributed to the low DO level of the feedwater. It appears that DO depletion of the feedwater in the module is so rapid due to its low initial level that the amount of oxygen transported across the membrane is dependent on the rate of delivery to the module.
  • Example 2 Based on the results discussed in Example 2 the following can be concluded. (1) The best performance achieved in Example 1 has been confirmed in an independent trial. (2) The invention is equally suited to oxygen removal from saturated and low concentration streams although relatively high feed flowrates are required in the latter case to reduce feed side resistance.
  • Example 3 In this example the effectiveness of the invention in producing very low levels of oxygen in the feed stream by recirculation through a single Hoechst Celanese Contractor was tested. The latter was identical to those used in Examples 1 and 2 but with a different membrane history.
  • a sample of lOOOmL of tap water which was saturated with air was pumped through the lumens of the hollow fiber module with recirculation back to the feed reservoir at 23°C.
  • a 5% w/v Na 2 SO 3 solution was pumped through the shell side of the module with recirculation back to the stripper tank.
  • the flowrate of each stream was 1000 mL/m.
  • the water feed was protected from reoxygenation by a blanket of carbon dioxide.
  • the DO meter was placed in the feed tank which was stirred by the returning oxygen- depleted feed.
  • Both streams were recirculated back to their respective feed containers at a rate of 450ml per minute.
  • the distilled water which had previously been allowed to become saturated with oxygen and carbon dioxide, was protected from further solubilisation of these gases by a blanket of nitrogen gas.
  • the temperatures of the water and stripper solutions were 23° C and 25°C respectively. Using a dissolved oxygen meter and pH meter for monitoring the water stream the following results were obtained.
  • This example demonstrates the effectiveness of the invention in the removal of oxygen from gas mixtures.
  • the particular application chosen for this experiment was the removal of oxygen from air.
  • Air was pumped through the lumens of a Terumo Capiox 350 hollow fiber module (polypropylene membrane, area 5m 2 ) at various flowrates in the range of 320 to 1160 mL/m.
  • the stripper solution (5% w/v Na 2 SO 3 ) was pumped through the shell side of the module in concurrent flow.
  • the gas exiting the module was sampled and analysed by a Fisher Gas Partitioner (Model 1200) with a thermal conductivity detector and a column temperature of 45°C.
  • a double headed peristaltic pump was used to cater for both the air and stripper streams and hence the volumetric stripper flowrate relating to each sample is equal to that of air.
  • the experiment was conducted at 21°C. Results
  • This invention provides a means for removing oxygen from liquids in which it is dissolved or from gas mixtures by transport across a micro porous, hydrophobic membrane to a stripping solution of an appropriate reducing agent such as sodium sulfite.
  • the oxygen is converted to a new chemical species by reaction with the reducing agent so that the partial pressure of oxygen at the membrane-stripper interface is effectively maintained at zero.
  • the resulting steep partial pressure gradient provides a driving force which is capable of reducing the dissolved oxygen content in the feed stream to very low levels.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Water Supply & Treatment (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Analytical Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)
  • Degasification And Air Bubble Elimination (AREA)
  • Gas Separation By Absorption (AREA)

Abstract

L'invention se rapporte à un procédé d'extraction des constituants volatils d'un courant d'alimentation, consistant à: (a) mettre une surface d'une membrane hydrophobe microporeuse en contact avec le courant d'alimentation; (b) mettre l'autre surface de la membrane en contact avec un courant d'extraction qui contient un réactif redox avec lequel le constituant volatil va réagir. Ce dernier se détache du courant d'alimentation, passe à travers la membrane et réagit avec le réactif redox dans le courant d'extraction.
PCT/AU1994/000038 1993-01-28 1994-01-28 Perstraction effectuee au moyen d'une reaction chimique WO1994016800A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AU59663/94A AU692759B2 (en) 1993-01-28 1994-01-28 Perstraction with chemical reaction

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
AUPL7006 1993-01-28
AUPL700693 1993-01-28

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WO1994016800A1 true WO1994016800A1 (fr) 1994-08-04

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Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1996004067A1 (fr) * 1994-08-02 1996-02-15 Fsm Technologies Ltd. Filtre a membrane
NL1000755C2 (nl) * 1995-07-07 1997-01-08 Tno Oxidatieve membraangasabsorptie.
WO1997002883A1 (fr) * 1995-07-07 1997-01-30 Nederlandse Organisatie Voor Toegepast- Natuurwetenschappelijk Onderzoek Tno Procede pour absorption de constituants gazeux oxydables ou reductibles a travers une membrane
US7377112B2 (en) 2005-06-22 2008-05-27 United Technologies Corporation Fuel deoxygenation for improved combustion performance
US7393388B2 (en) 2005-05-13 2008-07-01 United Technologies Corporation Spiral wound fuel stabilization unit for fuel de-oxygenation
US7435283B2 (en) 2005-05-18 2008-10-14 United Technologies Corporation Modular fuel stabilization system
US7465336B2 (en) 2005-06-09 2008-12-16 United Technologies Corporation Fuel deoxygenation system with non-planar plate members
US7569099B2 (en) 2006-01-18 2009-08-04 United Technologies Corporation Fuel deoxygenation system with non-metallic fuel plate assembly
US7582137B2 (en) 2006-01-18 2009-09-01 United Technologies Corporation Fuel deoxygenator with non-planar fuel channel and oxygen permeable membrane
US7615104B2 (en) 2005-11-03 2009-11-10 United Technologies Corporation Fuel deoxygenation system with multi-layer oxygen permeable membrane
US7824470B2 (en) 2006-01-18 2010-11-02 United Technologies Corporation Method for enhancing mass transport in fuel deoxygenation systems
WO2016154005A1 (fr) * 2015-03-24 2016-09-29 General Electric Company Appareil et procédé pour désoxygénation
EP3546043A1 (fr) * 2018-03-28 2019-10-02 Nederlandse Organisatie voor toegepast- natuurwetenschappelijk onderzoek TNO Procédé et appareil de désoxygénation de liquides

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4729773A (en) * 1986-03-04 1988-03-08 Erma Inc. Unit for degassing liquids
US4758416A (en) * 1986-12-30 1988-07-19 Shell Oil Company Removal of H2 S from gas streams
US4929357A (en) * 1989-08-09 1990-05-29 Exxon Research And Engineering Company Isocyanurate crosslinked polyurethane membranes and their use for the separation of aromatics from non-aromatics
US4962271A (en) * 1989-12-19 1990-10-09 Exxon Research And Engineering Company Selective separation of multi-ring aromatic hydrocarbons from distillates by perstraction

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4729773A (en) * 1986-03-04 1988-03-08 Erma Inc. Unit for degassing liquids
US4758416A (en) * 1986-12-30 1988-07-19 Shell Oil Company Removal of H2 S from gas streams
US4929357A (en) * 1989-08-09 1990-05-29 Exxon Research And Engineering Company Isocyanurate crosslinked polyurethane membranes and their use for the separation of aromatics from non-aromatics
US4962271A (en) * 1989-12-19 1990-10-09 Exxon Research And Engineering Company Selective separation of multi-ring aromatic hydrocarbons from distillates by perstraction

Cited By (17)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1996004067A1 (fr) * 1994-08-02 1996-02-15 Fsm Technologies Ltd. Filtre a membrane
NL1000755C2 (nl) * 1995-07-07 1997-01-08 Tno Oxidatieve membraangasabsorptie.
WO1997002883A1 (fr) * 1995-07-07 1997-01-30 Nederlandse Organisatie Voor Toegepast- Natuurwetenschappelijk Onderzoek Tno Procede pour absorption de constituants gazeux oxydables ou reductibles a travers une membrane
US6197269B1 (en) 1995-07-07 2001-03-06 Nederlandse Organisatie Voor Toegepast-Natuurwetenschappelijk Onderzoek (Tno) Method for absorbing gaseous oxidizable or reducible constituents through a membrane
US7393388B2 (en) 2005-05-13 2008-07-01 United Technologies Corporation Spiral wound fuel stabilization unit for fuel de-oxygenation
US7435283B2 (en) 2005-05-18 2008-10-14 United Technologies Corporation Modular fuel stabilization system
US7465336B2 (en) 2005-06-09 2008-12-16 United Technologies Corporation Fuel deoxygenation system with non-planar plate members
US7377112B2 (en) 2005-06-22 2008-05-27 United Technologies Corporation Fuel deoxygenation for improved combustion performance
US7615104B2 (en) 2005-11-03 2009-11-10 United Technologies Corporation Fuel deoxygenation system with multi-layer oxygen permeable membrane
US7569099B2 (en) 2006-01-18 2009-08-04 United Technologies Corporation Fuel deoxygenation system with non-metallic fuel plate assembly
US7582137B2 (en) 2006-01-18 2009-09-01 United Technologies Corporation Fuel deoxygenator with non-planar fuel channel and oxygen permeable membrane
US7824470B2 (en) 2006-01-18 2010-11-02 United Technologies Corporation Method for enhancing mass transport in fuel deoxygenation systems
WO2016154005A1 (fr) * 2015-03-24 2016-09-29 General Electric Company Appareil et procédé pour désoxygénation
CN106145231A (zh) * 2015-03-24 2016-11-23 通用电气公司 用于除氧的装置和方法
EP3546043A1 (fr) * 2018-03-28 2019-10-02 Nederlandse Organisatie voor toegepast- natuurwetenschappelijk onderzoek TNO Procédé et appareil de désoxygénation de liquides
WO2019190320A1 (fr) 2018-03-28 2019-10-03 Nederlandse Organisatie Voor Toegepast-Natuurwetenschappelijk Onderzoek Tno Procédé et appareil pour la désoxygénation de liquides
US12070703B2 (en) 2018-03-28 2024-08-27 Nederlandse Organisatie Voor Toegepast-Natuurwetenschappelijk Onderzoek Tno Method and apparatus for deoxygenation of liquids

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