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US20100155333A1 - Process for dewatering an aqueous organic solution - Google Patents

Process for dewatering an aqueous organic solution Download PDF

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Publication number
US20100155333A1
US20100155333A1 US12/317,163 US31716308A US2010155333A1 US 20100155333 A1 US20100155333 A1 US 20100155333A1 US 31716308 A US31716308 A US 31716308A US 2010155333 A1 US2010155333 A1 US 2010155333A1
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US
United States
Prior art keywords
solution
membrane
feed
draw
draw solution
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.)
Abandoned
Application number
US12/317,163
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English (en)
Inventor
Shabbir Husain
Prakhar Prakash
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.)
Chevron USA Inc
Chevron Corp
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Chevron USA Inc
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 Chevron USA Inc filed Critical Chevron USA Inc
Priority to US12/317,163 priority Critical patent/US20100155333A1/en
Assigned to CHEVRON CORPORATION reassignment CHEVRON CORPORATION ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: HUSAIN, SHABBIR, PRAKASH, PRAKHAR
Priority to US12/534,669 priority patent/US7955506B2/en
Priority to EP09837774.0A priority patent/EP2376394A4/de
Priority to PCT/US2009/064415 priority patent/WO2010080208A1/en
Priority to JP2011542178A priority patent/JP2012512740A/ja
Priority to CA2746637A priority patent/CA2746637A1/en
Publication of US20100155333A1 publication Critical patent/US20100155333A1/en
Abandoned legal-status Critical Current

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    • 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
    • B01D61/002—Forward osmosis or direct osmosis
    • B01D61/005—Osmotic agents; Draw solutions
    • 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
    • C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
    • C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2313/00—Details relating to membrane modules or apparatus
    • B01D2313/36—Energy sources
    • B01D2313/367—Renewable energy sources, e.g. wind or solar sources
    • 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
    • Y02P20/10—Process efficiency
    • 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

Definitions

  • the invention relates to a process for dewatering an aqueous organic solution.
  • ethanol suitable for blending with gasoline generally has a concentration of between about 95% and about 100% ethanol by weight and less than about 1% water by volume.
  • Known processes for dewatering ethanol solutions to achieve suitable concentrations include conventional distillation of a fermentation broth to raise the concentration of the broth, until an azeotropic solution is formed.
  • the concentration of ethanol in the broth may be raised using conventional distillation until an azeotrope is formed.
  • the distillation process can be followed by further processing to further remove water from the solution.
  • Such further processing includes distilling at lower than atmospheric pressure in order to derive more ethanol-rich solutions, extractive distillation in which the ethanol solution further includes a separation solvent or extracting agent having a high boiling point and being miscible with the ethanol solution which avoids formation of an azeotrope, and entrainer addition in which the ethanol-water azeotrope can be broken by the addition of a small quantity of benzene or cyclohexane which is followed by a fractional distillation process.
  • these processes are highly energy intensive.
  • a less energy intensive, alternative process for dewatering solutions uses a highly water selective pervaporation membrane, although heat input is required.
  • the invention is directed to a process for dewatering an aqueous organic solution, comprising the steps of:
  • the invention is directed to a system for dewatering an aqueous organic solution, comprising:
  • FIG. 1 is a schematic diagram of the process of the invention.
  • FIG. 2 is a plot of the rate of evaporation of water from the draw solution with changing reservoir surface temperature.
  • draw solutions Because of the stored mixing potential energy of concentrated solutions containing a water-soluble osmotic agent, herein referred to as draw solutions, such solutions can be used in conjunction with highly selective water/organic membranes to dewater low concentration aqueous organic solutions via forward osmosis, also referred to as direct osmosis.
  • the selectivity of the membrane is the degree to which the membrane allows a particular component or components to permeate the membrane while not allowing other components to permeate the membrane.
  • a highly selective water/organic membrane is selectively permeable to water and impermeable to the organic component of the solution.
  • the aqueous organic solution has higher water activity than the draw solution.
  • Water activity is defined as the ratio of the vapor pressure of water above a sample containing water to the saturation vapor pressure of pure water at the same temperature. Water activity is an indication of the degree to which unbound water is available in a solution. Water moves from an area of higher water activity to an area of lower water activity; therefore water from the aqueous organic solution moves across the membrane to the draw solution, thereby dewatering the organic solution and diluting the draw solution.
  • the draw solution can be stored in a reservoir at a desired concentration suitable to achieve the desired concentration of the aqueous organic solution via forward osmosis.
  • the diluted draw solution, resulting from the forward osmosis process can be returned to the reservoir. Within the reservoir, water is evaporated from the draw solution through the use of solar energy for re-concentration to the desired concentration.
  • a feed of the organic solution is delivered from a feed solution source 2 to the feed solution side of a membrane 6 .
  • the feed solution source 2 can be a storage tank or a fermentation tank when the organic solution is an alcohol.
  • Draw solution having a lower water activity than that of the feed solution is delivered from a reservoir 8 where it is concentrated to a desired concentration before being fed to the draw solution side of the membrane 6 .
  • water activity gradient across the membrane water moves from the feed solution to the draw solution, thus dewatering the organic solution and diluting the draw solution.
  • the resulting dewatered solution can then be removed for desired use, such as incorporation into fuels, transportation to further processing, storage, etc.
  • the diluted draw solution is returned to the reservoir 8 to be re-concentrated using solar energy and recycled to the membrane 6 .
  • the feed and draw solutions can be delivered via known means such as piping and pumps.
  • the feed solution can be delivered from the fermentation tank 2 to membrane 6 via gravity feed or pump 3 .
  • the draw solution can be delivered from reservoir 8 to membrane 6 via gravity feed or pump 5 , and the diluted draw solution can be returned to the reservoir via optional gravity feed or pump (not shown).
  • the aqueous organic feed solution can be an aqueous alcohol solution, e.g., comprising an alcohol having between 2 and 14 carbon atoms, or mixtures or isomers thereof.
  • the aqueous organic solution can be an aqueous ethanol solution.
  • the aqueous organic feed solution can have a concentration between about 0.1% and about 50% by volume, even between about 0.1% and about 15% by volume.
  • the resulting organic solution can have a concentration between about 1% and about 99% by volume, even between about 20% and about 99% of volume.
  • solids are removed from the feed solution using solids removal means 4 prior to contact with the membrane.
  • Such means can be any appropriate means including filter, centrifuge, gravity settling tank, membrane such as a microporous membrane or a dense membrane, etc.
  • the efficiency of the process can be improved by the use of an ethanol selective membrane for solids removal when the organic solution is an ethanol solution.
  • the ethanol selective membrane can be located within the fermentation tank 2 .
  • the process may be run continuously, semi-continuously or as a batch process. If the process is run continuously, the reservoir 8 should be sized to the optimal size to maintain essentially constant concentration of the draw solution stored within the reservoir.
  • essentially constant concentration is meant that the concentration of the draw solution in the reservoir varies somewhat but not so much as to require non-continuous operation.
  • the optimal size of reservoir 8 can be determined knowing the evaporation rate of the draw solution at the atmospheric conditions of temperature, humidity and air velocity. The evaporation rate can be approximated using equation (1), accounting for the various factors mentioned above.
  • the process can be run semi-continuously, by which is meant that the delivery of the feed solution to the membrane, the delivery of the draw solution to the membrane and/or the delivery of the diluted draw solution to the reservoir can be run intermittently in order to obtain the aqueous organic solution having the desired concentration.
  • the draw solution in the reservoir can be open to outdoor atmospheric conditions, such as in a pond or an open tank.
  • the open reservoir is advantageously located in an area where atmospheric conditions are conducive to high evaporation rates, e.g., warm temperature, low humidity and high air velocity.
  • the reservoir can be exposed to direct sunlight during the day. Solar energy is absorbed by the surface of the draw solution in the reservoir which drives the evaporation of the water in the draw solution.
  • the reservoir can be closed, as in a closed tank.
  • Solar energy can be concentrated with the use of mirrors and/or lenses to heat the draw solution to drive evaporation of the water in the draw solution.
  • the draw solution has sufficient osmotic pressure to extract water from the organic solution through the membrane.
  • the desired draw solution concentration will vary, depending on process parameters such as feed solution concentration, desired product concentration, flow rates, osmotic agent, etc.
  • the higher the osmotic pressure of the draw solution the greater the ability to extract water from the aqueous organic solution.
  • the draw solution has lower water activity than the organic solution. Water flows from a region of higher water activity to a region of lower water activity. The greater the water activity gradient between the aqueous organic feed solution and the draw solution, the greater the available driving force to move water across the membrane.
  • Saturation concentrations and osmotic pressure gradients for a number of draw solutions containing various osmotic agents when dewatering a 90% ethanol-water solution at room temperature are shown in Table 1.
  • Suitable osmotic agents for use in the draw solution are those which provide high osmotic pressure or water activity gradient across the membrane.
  • Suitable osmotic agents include halides, nitrates, sulfates, acetates and sugars.
  • sodium chloride, sodium acetate, magnesium nitrate and potassium acetate salts may be used as the osmotic agent.
  • Polyvalent salts may be preferred over monovalent salts as they offer a greater driving force.
  • Urea may also be used as the osmotic agent.
  • the temperature of the draw solution can advantageously be elevated to increase the osmotic agent solubility thereby increasing the osmotic pressure of the draw solution and decreasing the precipitation potential of the osmotic agent.
  • a saturated sodium chloride solution has an osmotic pressure of about 400 atm at 25° C., about 420 atm at 40° C., and about 440 atm at 55° C. Elevating the temperature of the draw solution also advantageously reduces the viscosity of the draw solution which in turn reduces the energy required to pump the draw solution.
  • Non-corroding, plastic pipes such as PVC pipes are well suited to handle corrosive salt solutions up to a temperature of 60° C. Chlorinated PVC pipes are suited to handle such solutions at higher temperatures.
  • the selection of the membrane for use in the invention is made after consideration of the requirements for stability, flux and separation efficiency in the forward osmosis process.
  • the membrane has a water/organic selectivity of at least 1. The actual water selectivity can vary depending on the combination of feed and draw solutions being used. When an aqueous alcohol solution is being dewatered, the water/alcohol selectivity is preferably at least about 50.
  • the membrane also has an osmotic agent rejection rate greater than 95%, meaning that membrane prevents at least 95% of the osmotic agent used in the draw solution from moving across the membrane to the feed solution side. A continuous dense membrane with few defects provides a high level of rejection, for example.
  • the membrane exhibits long term stability in high concentration environments, and resistance to plasticization by organic solvents.
  • Higher sorption of ethanol in glassy polymers of membranes results in a sharp loss in the separation selectivity of the membrane as a result of plasticization.
  • the use of membranes of higher glass transition aromatic polymers with or without physical (e.g. hydrogen bonding) or chemical (covalent) crosslinks may be favored for plasticization resistance.
  • the membrane preferably allows high water flux.
  • the water flux of the membrane preferably is at least about one liter per square meter per hour.
  • Water flux is a function of the intrinsic water permeability of the membrane material and the membrane skin thickness.
  • hydrophilic polymers are desired, having the added advantage of being less prone to membrane fouling.
  • trans-membrane pressure in forward osmosis is negligible, a minimal support structure is needed for the chosen membrane. Membranes with minimal support structure could be developed for maximum flux.
  • zeolite nanoparticles have been used in a polyamide matrix to increase water flux.
  • the zeolites are dispersed into the dense thin film polyamide layer which is formed on a porous support.
  • the zeolite particles can be dispersed in the porous support to increase its hydrophilicity.
  • such a design can also provide added strength from the high modulus of the zeolite.
  • zeolite nanoparticles can be used in the dense layer to provide solvent stability (plasticization resistance).
  • Other potential examples of membranes include crosslinked hydrophilic polymers.
  • the morphology and geometry of the membrane is preferably optimized for the particular separation application as would be within the skill level of one familiar with the use of membranes.
  • Suitable membranes include hollow fiber membranes, flat asymmetric membranes, multicomponent membranes and dense film membranes.
  • Known membrane module configurations for these membrane types can be used.
  • the membrane material can be selected from polymeric materials, metal-organic complexes, inorganic materials and combinations thereof.
  • the concentration of solute in the boundary layer adjacent the membrane on the draw solution side of the membrane can be lower than the concentration of ethanol in the boundary layer on the feed solution side of the membrane, due to an effect known as dilutive concentration polarization.
  • This effect works to reduce the osmotic pressure driving force across the separating layer of the membrane.
  • renewal of the membrane surface at both sides is needed. While this is easily done on the smooth outer side of the separation layer (skin layer) of an asymmetric membrane with a high flow rate, the renewal on the porous side of the skin is more challenging.
  • a thin or highly porous support layer is preferred to minimize the boundary layer thickness and thus maximize the driving force across the membrane.
  • the process according to the invention minimizes energy conversions thus reducing waste due to conversion inefficiencies.
  • the process takes advantage of freely available solar energy to concentrate the draw solution in evaporation ponds built on land that is barren or unsuitable for growing biofuel crops.
  • the solar energy is captured and stored as chemical potential in the draw solution.
  • the storage in the form of evaporation ponds or tanks is inexpensive.
  • a hypothetical reservoir is assumed to be an open evaporation pond located in an area with plenty of sunshine and the following average climatic conditions:
  • the draw solution is a 20 wt % solution of magnesium chloride in water. Absorbed solar energy leads to a rise in the temperature of the draw solution.
  • FIG. 2 shows the change in evaporation rate with change in temperature on the water surface. FIG. 2 indicates that by allowing solar heating to raise the temperature of water surface to 50° C., approximately 540 mL/hr/cm 2 of water can be removed. The pond area was determined by the surface area needed to evaporate water sufficient to attain draw solution concentration of 5M MgCl 2 in water.
  • a cellulose triacetate membrane is used in the osmosis process.
  • the membrane is assumed to be impermeable to ethanol.
  • a water/ethanol separation factor of approximately 95 was assumed to achieve a 99% ethanol recovery.
  • the effective membrane flux is estimated using a modified flux equation (2) which uses a logarithmic mean driving force for the osmotic pressure.
  • J w A w ( ( ⁇ 1 - ⁇ 2 ) Ln ⁇ ( ⁇ 1 ⁇ 2 ) ) ( 2 )
  • a w water permeability constant of the membrane
  • ⁇ 1 osmotic pressure differential at the inlet of the membrane
  • ⁇ 2 osmotic pressure differential at the outlet of the membrane
  • the modified flux equation was used to compute the flux based on an assumed water permeability of 3.07E ⁇ 12 m 3 /m 2 /Pa/s.
  • the subscripts denote osmotic driving force at positions 1 and 2 of the membrane.
  • the respective osmotic driving force is given in Table 2.
  • the calculated flux for the cellulose triacetate membrane is 553 liter/m 2 /hr of water permeating through the membrane, resulting in a membrane area requirement of approximately 650 m 2 (6,982 ft 2 ), assuming a 94.7% water recovery which is required to attain 50 wt % ethanol in the reject stream.
  • This composition is similar to that of an ethanol stream entering the rectifying column from the beer column in a typical ethanol dehydration process.
  • the energy required to dewater a 5 wt % aqueous ethanol solution to 50 wt % ethanol is significantly lower than that required by a beer column in a conventional distillation process.
  • the beer column consumes about 12,000 BTU/gallon of ethanol produced.
  • the energy typically required by distillation for dewatering a 5 wt % aqueous ethanol solution can be estimated as 21,505 BTU/gallon as disclosed in “The Alcohol Textbook” 4 th edition, edited by K. A. Jacques, et al.
  • the beer column consumes about 55% of the total energy consumption in ethanol dewatering, or approximately 12,000 BTU/gallon.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Water Supply & Treatment (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)
  • Heat Treatment Of Water, Waste Water Or Sewage (AREA)
US12/317,163 2008-12-18 2008-12-18 Process for dewatering an aqueous organic solution Abandoned US20100155333A1 (en)

Priority Applications (6)

Application Number Priority Date Filing Date Title
US12/317,163 US20100155333A1 (en) 2008-12-18 2008-12-18 Process for dewatering an aqueous organic solution
US12/534,669 US7955506B2 (en) 2008-12-18 2009-08-03 Process for dewatering an aqueous organic solution
EP09837774.0A EP2376394A4 (de) 2008-12-18 2009-11-13 Verfahren und syystem zur entwässerung einer wässrigen organischen lösung
PCT/US2009/064415 WO2010080208A1 (en) 2008-12-18 2009-11-13 Process and system for dewatering an aqueous organic solution
JP2011542178A JP2012512740A (ja) 2008-12-18 2009-11-13 有機水溶液を脱水するためのプロセス及びシステム
CA2746637A CA2746637A1 (en) 2008-12-18 2009-11-13 Process and system for dewatering an aqueous organic solution

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WO (1) WO2010080208A1 (de)

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US20130233797A1 (en) * 2012-03-09 2013-09-12 Great Salt Lake Minerals Corporation Methods for osmotic concentration of hyper saline streams
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