WO2020056847A1 - Ensemble membrane à étages multiples intégré à une pompe à chaleur à semi-conducteur et son utilisation dans la distillation à membrane - Google Patents

Ensemble membrane à étages multiples intégré à une pompe à chaleur à semi-conducteur et son utilisation dans la distillation à membrane Download PDF

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WO2020056847A1
WO2020056847A1 PCT/CN2018/112108 CN2018112108W WO2020056847A1 WO 2020056847 A1 WO2020056847 A1 WO 2020056847A1 CN 2018112108 W CN2018112108 W CN 2018112108W WO 2020056847 A1 WO2020056847 A1 WO 2020056847A1
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heat pump
membrane
permeate
membrane module
semiconductor heat
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PCT/CN2018/112108
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English (en)
Chinese (zh)
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关国强
姚成龙
江燕斌
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华南理工大学
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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
    • B01D61/36—Pervaporation; Membrane distillation; Liquid permeation
    • B01D61/364—Membrane distillation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • 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
    • B01D61/366—Apparatus therefor
    • 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
    • B01D61/368—Accessories; Auxiliary operations
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2311/00—Details relating to membrane separation process operations and control
    • B01D2311/10—Temperature control
    • B01D2311/103—Heating
    • B01D2311/1031—Heat integration, heat recovery or reuse within an apparatus
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2311/00—Details relating to membrane separation process operations and control
    • B01D2311/10—Temperature control
    • B01D2311/106—Cooling
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2313/00—Details relating to membrane modules or apparatus
    • B01D2313/22—Cooling or heating elements
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2313/00—Details relating to membrane modules or apparatus
    • B01D2313/22—Cooling or heating elements
    • B01D2313/221—Heat exchangers

Definitions

  • the invention relates to a membrane distillation technology, in particular to a multi-stage membrane module integrated with a semiconductor heat pump and its application in membrane distillation.
  • the multi-stage membrane module uses a semiconductor refrigeration sheet as a heat pump and is integrated in each stage of the membrane module.
  • Multi-stage membrane separation unit belongs to the technical field of energy conservation and environmental protection.
  • MD Membrane distillation
  • MD can be generally divided into direct contact (MDD), air gap (MDG), gas sweeping (MDMD), and vacuum (SGMD) vacuum MD, VMD).
  • MDD direct contact
  • MDG air gap
  • MDMD gas sweeping
  • SGMD vacuum vacuum MD
  • VMD vacuum MD
  • a typical DCMD system requires both heating of the feed liquid and cooling of the permeate, so the system requires both a heat source and a cold trap to operate.
  • the heat source required for heating can generally use the waste heat resources in the process industry (such as low-temperature steam, hot water, etc.), and heat the feed liquid through an external heat exchange device and enter the hot side of the membrane module; and after the permeate is cooled by the cold trap, Enter the cold side of the membrane module. Due to the evaporation and heat transfer of the liquid material on the hot side of the membrane module and the heat loss, the temperature of the hot side of the membrane module will decrease along the flow direction of the material liquid, while the temperature of the cold side will increase along the direction of the permeate flow, thereby causing two sides of the membrane surface.
  • the temperature difference distribution is not uniform, and the average temperature difference on the membrane surface (that is, the effective driving force for membrane separation) is smaller than the inlet temperature difference between the cold and hot sides of the membrane module (that is, the driving force provided by the process system).
  • the separation efficiency of DCMD membrane modules is low; at the same time, polarization exists on both the cold and hot sides of the membrane module (that is, the boundary layer phenomenon), which makes the temperature of the fluid on the hot-side membrane surface lower than the mainstream, and the fluid on the cold-side surface of the membrane The temperature is higher than the mainstream. This unavoidable polarization will further reduce the separation efficiency of DCMD membrane modules.
  • a heat pump is a device that transfers heat energy from a low-temperature system to a heating object. By simultaneously achieving efficient energy conversion between cooling and heating, the overall energy efficiency of the MD system can be significantly improved.
  • Chinese invention patent application CN105709601A discloses a two-effect membrane distillation device and method using a heat pump.
  • the two-effect DCMD membrane module is integrated in a traditional heat pump cycle, and the permeate-side refrigeration and the material-liquid-side heating are realized simultaneously using the heat pump principle.
  • Similar membrane distillation methods using heat pumps include: a DCMD system (CN206652392U) that integrates a heat pump cycle and a heat storage process, a DCMD system (CN205461826U) that integrates a single membrane module into a heat pump cycle, a DCMD system that integrates solar heating and heat pump cooling ( CN105749752A) and a method for improving the thermal efficiency of a heat pump membrane distillation system by optimizing a hollow fiber membrane (CN106582292A) and the like.
  • the semiconductor refrigeration chip using thermoelectric refrigeration has the advantages of small size, low cost, and easy realization of system miniaturization.
  • the semiconductor refrigeration chip uses the Peltier effect, and the current is applied to the semiconductor element to move the heat from the low-temperature heat absorption to the high-temperature heat radiation surface.
  • Chinese utility model patent CN203155103U discloses a membrane module for realizing multi-stage AGMD using thermoelectric refrigeration and a method for purifying water using solar energy.
  • the purpose of the present invention is to provide a multi-stage membrane module of an integrated semiconductor heat pump capable of significantly improving membrane separation efficiency while reducing the cost of adopting the DCMD method and its application in membrane distillation, so as to realize evaporation and concentration processes such as seawater desalination, sewage treatment, and food concentration. Energy consumption and costs are significantly reduced.
  • the invention uses a semiconductor refrigeration chip to replace the traditional heat pump circulation system, reduces the system configuration complexity and cost of the heat and cold source utilization method, and improves the film through "in-situ heat transfer" and optimized flow channel design for heat transfer near the film surface.
  • the average temperature difference between the two sides and the mitigation of polarization can reduce the cost of the DCMD system and increase the efficiency of separation and heat transfer.
  • the "in-situ heat transfer" of the present invention is to reduce the space-time interval of energy transfer, so that the energy of the input system is more efficiently transferred to the hot side of the membrane surface required for separation, and the heat on the cold side of the membrane surface is absorbed faster. Hot surface removal system.
  • the semiconductor refrigerating sheet of the present invention utilizes the Peltier effect to transfer heat from the low-temperature heat absorption of the refrigerating sheet to the high-temperature exothermic surface through the action of current.
  • the present invention adopts a method of directly cooling the permeate and utilizes the characteristic of the liquid thermal conductivity significantly higher than that of the gas, which effectively improves the heat transfer efficiency.
  • a multi-stage membrane module integrated with a semiconductor heat pump is mainly composed of an environmental heat absorption unit, an environmental heat dissipation unit and a multi-stage membrane module.
  • Each stage membrane module includes a semiconductor heat pump module and an in-situ heat transfer membrane separation unit;
  • the in-situ heat transfer membrane separation unit includes a hydrophobic microporous membrane, a hot-side volume, a cold-side volume, a material liquid inlet channel, a material liquid outlet channel, a permeate liquid inlet channel, and a permeate liquid outlet channel.
  • a hot-side volume and a cold-side volume are provided on both sides; one end of the hot-side volume is provided with a material-liquid inlet channel, and the other end is provided with a volume-liquid outlet channel; There are permeate outlet channels;
  • the heat-absorbing surface of the semiconductor heat pump module is attached to the cold-side volume of the upper-stage membrane module, and the heat-dissipating surface of the semiconductor heat pump module is attached to the hot-side of the next-stage membrane module.
  • the distance from the heat dissipation surface of the semiconductor heat pump component to the hydrophobic microporous membrane is 1 to 5 mm on the hot side cavity; the distance from the heat absorption surface of the semiconductor heat pump component to the hydrophobic microporous membrane is 1 ⁇ 5mm;
  • the environmental heat absorption unit is close to the heat absorption surface of the semiconductor heat pump module on the hot side cavity of the first-stage membrane module, and the heat dissipation surface of the semiconductor heat pump module is connected to the heat side cavity of the first-stage membrane module;
  • the unit is closely attached to the heat radiation surface of the semiconductor heat pump component on the cold side cavity of the last stage membrane module, and the heat absorption surface of the semiconductor heat pump component is connected to the cold side cavity of the last stage membrane module.
  • a plurality of material liquid inlet channels and material liquid outlet channels are respectively provided at both ends of the hot side cavity, and any material liquid inlet channel does not share an axis with any material liquid outlet channel. line.
  • a plurality of permeate inlet channels and permeate outlet channels are respectively provided at both ends of the cold-side volume, and any of the permeate inlet channels and the axis of any of the permeate outlet channels are not aligned.
  • the environmental heat absorption unit adopts a natural convection air heat exchanger
  • the environmental heat dissipation unit adopts a forced convection air radiator
  • the natural convection air heat exchanger uses a natural flow fin-type refrigeration heat exchanger; and the forced convection air radiator uses an aluminum fin fan cooler.
  • the semiconductor heat pump assembly includes a mounting frame and a semiconductor cooling sheet, wherein the semiconductor cooling sheet is selected as TEC1-19006 with a size of 40x40x4mm, and is embedded in a heat-resistant epoxy resin mounting frame.
  • the hydrophobic microporous membrane is a surface-modified super-hydrophobic polyvinylidene fluoride planar membrane, and the average membrane thickness is 0.018 mm.
  • the application of the multi-stage membrane module with integrated semiconductor heat pump in a direct contact membrane distillation system The multi-stage membrane module with integrated semiconductor heat pump and accessories form a direct contact membrane distillation system.
  • the direct contact membrane distillation system is mainly composed of Material liquid storage tank, hot-side circulation pump, multi-stage membrane module with integrated semiconductor heat pump, permeate storage tank, and permeate circulation; material liquid storage tank is connected to the hot-side circulation pump through a pipeline, and the hot-side circulation pump is connected to The material-liquid inlet channels of the multiple hot-side cavities of the integrated multistage membrane module of the semiconductor heat pump are connected, and the material-liquid outlet channels of the multiple hot-side cavities of the integrated multistage membrane module of the semiconductor heat pump are connected to the material-liquid storage tank through pipes.
  • the permeate storage tank is connected to the permeate circulation pump through a pipeline, and the permeate circulation pump is connected to the permeate inlet channels of multiple cold-side cavities of a multi-stage membrane module integrated with a semiconductor heat pump through a pipeline;
  • the permeate outlet channels of the multiple cold-side receptacles of the multi-stage membrane module are connected to the permeate storage tank through pipes, respectively.
  • seawater, sewage or liquid food to be concentrated is added to the feed liquid storage tank; ultrapure water is added to the feed liquid storage tank to realize seawater desalination, sewage treatment or food concentration.
  • the liquid food to be concentrated is milk.
  • the material liquid to be concentrated in the material liquid storage tank is sent to the hot-side volume chambers of the multistage membrane module integrated with the semiconductor heat pump through the material liquid circulation pump for heating;
  • the permeate is sent to the cold side cavity in the multi-stage membrane module of the integrated semiconductor heat pump through the permeate circulation pump.
  • the permeate vapor is driven by the temperature difference between the two sides of the membrane. Driven by the vapor pressure difference between the two sides of the membrane, the membrane migrates from the hot side to the cold side through the membrane, thereby achieving the evaporation and concentration of the feed liquid and the condensation and enrichment of the permeate.
  • the heating and cooling processes of the feed liquid and permeate in the multi-stage membrane module of the present invention are described in detail as follows: the heat is absorbed by the first-stage semiconductor heat pump module from the ambient heat absorption unit and transferred to the first-stage in-situ heat transfer membrane separation unit; The side volume cavity transfers heat to heat the material liquid in the hot side volume cavity; the permeate in the cold side volume cavity is cooled by the next-stage semiconductor heat pump assembly, and the heat absorbed by it is transferred to the next-stage in-situ heat transfer membrane separation unit Heat-side cavity transfer; by analogy, the semiconductor heat pump components of each level absorb heat from the cold-side volume of the in-situ heat transfer membrane separation unit at the previous level and release heat to the heat-side volume of the in-situ heat transfer membrane separation unit at that level ; The heat of the cold side cavity of the last-stage in-situ heat transfer membrane separation unit transfers heat to the environmental heat-dissipating unit through the last-stage semiconductor heat pump assembly, thereby realizing heating
  • the present invention has the following advantages and effects:
  • the energy transfer required for the membrane separation of the conventional DCMD system is completed by a heater and a cooler outside the membrane module, and there is a large space-time interval between the supply and use of energy.
  • the present invention finds that in the hot-side cavity, the distance from the heat-radiating surface of the semiconductor heat pump component to the hydrophobic microporous membrane is 1 to 5 mm; in the cold-side cavity, the heat-absorbing surface of the semiconductor heat pump component is controlled to the hydrophobic microporous membrane.
  • the distance is 1 to 5 mm; the two adjacent membrane modules are spaced apart; the heat absorption surface of the upper membrane module and the heat radiation surface of the lower membrane module are spaced 1 to 5 mm; the distance between the heat transfer surface and the membrane surface should be less than
  • the width of the temperature boundary layer can achieve "in-situ heat transfer" and effectively improve the thermal efficiency of the DCMD process.
  • the energy supply position that is, the heat transfer surface
  • the energy use position that is, the film surface
  • the heat absorption surface of the semiconductor heat pump assembly of the present invention is in direct contact with the permeate, which avoids high heat transfer resistance caused by air gap heat transfer, and improves the effective temperature difference between the hot and cold sides of the film surface fluid.
  • the heat absorbing surface and the heat radiating surface of the semiconductor heat pump module of the present invention perform heat exchange through the heat radiating surface and the heat absorbing surface of the adjacent semiconductor heat pump module, respectively, which shortens the space distance for energy supply and use, and avoids the need for external installation.
  • the energy loss caused by the two fluid transport links from the heat exchange equipment to the membrane module and from the membrane module inlet to the membrane surface also slows down the effect of polarization.
  • the present invention uses economical semiconductor refrigeration chips to replace the traditional heat pump cycle, which can conveniently develop a multi-stage DCMD system at a lower cost.
  • membrane separation units at all levels have only two cold and hot sides with a thickness not exceeding 5mm, and there are no internal components such as metal fins in the cavity. Effectively reduce the size of the membrane module, and can completely use lightweight materials such as plastic to manufacture membrane units at all levels, achieving compactness and lightness of the DCMD system, and significantly reducing the configuration cost of the MD system.
  • the present invention effectively avoids the "dead zone” and “short circuit” phenomena without significantly increasing the flow energy consumption, and further improves the separation efficiency of the membrane module.
  • FIG. 1 is a schematic structural diagram of a multi-stage membrane module with an integrated semiconductor heat pump according to the present invention
  • FIG. 2 is a schematic structural diagram of a combination of an in-situ heat transfer membrane separation unit and a semiconductor heat pump assembly
  • FIG. 3 is a schematic structural diagram of a membrane distillation system established by applying a multi-stage membrane module of an integrated semiconductor heat pump of the present invention
  • FIG. 4 is a schematic structural diagram of a conventional two-stage parallel DCMD system and membrane separation units at each stage in Comparative Examples 1, 2 and 3;
  • FIG. 5 is a schematic structural diagram of a two-stage membrane module of an integrated semiconductor heat pump described in Examples 1, 2 and 3;
  • FIG. 6 is a schematic structural diagram of a membrane distillation system established by using an integrated semiconductor heat pump secondary membrane module in Examples 1, 2 and 3;
  • FIG. 7 is a curve of the concentration rate with time of Comparative Example 1 and Example 1;
  • FIG. 9 is a curve of the concentration rate with time of Comparative Example 3 and Example 3.
  • a multi-stage membrane module integrated with a semiconductor heat pump is composed of an environmental heat absorption unit 11, an environmental heat dissipation unit 12, and a multi-stage membrane module.
  • the multi-stage membrane module includes a plurality of in-situ heat transfer membrane separation units 14 separated by a semiconductor heat pump module 13.
  • the structure of each in-situ heat transfer membrane separation unit 14 is shown in FIG. 2.
  • the in situ heat transfer membrane separation unit 14 includes a hydrophobic microporous membrane 21, a hot-side volume 25, a cold-side volume 29, a material liquid inlet channel 22, a material liquid outlet channel 26, a permeate liquid inlet channel 23, and a permeate liquid outlet channel 27. .
  • a hot-side volume 25 and a cold-side volume 29 are respectively provided; the hot-side volume 25 is provided with a material liquid inlet channel 22 at one end and a material-liquid outlet channel 26 at the other end; the cold-side volume 29 One end is provided with a permeate inlet channel 23 and the other end is provided with a permeate outlet channel 27.
  • a semiconductor heat pump module 13 is arranged between two adjacent membrane modules, and the heat absorption surface of the semiconductor heat pump module 13 is closely attached to the first stage membrane module. On the cold side cavity 29, the heat dissipation surface of the semiconductor heat pump module 13 is closely adjacent to the heat side cavity 25 of the next-stage membrane module.
  • the distance from the heat dissipation surface 24 of the semiconductor heat pump module to the hydrophobic microporous membrane 21 is 1 to 5 mm; the distance from the heat-absorbing surface 28 of the semiconductor heat pump module to the hydrophobic microporous membrane 21 is 1 to 5 mm in the cold-side chamber 29; the environmental heat absorption unit 11 is close to the hot-side chamber of the first-stage membrane module
  • the heat absorption surface of the semiconductor heat pump module 13 and the heat radiation surface of the semiconductor heat pump module 13 are connected to the first-stage membrane module hot-side volume 25; the ambient heat-dissipating unit 12 is close to the semiconductor heat pump of the last-stage membrane module cold-side volume.
  • the heat radiation surface of the module 13 and the heat absorption surface of the semiconductor heat pump module 13 The cold-side volume 19 of the latter-stage membrane module is connected.
  • the present invention uses "in-situ heat transfer" to directly transfer heat near the membrane, that is, the heat dissipation surface 24 and heat absorption surface 28 of the semiconductor heat pump module 13 to the hydrophobic microporous membrane
  • the distances of 21 are 1 to 5 mm, respectively, so that the heated and cooled fluid directly contacts the heat dissipation surface and the heat absorption surface, and by reducing the space-time distance of energy transmission and conversion, the average temperature difference between the two sides of the hydrophobic microporous membrane 21 is increased. It also relieves the polarization effect, thereby improving heat transfer and separation efficiency.
  • the environmental heat absorption unit of the present invention may use a natural convection air heat exchanger, and the environmental heat dissipation unit may use a forced convection air radiator.
  • the natural convection air heat exchanger preferably adopts a natural flow fin-type refrigeration heat exchanger, and the fin size is 60x10x1.5mm.
  • the forced convection air radiator adopts aluminum fin fan cooler. The cooling fan comes with a standard 5V power management function, and the maximum cooling power is 360W.
  • Each of the semiconductor heat pump components 13 includes a mounting frame and a semiconductor refrigerating sheet.
  • the semiconductor refrigerating sheet uses a model number of TEC1-19006 with a size of 40x40x4mm and is embedded in a heat-resistant epoxy resin mounting frame.
  • the semiconductor heat pump module 13 uses a thermoelectric effect (Peltier effect) to transfer heat from a low-temperature heat absorption surface 28 to a high-temperature heat radiation surface 24.
  • multiple material liquid inlets are provided at both ends of the hot side cavity 25, respectively.
  • Channel 22 and material liquid outlet channel 26 the axis of any material liquid inlet channel 22 and any material liquid outlet channel 26 are not collinear; a plurality of permeate liquid inlet channels 23 are respectively provided at both ends of the cold-side volume cavity 29
  • the permeate outlet channel 27 the axis of any of the permeate inlet channel 23 and the axis of any of the permeate outlet channel 27 are not collinear.
  • the material liquid enters the hot-side volume cavity 25 through the material-liquid inlet channel 22, and is heated and heated by the semiconductor heat pump component 13; the permeate enters the cold-side volume through the permeate inlet channel 23.
  • the cavity 29 is cooled by the heat absorption of the semiconductor heat pump module 13.
  • a temperature difference is formed on both sides of the hydrophobic microporous membrane 21, that is, the water vapor pressure on the material liquid side is higher than that on the permeate side, and the water vapor in the membrane pores is moved from the material liquid side to the permeation side by the vapor pressure difference, thereby realizing the material
  • the liquid-side evaporation is concentrated and water is enriched on the permeate side.
  • a multi-stage membrane module integrated with a semiconductor heat pump is used to make the hot side chambers of the in-situ heat transfer membrane separation units of the multi-stage membrane module integrated with the semiconductor heat pump in parallel, and the parallel ends are respectively connected to the material and liquid storage.
  • the tank is connected to the hot-side circulation pump, and the material-liquid storage tank and the hot-side circulation pump are connected through pipelines; at the same time, the cold-side storage chambers of the in-situ heat transfer membrane separation units of the multi-stage membrane module integrated with the semiconductor heat pump are connected in parallel and in parallel.
  • the ends are respectively connected to the permeate storage tank and the permeate circulation pump, and the permeate storage tank and the permeate circulation pump are connected through pipelines; an economical, efficient and new DCMD system is formed.
  • the new DCMD system is mainly composed of a feed liquid storage tank 31, a hot-side circulation pump 32, a multi-stage membrane module 33 integrated with a semiconductor heat pump, a permeate storage tank 34, and a permeate circulation pump 35.
  • the side circulation pump 32 is connected, and the hot side circulation pump 32 is connected to the material and liquid inlet channels of the multiple heat side cavities of the multi-stage membrane module 33 integrated with the semiconductor heat pump through pipes.
  • the material-liquid outlet channel of the hot-side volume is connected to the material-liquid storage tank 31 through pipes; the permeate liquid storage tank 34 is connected to the permeate liquid circulation pump 35 through the pipes, and the permeate liquid circulation pump 35 is connected to the multi-stage membrane of the integrated semiconductor heat pump through the pipes.
  • the permeate inlet channels of multiple cold-side containers of module 33 are connected; the permeate outlet channels of multiple cold-side containers of multiple multi-stage membrane modules 33 with integrated semiconductor heat pumps are connected to the permeate storage tank 34 through pipes, respectively.
  • the feed liquid is heated by an external heater, and the permeate is cooled by an external cooler and flows into the membrane module.
  • the membrane module With the heat and mass transfer from the hot side to the cold side, the temperature of the material liquid in the hot side cavity decreases, while the temperature of the permeate in the cold side cavity increases, which reduces both sides of the DCMD membrane. Temperature difference.
  • the polarization effect near the membrane surface further reduces the effective temperature difference between the two sides of the DCMD membrane, so the separation efficiency of traditional DCMD is lower.
  • a traditional two-stage parallel DCMD system as shown in Fig. 4 is established.
  • the traditional DCMD system specifically includes a material-liquid storage tank 41 with a volume of 500 mL and a polypropylene material, a Cole-Parmer company's Masterflex L / S type material-liquid circulation pump 42, a 2kW electric heating system 43, and a DCMD Two-stage parallel membrane module 44, 500mL volume, permeate tank 45 made of polypropylene with overflow outlet, Masterflex L / S type permeate circulation pump 46 from Cole-Parmer Company, Polystat 12122 from Cole-Parmer Company, USA Type 58 low temperature circulating water bath 47, computer 48 for data acquisition and monitoring, and analytical balance 49 for permeate overflow measurement.
  • the conventional DCMD two-stage parallel membrane module 44 includes a first-stage traditional DCMD membrane separation unit 441 and a second-stage traditional DCMD membrane separation unit 442 arranged in parallel.
  • the two-stage traditional DCMD membrane separation unit has the same structure and is made of colorless and transparent plexiglass, which includes a hot-side volume 4411 and a cold-side volume 4412 each having a size of 40x40x5mm (this structure is mainly for the convenience of the present invention. It is more convenient.
  • the width of the hot side cavity 4411 and cold side cavity 4412 is not required by the traditional DCMD system. Generally, it is much larger than this width.
  • Porous membrane 4413 is a surface modified super-hydrophobic polyvinylidene fluoride planar membrane provided by Singapore Membrane Technology Center. Its effective size is 40x40mm and the average membrane thickness is 0.018mm. Both the cold and hot sides of the cavity are provided with fluid outlet channels 4414 and fluid. Entrance channel 4415.
  • the traditional two-stage DCMD system shown in Figure 4 was used to desalinate and desalinate the sodium chloride aqueous solution.
  • the sodium chloride aqueous solution was concentrated to saturation and purified water was obtained.
  • the specific operating methods and process parameters are as follows:
  • the 3% sodium chloride aqueous solution prepared in advance is placed in the material liquid storage tank 41, the material liquid is sent to the electric heating system 43 through the material liquid circulation pump 42, and then input into the hot-side accommodating chambers 4411 of the two-stage parallel membrane module 44;
  • the ultrapure water placed in the permeate storage tank 45 is sent to the low-temperature circulating water bath 47 through the permeate circulation pump 46, and is input to the cold-side accommodating chambers 4412 of the two-stage parallel membrane module 44 after being cooled by coil heat exchange.
  • the flow rate of the liquid and permeate circulation pumps to 120 mL / min, adjust the electric heater 43 and the low-temperature circulating water bath 47 so that the two-stage parallel DCMD membrane module 44 has a hot-side chamber temperature of 57-59 ° C.
  • the permeate inlet temperature of the cold-side volume is 20 to 21 ° C.
  • the inlet and outlet temperatures of the membrane module are collected and recorded by a computer 48. In the in-situ heat transfer membrane separation units at all levels, the temperature difference between the inlets of the hot-side and cold-side chambers is about 38 ° C.
  • the film of the feed liquid in the hot-side chambers evaporates and transfers heat and mass to the cold side, thereby increasing the permeate, and the produced permeate flows out through the overflow pipe of the permeate storage tank 45, and the amount of permeate produced per unit time is measured by the balance 49.
  • the saltwater concentration rate of the DCMD system is the amount of permeate produced per unit time, and its variation curve with time is shown in FIG. 7.
  • the results show that the membrane distillation system can concentrate the sodium chloride aqueous solution to achieve desalination and desalination of the brine.
  • the traditional DCMD system initially concentrated the brine at a rate of about 18 grams per hour. With the concentration of the salt solution continuously increasing, the continuous operation After 20 hours, the sodium chloride aqueous solution was nearly saturated, and the concentration ability was reduced to 13 grams per hour due to the increase in the concentration of the feed solution.
  • the total soluble salt TDS content of wastewater is about 100g / L, mainly Mg 2+ , Fe 3+ and SO 4 2- plasma.
  • the sample wastewater is placed in the feed liquid storage tank 41, and the feed liquid is sent to the electric heating system 43 through the feed liquid circulation pump 42 and then input into the hot-side accommodating chambers of the conventional two-stage parallel membrane module 44;
  • the ultrapure water is sent to the low-temperature circulating water bath 47 through the permeate circulation pump 46, and is input to the cold-side accommodating chambers of the two-stage parallel membrane module 44 after being cooled by coil heat exchange.
  • the flow rates of the material liquid and permeate circulation pumps to 100 mL / min, adjust the electric heater 43 and the low-temperature circulating water bath 47 so that the two-stage parallel traditional DCMD membrane module 44 has a hot-side chamber temperature of 54 ⁇ 55 °C, and the permeate inlet temperature of the cold-side volume is 20 ⁇ 21 °C.
  • the inlet and outlet temperatures of the membrane module are collected and recorded by a computer 48.
  • the temperature difference between the inlets of the hot-side and cold-side chambers is about 34 ° C.
  • the feed liquid evaporates on the membrane surface of the hot-side chamber and moves towards the membrane surface.
  • the cold-side heat and mass transfer increases the permeate, and the produced permeate flows out through the overflow pipe of the permeate storage tank 45, and the amount of permeate produced per unit time is measured by the balance 49.
  • the wastewater treatment volume of the DCMD system is the permeate generation amount per unit time, and its variation curve with time is shown in FIG. 8.
  • a conventional DCMD system with a membrane area of 32 cm 2 was used for 2 hours of continuous operation, and the wastewater treatment capacity was about 14 to 15 grams per hour.
  • the milk was concentrated to increase the protein content of the milk from 5% to 10%.
  • the sample milk is placed in the feed liquid storage tank 41, and the feed liquid is sent to the electric heating system 43 through the feed liquid circulation pump 42 and then input into the hot-side accommodating chambers of the conventional two-stage parallel membrane module 44;
  • the ultrapure water is sent to the low-temperature circulating water bath 47 through the permeate circulation pump 46, and is input to the cold-side accommodating chambers of the two-stage parallel membrane module 44 after being cooled by coil heat exchange.
  • Set the flow rate of the material liquid and permeate circulation pumps to 100 mL / min, adjust the electric heater 43 and the low temperature circulating water bath 47 to make the two-stage parallel DCMD membrane module 44 feed temperature of the hot-side volume of each stage is 55-56.
  • the permeate inlet temperature of the cold-side volume is 20 ⁇ 21 °C.
  • the inlet and outlet temperatures of the membrane module are collected and recorded by a computer 48.
  • the temperature difference between the inlets of the hot-side and cold-side chambers is about 35 ° C.
  • the feed liquid evaporates on the membrane surface of the hot-side chamber and moves towards the membrane surface.
  • the cold-side heat and mass transfer increases the permeate, and the produced permeate flows out through the overflow pipe of the permeate storage tank 45, and the amount of permeate produced per unit time is measured by the balance 49.
  • the milk concentration rate of the DCMD system is the amount of permeate produced per unit time, and its change curve with time is shown in FIG. 9.
  • the milk concentration rate was about 13 to 14 grams per hour through continuous operation for 6 hours.
  • the two-stage membrane module with integrated semiconductor heat pump shown in FIG. 5 is established according to the structure of FIGS. 1-3.
  • the two-stage membrane module 50 with integrated semiconductor heat pump includes: an environmental heat absorption unit 51, a first-stage semiconductor heat pump module 52, and a first The first-stage in-situ heat transfer membrane separation unit 53, the second-stage semiconductor heat pump assembly 54, the second-stage in-situ heat transfer film separation unit 55, the third-stage semiconductor heat-pump assembly 56, and the ambient heat dissipation unit 57.
  • the environmental heat absorbing unit 51 uses an aluminum natural flow fin refrigeration heat exchanger, and the fin size is 60x10x1.5mm.
  • the first-stage semiconductor heat pump assembly 52, the second-stage semiconductor heat pump assembly 54 and the third-stage semiconductor heat pump assembly 56 have the same structure, and all include a mounting frame and a semiconductor refrigeration sheet.
  • the semiconductor refrigeration sheet is selected as TEC1-19006 and has a size of TEC1-19006. 40x40x4mm, mounted on heat-resistant epoxy mounting frame.
  • the first-stage in-situ heat-transfer membrane separation unit 53 and the second-stage in-situ heat-transfer membrane separation unit 54 have the same structure and are made of plexiglass.
  • the dimensions of the hot-side and cold-side chambers are both 40x40x5mm.
  • the effective volume is 8 mL (for ease of comparison, the dimensions of the membrane modules of each stage in Example 1 are the same as those described in Comparative Example 1).
  • the diameter of the hot side cavity is uniformly distributed on the side of the feed.
  • 10 diameter environmental cooling units 57 adopts aluminum fin fan cooler, and the cooling fan comes with a standard 5V power management function, the maximum cooling power is 360W. It is a 1.8mm feed channel. Nine discharge channels with a diameter of 1.8mm are evenly distributed on the discharge side, and none of the inlet channels coincide with the axis of the outlet channel. The feed side of the cold-side cavity is evenly distributed.
  • 1.8mm diameter feeding channels 10 discharge channels with a diameter of 1.8mm are evenly distributed on the discharge side, and none of the inlet channels coincide with the axis of the outlet channel; for better monitoring of the membrane separation status,
  • PT100 thermal resistance temperature sensors connected to the computer acquisition system in the hot-side and cold-side chambers of the in-situ heat transfer membrane separation units at all levels;
  • the hydrophobic microporous membrane uses surface-modified super-hydrophobic polyisotropic provided by Thermo Fluoroethylene flat film (product number 88518), effective size after cutting is 40x40mm, average film thickness is 0.018mm.
  • the DCMD system shown in FIG. 6 was developed for desalination of sodium chloride brine according to the process shown in FIG. 3, and the purpose of the process was the same as that of Comparative Example 1, that is, the concentrated salt solution was saturated to obtain purified water.
  • the DCMD system specifically includes a material-liquid storage tank 61 with a volume of 500 mL and a material of polypropylene, a set of Masterflex L / S type material-liquid circulation pumps 62 from the Cole-Parmer Company in the United States, and a set of FIG.
  • a two-stage membrane module 63 with integrated semiconductor heat pump shown (the specific structure is shown in Figure 5), a permeate storage tank 64 with a volume of 500 mL, made of polypropylene with an overflow outlet, and a set of Masterflex from Cole-Parmer L / S type permeate circulation pump 65;
  • it also includes three DC adjustable power supplies 66 with a rated power of 300W, a computer 67 for data acquisition and monitoring, and an analytical balance for permeate overflow measurement.
  • An analytical balance 68 for permeate overflow measurement is connected to the permeate storage tank 64.
  • Pre-prepared 3% sodium chloride aqueous solution and ultrapure water are placed in the material liquid storage tank 61 and the permeate liquid storage tank 64, respectively.
  • the material liquid and ultrapure water are passed through the hot-side circulation pump 62 and the cold-side circulation pump 65, respectively.
  • the hot- and cold-side receptacles in the two-stage membrane module 63 are input. Set the output voltage of the DC power supply driven by the semiconductor heat pump components at all levels to be constant 24V, adjust the flow of the hot-side circulation pump 62 and the cold-side circulation pump 65, so that the temperature of the material liquid in the hot-side volume is stabilized at 57 ° C, and the cold-side volume
  • the temperature of the ultrapure water in the cavity was about 20 ° C.
  • the temperature of the cold and hot-side containers of the in-situ heat transfer membrane separation units at each level is collected and recorded by the computer 67 (the computer temperature acquisition module is connected to the thermal resistance of the two-stage membrane module at each level), and the average temperature of the hot-side storage cavity is maintained to be lower than that of the cold-side.
  • the cavity is 37 ° C high.
  • the feed liquid evaporates on the membrane surface of the hot side cavity and transfers heat and mass to the cold side, thereby increasing the permeate, and the produced permeate passes through the permeate storage
  • the overflow pipe of the tank 64 flows out, and the amount of permeate generation per unit time is measured by the balance 68.
  • the saltwater concentration rate of the DCMD system is the amount of permeate produced per unit time, and its variation curve with time is shown in FIG. 7.
  • the results show that the two-stage membrane distillation system with integrated semiconductor heat pump can concentrate the sodium chloride aqueous solution to achieve desalination of brine.
  • a membrane system with a membrane area of 32 cm 2 was used to initially concentrate the brine at a rate of approximately At 25 grams per hour, the salt concentration of the feed liquid is continuously increasing with concentration. After 20 hours of continuous operation, the sodium chloride aqueous solution is nearly saturated, and the concentration ability is reduced to 18 grams of water per hour due to the increase in the concentration of the feed liquid.
  • Example 1 demonstrates that the multi-stage membrane distillation system with integrated semiconductor heat pump can run stably for a long time, and at the same time realize the concentration of sodium chloride aqueous solution and the production of pure water, thereby indicating that the method of the present invention can be expected to be applied to mineral salt recovery and seawater Desalination and other fields.
  • the present invention Compared with the conventional membrane distillation system described in Comparative Example 1, the present invention has higher membrane separation efficiency. For the same membrane material and membrane area, under the same operating conditions as shown in FIG. 7, the concentration capacity of the sodium chloride solution of Example 1 is increased by more than 1/3 than that of Comparative Example 1. This is because the two-stage membrane module with integrated semiconductor heat pump described in Example 1 (as shown in FIG. 5) applied the "in-situ heat transfer" method and optimized the flow channel design scheme, thereby effectively improving the heat and mass transfer efficiency. .
  • the multi-stage membrane module of the present invention (as shown in Figure 1, Figure 2 and Figure 5) (Shown in Figure 3) and the membrane distillation system (shown in Figures 3 and 6) built thereby not only avoids the use of compressors, cold and heat exchangers and other components necessary in traditional heat pump methods, but also avoids the use of complex membrane groups
  • the components effectively reduce the module size, thereby significantly reducing the complexity and cost of the system configuration, which is convenient for the system to be enlarged and applied to the actual industrial field.
  • Example 2 The same DCMD system as in Example 1 was used to treat the same salt-containing wastewater from a steel plant as described in Comparative Example 2.
  • Example 2 Using a similar operation method as in Example 1, the salt-containing wastewater and the ultrapure water were respectively placed in the material liquid storage tank 61 and the permeate liquid storage tank 64, and the material liquid (salt-containing wastewater) and the ultrapure water were passed through the hot-side circulation pump, respectively.
  • 62 and the cold-side circulation pump 65 are input to the hot-side and cold-side accommodating chambers in the two-stage membrane module 63, respectively.
  • the temperature of the feed liquid and the permeate is the same, that is, the temperature of the hot side cavity is 54 to 55 ° C, and the temperature of the cold side cavity is 20 to 21 ° C.
  • the temperature of the cold and hot-side containers of the in-situ heat transfer membrane separation units at each level is collected and recorded by the computer 67 (the computer temperature acquisition module is connected to the thermal resistance of the two-stage membrane module at each stage), and the average temperature of the hot-side volume is maintained to be lower than that of the cold-side
  • the cavity is 34 ° C high.
  • the feed liquid evaporates on the membrane surface of the hot side cavity and transfers heat and mass to the cold side, thereby increasing the permeate, and the produced permeate passes through the permeate storage
  • the overflow pipe of the tank 64 flows out, and the amount of permeate generation per unit time is measured by the balance 68.
  • the wastewater treatment volume of the DCMD system is the permeate generation amount per unit time, and its variation curve with time is shown in FIG. 8.
  • the results show that the two-stage membrane distillation system with integrated heat pump can stably process salt-containing wastewater.
  • a membrane system with a membrane area of 32 cm 2 was continuously operated for 2 hours and the wastewater treatment capacity was stabilized at 19-20 grams. This indicates that the method of the present invention can be expected to be applied to the fields of saline wastewater treatment and the like.
  • the present invention Compared with the conventional membrane distillation system described in Comparative Example 2, the present invention has higher membrane separation efficiency. As shown in FIG. 8, the membrane module described in Example 2 and Comparative Example 2 have the same membrane area, and the processing capacity of the salt-containing wastewater has increased by more than 40% under the same feed temperature. This is due to Example 1
  • the two-stage membrane module of the integrated heat pump (as shown in FIG. 5) applies the “in-situ heat transfer” method and optimizes the flow channel design scheme, thereby effectively improving the heat and mass transfer efficiency of the process.
  • the method of the invention has the advantages of economy and easy configuration, and it is expected to be applied to practical industrial fields through multi-stage amplification.
  • the milk sample and ultrapure water were placed in the feed liquid storage tank 61 and the permeate liquid storage tank 64, respectively.
  • the feed liquid (milk) and ultrapure water were passed through the hot-side circulation pump 62 and cold respectively.
  • the side circulation pump 65 is input into a hot-side and a cold-side volume in the two-stage membrane module 63, respectively.
  • the temperature of the cold and hot-side containers of the in-situ heat transfer membrane separation units at each level is collected and recorded by a computer 67 (the computer temperature acquisition module is connected to the thermal resistance of the two-stage membrane module at each level), and the average temperature of the hot-side cavity is maintained to be lower than that of the cold-side
  • the cavity is 35 ° C high.
  • the feed liquid evaporates on the membrane surface of the hot side cavity and transfers heat and mass to the cold side, thereby increasing the permeate, and the produced permeate passes through the permeate storage
  • the overflow pipe of the tank 64 flows out, and the amount of permeate generation per unit time is measured by the balance 68.
  • the milk concentration of the DCMD system is the amount of permeate produced per unit time, and its change curve with time is shown in FIG. 9.
  • the results show that the two-stage membrane distillation system with integrated heat pump can stably concentrate milk.
  • a membrane system with a membrane area of 32 cm 2 was continuously operated for 7 hours and the milk concentration was stabilized at 20 to 22 g / hour. This shows that the method of the present invention is expected to be applied to the field of food concentration such as milk juice.
  • the present invention Compared with the conventional membrane distillation system described in Comparative Example 3, the present invention has higher membrane separation efficiency. As shown in FIG. 9, the membrane modules described in Example 3 and Comparative Example 3 have the same membrane area, and the processing capacity of milk increases by nearly 50% under the same feed temperature condition. This is due to the integration described in Example 1.
  • the two-stage membrane module of the heat pump (as shown in Figure 5) applied the "in-situ heat transfer" method and optimized the flow channel design scheme, thereby effectively improving the heat and mass transfer efficiency of the process.
  • the invention also has the advantages of economy and easy configuration, and is expected to be applied to the actual industrial production field through multi-stage amplification.

Abstract

L'invention concerne un ensemble membrane à étages multiples intégré à une pompe à chaleur à semi-conducteur et son utilisation dans la distillation à membrane. L'ensemble membrane à étages multiples intégré à la pompe à chaleur à semi-conducteur est principalement constitué d'une unité d'absorption de chaleur d'environnement (11), d'une unité de dissipation de chaleur d'environnement (12) et d'un ensemble membrane à étages multiples ; une unité de séparation de membrane de transfert de chaleur in situ (14) comprend une membrane microporeuse hydrophobe (21), une cavité côté chauffage (25), une cavité côté refroidissement (29) et un canal d'entrée et de sortie de fluide ; la cavité côté chauffage (25) et la cavité côté refroidissement (29) sont disposées sur deux côtés de la membrane microporeuse hydrophobe (21), respectivement ; un ensemble pompe à chaleur à semi-conducteur (13) est disposé entre deux étages adjacents d'ensembles membrane, une surface d'absorption de chaleur de l'ensemble pompe à chaleur à semi-conducteur (13) étant fixée à la cavité côté refroidissement (29) de l'étage supérieur de l'ensemble membrane, et une surface de dissipation de chaleur de l'ensemble pompe à chaleur à semi-conducteur (13) étant fixée à la cavité côté chauffage (25) de l'étage inférieur de l'ensemble membrane ; et la distance entre la surface de dissipation de chaleur ou la surface d'absorption de chaleur de l'ensemble pompe à chaleur à semi-conducteur (13) et la membrane microporeuse hydrophobe (21) étant de 1 à 5 mm La chaleur nécessaire à la séparation est directement transférée à une région adjacente à la membrane, améliorant l'efficacité de séparation de membrane, réduisant la consommation d'énergie et le coût d'utilisation du procédé de distillation à membrane pour le processus d'évaporation et de concentration tel que le dessalement de l'eau de mer, le traitement des eaux d'égout et la concentration d'aliments.
PCT/CN2018/112108 2018-09-21 2018-10-26 Ensemble membrane à étages multiples intégré à une pompe à chaleur à semi-conducteur et son utilisation dans la distillation à membrane WO2020056847A1 (fr)

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