CN102989319A - Apparatus and method for microwave enhanced membrane distillation process - Google Patents
Apparatus and method for microwave enhanced membrane distillation process Download PDFInfo
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- CN102989319A CN102989319A CN2011102748189A CN201110274818A CN102989319A CN 102989319 A CN102989319 A CN 102989319A CN 2011102748189 A CN2011102748189 A CN 2011102748189A CN 201110274818 A CN201110274818 A CN 201110274818A CN 102989319 A CN102989319 A CN 102989319A
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Abstract
The present invention provides an apparatus and a method for a microwave enhanced membrane distillation process. According to the present invention, a microwave reaction chamber for microwave and negative pressure operation is manufactured, and comprises six parts such as a chamber, a chamber top cover, a microwave head interface, a component fixation flange, a pressing flange and a membrane head locking member; a membrane assembly for operation in a microwave field is designed and manufactured, penetrates through the component fixation flange on the chamber, and is fixed through the pressing flange, the membrane head locking member, a silica gel gaskets and other accessories; a microwave magnetron is connected with the chamber top cover through the microwave head interface so as to achieve a microwave environment in the chamber; and a water circulating pump, steam catching, condensation and other equipment are complemented so as to achieve organic combination of microwave radiation, the membrane assembly and the membrane distillation process, such that the microwave enhanced membrane distillation process can be achieved, and microwave-assisted online cleaning and drying of pollution films can be concurrently achieved.
Description
One technical field
The invention belongs to the film distillation technology field, specially refer to a kind of method and apparatus of microwave auxiliary film distillation desalting technology.
Two background technologies
The fast development of film distillation (MD) technology since nearly 30 years driven the continuous breakthrough of hydrophobic microporous membrane preparation technology.The advantages such as wherein, hollow-fibre membrane is with its higher loading density, and assembly is easy to fitting operation, and floor space is little become the film distillation gradually with the first-selection of film.Although the film distillation technology development is very fast, study also more and more extensive, but the film distillation to be applied to actual production, still face three problem demanding prompt solutions: 1) hollow fiber hydrophobic membrane of current phase inversion commonly used preparation is for pursuing membrane flux, and so that membranous wall is thick thinner, cause film silk mechanical strength lower, actual life is shorter; 2), in the film distillation running, temperature polarization, concentration polarization, channelling effect cause membrane flux to descend; 3) film pollutes and the film wetting phenomena is difficult to avoid, and currently there is no efficient cleaning and drying means, so that film distillation stable operating performance is relatively poor.Address the above problem, can be from two aspects, the one, by improving existing hydrophobic membrane technology of preparing, prepare the more better film distillation of high hydrophobicity doughnut membrane material of intensity, bibliographical information is arranged, carry out the surface super hydrophobic modification of pvdf membrane by adopting solution phase to shift cladding process, can change the physical aspect structure on film surface, can reach 160 ° so that the contact angle of PVDF hydrophobic membrane is the highest; The 2nd, by the membrane distillation technique system of development of new, affect the phenomenon of membrane flux in the hope of alleviating film pollution and temperature difference polarization etc., come the reinforced film still-process.There is no under the prerequisite of important breakthrough in the membrane material preparation, the membrane distillation technique system of development of new just seems particularly important, and this mainly comprises the design of membrane module and the design of reactor.The foreign study personnel pass through to add the members such as graticule mesh in runner, or make film silk configuration complicated to alleviate temperature polarization and the concentration polarization phenomenon in the film still-process, have strengthened mass transport process.Bibliographical information is also arranged, adopt ultrasonic technology to strengthen the vacuum membrane distillation process and obtained good result, but the ultra sonic machinery oscillation action is comparatively serious to the membrane material damage, and noise is large in the operating process, ultrasonic thermal energy loss is large, and its application prospect is also pessimistic.
Microwave technology is a very ripe technology, has been widely used in the various aspects of social life, such as medical treatment, and drying sterilizing, solid waste is processed, heating of food etc.The operation principle of microwave can be summed up as the effect of two aspects, fuel factor and non-thermal effect, fuel factor refers to material even Fast Heating in microwave field, the principle of heating using microwave is, when polar molecule is in the microwave electric field, can induce the generation electric dipole, and electric dipole can be along with the several hundred million inferior high speed break-ins of the alternating electric field generation per second that microwave produces, in the break-in process, friction generates heat between adjacent molecule, the apparent upper so that Fast Heating of material own, namely fuel factor is mainly reflected in rapidity and the uniformity of heating; Non-thermal effect refers to polar molecule at the microwave field microwave energy absorbing, so that the locomitivity of molecule is strengthened.Our result of study shows that microwave technology and film distillation technology are integrated, can alleviate the temperature polarization phenomena of MD, and strengthens the mass transfer rate of MD, and then can improve the MD membrane flux, improves the quick separation of volatile solutes in the solution; Also can utilize microwave technology to realize auxiliary Rapid Cleaning and the rapid draing of film.Therefore, integrated three the main key issues that are expected to solve above-mentioned restriction MD industrial applications by microwave technology and MD technology.
In a word, method and the relevant apparatus of microwave reinforced film still-process have not yet to see report, and this invention has obvious novelty and application prospect.
Three summary of the invention
The present invention proposes microwave technology and film distillation technology are coupled, and designs and produces out a kind of on-line cleaning that realizes the high yield water flux, realizes polluted membrane with dry, and the membrane distillation technique device of large-scale application prospect can be arranged in actual production.The capital equipment and the material that adopt comprise: dewatering microporous film, microwave reaction chamber, microwave magnetron and respective accessory etc.
Starting point of the present invention is to solve to a certain extent some problems that exist in the film still-process, mainly is the problem that membrane flux was low and film pollutes after scale was used here.Wherein, the basic restraining factors of membrane flux are the temperature on feed liquid side form surface, that the assembly import and export temperature difference was larger after membrane module amplified on the one hand, cause the membrane flux of unit effective film area lower, the membrane area utilization rate descends, the problem of temperature polarization on the other hand, so-called temperature polarization refers in the film still-process, owing to distillation is constantly taken away heat and caused face place feed temperature to be lower than the temperature of feed liquid main body, the correlative study of film distillation is verified, and the temperature polarization is to affect the very important phenomenon of flux of membrane distillation.
It also is a key factor of restriction film still-process that film pollutes, film pollutes and comes from the film distillation long-play process, solute in the feed liquid to be separated is in the deposition on film surface, can affect the flux of film distillation and the purity of product after film is seriously polluted, pollute at present membrane washing and the dry also main conventional method that adopts, namely adopt the chemical acid alkali cleaning agent to clean polluted membrane, the wet film after the cleaning or natural drying or dry up with air compressor, efficient is lower.
Address the above problem, the current feed liquid side that mainly relies on increases " disturbance factor ", as increasing feed velocity, graticule mesh etc. is set.But especially import and export the long membrane module of flow process for scale, the mechanical disturbance effect is limited after all, and increases the consumption that mechanical disturbance can increase power, makes the aggravation of technical construction complexity.
Coupling integration by microwave and film distillation can address the above problem better, efficient all heat phase of microwave and " mechanical little stirring " effect can realize in long membrane module flow process the homogeneity of temperature, and can alleviate to a certain extent temperature polarization and film contamination phenomenon, and help to pollute membrane washing and drying.
Manufacturing and designing of apparatus of the present invention need be considered emphatically the following aspects: the dewatering microporous film that adopt (1) should have very good nonpolar on the porous basis; (2) designed microwave reactor should be to be convenient to membrane module install, and can guarantee the dual-seal of gas and microwave; (3) designed device should have very good practical large-scale application prospect.
Basic ideas of the present invention are at first to design the membrane module that profile is applicable to operate in the microwave field, and design and produce out the microwave reaction chamber that can realize microwave and gas double sealing according to the actual size of membrane module profile; In view of security and the sealing requirements under the microwave operation, the collection of crossing film steam need be adopted the mode of gas trapping, cavity condensed exterior; And then be aided with corresponding accessory to finish this cover process unit.Based on design philosophy of the present invention, adopt doughnut film production membrane module to be convenient to realize the installation of assembly most.The below elaborates content of the present invention.
Fig. 3 has described the course of work of hollow-fibre membrane microwave distillation device, pending feed liquid enters from an end of hollow fiber film assembly 14, flow out from the other end, and be connected to form circulation with outside water pump and firing equipment, also can realize the auxiliary on-line cleaning of microwave that film pollutes by extraneous cleaning fluid storage tank, the film after the cleaning can carry out the microwave online dry; Magnetron 11 externally microwave source excites lower generation alternating electromagnetic field, enters the microwave reaction chamber through microwave head 13 hollow fiber film assembly is carried out irradiation, and radiator fan 12 is the magnetron heat radiation; Steam catching apparatus interface 9 connects external equipment with being connected, and collects film steam to the cavity condensed exterior.
Its form of described hollow fiber film assembly is that two ends have screw-type film head, wrap up without shell the centre, namely except two terminal membrane heads, the film of middle actual membrane distillation work part is naked state, namely crossing the film side is directly exposed in the microwave environment, be convenient to the microwave energy direct effect to the film silk on the one hand, avoided on the other hand increase gas collection pipeline, simplified the inside cavity structure; The film head adopts polytetrafluoroethylene (PTFE) (PTFE) material to make, because PTFE's is nonpolar good, absorbing microwave hardly, and stable in properties, the part of film head is external thread structure, this structure makes assembly be convenient to be connected with external pipe, and is convenient to it and passes assembly mounting flange on the microwave reaction chamber; Membrane module needs bonding portion to adopt epoxy resin and contracting amine hardener hard rubber to reach not two kinds of binding agents of polyurethane soft balsam of absorbing microwave, hard rubber partly is convenient to the follow-up cutting processing of assembly after solidifying, this partially absorbs microwave, be in the outside, microwave reaction chamber, but soft balsam part diaphragm is subject to damage not, this part is absorbing microwave not, and is inboard near the microwave reaction chamber; The film silk evenly distributes, and keeps certain distance between adjacent two film silks, the resistance that transmits to the external world to reduce steam and heat.
Except hollow fiber film assembly, the present invention also can adopt plate film assembly and tubular membrane component.
Described microwave reaction chamber is core of the present invention, and concrete specification is set according to the filling number of membrane module; The cavity top cover is connected in the flange mode with cavity, is easy for installation and removal with realization, is convenient to the inside cavity membrane module is installed into line operate; The assembly mounting flange is the position of membrane module in cavity fixedly, and by supported flange and the tight latch fitting locking of film head membrane module, and realization comprises the sealing of microwave field and the sealing of gas to the sealing of cavity; The cavity part directly contacts with steam, and corrosion resistance requires high, for strengthening the security of cavity under negative-pressure operation, adopts thick high-quality 316 corrosion resistant plates of 3mm to make, and according to actual requirement, reinforcement can be installed in the cavity outside; Other accessory requires lower relatively, adopts 304 stainless steels to make.All parts that contact with microwave of device interior need polish smooth, and prevent from striking sparks in microwave field.
Described microwave reaction chamber is according to the requirement of microwave cavity, and profile can be designed as cylinder, cuboid, cube etc.
The installation of described hollow fiber film assembly microwave film distillation as shown in Figure 3.Microwave magnetron and radiator fan are attached to inner on the microwave head of cavity, the magnetron utmost point embeds microwave head, the cavity of microwave energy by microwave head enters the microwave reaction chamber and acts on the membrane module, wherein, it is the pad of the PTFE material of 3mm that recess between microwave head and microwave head interface embeds thickness, play on the one hand sealing function, and PTFE material excessive distortion of unlikely generation in the subnormal ambient of cavity that rigidity is stronger, the PTFE material is very weak to the absorption of microwave on the other hand, can obviously not weaken microwave energy; When many assemblies are installed in the microwave reaction chamber, need evenly to install, and keep the distance of about 2cm between adjacent component, transmit the space to increase steam, avoid accumulating the vapor absorption microwave energy and cause heat in cavity, to gather in a large number, increase resistance to mass tranfer.
Based on the difference of crossing film distillation vapour Trapping ways, the present invention can adopt gas to sweep the distillation of formula film and two kinds of modes of operation of vacuum membrane distillation, and in view of the vacuum membrane distillation flux is higher, its application prospect is better.
In sum, basic goal of the present invention is that microwave and film still-process are combined, membrane module by designing and producing microwave reaction chamber and respective shapes is to realize this purpose, thereby realize increasing membrane flux, alleviate the target that temperature polarization and film pollute, prolong the stable operation cycle of film still-process, and inhibition and the on-line cleaning polluted for film provide brand-new thinking and method with drying.
Four description of drawings
Accompanying drawing 1 is suction type hollow fiber film assembly figure; Accompanying drawing 2 is microwave reaction chamber and accessory figure; Accompanying drawing 3 is hollow fiber film assembly microwave vacuum film distillation installations diagram.Wherein, the thin camber line in whole accompanying drawings represents external screw thread.
Accompanying drawing 1 be among the present invention without shell type hollow fiber film assembly structural representation.Among the figure, the 1st, screw-type film head, the heavy line in 2 represents hollow fiber film thread.
Accompanying drawing 2 is the capital equipment microwave reaction chambeies among the present invention, is all made by stainless steel.Among the figure, the 3rd, the cavity top cover, the 4th, the microwave head interface, the 5th, the tight latch fitting of film head, the 6th, supported flange, the 7th, the assembly mounting flange, the 8th, cavity, the 9th, the vacuum meter interface, 9 and 10 is the gas apparatus interface.Microwave head interface 4 is welded on the cavity top cover, assembly mounting flange 7 be welded on the cavity.
Five specific embodiment
In view of vacuum membrane distillation process flux is larger, present embodiment adopts respectively vacuum membrane distillation and microwave vacuum film distillation procedure, and carries out the auxiliary on-line cleaning of microwave and the drying of polluted membrane, and concrete range of application of the present invention is not subjected to the restriction of present embodiment.The below verifies exploitativeness of the present invention take sodium-chloride water solution as feeding liquid by comparative test.
Primary condition:
(1) feeding liquid: the NaCl aqueous solution, electrical conductivity are about 6000 μ s/cm; Cleaning fluid: deionized water, electrical conductivity are about 2 μ s/cm; Microwave power 1000W;
(2) cavity parameters: cavity specification 350mm * 215mm * 330mm, cavity volume 25L;
(3) hollow fiber film assembly parameter: PVDF hollow fiber film assembly, film head diameter 320mm, effective active length 180mm, effective film area 0.107m
2
(4) in the running, ignore micro-feed liquid loss.
Operational mode:
(1) film distillation
Setting feeding temperature is 60 ℃, and vacuum is-96kPa charging flow velocity 0.14m/s.
Operation and operation: respectively with the external microwave source of magnetron, water pump, material liquid tank and firing equipment outside the membrane module two ends, the external condensation of vacuum equipment interface and vaccum-pumping equipment are to form the continuous operation mode of device.The NaCl aqueous solution circulates in membrane module and material liquid tank, and vacuum equipment makes the subnormal ambient of cavity formation-96kPa, crosses the film water steam and enters condensing plant condensation collection by pipeline, moves respectively the film still-process before microwave starting and after starting.
In the vacuum membrane distillation running, the feed liquid in the material liquid tank can constantly reduce, and adopts successional moisturizing facility to replenish pure water here in tank, to keep the constant concentration of feed liquid.Carried out respectively vacuum membrane distillation and microwave vacuum film still-process each 100 hours, and continuous monitoring electrical conductivity, the result shows, both product water conductivities are all basicly stable about 2 μ s/cm, but the membrane flux of microwave vacuum film still-process is 1.9 times of vacuum membrane distillation, forgo microwave to the heating factor of feed liquid by calculating, and microwave still makes the mass tranfer coefficient of vacuum membrane distillation improve 26%.But proved microwave action reinforced film distillation mass transport process, therefore can realize the purpose of high yield water flux.
(2) the auxiliary on-line cleaning of the microwave of polluted membrane and drying
Setting rinse liquid temperature is 30 ℃, and flow velocity is 0.40m/s.
Operation and operation: at first with high concentration NaCl aqueous solution operation long period film still-process, when membrane flux drops to about 50% of initial flux, when namely obviously a large amount of NaCl crystalline solid appears in face, the stopper film still-process.Junctional membrane pollutes cleaning equipment and pipeline, the pipeline connected mode is similar to above-mentioned film still-process, just change material liquid tank into cleaning fluid tank, in cleaning fluid tank, add washed with de-ionized water liquid 500mL, carry out respectively 10 minutes conventional the cleaning and the auxiliary cleaning of microwave of polluted membrane, before cleaning and in the cleaning process, can two kinds of import and export rinse liquid temperature mean values under the cleaning condition all be remained on about 30 ℃ by regulating firing equipment, to guarantee except microwave two kinds of uniformity of cleaning other condition.Wash result is, the electrical conductivity of washed with de-ionized water liquid is increased to 520 μ s/cm after conventional the cleaning, and after microwave cleaned, the electrical conductivity of washed with de-ionized water liquid was increased to 780 μ s/cm, and this shows that the efficient that microwave cleans is conventional 1.5 times of cleaning.
Above comparative test has proved exploitativeness of the present invention.
Claims (7)
1. the device and method of a microwave reinforced film still-process comprises membrane module, microwave reaction chamber, microwave magnetron and related accessory; Membrane module and outside water pump, firing equipment and material liquid tank are connected to form circulation; By microwave source and corresponding mulch film distillation procedure mode, to realize microwave reinforced film still-process.
2. the device and method of a microwave reinforced film still-process is characterized in that: only the material liquid tank that membrane module is connected with external equipment need to be changed and do cleaning fluid tank, just can realize cleaning and drying that film in the film still-process is polluted under microwave action.
3. according to microwave reaction claimed in claim 1 chamber, it is characterized in that: cavity geometry can be cylinder, and cube and cuboid, the volume of reaction chamber are 0.02m
3～20m
3
4. according to membrane module claimed in claim 1, it is characterized in that: adopt epoxy resin 711,618 and curing agent contracting amine 105, and two kinds of glue of polyurethane are the bonding making membrane module of binding agent; Assembly two terminal membrane heads are connected with external equipment with external thread type; The length of membrane module feed liquid flow process is 0.2m～2m; Membrane module can adopt flat, tubular type and doughnut formula membrane module.
5. according to membrane module claimed in claim 1, it is characterized in that: membrane material can adopt Kynoar (PVDF), polypropylene (PP), and polytetrafluoroethylene (PTFE) (PTFE) and other nonpolar hydrophobic membrane material, micropore size is 0.05～0.5 μ m.
6. according to the device and method of a kind of microwave reinforced film still-process claimed in claim 1, it is characterized in that: according to the actual production requirement, can adopt gap membrane distillation and vacuum membrane distillation operation; Can place many membrane modules in the cavity, distance is greater than 2cm between the assembly; And around the cavity except the two sides that membrane module occupies, branched microwave magnetron is installed, realization is to the Omnidirectional radiation of inside cavity; Microwave frequency can adopt 915MHz and 2450MHz.
7. according to the device and method of a kind of microwave reinforced film still-process claimed in claim 1, it is characterized in that: membrane module feed liquid effluent speed is 0.05m/s～0.5m/s, feed temperature is 50 ℃～80 ℃, and for the vacuum membrane distillation operating process, vacuum is greater than-96Kpa.
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Cited By (1)
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| CN104607065A (en) * | 2015-02-03 | 2015-05-13 | 湖州森诺膜技术工程有限公司 | PTFE (polytetrafluoroethylene) hydrophobic membrane reduction system |
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| CN101342425A (en) * | 2008-08-27 | 2009-01-14 | 武汉大学 | Microwave separation method and apparatus used thereof |
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Application publication date: 20130327 |