CN102179175B - Device and method for integrally modifying membrane module by using remote plasma - Google Patents
Device and method for integrally modifying membrane module by using remote plasma Download PDFInfo
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- CN102179175B CN102179175B CN 201110066542 CN201110066542A CN102179175B CN 102179175 B CN102179175 B CN 102179175B CN 201110066542 CN201110066542 CN 201110066542 CN 201110066542 A CN201110066542 A CN 201110066542A CN 102179175 B CN102179175 B CN 102179175B
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Abstract
The invention relates to a device and method for integrally modifying a membrane module by using remote plasma, belonging to the fields of membrane separation and plasma. The device provided by the invention comprises a vacuum pump, a discharge tube, a gas storage tank and the membrane module, wherein the discharge tube is in pipeline connection with the gas storage tank and is respectively in pipeline connection with an axial gas/liquid inlet and a lateral gas/liquid inlet of the membrane module through three-way control valves; and the axial gas/liquid outlet and the lateral gas/liquid outlet of the membrane module are simultaneously in pipeline connection with the vacuum pump through three-way control valves. The method provided by the invention comprises the following steps that: the unpolymerized gas in the gas storage tank is activated into active particles in the discharge tube; and the active particles flow through the membrane module by adopting the vacuum pump and controlling through adjusting the three-way control valves; and then the modification to the integral membrane module is realized. The invention realizes the scale modification to the integral membrane module consisting of a plurality of flat membranes or tubular membranes, thereby greatly increasing the efficiency; in addition, the directional integral modification to the inner and the outer surfaces and the hole walls of a membrane can be carried out.
Description
Technical field
The present invention relates to a kind of remote plasma that utilizes membrane module is carried out bulk modified device and method, belong to membrane separation technique and technical field of plasma.
Background technology
Membrane separation technique be utilize film to the selectivity of each component in mixture separate, the new separation technology of purification and concentrated purpose product.Energy consumption is low, separative efficiency is high, equipment is simple owing to having, convenient operation and control and the advantage such as free from environmental pollution, has been widely used in the fields such as chemical industry, medicine, light industry, food, weaving, electronics, metallurgy.So-called membrane module be membrane component with certain area with the membrane separator spare that certain form is assembled into, be the elementary cell of in the middle of engineering is used, film being installed.Film has flat sheet membrane and tubular film two classes by its shape, and wherein, tubular film has hollow-fibre membrane, periosteum, capillary-pipe film.Membrane module can be divided into three kinds of sheet frame configuration, wound configuration and tubular type configurations.Plate and frame and rolled membrane module all use flat sheet membrane, and tubular type configuration assembly can use hollow-fibre membrane, periosteum or capillary-pipe film, and corresponding membrane module is called hollow fiber film assembly, tubular membrane component and capillary-pipe film assembly.
Development along with membrane separation technique, single membrane material can not satisfy in practical application the needs to the combination properties such as PSPP, chemical stability, mechanical strength and anti-pollution and some particular separation performances, and the development of new material need expend a large amount of energy and financial resources with the film for preparing different performance, therefore, to macromolecule member material, usually adopt the method for membrane surface modification, introduce specific group or polymer side chain on the film matrix material, with the separating property of improving film or make film surface-functionalized.
The principle of plasma surface modification be non-polymerization gas in plasma reactor by plasma exciatiaon, generate the various active particles such as ion, excited state molecule, free radical, these active particle bombardment membrane materials are surperficial, produce surface free radical or form cross-linked structure, can introduce the particular functional group on the film surface, even further by with organic monomer reaction, graft polymerization, form new polymer side chain on the film surface.Plasma grafting due to have can select the monomer scope extensively, only effects on surface modification, introduce the characteristics such as the grafting layer is thin and even and get more and more people's extensive concerning.
Remote plasma is the new technology of utilizing plasma treatment that occurs the nineties in last century.Process different from traditional plasma, sample is not to be positioned over region of discharge, but leave region of discharge one segment distance, because the free radical in plasma has than electronics and longer life-span of ion, therefore, in the position away from region of discharge, the concentration of free radical is higher, and the concentration of electronics, ion is lower, thereby has reduced the damage that the bombardment of sample is caused due to high energy active particles such as electronics, ions, be conducive to control goal response, particularly strengthen the chemical reaction that free radical causes.
The utility model patent (CN101530777A) that the domestic Chen Jie Rong of Xi'an Communications University applies for discloses a kind of Plasma chemical reaction device, comprises vavuum pump, discharge reaction tube, is wrapped in inductance coil, radio-frequency power supply and air accumulator on the import pipeline section of discharge reaction tube.It is characterized in that, also comprise the radical reaction chamber as remote locations, its outlet is communicated with vavuum pump, and import is communicated with the outlet of discharge reaction tube.Discharge reaction tube is region of discharge by inducer, is the diffusion region by outlet section.The as a whole pipeline section of discharge reaction tube and radical reaction chamber.Adopt this covering device, this group member utilizes the remote plasmas such as argon, nitrogen successfully to carry out modification to materials such as polytetrafluoroethylene (PTFE) (PTFE), polyvinyl chloride (PVC) and NACFs.
But, the film individual (comprising hollow-fibre membrane, periosteum, capillary-pipe film and flat sheet membrane) that present remote plasma body technique is only limited to being positioned in discharge reaction tube carries out surface modification, can't modify hollow fiber film assembly, tubular membrane component or the capillary-pipe film assembly scale of carrying out that is consisted of by many/single film assembling, also can't modify assembled the plate and frame module that the consists of scale of carrying out by many/monolithic flat sheet membrane.
Summary of the invention
The objective of the invention is to carry out to the whole membrane module of many flat sheet membrane or tubular film composition the shortcoming that scale is modified in order to solve existing remote plasma surface modification device, and provide a kind of remote plasma that utilizes to carry out bulk modified device and method to membrane module.
The objective of the invention is to be achieved through the following technical solutions:
A kind of remote plasma that utilizes of the present invention carries out the whole device of modifying to membrane module, comprise vavuum pump, discharge tube, air accumulator, be wrapped in the inductance coil on discharge tube, the radio circuit that is connected with inductance coil, the air admission hole of discharge tube is connected with the air accumulator pipeline with flowmeter by flow control valve, and the air admission hole of discharge tube is provided with vacuum meter; Also comprise membrane module, the venthole of discharge tube advances gas/liquid hole pipeline with the axial admission of membrane module air inlet one side/liquid hole and side direction respectively by three-way control valve and is connected, and give vent to anger Axial-running Out gas/liquid hole and the side direction of a side of membrane module goes out the gas/liquid hole and be connected with vacuum pump pipeline by three-way control valve simultaneously.
Wherein, described vacuum meter also can be arranged on pipeline between discharge tube and membrane module.
Distance between described discharge tube and membrane module is 0～40cm.
Described membrane module is hollow fiber film assembly, tubular film assembly, capillary-pipe film assembly, plate film assembly.
Film in described membrane module is the tubulose inoranic membrane that polymeric membrane, surface recombination have macromolecule member material.
The non-polymerization gas for generation of plasma that stores in described air accumulator is air, CO
2, nitrogen, ammonia, argon gas, oxygen, hydrogen, steam.
Adopt device of the present invention various membrane modules to be carried out the method for plasma surface modification, concrete grammar is:
With the non-polymerization gas in air accumulator in discharge tube by plasma exciatiaon, generate the various active particles such as ion, excited state molecule, free radical, the swabbing action by vavuum pump makes the active particle in discharge tube flow through membrane module; According to the kind of membrane module and the position of film needs modification, regulate each three-way control valve and control the flow direction of active particle in membrane module, realize the plasma surface modification to whole membrane module; The mobile concrete direction of active particle in different membrane modules is:
When the film inner surface of hollow fiber film assembly, tubular film assembly, capillary-pipe film assembly is carried out modification, by regulating each three-way control valve, control active particle stream and advance from the axial admission of membrane module/liquid hole (being the tube side entrance), through going out from Axial-running Out gas/liquid hole (being the tube side outlet) after membrane module;
When the film outer surface of hollow fiber film assembly, tubular film assembly, capillary-pipe film assembly is carried out modification, by regulating each three-way control valve, control active particle stream enters gas/liquid hole (being the shell side entrance) from the side direction of membrane module and advances, and goes out through going out gas/liquid hole (being the shell side outlet) from side direction after membrane module;
When film inner surface, outer surface and the fenestra of hollow fiber film assembly, tubular film assembly, capillary-pipe film assembly carried out modification simultaneously, by regulating each three-way control valve, controlling active particle stream advances, goes out through going out gas/liquid hole (being the shell side outlet) from side direction after membrane module from the axial admission of membrane module/liquid hole (being the tube side entrance);
When the one side of plate film assembly is carried out modification, by regulating each three-way control valve, control active particle stream and enter the gas/liquid hole from the side direction of membrane module and advance, go out through going out the gas/liquid hole from side direction after membrane module;
When the upper surface of plate film assembly and fenestra are carried out modification simultaneously, by regulating each three-way control valve, control active particle stream and enter the gas/liquid hole from the side direction of membrane module and advance, through going out from Axial-running Out gas/liquid hole after membrane module.
Wherein, active particle is identical with the vavuum pump suction time discharge time in discharge tube, is 5～1200s, is preferably 10～300s;
Radio-frequency power 10～1000W in discharge tube is preferably 40～300W;
The air inlet air pressure of membrane module is 0.5～100Pa, is preferably 2～50Pa.
Beneficial effect
(1) advantage of maximum of the present invention is to modify on overall size membrane module, has broken through the limitation that prior art can only be modified individual flat sheet membrane or single tubular membrane, thereby has greatly improved efficient.
(2) existing technology once can only be modified for the surface of flat sheet membrane or the outer surface of tubular film, and the present invention can carry out bulk modified targetedly to inside and outside surface and the hole wall of film, particularly can also modify the hole wall of inner surface, hole wall and the flat sheet membrane of tubular film with membrane module integral body, and well-known be that the specific area of hole wall is more much bigger than the external surface area of film.
(3) because the free radical in plasma had than electronics and longer life-span of ion, therefore, by plasma is drawn discharge tube, can utilize the film surface in high concentration, long-life radical pair membrane module to modify, can reduce the damage that the bombardment of sample is caused due to high energy active particles such as electronics, ions, be conducive to control goal response, particularly strengthen the chemical reaction that free radical causes.
Description of drawings
Fig. 1 carries out bulk modified installation drawing to a kind of remote plasma that utilizes of the present invention to membrane module;
Wherein, 1-air accumulator; The 2-pressure-reducing valve; The 3-flow controller; The 4-discharge tube; The 5-inductance coil; The 6-radio frequency adaptation; The 7-radio-frequency power supply; The 8-vacuum meter; 9-three-way control valve A; The 10-membrane module; 11-three-way control valve B; The 12-vavuum pump; 101-axial admission/liquid hole; The 102-side direction is entered the gas/liquid hole; The 103-side direction goes out the gas/liquid hole; 104-Axial-running Out gas/liquid hole.
The specific embodiment
Below in conjunction with drawings and Examples, content of the present invention is described further.
Embodiment 1
A kind of remote plasma that utilizes of the present invention carries out the whole device of modifying to membrane module, as shown in Figure 1, comprise vavuum pump 12, membrane module 10, discharge tube 4, air accumulator 1, be wrapped in the inductance coil 5 on discharge tube, the radio frequency adaptation 6 that is connected with inductance coil and radio-frequency power supply 7, the air admission hole of discharge tube 4 is connected with flow controller and is connected with air accumulator 1 by pressure-reducing valve 2, is provided with vacuum meter 8 on the pipeline between discharge tube 4 and membrane module 10; The venthole of discharge tube 4 advances gas/liquid hole 102 pipelines with the axial admission of membrane module air inlet one side/liquid hole 101 and side direction respectively by three-way control valve 9 and is connected, and give vent to anger Axial-running Out gas/liquid hole 104 and the side direction of a side of membrane module goes out gas/liquid hole 103 and be connected with vavuum pump 12 pipelines by three-way control valve 11 simultaneously.
Adopt this device to carry out modifying inner surface to the hollow fiber film assembly of polytetrafluoroethylmaterial material: to regulate three-way control valve A9, the venthole of discharge tube 4 101 is opened to the axial admission of membrane module 10/liquid hole, and the venthole of discharge tube 4 enters gas/liquid hole 102 to the side direction of membrane module 10 and closes; Regulate three-way control valve B11, the Axial-running Out gas/liquid hole 104 of membrane module 10 is opened to vavuum pump 12, the side direction of membrane module 10 goes out gas/liquid hole 103 and closes to vavuum pump 12; The non-polymerization gas for generation of plasma that stores in air accumulator 1 is argon gas; By regulating the flow controller 3 of vavuum pump 12 and discharge tube 4 front ends, make the air pressure in discharge tube 4 exits remain on 20Pa; Non-polymerization gas by plasma exciatiaon, generates the various active ions such as ion, excited state molecule, free radical, radio-frequency power 80W in discharge tube 4; Under the swabbing action of vavuum pump, these active particles 101 flow into from the axial admission of membrane module 10/liquid hole, flow out from the Axial-running Out gas/liquid hole 104 of membrane module 10, and be 2min discharge time, thereby realize the modification to the inner surface of hollow fiber film assembly.
A kind of remote plasma that utilizes of the present invention carries out the whole device of modifying to membrane module, and structure adopts this device to carry out the outer surface modification to the hollow fiber film assembly of polyvinylidene fluoride material with embodiment 1:
Regulate three-way control valve A9, the venthole of discharge tube 4 101 is closed to the axial admission of membrane module 10/liquid hole, the venthole of discharge tube 4 is opened to the logical gas/liquid of the side direction hole 102 of membrane module 10; Regulate three-way control valve B11, the Axial-running Out gas/liquid hole 104 of membrane module 10 is closed to vavuum pump 12, the side direction of membrane module 10 goes out gas/liquid hole 103 and opens to vavuum pump 12; The non-polymerization gas for generation of plasma that stores in air accumulator 1 is nitrogen; By regulating the flow controller 3 of vavuum pump 12 and discharge tube 4 front ends, make the air pressure in discharge tube 4 exits remain on 15Pa; Non-polymerization gas by plasma exciatiaon, generates the various active ions such as ion, excited state molecule, free radical, radio-frequency power 70W in discharge tube 4; Under the swabbing action of vavuum pump, these active particles enter gas/liquid hole 102 from the side direction of membrane module 10 and flow into, and go out gas/liquid hole 103 from the side direction of membrane module 10 and flow out, and be 4min discharge time, thereby realize the modification to the outer surface of hollow fiber film assembly.
Embodiment 3
A kind of remote plasma that utilizes of the present invention carries out the whole device of modifying to membrane module, structure is with embodiment 1, adopt this device to carry out simultaneously inside and outside surface and fenestra modification to the hollow fiber film assembly integral body of polypropylene material: to regulate three-way control valve A9, the venthole of discharge tube 4 101 is opened to the axial admission of membrane module 10/liquid hole, and the venthole of discharge tube 4 enters gas/liquid hole 102 to the side direction of membrane module 10 and closes; Regulate three-way control valve B11, the Axial-running Out gas/liquid hole 104 of membrane module 10 is closed to vavuum pump 12, the side direction of membrane module 10 goes out gas/liquid hole 103 and opens to vavuum pump 12; The non-polymerization gas for generation of plasma that stores in air accumulator 1 is ammonia; By regulating the flow controller 3 of vavuum pump 12 and discharge tube 4 front ends, make the air pressure in discharge tube 4 exits remain on 25Pa; Non-polymerization gas by plasma exciatiaon, generates the various active ions such as ion, excited state molecule, free radical, radio-frequency power 85W in discharge tube 4; Under the swabbing action of vavuum pump, these active particles 101 flow into from the axial admission of membrane module 10/liquid hole, go out gas/liquid hole 103 outflows from the side direction of membrane module 10, be 3min discharge time, thereby realize inner surface, outer surface and the fenestra modification simultaneously to hollow fiber film assembly.
A kind of remote plasma that utilizes of the present invention carries out the whole device of modifying to membrane module, structure is with embodiment 1, adopt this device to carry out the upper surface modification to the plate and frame module of the polythene material of 2 horizontal positioned: to regulate three-way control valve A9, the venthole of discharge tube 4 101 is closed to the axial admission of membrane module 10/liquid hole, and the venthole of discharge tube 4 is opened to the side direction feed liquor/pore 102 of membrane module 10; Regulate three-way control valve B11, the Axial-running Out gas/liquid hole 104 of membrane module 10 is closed to vavuum pump 12, the side direction of membrane module 10 goes out gas/liquid hole 103 and opens to vavuum pump 12; The non-polymerization gas for generation of plasma that stores in air accumulator 1 is CO
2By regulating the flow control valve of vavuum pump 12 and discharge tube 4 front ends, make the air pressure in discharge tube 4 exits remain on 30Pa; Non-polymerization gas by plasma exciatiaon, generates the various active ions such as ion, excited state molecule, free radical, radio-frequency power 50W in discharge tube 4; Under the swabbing action of vavuum pump, these active particles flow into from the side direction feed liquor/pore 102 of membrane module 10, go out gas/liquid hole 103 from the side direction of membrane module 10 and flow out, and be 3min discharge time, thereby realize the modification to the upper surface of plate and frame module.
A kind of remote plasma that utilizes of the present invention carries out the whole device of modifying to membrane module, structure is with embodiment 1, adopt this device to carry out simultaneously film upper surface and fenestra modification to the plate and frame module of the polythene material of 4 horizontal positioned: to regulate three-way control valve A9, the venthole that makes discharge tube 4 enters gas/liquid hole 102 to the side direction of membrane module 10 to be opened, and the venthole of discharge tube 4 101 is closed to the axial admission of membrane module 10/liquid hole; Regulate three-way control valve B11, the Axial-running Out gas/liquid hole 104 of membrane module 10 is opened to vavuum pump 12, the side direction of membrane module 10 goes out gas/liquid hole 103 and closes to vavuum pump 12; The non-polymerization gas for generation of plasma that stores in air accumulator 1 is air; By regulating the flow control valve of vavuum pump 12 and discharge tube 4 front ends, make the air pressure in discharge tube 4 exits remain on 20Pa; Non-polymerization gas by plasma exciatiaon, generates the various active ions such as ion, excited state molecule, free radical, radio-frequency power 75W in discharge tube 4; Under the swabbing action of vavuum pump, these active particles advance gas/liquid hole 102 inflows from the side direction of membrane module 10, from Axial-running Out gas/liquid hole 104 outflows of membrane module 10, be 4min discharge time, thus modification when realizing plate and frame module inner surface and fenestra.
Claims (3)
1. one kind is utilized remote plasma to carry out the whole device of modifying to membrane module, comprise vavuum pump, discharge tube, air accumulator, be wrapped in the inductance coil on discharge tube, the radio circuit that is connected with inductance coil, the air admission hole of discharge tube is connected with the air accumulator pipeline with flowmeter by flow control valve, and the air admission hole of discharge tube is provided with vacuum meter; It is characterized in that: also comprise membrane module, the venthole of discharge tube advances gas/liquid hole pipeline with the axial admission of membrane module air inlet one side/liquid hole and side direction respectively by three-way control valve and is connected, and give vent to anger Axial-running Out gas/liquid hole and the side direction of a side of membrane module goes out the gas/liquid hole and be connected with vacuum pump pipeline by three-way control valve simultaneously;
Wherein, the distance of the pipeline between described discharge tube and membrane module is 0～40cm;
Described membrane module is hollow fiber film assembly, tubular film assembly, capillary-pipe film assembly, plate film assembly;
The non-polymerization gas for generation of plasma that stores in described air accumulator is air, CO
2, nitrogen, ammonia, argon gas, oxygen, hydrogen, steam,
Film in described membrane module is the tubulose inoranic membrane that polymeric membrane, surface recombination have macromolecule member material,
The vacuum meter of described discharge tube air admission hole setting also can be arranged on pipeline between discharge tube and membrane module.
2. adopt and install as claimed in claim 1 the method for various membrane modules being carried out plasma surface modification, it is characterized in that concrete grammar is:
Non-polymerization gas in air accumulator is become active particle by plasma exciatiaon in discharge tube, the swabbing action by vavuum pump makes the active particle in discharge tube flow through membrane module; According to the kind of membrane module and the position of film needs modification, regulate each three-way control valve and control the flow direction of active particle in membrane module, realize the plasma surface modification to whole membrane module; The mobile concrete direction of active particle in different membrane modules is:
When the film inner surface of hollow fiber film assembly, tubular film assembly, capillary-pipe film assembly is carried out modification, by regulating each three-way control valve, control active particle stream and advance from the axial admission of membrane module/liquid hole, through going out from Axial-running Out gas/liquid hole after membrane module;
When the film outer surface of hollow fiber film assembly, tubular film assembly, capillary-pipe film assembly is carried out modification, by regulating each three-way control valve, control active particle stream and enter the gas/liquid hole from the side direction of membrane module and advance, go out through going out the gas/liquid hole from side direction after membrane module;
When film inner surface, outer surface and the fenestra of hollow fiber film assembly, tubular film assembly, capillary-pipe film assembly carried out modification simultaneously, by regulating each three-way control valve, control active particle stream and advance from the axial admission of membrane module/liquid hole, go out through going out the gas/liquid hole from side direction after membrane module;
When the one side of plate film assembly is carried out modification, by regulating each three-way control valve, control active particle stream and enter the gas/liquid hole from the side direction of membrane module and advance, go out through going out the gas/liquid hole from side direction after membrane module;
When the upper surface of plate film assembly and fenestra are carried out modification simultaneously, by regulating each three-way control valve, control active particle stream and enter the gas/liquid hole from the side direction of membrane module and advance, through going out from Axial-running Out gas/liquid hole after membrane module;
Wherein, active particle is identical with the vavuum pump suction time discharge time in discharge tube, is 5～1200s; Radio-frequency power 10～1000W in discharge tube; The air inlet air pressure of membrane module is 0.5～100Pa.
3. method of various membrane modules being carried out plasma surface modification as claimed in claim 2 is characterized in that: described active particle is preferably 10～300s the discharge time in discharge tube; Radio-frequency power in discharge tube is preferably 40～300W; The air inlet air pressure of membrane module is preferably 2～50Pa.
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| WO2013096714A1 (en) * | 2011-12-22 | 2013-06-27 | Dow Global Technologies Llc | Microcapillary films and foams suitable for capillary action fluid transport |
| CN102773020B (en) * | 2012-07-18 | 2014-07-23 | 北京理工大学 | Method for wholly chemically grafting membrane component by utilizing remote plasma |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2783707Y (en) * | 2005-04-04 | 2006-05-24 | 应用材料股份有限公司 | Prepared gas bypassing device for long distance plasma reactor |
| CN101628203A (en) * | 2009-08-12 | 2010-01-20 | 江苏中科膜技术有限公司 | Hollow fiber membrane assembly for submerged membrane bioreactor |
| CN202028342U (en) * | 2011-03-18 | 2011-11-09 | 北京理工大学 | Device for overall modifying membrane module by long-range plasmas |
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| JP4186827B2 (en) * | 2004-01-30 | 2008-11-26 | 日立電線株式会社 | Semiconductor manufacturing method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2783707Y (en) * | 2005-04-04 | 2006-05-24 | 应用材料股份有限公司 | Prepared gas bypassing device for long distance plasma reactor |
| CN101628203A (en) * | 2009-08-12 | 2010-01-20 | 江苏中科膜技术有限公司 | Hollow fiber membrane assembly for submerged membrane bioreactor |
| CN202028342U (en) * | 2011-03-18 | 2011-11-09 | 北京理工大学 | Device for overall modifying membrane module by long-range plasmas |
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| JP特开2005-217220A 2005.08.11 |
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