CN103752181A - Preparation method and equipment of composite hollow fiber membrane - Google Patents
Preparation method and equipment of composite hollow fiber membrane Download PDFInfo
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- CN103752181A CN103752181A CN201410002960.1A CN201410002960A CN103752181A CN 103752181 A CN103752181 A CN 103752181A CN 201410002960 A CN201410002960 A CN 201410002960A CN 103752181 A CN103752181 A CN 103752181A
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Abstract
The invention discloses a preparation method and equipment of a composite hollow fiber membrane. The equipment is rotary coating equipment which comprises main components such as a membrane liquid storage tank, a hollow fiber membrane fixing rack, a shaft, a connector, a gear motor and the like, wherein the hollow fiber membrane fixing rack is two discs which are connected through a stainless steel shaft and provided with dense micro pores; the shaft of the hollow fiber membrane fixing rack is connected with the gear motor through the connector. The composite hollow fiber membrane is prepared by dipping the hollow fiber membrane fixing rack on which the hollow fiber membrane is fixed into the membrane liquid storage tank, coating polymer film liquid, and subsequently heating in a slow rotation state so as to coat on the outer surface of the hollow fiber membrane with the membrane liquid to obtain the composite hollow fiber membrane. The composite hollow fiber membrane prepared by using the method can be applied to membrane processes of pervaporation, vapor permeation, gas separation and the like.
Description
Technical field
The present invention relates to a kind of preparation method who is applied to the hollow fiber composite membrane of film separation process, the invention still further relates to a kind of Preparation equipment of hollow fiber composite membrane.
Background technology
In recent years, the research of membrane technology and application obtain fast development.According to the shape of film, can be divided into three kinds of flat sheet membrane, hollow-fibre membrane and tubular membrane.It is simple that hollow-fibre membrane has preparation technology, and structure is easy to control, and therefore the advantages of higher of membrane area in unit volume is widely used in the fields such as the pretreatment of wastewater treatment, ultra-pure water preparation, desalinization, brackish water desalination and membrane bioreactor.These films are all micro-filtration, the milipore filters based on pore size difference.1974, Henis made supporting layer with polysulfone hollow fibre milipore filter, adopted the method that vacuumizes coating silicon rubber to make N
2/ O
2separated gas separation membrane, this film is high pressure resistant, and separation is high, and permeation flux is large, has from then on opened the new application of hollow fiber composite membrane.
Hollow fiber composite membrane is the novel film materials at the outer surface of Hollow Fiber Ultrafiltration or microfiltration membranes or the compound one deck densified polymer of inner surface film.Hollow Fiber Ultrafiltration or microfiltration membranes play a supportive role, and the densified polymer rete of inner surface or outer surface plays centrifugation, and both can be same materials, can be also different materials.Be widely used in organic matter osmotic, evaporating and dewatering, the recovery of volatile organic matter, N in liquid mixture
2/ O
2the removing of micro quantity organic pollutant, organic/fields such as organic mixture separation in separated (gas is separated), water.
How quick, the convenient hollow fiber composite membrane that makes ultra-thin active separating layer is the target that film researcher pursues always.Guo Yong (Guo Yong etc., the preparation and property research of silicon rubber-polysulfone hollow fibre composite membrane, membrane science and technology, 2002,22 (5): 58-60) etc. in laboratory adopts pressurization, be coated with legal system for the hollow fiber composite membrane of dimethyl silicone polymer/polysulfones; Li Bingbing (Li Bingbing etc., the preparation of PDMS/PES doughnut osmosis vaporizing compound membrane, membrane science and technology, 2009,29 (5): 29-32) etc. at polyether sulphone hollow fibre film outer surface, apply one deck dimethyl silicone polymer and make hollow fiber composite membrane.These methods are all to belong to physics to apply, and once can only apply a small amount of film, and after applying, because the mobility of film liquid causes coat film layer thickness inhomogeneous.Therefore film researcher attempts adopting the method for chemical modification to carry out the preparation of active separating layer on the inside and outside surface of hollow-fibre membrane.Xu Zhikang (Z. K. Xu, et al. Microporous polypropylene hollow fiber membranes part II:pervaporation separation of water/ethanol mixtures by the poly (acrylic acid) grafted membranes, J.Membr.Sci.2003,214 (1): 71-81) etc. adopt the mode of plasma polymerization at polypropylene hollow fiber milipore filter surface-grafted polyacrylic acid, make poly propenoic acid propylene doughnut osmosis vaporizing compound membrane; Xie Jingyuan (Xie Jingyuan etc., cross-linking radiation is prepared polymethylacrylic acid-N, N-dimethylaminoethyl/polysulfone hollow fibre Nano filtering composite membrane, Tianjin University of Technology's journal, 2008,27 (1): 1-4) with irradiation crosslinking, on ps hollow fiber uf membrane surface, prepared polymethylacrylic acid-N, N dimethylaminoethyl/polysulfones Nano filtering composite membrane.Although preparing the method for hollow fiber composite membrane, chemical modification there is favorable reproducibility, membrane structure is easy to control, but also there is the shortcomings such as modified monomer limited amount, therefore in the urgent need to finding a kind of novel preparation method of hollow fiber composite membrane of quick, convenient, applicable multiple polymers.
The present invention is on the basis of ZL200610053745.X, by designing a kind of spin coating equipment, by parallel being fixed on the hollow-fibre membrane fixed mount with two disks of hollow-fibre membrane, then immerse in polymer film solution, with reducing motor, drive hollow-fibre membrane fixed mount to rotate in film liquid, thereby film liquid is coated in to doughnut film outer surface, then by more than film liquid emit, stick to the film liquid of doughnut film outer surface along the central shaft rotation of film, thereby film liquid is evenly applied at film outer surface, by heating and attemperating unit, allow solvent evaporates in film liquid, make film liquid at doughnut film outer surface, form the diffusion barrier of one deck homogeneous, thereby obtain hollow fiber composite membrane.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of hollow fiber composite membrane, the present invention also aims to provide a kind of Preparation equipment of hollow fiber composite membrane, described equipment is a kind of spin coating equipment.
The present invention is achieved like this.A kind of spin coating equipment for the preparation of hollow fiber composite membrane, it comprises film liquid storage tank, film liquid storage tank outer cover, heater, hollow-fibre membrane fixed mount, reducing motor and connector, it is characterized in that hollow-fibre membrane fixed mount consists of hollow-fibre membrane fixed disk and axle, described axle is through the fixing hole at two hollow-fibre membrane fixed disk centers, and the position of hollow-fibre membrane fixed disk is fixed with the pin on axle; The bottom of described film liquid storage tank is provided with film liquid storage tank valve, and the two ends of described film liquid storage tank are respectively equipped with bearing; Described hollow-fibre membrane fixed mount is placed in film liquid storage tank, and by the axle of bearings hollow-fibre membrane fixed mount, described axle is connected with reducing motor by connector, and film liquid storage tank outside housing cover is on film liquid storage tank, and film liquid storage tank outer cover is provided with heater.
On described hollow-fibre membrane fixed disk, be covered with micropore.
Use above-mentioned spin coating equipment to prepare a method for hollow fiber composite membrane, its step is as follows:
(1) hollow-fibre membrane is passed from two hollow-fibre membrane fixed disks that stack;
(2) by two hollow-fibre membrane fixed disks that stack to hollow-fibre membrane two ends separately, after suitable length, the stainless steel shaft in hollow-fibre membrane fixed mount is passed from the fixing hole at hollow-fibre membrane fixed disk center, stuck with pin;
(3) end face of hollow-fibre membrane fixed disk is fixed hollow-fibre membrane with Instant cement, guaranteed that film is arranged in parallel, and does not contact to each other mutually;
(4) the polymer film liquid configuring is poured in the semi-cylindrical film liquid storage tank keeping flat;
(5) the hollow-fibre membrane fixed mount of having fixed hollow-fibre membrane is put into the film liquid storage tank that fills polymer film liquid;
(6) axle on hollow-fibre membrane fixed mount and reducing motor are coupled together with connector;
(7) open reducing motor, adjust the rotating speed of 1-50r/min, allow every film all apply last layer polymer film solution;
(8) open film liquid storage tank valve, unnecessary film liquid is emitted from film liquid storage tank, in order to applying next time, use; And cover film liquid storage tank outer cover, and open heater, make solvent in the film liquid 1-24h that volatilizees at 30-100 ℃;
(9) after the solvent evaporates in film liquid completes, close reducing motor, the composite membrane on hollow-fibre membrane fixed mount is cut with scissors, carry out encapsulation and the performance test of membrane module.
Technique effect of the present invention: can quick, convenient, applicable multiple polymers prepare hollow fiber composite membrane, thicknesses of layers is realized by control Immersion time, film fluid viscosity, reducing motor rotating speed.Prepared hollow fiber composite membrane even thickness, defect is few, can be used for the membrane process such as infiltration evaporation, steam infiltration, gas separation.
Accompanying drawing explanation
Fig. 1. spin-coating equipment schematic diagram
Fig. 2. film liquid storage tank schematic diagram
Fig. 3. hollow-fibre membrane fixed mount and axle schematic diagram
Fig. 4. hollow-fibre membrane fixed disk and film be schematic diagram fixedly
In figure: 101-film liquid storage tank, 102-film liquid storage tank outer cover, 2-bearing, 3-film liquid storage tank valve, 4-heater, 5-axle, 6-pin, 7-hollow-fibre membrane fixed disk, 8-hollow-fibre membrane, 9-reducing motor, 10-connector.
The specific embodiment
As shown in Figures 1 to 4, a kind of spin coating equipment for the preparation of hollow fiber composite membrane, it comprises film liquid storage tank (101), film liquid storage tank outer cover (102), hollow-fibre membrane fixed mount, heater (4), reducing motor (9) and connector (10), it is characterized in that hollow-fibre membrane fixed mount consists of hollow-fibre membrane fixed disk (7) and axle (5), described axle (5) is through the fixing hole at two hollow-fibre membrane fixed disks (7) center, and the pin (6) on the axle for position (5) of hollow-fibre membrane fixed disk (7) is fixing; The bottom of described film liquid storage tank (101) is provided with film liquid storage tank valve (3), and the two ends of described film liquid storage tank (101) are respectively equipped with bearing (2); Described hollow-fibre membrane fixed mount is placed in film liquid storage tank (101), axle (5) by bearing (2) support hollow tunica fibrosa fixed mount, described axle (5) is connected with reducing motor (9) by connector (10), film liquid storage tank outer cover (102) covers at film liquid storage tank (101) upper, and film liquid storage tank outer cover (102) is provided with heater (4).On described hollow-fibre membrane fixed disk (7), be covered with micropore.
Use above-mentioned spin coating equipment to prepare a method for hollow fiber composite membrane, its step is as follows:
(1) hollow-fibre membrane (8) is passed from two hollow-fibre membrane fixed disks (7) that stack;
(2) by two hollow-fibre membrane fixed disks (7) that stack to hollow-fibre membrane (8) two ends separately, after suitable length, stainless steel shaft in hollow-fibre membrane fixed mount (5) is passed from the fixing hole at hollow-fibre membrane fixed disk (7) center, stuck with pin (6);
(3) end face of hollow-fibre membrane fixed disk (7) is fixing hollow-fibre membrane (8) with Instant cement, guarantee that film is arranged in parallel, and does not contact to each other mutually;
(4) the polymer film liquid configuring is poured in the semi-cylindrical film liquid storage tank (101) keeping flat;
(5) the hollow-fibre membrane fixed mount of having fixed hollow-fibre membrane (8) is put into the film liquid storage tank (101) that fills polymer film liquid;
(6) axle on hollow-fibre membrane fixed mount (5) and reducing motor (9) are coupled together with connector (10);
(7) open reducing motor (9), adjust the rotating speed of 1-50r/min, allow every film all apply last layer polymer film solution;
(8) open film liquid storage tank valve (3), unnecessary film liquid is emitted from film liquid storage tank (101), in order to applying next time, use; And cover film liquid storage tank outer cover (102), and open heater (4), make solvent in the film liquid 1-24h that volatilizees at 30-100 ℃;
(9) after the solvent evaporates in film liquid completes, close reducing motor (9), the composite membrane on hollow-fibre membrane fixed mount is cut with scissors, carry out encapsulation and the performance test of membrane module.
embodiment 1
In hole by 500 root polypropylene nitrile hollow-fibre membranes (8) from two hollow-fibre membrane fixed disks (7) that stack, pass, then two hollow-fibre membrane fixed disks (7) are stretched to 80cm to hollow-fibre membrane (8) two ends, then axle (5) is passed in the hole from hollow-fibre membrane fixed disk (7), arrive the long place of 80cm, with the pin (6) on axle (5), fix; Then the Instant cement of falling one deck in hollow-fibre membrane fixed disk (7) both ends of the surface, is fixed on hollow-fibre membrane on hollow-fibre membrane fixed disk (7).The polyvinyl alcohol coating solution preparing by 10% concentration by deionized water is poured in film liquid storage tank (101), before pouring into, first closed the film liquid storage tank valve (3) of film liquid storage tank (101) lower end.Then two bearings (2) that the axle (5) of having fixed the fixed mount of polyacrylonitrile hollow fiber membrane (8) are placed in film liquid storage tank (101) are upper, with connector (10), hollow-fibre membrane fixed mount and reducing motor (9) coupled together.Open reducing motor (9) power switch, and the rotating speed that regulates reducing motor (9) is 10r/min, when every hollow-fibre membrane (8) has all applied after film liquid, open the film liquid storage tank valve (3) of film liquid storage tank (101) lower end, emit wherein remaining poly-vinyl alcohol solution; Then cover film liquid storage tank outer cover (102), setting baking temperature is 70 ℃, open heater (4), regulating reducing motor (9) rotating speed is 20r/min, after dry 5h, open film liquid storage tank outer cover (102), the actual conditions that apply according to hollow-fibre membrane (8) determine whether to carry out secondary coating.After coating completes, with scissors, polyvinyl alcohol/polyacrylonitrile hollow fiber composite membrane is cut from fixed disk, carried out the encapsulation of membrane module.
embodiment 2
In hole by 300 ps hollow fiber uf membrane (8) from two two hollow-fibre membrane fixed disks (7) that stack, pass, then two hollow-fibre membrane fixed disks (7) are stretched to 100cm to hollow-fibre membrane (8) two ends, then axle (5) is passed in the hole from hollow-fibre membrane fixed disk (7), arrive the long place of 100cm, with the pin (6) on axle (5), fix; Then the Instant cement of falling one deck in hollow-fibre membrane fixed disk (7) both ends of the surface, is fixed on hollow-fibre membrane (8) on hollow-fibre membrane fixed disk (7).The PDMS membrane solution preparing by 15% concentration with n-hexane water is poured in film liquid storage tank (101), before pouring into, first closed film liquid storage tank valve (3).Then two bearings (2) that the axle (5) of having fixed the fixed mount of ps hollow fiber uf membrane (8) are placed in film liquid storage tank (101) are upper, with connector (10), hollow-fibre membrane fixed mount and reducing motor (9) coupled together.Open reducing motor (9) power switch, and to regulate the rotating speed of reducing motor (9) be 5r/min, when every hollow-fibre membrane (8) has all applied after film liquid, open film liquid storage tank valve (3), emit wherein remaining dimethyl silicone polymer solution; Then cover film liquid storage tank outer cover (102), setting baking temperature is 40 ℃, opens heater (4), regulating reducing motor rotating speed is 20r/min, after dry 20h, open film liquid storage tank outer cover (102), the actual conditions that apply according to film determine whether to carry out secondary coating.After coating completes, with scissors, dimethyl silicone polymer/polysulfone hollow fibre composite membrane is cut from fixed disk, carried out the encapsulation of membrane module.
By 100 Al
2o
3hollow-fibre membrane (8) passes in the hole from two hollow-fibre membrane fixed disks (7) that stack, then two hollow-fibre membrane fixed disks (7) are stretched to 60cm to hollow-fibre membrane (8) two ends, then axle (5) is passed in the hole from hollow-fibre membrane fixed disk (7), arrive the long place of 60cm, with the pin (6) on axle (5), fix; Then the Instant cement of falling one deck in hollow-fibre membrane fixed disk (7) both ends of the surface, is fixed on hollow-fibre membrane (8) on hollow-fibre membrane fixed disk (7).The polyurethane film solution preparing by 12% concentration with oxolane is poured in film liquid storage tank (1), before pouring into, first closed film liquid storage tank valve (3).Then will fix Al
2o
3two bearings (2) that the axle (5) of the fixed mount of hollow-fibre membrane (8) is placed in film liquid storage tank (1) are upper, with connector (10), hollow-fibre membrane fixed mount and reducing motor (9) coupled together.Open reducing motor (9) power switch, and to regulate reducing motor rotating speed be 10r/min, when every film has all applied after film liquid, open film liquid storage tank valve (3), emit wherein remaining polyurethane film solution; Then cover film liquid storage tank outer cover (102), setting baking temperature is 30 ℃, opens heater (4), regulating reducing motor rotating speed is 30r/min, after dry 2h, open film liquid storage tank outer cover (102), the actual conditions that apply according to film determine whether to carry out secondary coating.After coating completes, by polyurethane/Al
2o
3hollow fiber composite membrane takes off from fixed disk, carries out the encapsulation of membrane module.
Claims (4)
1. the preparation method of a hollow fiber composite membrane, it is characterized in that hollow-fibre membrane to be fixed on spin coating equipment, in spin coating equipment, add polymer film solution, by driven by motor, hollow-fibre membrane is rotated, polymer film solution is coated in to doughnut film outer surface, then discharge polymer film solution remaining in spin coating equipment, the polymer film solution of heating, drying doughnut film outer surface, after solvent volatilizees completely in the film liquid of film surface attachment, obtain hollow fiber composite membrane.
2. the spin coating equipment for the preparation of hollow fiber composite membrane, it comprises film liquid storage tank, film liquid storage tank outer cover, hollow-fibre membrane fixed mount, heater, reducing motor and connector, it is characterized in that hollow-fibre membrane fixed mount consists of hollow-fibre membrane fixed disk and axle, described axle is through the fixing hole at two hollow-fibre membrane fixed disk centers, and the position of hollow-fibre membrane fixed disk is fixed with the pin on axle; The bottom of described film liquid storage tank is provided with film liquid storage tank valve, and the two ends of described film liquid storage tank are respectively equipped with bearing; Described hollow-fibre membrane fixed mount is placed in film liquid storage tank, and by the axle of bearings hollow-fibre membrane fixed mount, described axle is connected with reducing motor by connector, and film liquid storage tank outside housing cover is on film liquid storage tank, and film liquid storage tank outer cover is provided with heater.
3. the spin coating equipment for the preparation of hollow fiber composite membrane according to claim 2, is characterized in that being covered with micropore on described hollow-fibre membrane fixed disk.
4. the preparation method of a kind of hollow fiber composite membrane according to claim 1, is characterized in that right to use requires the spin coating equipment described in 2 to prepare hollow fiber composite membrane, and concrete steps are as follows:
Hollow-fibre membrane is passed from two hollow-fibre membrane fixed disks that stack;
By two hollow-fibre membrane fixed disks that stack to hollow-fibre membrane two ends separately, after suitable length, the stainless steel shaft in hollow-fibre membrane fixed mount is passed from the fixing hole at hollow-fibre membrane fixed disk center, stuck with pin;
The end face of hollow-fibre membrane fixed disk is fixed hollow-fibre membrane with Instant cement, guaranteed that film is arranged in parallel, and does not contact to each other mutually;
The polymer film liquid configuring is poured in the semi-cylindrical film liquid storage tank keeping flat;
The hollow-fibre membrane fixed mount of having fixed hollow-fibre membrane is put into the film liquid storage tank that fills polymer film liquid;
Axle on hollow-fibre membrane fixed mount and reducing motor are coupled together with connector;
Open reducing motor, adjust the rotating speed of 1-50r/min, allow every film all apply last layer polymer film solution;
Open film liquid storage tank valve, unnecessary film liquid is emitted from film liquid storage tank, in order to applying next time, use; And cover film liquid storage tank outer cover, and open heater, make solvent in the film liquid 1-24h that volatilizees at 30-100 ℃;
After the solvent evaporates in film liquid completes, close reducing motor, the composite membrane on hollow-fibre membrane fixed mount is cut with scissors, carry out encapsulation and the performance test of membrane module.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109234833A (en) * | 2018-08-17 | 2019-01-18 | 东华大学 | With the Porous hollow polyurethane fiber of fine and close clad structure and its preparation and application |
| CN109231365A (en) * | 2018-08-31 | 2019-01-18 | 浙江工业大学 | A kind of application of PIMs superthin layer composite hollow fiber membrane in separation alcohol water |
| CN109248567A (en) * | 2018-08-31 | 2019-01-22 | 浙江工业大学 | A kind of PIMs superthin layer composite hollow fiber membrane and preparation and application |
| CN111482091A (en) * | 2020-05-18 | 2020-08-04 | 浙江长兴求是膜技术有限公司 | Preparation method of high-performance MABR hollow fiber composite membrane |
| CN112261987A (en) * | 2018-06-08 | 2021-01-22 | 可隆工业株式会社 | Method for manufacturing hollow fiber membrane module and hollow fiber membrane module manufactured thereby |
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| CN111482091A (en) * | 2020-05-18 | 2020-08-04 | 浙江长兴求是膜技术有限公司 | Preparation method of high-performance MABR hollow fiber composite membrane |
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