CN111111462A - Fiber-reinforced hollow fiber multi-core membrane and preparation method thereof - Google Patents
Fiber-reinforced hollow fiber multi-core membrane and preparation method thereof Download PDFInfo
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- CN111111462A CN111111462A CN202010010147.4A CN202010010147A CN111111462A CN 111111462 A CN111111462 A CN 111111462A CN 202010010147 A CN202010010147 A CN 202010010147A CN 111111462 A CN111111462 A CN 111111462A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/08—Hollow fibre membranes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0002—Organic membrane manufacture
- B01D67/0009—Organic membrane manufacture by phase separation, sol-gel transition, evaporation or solvent quenching
- B01D67/0016—Coagulation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/24—Mechanical properties, e.g. strength
Abstract
The invention belongs to the technical field of membrane separation, and particularly relates to and discloses a fiber-reinforced hollow fiber multi-core membrane which is provided with a plurality of hollow inner cores, wherein the inner membrane layer is a hollow inner core surface layer, a supporting layer is positioned between the outer membrane layer and the inner membrane layer, at least one reinforcing fiber is embedded in the supporting layer, and the reinforcing fiber, the outer membrane layer, the inner membrane layer and the supporting layer are manufactured in an integrated forming mode. The invention also discloses a preparation method of the fiber-reinforced hollow fiber multi-core membrane, which comprises the following steps: 1) preparing a polymer solution; 2) preparing an inner diameter maintaining agent and reinforcing fibers; 3) preliminarily forming through a hollow multi-core spinneret die; 4) and curing through a solidification medium. According to the fiber-reinforced hollow fiber multi-core membrane and the preparation method thereof, the risk that the membrane is easy to peel from the support body is overcome, the integrity of the inner surface and the outer surface of the membrane can be effectively improved, the total cross section area is larger, the mechanical strength is better, and the permeation flux of the membrane is larger.
Description
Technical Field
The invention belongs to the technical field of membrane separation, and particularly relates to a fiber-reinforced hollow fiber multi-core membrane and a preparation method thereof.
Background
With the global urbanization and rapid population growth, the demand for drinking water is increasing, and the interest in wastewater recovery and brine desalination is also stimulated. The membrane technologies such as microfiltration, ultrafiltration, nanofiltration and reverse osmosis are widely used, and various types of separation membranes such as flat membrane, tubular membrane and hollow fiber membrane are developed. These separation membranes are usually formed by solidifying a polymer solution by a phase inversion method such as a dry method, a wet method, a thermal method, or an interfacial polymerization method, and are required to have excellent permselectivity and high mechanical strength in practical use.
Compared with membrane structures such as flat membrane, tubular membrane and the like, the hollow fiber membrane can realize a self-supporting structure, other supporting bodies are not needed, the preparation process of the component is simple, and the unit volume can provide larger specific surface area. However, in the practical application process, the hollow fiber membrane is continuously subjected to positive flushing, back flushing, gas scrubbing and chemical cleaning, the self-supporting membrane has insufficient mechanical strength and is easy to break, and finally the effluent quality of the membrane system is reduced and even collapses.
In order to improve the mechanical strength of the hollow fiber membrane, it is effective to use a knitted fiber tube (woven tube or crocheted tube) for the inner support as a membrane support. The knitted fiber tube of the inner support is mostly made of polyester materials, the adhesion with coating materials is poor, the film is easy to stay on the outer surface of the knitted fiber tube, and the risk of easy peeling exists in the actual use process. In addition, when a low-viscosity polymer membrane solution is coated, the situation that the inner supporting knitted fiber tube is excessively seeped and even the core hole is blocked easily occurs. In short, the internal-supported knitted fiber tube has many disadvantages such as high membrane cost, easy defect damage on the outer surface of the membrane, and unsuitability for internal pressure filtration, although the mechanical strength of the hollow membrane is improved.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides the fiber-reinforced hollow fiber multi-core membrane which has high mechanical strength, low cost, high integrity of the inner surface and the outer surface and high permeation flux of the membrane under the condition of internal pressure use and the preparation method thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
the utility model provides a hollow fiber multicore membrane of fibre reinforcement, has a plurality of cavity inner cores, includes membrane skin, membrane inlayer and supporting layer, the membrane inlayer is cavity inner core superficial layer, and the supporting layer is located between membrane skin, the membrane inlayer, and it has at least one reinforcing fiber to inlay on the supporting layer, and reinforcing fiber makes with membrane skin, membrane inlayer and supporting layer integrated into one piece. The membrane strength is improved on the basis of ensuring the integrity of the inner surface and the outer surface of the membrane without using an additional support body.
Preferably, the volume of the reinforcing fiber is 1-30% of that of the support layer. The strength of the membrane can be ensured without additional support bodies.
Preferably, the diameter of the reinforcing fiber is 0.05-1 mm, and the breaking strength is 10-200N. The strength is good, and the integrity of the film is not influenced.
Preferably, the reinforcing fibers are polytetrafluoroethylene, polyvinylidene fluoride, basalt, carbon fibers, polyethylene terephthalate, polybutylene terephthalate, polystyrene, polyolefin, polymethacrylate, polyvinyl chloride, polyamide, or polyimide fibers. The reinforced fiber material has wide selectable range, ensures the mechanical strength and can be made of economical and convenient materials.
Preferably, the number of the hollow inner cores is 3-12, and the aperture of the inner layer hole of the membrane is 0.5-500 nm. The multi-core membrane has larger total cross-sectional area, enhanced tensile load and reversible maximum load, can provide better mechanical strength, and in the case of feed-to-inner surface contact, if the outer diameters of two hollow fibers are similar, the effective contact area of the multi-core membrane can be many times larger than that of the currently commonly used single-core membrane, and the permeation flux of the membrane is larger.
A method for preparing a fiber-reinforced hollow fiber multi-core membrane, comprising the steps of:
1) preparing a polymer solution: dissolving a solid polymer material in a solvent or diluent at the temperature of 40-300 ℃, and adding a non-solvent additive to prepare a polymer solution, wherein the mass percent concentration of the polymer material is 8-40%, the mass percent concentration of the non-solvent additive is 1-40%, and the mass percent concentration of the solvent or diluent is 20-80%;
2) preparing an inner diameter maintaining agent and reinforcing fibers, wherein the inner diameter maintaining agent is liquid or gas;
3) preliminary molding through a hollow multi-core spinning die: the hollow multi-core spinning die comprises a conventional high polymer solution channel, a plurality of spray needle channels and at least one reinforced fiber channel, wherein the reinforced fiber channel is communicated with the high polymer solution channel, the structures of the high polymer solution channel and the plurality of spray needle channels are adapted to the structure of a hollow multi-core membrane to be obtained, the high polymer solution prepared in the step 1) is extruded from the high polymer solution channel, an inner diameter maintaining agent is sprayed out through the spray needle channels, and meanwhile, the reinforced fiber and the high polymer solution are subjected to composite forming through the reinforced fiber channels;
4) curing by a setting medium: and 3) after leaving the die, the preliminarily formed hollow fiber membrane obtained in the step 3) passes through an air gap, then is immersed into a solidification medium for solidification and formation, and the preliminarily formed membrane is drawn and wound in the solidification medium to obtain the fiber-reinforced hollow fiber multi-core membrane.
Preferably, the polymer material in step 1) is at least one selected from polysulfone, sulfonated polysulfone, polyethersulfone, cellulose acetate, polyetheretherketone, polyvinylidene fluoride, polytetrafluoroethylene, polyacrylonitrile, polyvinyl chloride, polyolefin, polysiloxane, polyamide and polyimide.
Preferably, the reinforcing fiber in step 2) is one of polytetrafluoroethylene, polyvinylidene fluoride, basalt, carbon fiber, polyethylene terephthalate, polybutylene terephthalate, polystyrene, polyolefin, polymethacrylate, polyvinyl chloride, polyamide or polyimide fiber.
Preferably, the diameter of the polymer solution channel in the step 3) is 0.5-10 mm, the diameter of the spray needle channel is 0.1-2 mm, the number of the spray needle channels is 3-12, and the diameter of the reinforced fiber channel is 0.05-2 mm.
Preferably, the air interval length in the step 4) is 0-50 cm, the temperature of the solidification medium is 0-80 ℃, and the traction winding speed is 10-100 m/min.
The fiber-reinforced hollow fiber multi-core membrane and the preparation method thereof not only can effectively solve the risk that the membrane is easy to peel from the support body, but also can effectively improve the integrity of the inner surface and the outer surface of the membrane, and can prepare the membranes in various forms suitable for external pressure filtration and internal pressure filtration. In addition, fiber reinforced multi-core films have a larger total cross-sectional area, increased tensile load and reversible maximum load, which can provide better mechanical strength. In the case of feed in contact with the inner surface, if the outer diameters of the two hollow fibers are similar, the effective contact area of the multi-core membrane can be many times larger than that of the currently commonly used single-core membrane, and the permeation flux of the membrane is larger.
Drawings
Fig. 1 is a schematic structural view of a fiber-reinforced hollow fiber multi-core membrane described in example 1.
Fig. 2 is a schematic structural view of the hollow multicore spinning die according to embodiment 1.
FIG. 3 is a top view of the hollow multi-core spinning die of example 1.
Fig. 4 is a schematic structural view of the fiber-reinforced hollow fiber multi-core membrane described in example 2.
Fig. 5 is a schematic structural view of the fiber-reinforced hollow fiber multi-core membrane described in example 3.
The figure is as follows: 1: an outer membrane layer; 2: a support layer; 3: an inner membrane layer; 4: a reinforcing fiber; 5: a polymer solution channel; 6: a needle channel; 7: a reinforcing fiber channel; 8: a hollow inner core; 9: hollow multicore spouts a mould.
Detailed Description
The present invention will be further described with reference to FIGS. 1 to 5 and the following detailed description.
Example 1
A fiber-reinforced hollow fiber multi-core membrane is shown in figure 1 and comprises three hollow inner cores 8 and comprises an outer membrane layer 1, an inner membrane layer 3 and a supporting layer 2, wherein the inner membrane layer 3 is a surface layer of the hollow inner core 8, the supporting layer 2 is positioned between the outer membrane layer 1 and the inner membrane layer 3, the outer membrane layer 1 and the inner membrane layer 3 are concentric circular arcs, the diameter of the hollow inner core 8 is 0.5mm, the diameter of the outer membrane layer 1 is 2.5mm, a reinforcing fiber 4 is embedded in the supporting layer 2, and the reinforcing fiber 4 is integrally formed with the outer membrane layer 1, the inner membrane layer 3 and the supporting layer 2. The reinforcing fibers 4 had a diameter of 0.4mm, a volume of 4% of the volume of the support layer 2, and a breaking strength of 20N.
The reinforced fiber 4 is made of Polytetrafluoroethylene (PTFE), the membrane material is made of polyvinylidene fluoride (PVDF), the strength of the whole membrane is 28N, and the average pore diameter of 3 pores in the inner layer of the membrane is 10 nm.
A method for preparing a fiber-reinforced hollow fiber multi-core membrane, which is used for preparing the fiber-reinforced hollow fiber multi-core membrane of the embodiment, comprises the following steps:
1) preparing a polymer solution: the temperature is kept at 150 ℃, solid polymer material polyvinylidene fluoride (PVDF, Suwei 6010) is dissolved in diluent triethyl phosphate (TEP), and a non-solvent additive polyethylene glycol (PEG600) is added to prepare a polymer solution, wherein the mass percentage concentration of the PVDF is 35%, the mass percentage concentration of the PEG600 is 10%, and the mass percentage concentration of the TEP is 55%;
2) preparing polyethylene glycol (PEG600) liquid as an inner diameter maintainer and Polytetrafluoroethylene (PTFE) as a reinforcing fiber;
3) preliminary forming by a hollow multicore spinning die 9: as shown in the attached fig. 2 and 3, the hollow multi-core spinneret mold 9 includes a conventional polymer solution channel 5, three nozzle needle channels 6, and further includes a reinforced fiber channel 7, the reinforced fiber channel 7 is communicated with the polymer solution channel 5, the structures of the polymer solution channel 5 and the three nozzle needle channels 6 are adapted to the structure of the hollow multi-core membrane to be obtained, the polymer solution prepared in step 1) is extruded from the polymer solution channel 5, the internal diameter maintaining agent is sprayed out through the nozzle needle channels 6, and simultaneously the reinforced fiber and the polymer solution are subjected to composite molding through the reinforced fiber channel 7; wherein the outer diameter of the macromolecule solution channel 5 is 3.0mm, the diameter of the spray needle channel 6 is 0.6mm, and the diameter of the reinforced fiber channel 7 is 0.05 mm.
4) Curing by a setting medium: and (3) after leaving the hollow multi-core spinneret mold 9, the preliminarily formed hollow fiber membrane obtained in the step 3) passes through an air gap, then is immersed into a solidification medium for solidification and formation, and the preliminarily formed membrane is drawn and wound in the solidification medium to obtain the fiber-reinforced hollow fiber multi-core membrane. Wherein the air interval length is 30 cm, the solidification medium is water, the temperature of the solidification water bath is 50 ℃, and the speed of traction and winding is 30 m/min.
Example 2
A structure of a fiber-reinforced hollow fiber multi-core membrane, the other parts being the same as those of example 1, except that:
as shown in figure 4, the membrane has five hollow inner cores 8, the diameter of the hollow inner core 8 is 0.9mm, the diameter of the membrane outer layer 1 is 4mm, the diameter of the reinforcing fiber 4 is 0.5mm, the volume of the reinforcing fiber is 6 percent of the volume of the support layer 2, and the breaking strength is 30N.
Polyvinylidene fluoride (PVDF) is selected as the reinforcing fiber 4, polyether sulfone (PES) is used as a membrane material, the strength of the whole membrane is 37N, and the average pore diameter of 3 pores in the inner layer of the membrane is 20 nm.
A method of producing a fiber-reinforced hollow fiber multi-core membrane, the method of producing the fiber-reinforced hollow fiber multi-core membrane of the present example being the same as example 1 except that:
step 1), the temperature is kept at 60 ℃, the high polymer material adopts polyether sulfone (PES, Basff E6020P), the solvent adopts N, N-dimethyl acetamide (DMAc), the non-solvent additive adopts polyvinylpyrrolidone (PVPK30), wherein the mass percent concentration of the PES is 25 percent, the mass percent concentration of the DMAc is 70 percent, and the mass percent concentration of the PVPK30 is 5 percent
And 2) adopting a 50% DMAc aqueous solution as an inner diameter maintaining agent, and adopting polyvinylidene fluoride fibers (PVDF long fibers, the diameter of which is 0.5mm, and the breaking strength of which is 30N) as reinforcing fibers.
And step 3) the mould is provided with five spray needle channels 6, wherein the outer diameter of the polymer solution channel 5 is 4.2mm, the diameter of the spray needle channel 6 is 1.0mm, and the diameter of the reinforced fiber channel 7 is 0.5 mm.
And 4) in the step, the air interval length is 20 cm, the solidification medium is a 30% DMAc aqueous solution, the temperature is 40 ℃, and the traction winding speed is 20 m/min.
Example 3
A structure of a fiber-reinforced hollow fiber multi-core membrane, the other parts being the same as those of example 1, except that: as shown in fig. 5, the number of the reinforcing fibers 4 is four, and the reinforcing fibers are approximately uniformly distributed at different positions on the support layer 2, the diameter of the hollow inner core 8 is 0.8 mm, the diameter of the membrane outer layer 1 is 4.8mm, the diameter of the reinforcing fibers 4 is 0.5mm, the volume of the reinforcing fibers is 10% of the volume of the support layer 2, and the total breaking strength is 60N.
Basalt is selected as the reinforcing fiber 4, polymethylpentene (TPX) is used as a membrane material, the strength of the whole membrane is 120N, and the average pore diameter of 3 pores in the membrane inner layer is 1 nm.
A method of producing a fiber-reinforced hollow fiber multi-core membrane, the method of producing the fiber-reinforced hollow fiber multi-core membrane of the present example being the same as example 1 except that:
step 1), keeping the temperature at 250 ℃, wherein the polymer material is polymethylpentene (TPX, Mitsui DX310), the diluent dioctyl adipate (DOA) and the non-solvent additive nano-silica (with the average particle size of 50 nm), the mass percentage concentration of TPX is 8%, the mass percentage concentration of nano-silica is 40%, and the mass percentage concentration of DOA is 52%;
and 2) adopting nitrogen as an inner diameter maintaining agent, adopting basalt fiber long fiber as a reinforcing fiber, wherein the diameter of the basalt fiber long fiber is 0.5mm, and the total breaking strength of the basalt fiber long fiber is 60N).
And step 3) the die is provided with four reinforced fiber channels 7, wherein the outer diameter of the polymer solution channel 5 is 5.0mm, the diameter of the spray needle channel 6 is 0.9mm, and the diameter of the reinforced fiber channel 7 is 1 mm.
And 4) in the step, the air interval length is 40 cm, the solidification medium is isopropanol solution, the temperature is 30 ℃, and the traction winding speed is 50 m/min.
The measurement method used in each example is as follows: the measurements were carried out at 25 ℃ unless otherwise mentioned.
(1) Determination of the diameter of the hollow inner core 8, the diameter of the membrane outer layer 1, the diameter of the reinforcing fibers 4 and the volume of the reinforcing fibers 4 in the support layer 2 of the fiber-reinforced hollow fiber multi-core membrane: measuring the diameter of the inner core, the outer diameter and the diameter of the reinforcing fiber 4 of the cross section of the membrane by using a microscope, and determining the diameter of the hollow inner core 8, the diameter of the outer layer 1 of the membrane and the diameter of the reinforcing fiber 4 by means of multiple times of average measurement; the volume of the support layer 2 occupied by the reinforcing fibers 4 is the average of the ratio of the cross-sectional areas thereof.
(2) Determination of breaking force
The reinforcing fiber 4 and the fiber-reinforced hollow multi-core membrane were tested on a tensile tester at a fixed length of 10 cm and a length of 100 mm/min.
(3) Determination of the average pore diameter
The average pore diameter of the inner layer 3 of the membrane is determined by adopting an image analysis technology and the characterization of trapped substances with different molecular weights, such as polyethylene glycol with different molecular weights and proteins (lysozyme, chicken protein and bovine serum albumin) with different molecular weights. The average pore size is the arithmetic average of the pores visible on the membrane under a certain magnification and the pore size corresponding to the cut molecular weight at 90% interception position characterized by the retention substances with different molecular weights.
In summary, the present invention is only a preferred embodiment, and is not intended to limit the scope of the invention, and all equivalent changes and modifications made in the content of the claims should be considered as the technical scope of the invention.
Claims (10)
1. A fiber-reinforced hollow fiber multi-core membrane having a plurality of hollow inner cores (8), comprising an outer membrane layer (1), an inner membrane layer (3) and a support layer (2), wherein the inner membrane layer (3) is a surface layer of the hollow inner cores (8), and the support layer (2) is located between the outer membrane layer (1) and the inner membrane layer (3), characterized in that: at least one reinforcing fiber (4) is embedded in the supporting layer (2), and the reinforcing fiber (4) is integrally formed with the outer membrane layer (1), the inner membrane layer (3) and the supporting layer (2).
2. A fiber-reinforced hollow fiber multicore membrane according to claim 1, wherein: the volume of the reinforced fiber (4) is 1-30% of that of the support layer (2).
3. A fiber-reinforced hollow fiber multicore membrane according to claim 1, wherein: the diameter of the reinforced fiber (4) is 0.05-1 mm, and the breaking strength is 10-200N.
4. A fiber-reinforced hollow fiber multicore membrane according to claim 1, wherein: the reinforced fiber (4) is polytetrafluoroethylene, polyvinylidene fluoride, basalt, carbon fiber, polyethylene terephthalate, polybutylene terephthalate, polystyrene, polyolefin, polymethacrylate, polyvinyl chloride, polyamide or polyimide fiber.
5. A fiber-reinforced hollow fiber multicore membrane according to claim 1, wherein: the number of the hollow inner cores (8) is 3-12, and the aperture of the inner membrane layer (3) is 0.5-500 nm.
6. A method of producing a fiber-reinforced hollow fiber multicore membrane according to any one of claims 1 to 5, characterized in that: the method comprises the following steps:
1) preparing a polymer solution: dissolving a solid polymer material in a solvent or diluent at the temperature of 40-300 ℃, and adding a non-solvent additive to prepare a polymer solution, wherein the mass percent concentration of the polymer material is 8-40%, the mass percent concentration of the non-solvent additive is 1-40%, and the mass percent concentration of the solvent or diluent is 20-80%;
2) preparing an inner diameter maintaining agent and reinforcing fibers, wherein the inner diameter maintaining agent is liquid or gas;
3) preliminary molding through a hollow multi-core spinning die: the hollow multi-core spinning die comprises a conventional high polymer solution channel, a plurality of spray needle channels and at least one reinforced fiber channel, wherein the reinforced fiber channel is communicated with the high polymer solution channel, the structures of the high polymer solution channel and the plurality of spray needle channels are adapted to the structure of a hollow multi-core membrane to be obtained, the high polymer solution prepared in the step 1) is extruded from the high polymer solution channel, an inner diameter maintaining agent is sprayed out through the spray needle channels, and meanwhile, the reinforced fiber and the high polymer solution are subjected to composite forming through the reinforced fiber channels;
4) curing by a setting medium: and 3) after leaving the die, the preliminarily formed hollow fiber membrane obtained in the step 3) passes through an air gap, then is immersed into a solidification medium for solidification and formation, and the preliminarily formed membrane is drawn and wound in the solidification medium to obtain the fiber-reinforced hollow fiber multi-core membrane.
7. The method of producing a fiber-reinforced hollow fiber multicore membrane according to claim 6, wherein: the polymer material in the step 1) is at least one selected from polysulfone, sulfonated polysulfone, polyethersulfone, cellulose acetate, polyetheretherketone, polyvinylidene fluoride, polytetrafluoroethylene, polyacrylonitrile, polyvinyl chloride, polyolefin, polysiloxane, polyamide and polyimide.
8. The method of producing a fiber-reinforced hollow fiber multicore membrane according to claim 6, wherein: and 2) the reinforced fiber is one of polytetrafluoroethylene, polyvinylidene fluoride, basalt, carbon fiber, polyethylene terephthalate, polybutylene terephthalate, polystyrene, polyolefin, polymethacrylate, polyvinyl chloride, polyamide or polyimide fiber.
9. The method of producing a fiber-reinforced hollow fiber multicore membrane according to claim 6, wherein: the diameter of the polymer solution channel in the step 3) is 0.5-10 mm, the diameter of the spray needle channel is 0.1-2 mm, the number of the spray needle channels is 3-12, and the diameter of the reinforced fiber channel is 0.05-2 mm.
10. The method of producing a fiber-reinforced hollow fiber multicore membrane according to claim 6, wherein: the air interval length in the step 4) is 0-50 cm, the temperature of the solidification medium is 0-80 ℃, and the traction winding speed is 10-100 m/min.
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