CN112915803A - Preparation method of microwave wave-shaped hollow fiber nanofiltration membrane - Google Patents
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Abstract
The invention discloses a preparation method of a microwave wave-shaped hollow fiber nanofiltration membrane, which is characterized by comprising the following steps of 1) extruding a membrane casting solution and a core solution from a membrane casting solution port and a core solution port of a spinneret respectively to form a hollow tubular liquid membrane; 2) the liquid membrane enters the gel device to form a gel-state primary membrane wire after passing through the air gap, a wire winding fence is arranged in the gel device, the primary membrane wire forms a micro-wave-shaped membrane wire after passing through the wire winding fence, and the micro-wave-shaped membrane wire is washed and cured after exiting the gel device to obtain the micro-wave-shaped hollow fiber ultrafiltration basal membrane. The membrane filaments in the micro-wave shape can be closely arranged, the degree of freedom is low, the impact of water flow on certain positions is reduced, and the filament breakage condition is well avoided; the effective area of the nanofiltration membrane in the filter element is increased, and the flux of the filter element is improved; the preparation method is simple, low in investment and convenient for industrialization.
Description
Technical Field
The invention belongs to the technical field of filtering membranes, and particularly relates to a preparation method of a microwave-wave-shaped hollow fiber nanofiltration membrane.
Background
Nanofiltration membranes are a new membrane separation technology that has developed relatively rapidly in recent years. The hollow fiber nanofiltration membrane combines the advantages of the hollow fiber and the composite nanofiltration membrane, is of a self-supporting structure, has low membrane component operating pressure, higher membrane filling density and simpler pretreatment and maintenance than a roll type membrane, can be widely applied to the fields of softened water, brackish water desalination, food processing, electronic industry and the like, and is a hotspot of the research in the field of nanofiltration membranes in recent years. The existing hollow fiber nanofiltration membranes are all straight cylinders, in the structure of the filter element assembly, gaps between membrane filaments are large, and the membranes have high degree of freedom and are easy to break during the water flowing process; in addition, the effective area of the straight cylinder membrane is limited, so that the assembled filter element component has small flux.
Chinese patent CN111282455A (with the patent number CN202010125683.9) discloses a preparation method of an external pressure type hollow fiber industrial nanofiltration membrane, which comprises the following steps: respectively injecting the casting solution and the core solution into a spinning nozzle through a gear pump from a casting solution channel and a core solution channel, extruding a hollow tubular liquid film through a casting solution port and a core solution port of the spinning nozzle, allowing the liquid film to pass through an air gap and then pass through two coagulation baths in sequence, winding the liquid film on a winding wheel, performing phase change to form an external pressure type hollow fiber nanofiltration membrane wire, sequentially passing through water and glycerol for soaking the hollow fiber membrane wire, and then airing the hollow fiber membrane wire in air, wherein the casting solution comprises hydrophilic polymers, a feed solution solvent and an auxiliary agent, wherein the casting solution comprises a high polymer, a hydrophilic polymer, a feed solution solvent and an auxiliary agent, and the high polymer at least comprises one of polyether sulfone and polysulfone; the hydrophilic polymer at least comprises one of sulfonated polyethersulfone, sulfonated polysulfone and polyethyleneimine, the solute content of the hydrophilic polymer is 5-30 wt%, and the molecular weight is between 500000-800000 Da; the feed liquid solvent comprises at least one of dimethylformamide, dimethylacetamide and N-methylpyrrolidone, and the auxiliary agent comprises at least one of polyethylene glycol, ethylene glycol, lithium chloride and lithium bromide. In the scheme, the liquid film passes through the air gap and then sequentially passes through the two coagulation baths and then is wound on the wire winding wheel, the hollow fiber nanofiltration membrane prepared by the method is in a straight cylindrical shape, and in the structure of the filter element assembly, the hollow fiber nanofiltration membrane is easy to break and the flux of the assembled assembly is small.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of a microwave wave-shaped hollow fiber nanofiltration membrane, which can increase the effective area of the nanofiltration membrane in a filter element assembly and improve the flux of the filter element, aiming at the current situation of the prior art.
The technical scheme adopted by the invention for solving the technical problems is as follows: a preparation method of a microwave wave-shaped hollow fiber nanofiltration membrane is characterized by comprising the following steps:
1) respectively extruding the casting solution and the core solution from a casting solution port and a core solution port of a spinning nozzle to form a hollow tubular liquid film;
2) the liquid membrane enters a gel device to form a gel-state primary membrane wire after passing through an air gap, a wire winding fence is arranged in the gel device, the primary membrane wire forms a micro-wave-shaped membrane wire after passing through the wire winding fence, and the micro-wave-shaped membrane wire is washed and cured after exiting the gel device to obtain a micro-wave-shaped hollow fiber ultrafiltration basal membrane;
3) immersing the microwave wave-shaped hollow fiber ultrafiltration base membrane into the water phase solution for a period of time, taking out and drying the base membrane to remove redundant water, immersing the base membrane into the prepared oil phase solution to generate interfacial polymerization reaction, taking out and heating and drying the base membrane to obtain the microwave wave-shaped hollow fiber nanofiltration membrane.
Preferably, the pressure of the casting film in the step 1) is 0.5-2 bar, the temperature is 45-60 ℃, the flow rate is 5-15 g/min, the pressure of the core liquid is 0.1-0.5 bar, the temperature is 45-60 ℃, and the flow rate is 0.5-1 g/min; the inner diameter of the spinning nozzle is 0.2-0.4 mm, the outer diameter of the spinning nozzle is 0.4-0.6 mm, and the temperature of the spinning nozzle is 45-65 ℃; the height of the air gap in the step 2) is 5-10 cm, and the temperature is 20-30 ℃; the temperature of the gel device is 40-60 ℃, the water washing is four-stage, and the temperatures are 75-80 ℃, 80-85 ℃, 85-90 ℃ and 90-95 ℃ respectively.
Preferably, the membrane casting solution in step 1) comprises a high molecular polymer, a hydrophilic additive, a non-solvent additive and a solvent, wherein the high molecular polymer at least comprises one of polysulfone and polyethersulfone; the hydrophilic additive comprises one or more of polyvinylpyrrolidone and polyethylene glycol; the non-solvent additive is pure water; the solvent comprises one of N, N-dimethylacetamide, dimethyl pyrrolidone, N-dimethylformamide, dimethyl sulfoxide and tetrahydrofuran; the core liquid comprises a solvent and water, and the solvent of the core liquid is the same as the added solvent of the casting solution.
Preferably, the molecular weight of the polymer in the casting solution in the step 1) is 7 to 9 ten thousand, the molecular weight of the hydrophilic additive polyvinylpyrrolidone is 0.5 to 5 ten thousand, and the molecular weight of the polyethylene glycol is 200 to 2000.
Preferably, the casting solution in the step 1) comprises the following components in percentage by mass: 18-25% of high molecular polymer, 5-20% of hydrophilic additive, 3-8% of non-solvent additive and 47-74% of solvent; the core liquid comprises the following components in percentage by mass: 50-85% of solvent and the balance of water.
The prepared microwave wave-shaped membrane filaments can be regarded as a shape consisting of sine functions, and in order to control the amplitude and the period of the microwave wave-shaped membrane filaments, the filament winding fences in the step 2) preferably comprise 2 or more than 2 polished rods which are transversely, parallelly and alternately arranged, the radius of each polished rod is 0.5-3 cm, the horizontal distance of each polished rod is 0.3-4 cm, and the vertical distance of each polished rod is 0-2.5 cm. Too large amplitude or too small period of the membrane filaments are seriously bent, the membrane filaments are staggered when the membrane filaments are assembled into a component, the component is easily disordered and seriously influences the performance of the component, and the too small amplitude or too large period of the membrane filaments cannot show the action of micro waves, so the numerical values of the radius and the distance need to be in the range.
Preferably, the wire winding fence comprises vertically arranged mounting supports, the polished rod is arranged between the mounting supports, a support frame detachably connected with the gel device is arranged on the mounting supports, and a limit groove is formed in the polished rod along the circumferential direction. The limiting groove is arranged to limit the left and right movement of the membrane wire.
Preferably, the temperature of the light bar in the step 2) is 5-50 ℃. The purpose of the heating is to slow down the speed of the phase separation of the film filaments and slow down the degree of solidification, so that the micro-wave shape can be formed on the fence with enough time.
Preferably, the aqueous phase solution in step 3) includes polyamine monomer and pure water, the polyamine monomer is selected from at least one of piperazine, m-phenylenediamine, p-phenylenediamine and ethylenediamine, the oil phase solution includes polyacyl chloride monomer and organic solvent, the polyacyl chloride monomer is selected from at least one of trimesoyl chloride, terephthaloyl chloride and isophthaloyl chloride, and the organic solvent is selected from at least one of pentane, n-hexane, cyclohexane and heptane.
Preferably, the aqueous phase solution comprises the following components in percentage by mass: 2-5% of polyamine monomer, and the balance of water; the oil phase solution comprises the following components in percentage by mass: 0.2-1% of polyacyl chloride monomer, and the balance of organic solvent.
Compared with the prior art, the invention has the advantages that: the casting film liquid is subjected to phase transformation to form a gel-state primary film wire, the film wire is not completely cured and is soft, and then the film wire is wound by a wire winding fence to form a micro-wave-shaped film wire, the micro-wave-shaped film wire and the film wire can be tightly arranged, the degree of freedom is low, the impact of water flow on certain positions is reduced, and the wire breaking condition is well avoided; the effective area of the nanofiltration membrane in the filter element is increased, and the flux of the filter element is improved; the preparation method is simple, low in investment and convenient for industrialization.
Drawings
FIG. 1 is a schematic view of a wire-wrapping fence in an embodiment of the present invention. Wherein 1 is a polish rod, 3 is a mounting bracket, and 4 is a supporting frame.
Fig. 2 is an enlarged view of a portion I of fig. 1. And 2 is a limit groove.
FIG. 3 shows the arrangement of the light bar and the filament winding in embodiment 1 of the present invention. Wherein 1 is a polish rod, and 5 is a membrane filament.
Fig. 4 shows the arrangement of the light bar and the filament winding in embodiments 2 and 3 of the present invention. Wherein 1 is a polish rod, and 5 is a membrane filament.
Fig. 5 is a picture of a hollow fiber nanofiltration membrane according to example 1 and comparative example of the present invention.
Detailed Description
The invention is described in further detail below with reference to the accompanying examples.
Example 1:
1) preparing a casting solution by mixing 25%, 47%, 20% and 8% of polysulfone (PSf) high polymer (with a molecular weight of 7 ten thousand), N-dimethylacetamide (DMAc), a pore diameter regulator polyvinylpyrrolidone (PVP) (with a molecular weight of 1 ten thousand) and pure water in sequence according to mass percentage; mixing 50% and 50% of N, N-dimethylacetamide and pure water by mass percent to prepare core liquid; respectively injecting the membrane casting solution and the core solution into a spinning nozzle through a gear pump from a membrane casting solution channel and a core solution channel, and extruding a hollow tubular liquid membrane through a membrane casting solution port and a core solution port of the spinning nozzle, wherein the inner diameter and the outer diameter of a membrane wire are 0.2/0.4mm, the pressure of the membrane casting solution is 2bar, the temperature is 45 ℃, the flow rate is 15g/min, the pressure of the core solution is 0.5bar, the temperature is 45 ℃, the flow rate is 1g/min, and the temperature of the spinning nozzle is 45 ℃.
2) The liquid membrane enters a gel tank (a gel device) after passing through an air gap, the height of the air gap is 5cm, the temperature is 30 ℃, the temperature of the gel tank is 40 ℃, the hollow tubular liquid membrane enters the gel tank to be subjected to split-phase curing to form a primary membrane wire, then the primary membrane wire passes through a wire winding fence shown in figure 1, as shown in figure 3, the radius r of a polish rod is 0.5cm, the horizontal direction distance d is 0.3cm as shown in figure 3, the temperature of the polish rod is 25 ℃, the membrane wire in the shape of micro waves exits the gel tank, then the membrane wire is washed by water and wound by a wire winding wheel, and the temperatures of a four-level water washing tank are 75 ℃, 80 ℃, 85 ℃ and 90 ℃ respectively, so that the microwave wave-shaped hollow.
3) Preparing aqueous phase solution with piperazine (PIP) and water respectively accounting for 2% and 98% by mass, and oil phase solution with trimesoyl chloride (TMC) and pentane respectively accounting for 0.2% and 99.8% by mass; and then immersing the microwave wave-shaped hollow fiber ultrafiltration base membrane prepared in the step 2) into a water phase for 10min, taking out the membrane from the air, airing the membrane for 5min, immersing the membrane into an oil phase for 30s, taking out the membrane from an oven, and drying the membrane for 1min at 50 ℃ to obtain the micro-wave-shaped hollow fiber nanofiltration membrane.
Example 2:
1) preparing a casting solution by mixing 18 percent, 74 percent, 5 percent and 3 percent of polysulfone (PSf) high polymer (with the molecular weight of 9 ten thousand), N-dimethylacetamide (DMAc), a pore diameter regulator polyvinylpyrrolidone (PVP) (with the molecular weight of 2 ten thousand) and pure water in sequence according to mass percentage; mixing N, N-dimethylacetamide and pure water according to the mass percentage of 60% and 40% respectively to prepare core liquid; respectively injecting the membrane casting solution and the core solution into a spinning nozzle through a gear pump from a membrane casting solution channel and a core solution channel, extruding a hollow tubular liquid membrane through a membrane casting solution port and a core solution port of the spinning nozzle, wherein the inner diameter and the outer diameter of a membrane wire are 0.4/0.6mm, the pressure of the membrane casting solution is 1bar, the temperature is 45 ℃, the flow rate is 5g/min, the pressure of the core solution is 0.5bar, the temperature is 45 ℃, the flow rate is 1g/min, and the temperature of the spinning nozzle is 45 ℃.
2) The liquid membrane enters a gel tank (a gel device) after passing through an air gap, the height of the air gap is 10cm, the temperature is 23 ℃, the temperature of the gel tank is 40 ℃, the hollow tubular liquid membrane enters the gel tank to be subjected to split-phase curing to form a nascent membrane filament, then the nascent membrane filament passes through a filament winding fence shown in figure 1, as shown in figure 4, the radius r of a polished rod is 1cm, the horizontal direction distance d is 1cm, as shown in figure 4, the vertical distance e of the polished rod is 1cm, the temperature of the polished rod is 50 ℃, the microwaved membrane filament is wound by a filament winding wheel after exiting the gel tank, the temperature of a four-stage water washing tank is 75 ℃, 80 ℃, 85 ℃ and 90 ℃, and the microwave-wave-shaped hollow fiber ultrafiltration basal membrane is obtained after curing.
3) Preparing aqueous phase solution with the mass percentages of piperazine (PIP) and water of 2 percent and 98 percent respectively, and oil phase solution with the mass percentages of trimesoyl chloride (TMC) and pentane of 0.2 percent and 99.8 percent respectively; and then immersing the microwave wave-shaped hollow fiber ultrafiltration membrane prepared in the step 2) into a water phase for 10min, taking out the hollow fiber ultrafiltration membrane from the air, airing the hollow fiber ultrafiltration membrane for 5min, immersing the hollow fiber ultrafiltration membrane into an oil phase for 30s, taking out the hollow fiber ultrafiltration membrane from an oven, and drying the hollow fiber ultrafiltration membrane for 1min at 50 ℃ to obtain the micro wave-shaped hollow fiber nanofiltration membrane.
Example 3:
1) mixing polyether sulfone (PES) high polymer (with the molecular weight of 9 ten thousand), dimethyl sulfoxide (DMSO), pore-size regulator polyethylene glycol (PEG) (with the molecular weight of 2000) and pure water according to the mass percentages of 18%, 74%, 5% and 3% in sequence to prepare a casting solution; mixing 75% and 25% dimethyl sulfoxide and pure water by mass percent to prepare core liquid; respectively injecting the membrane casting solution and the core solution into a spinning nozzle through a gear pump from a membrane casting solution channel and a core solution channel, extruding a hollow tubular liquid membrane through a membrane casting solution port and a core solution port of the spinning nozzle, wherein the inner diameter and the outer diameter of a membrane wire are 0.4/0.6mm, the pressure of the membrane casting solution is 1bar, the temperature is 50 ℃, the flow rate is 10g/min, the pressure of the core solution is 0.3bar, the temperature is 55 ℃, the flow rate is 0.7g/min, and the temperature of the spinning nozzle is 45 ℃.
2) The liquid membrane enters a gel tank (a gel device) after passing through an air gap, the height of the air gap is 10cm, the temperature is 20 ℃, the temperature of the gel tank is 55 ℃, the hollow tubular liquid membrane enters the gel tank to be subjected to split-phase curing to form a nascent membrane filament, then the nascent membrane filament passes through a filament winding fence shown in figure 1, as shown in figure 2, the radius r of a polished rod is 3cm, the horizontal direction distance d is 4cm as shown in figure 4, the vertical distance e of the polished rod is 2.5cm, the temperature of the polished rod is 50 ℃, the microwaved membrane filament passes through the gel tank to be washed and wound by a filament winding wheel, and the temperatures of four-level water washing tanks are 75 ℃, 80 ℃, 85 ℃ and 90 ℃, respectively, and the microwave-wave-shaped hollow fiber ultrafiltration basal membrane is obtained.
3) Preparing water phase solution with piperazine (PIP) and water respectively 5% and 95% in mass percentage, and oil phase solution with trimesoyl chloride (TMC) and pentane respectively 1% and 99% in mass percentage; and then immersing the microwave wave-shaped hollow fiber ultrafiltration membrane prepared in the step 2) into a water phase for 10min, taking out the hollow fiber ultrafiltration membrane from the air, airing the hollow fiber ultrafiltration membrane for 5min, immersing the hollow fiber ultrafiltration membrane into an oil phase for 30s, taking out the hollow fiber ultrafiltration membrane from an oven, and drying the hollow fiber ultrafiltration membrane for 1min at 50 ℃ to obtain the micro wave-shaped hollow fiber nanofiltration membrane.
Comparative example: the preparation steps, related substances and parameter control are the same as those of the comparative example 1, except that the liquid film in the step 2) enters a gel tank after passing through an air gap, passes through the gel tank, then passes through a water washing tank, is wound by a winding wheel, and is cured to obtain the microwave-wave-shaped hollow fiber ultrafiltration basal membrane.
The hollow fiber nanofiltration membranes of the examples and the comparative examples were assembled into modules, and the flux levels of the modules were tested. The testing steps are as follows: the prepared hollow fiber nanofiltration membrane is prepared into filter elements with the same specification (1812 model), the filter elements are assembled into a component and placed into an external pressure type hollow fiber industrial nanofiltration membrane testing device, as the dense selection layer is positioned at the outer side of the composite hollow fiber, the original solution circulates through the inner cavity side of the membrane component under the membrane inlet pressure of 6bar, and the produced water flows out from the outer cavity side of the membrane component. Deionized water is used as a raw water solution to obtain the purified water permeability of the composite membrane, and then the purified water permeability is changed into a magnesium sulfate solution with 250ppm to test the desalination rate.
Table 1 flux and salt rejection for assembly of hollow fiber nanofiltration membranes into modules of examples and comparative examples
| Numbering | flux/G | Percent of magnesium sulfate salt rejection |
| Example 1 | 430 | 95.0 |
| Example 2 | 446 | 96.3 |
| Example 3 | 472 | 95.2 |
| Comparative example | 395 | 95.9 |
Claims (10)
1. A preparation method of a microwave wave-shaped hollow fiber nanofiltration membrane is characterized by comprising the following steps:
1) respectively extruding the casting solution and the core solution from a casting solution port and a core solution port of a spinning nozzle to form a hollow tubular liquid film;
2) the liquid membrane enters a gel device to form a gel-state primary membrane wire after passing through an air gap, a wire winding fence is arranged in the gel device, the primary membrane wire forms a micro-wave-shaped membrane wire after passing through the wire winding fence, and the micro-wave-shaped membrane wire is washed and cured after exiting the gel device to obtain a micro-wave-shaped hollow fiber ultrafiltration basal membrane;
3) immersing the microwave wave-shaped hollow fiber ultrafiltration base membrane into the water phase solution for a period of time, taking out and drying the base membrane to remove redundant water, immersing the base membrane into the prepared oil phase solution to generate interfacial polymerization reaction, taking out and heating and drying the base membrane to obtain the microwave wave-shaped hollow fiber nanofiltration membrane.
2. The method of preparing a microwave wave-shaped hollow fibrous nanofiltration membrane according to claim 1, wherein: in the step 1), the pressure of the casting film is 0.5-2 bar, the temperature is 45-60 ℃, the flow rate is 5-15 g/min, the pressure of the core liquid is 0.1-0.5 bar, the temperature is 45-60 ℃, and the flow rate is 0.5-1 g/min; the inner diameter of the spinning nozzle is 0.2-0.4 mm, the outer diameter of the spinning nozzle is 0.4-0.6 mm, and the temperature of the spinning nozzle is 45-65 ℃; the height of the air gap in the step 2) is 5-10 cm, and the temperature is 20-30 ℃; the temperature of the gel device is 40-60 ℃, the water washing is four-stage, and the temperatures are 75-80 ℃, 80-85 ℃, 85-90 ℃ and 90-95 ℃ respectively.
3. The method of preparing a microwave wave-shaped hollow fibrous nanofiltration membrane according to claim 1, wherein: the membrane casting solution in the step 1) comprises a high molecular polymer, a hydrophilic additive, a non-solvent additive and a solvent, wherein the high molecular polymer at least comprises one of polysulfone and polyethersulfone; the hydrophilic additive comprises one or more of polyvinylpyrrolidone and polyethylene glycol; the non-solvent additive is pure water; the solvent comprises one of N, N-dimethylacetamide, dimethyl pyrrolidone, N-dimethylformamide, dimethyl sulfoxide and tetrahydrofuran; the core liquid comprises a solvent and water, and the solvent of the core liquid is the same as the added solvent of the casting solution.
4. The method of preparing a microwave wave-shaped hollow fibrous nanofiltration membrane according to claim 3, wherein: the molecular weight of the high molecular polymer in the membrane casting solution in the step 1) is 7-9 ten thousand, the molecular weight of the hydrophilic additive polyvinylpyrrolidone is 0.5-5 ten thousand, and the molecular weight of the polyethylene glycol is 200-2000.
5. The method of preparing a microwave wave-shaped hollow fibrous nanofiltration membrane according to claim 3, wherein: the casting solution in the step 1) comprises the following components in percentage by mass: 18-25% of high molecular polymer, 5-20% of hydrophilic additive, 3-8% of non-solvent additive and 47-74% of solvent; the core liquid comprises the following components in percentage by mass: 50-85% of solvent and the balance of water.
6. The method of preparing a microwave wave-shaped hollow fibrous nanofiltration membrane according to claim 1, wherein: the wire winding fence in the step 2) comprises polished rods which are 2 or more than 2 in number, are arranged transversely, parallelly and at intervals, the radius of each polished rod is 0.5-3 cm, the horizontal distance between the polished rods is 0.3-4 cm, and the vertical distance between the polished rods is 0-2.5 cm.
7. The method of preparing a microwave wave-shaped hollow fibrous nanofiltration membrane according to claim 6, wherein: the wire winding fence comprises vertically arranged mounting supports, the polished rod is arranged between the mounting supports, a support frame detachably connected with the gel device is arranged on the mounting supports, and a limit groove is formed in the polished rod along the circumferential direction.
8. The method of preparing a microwave wave-shaped hollow fibrous nanofiltration membrane according to claim 6, wherein: the temperature of the light bar in the step 2) is 5-50 ℃.
9. The method of preparing a microwave wave-shaped hollow fibrous nanofiltration membrane according to claim 1, wherein: the water phase solution in the step 3) comprises polyamine monomers and pure water, the polyamine monomers are selected from at least one of piperazine, m-phenylenediamine, p-phenylenediamine and ethylenediamine, the oil phase solution comprises polybasic acyl chloride monomers and an organic solvent, the polybasic acyl chloride monomers are selected from at least one of trimesoyl chloride, terephthaloyl chloride and isophthaloyl chloride, and the organic solvent is selected from at least one of pentane, n-hexane, cyclohexane and heptane.
10. The method for preparing a microwave-shaped hollow fiber nanofiltration membrane according to claim 9, wherein the aqueous phase solution comprises the following components in percentage by mass: 2-5% of polyamine monomer, and the balance of water; the oil phase solution comprises the following components in percentage by mass: 0.2-1% of polyacyl chloride monomer, and the balance of organic solvent.
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| CN113529271A (en) * | 2021-08-27 | 2021-10-22 | 浙江三创无纺布科技有限公司 | Method for manufacturing non-woven fabric with excellent elasticity and applied to baby wet tissue |
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| CN105396470A (en) * | 2015-12-10 | 2016-03-16 | 广州中国科学院先进技术研究所 | Hollow fiber composite nanofiltration membrane and preparation method thereof |
| CN108697986A (en) * | 2016-03-01 | 2018-10-23 | 费森尤斯医疗护理德国有限责任公司 | Hollow-fiber film with three-dimensional crimp portion |
| CN109692576A (en) * | 2017-10-20 | 2019-04-30 | 宁波方太厨具有限公司 | The interface-cross-linked modification method for preparing of hollow fiber ultrafiltration membrane |
| CN211562524U (en) * | 2020-07-27 | 2020-09-25 | 天津膜天膜科技股份有限公司 | Wave type hollow fiber membrane manufacturing membrane assembly and membrane assembly thereof |
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