CN111888951A - Method for preparing PVDF hollow fiber composite membrane - Google Patents
Method for preparing PVDF hollow fiber composite membrane Download PDFInfo
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- CN111888951A CN111888951A CN202010758883.8A CN202010758883A CN111888951A CN 111888951 A CN111888951 A CN 111888951A CN 202010758883 A CN202010758883 A CN 202010758883A CN 111888951 A CN111888951 A CN 111888951A
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- hollow fiber
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/30—Polyalkenyl halides
- B01D71/32—Polyalkenyl halides containing fluorine atoms
- B01D71/34—Polyvinylidene fluoride
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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
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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
- B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
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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
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/12—Composite membranes; Ultra-thin membranes
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- Separation Using Semi-Permeable Membranes (AREA)
- Artificial Filaments (AREA)
Abstract
The invention discloses a method for preparing a PVDF hollow fiber composite membrane, which comprises the steps of adding PVDF powder into a mixed solution of propanol, dimethylacetamide and lithium chloride powder, adding a small amount of distilled water, uniformly stirring by using a magnetic stirrer, spinning by using a hollow fiber spinning machine to prepare the hollow fiber composite membrane, soaking in pure water to remove residual solvent, and then placing in a glycerol aqueous solution for storage. The method has simple process flow and low cost of preparation materials, and the prepared composite membrane has the characteristics of high temperature resistance, good flexibility, good mechanical stability, high mechanical strength, long service life, high permeability, high packing density and the like, so the prepared composite membrane has the advantages of greatly improved filtration efficiency, higher practicability and popularization and extremely high market economic value.
Description
Technical Field
The invention belongs to the field of nano materials, and particularly relates to a method for preparing a PVDF hollow fiber composite membrane.
Background
The membrane separation technology is a novel separation technology, uses external energy as power to separate solute and solvent of various components, and has the characteristics of high efficiency, low energy consumption and simple process compared with the conventional filtration method. Polyvinylidene fluoride (PVDF) has the advantages of high temperature resistance, good toughness, stable chemical properties, good film forming capability and the like, and is widely applied to preparation of separation membranes in various research fields. The common preparation method for preparing the PVDF separation membrane in China comprises a sintering method, a stretching method, a track etching method, a phase inversion method and the like, and because the process conditions are different, the domestic separation membrane is slightly lagged in the aspects of mechanical toughness, hardness, permeability and the like, and the defects cause little influence on the service life of the membrane, the efficiency during filtration and the energy consumption.
The common membrane forms in the industry at present include the following flat plate type, roll type, tubular type and hollow fiber type. Wherein, the filling density of the hollow micron fiber composite is very high, and the filtering efficiency is excellent. The pressure resistance depends on the ratio of the inner diameter to the outer diameter of the pipe wall, so that no support is needed, the assembly structure is compact, the size is small, the weight is light, the process is simple, and the production cost is generally lower than that of other types of membranes. Compared with the traditional nanometer membrane structure, the hollow fiber structure has more practical value. The invention makes up the defects of poor mechanical strength, low permeability and the like of the traditional PVDF fiber membrane by manufacturing the PVDF separation membrane with a hollow fiber structure.
Disclosure of Invention
The invention aims to overcome the defects of poor mechanical strength and low permeability of the traditional PVDF fiber membrane and provides a method for preparing a PVDF hollow fiber composite membrane.
The invention adopts the following technical scheme: the method for preparing the PVDF hollow fiber composite membrane is characterized by comprising the following steps:
s1, putting PVDF powder into a vacuum drying oven for drying;
s2, mixing the dried PVDF powder with lithium chloride powder, dimethylacetamide and propanol, then adding a proper amount of distilled water, and uniformly stirring to form a mixed solution;
s3, standing and defoaming the mixed solution in a vacuum drying oven to form a mixture;
s4, adding the defoamed mixture into a hollow fiber spinning machine to spin a hollow fiber composite membrane;
s5, soaking the hollow fiber composite membrane prepared in the step S4 in distilled water for 48 hours, and storing the soaked hollow fiber composite membrane in an aqueous solution containing 30 wt% of glycerol.
Preferably, in step S1, the PVDF powder needs to be dried in a vacuum drying oven at 60 ℃ for 24-36 hours, so as to ensure complete removal of moisture in the PVDF powder.
Preferably, when the mixed solution is prepared in step S2, the mixture is stirred for 8h with a magnetic stirrer at the temperature of 50-60 ℃ and the rotation speed of 400-500rmp until the solution is mixed uniformly.
Preferably, after the preparation of the mixed solution in step S2 is completed, the mixed solution comprises, by mass, 13 wt% of PVDF powder, 5 wt% of acetone, 30-37 wt% of dimethylacetamide, 1-3 wt% of lithium chloride powder, and 1-1.5 wt% of distilled water.
Preferably, the bore fluid used in the hollow fiber spinning machine in the step S4 is 1-3 wt.% NH4The Cl solution has a working temperature of 15-23 ℃ and the flow rate is controlled in1.5-3ml/h, 0.2-5Mpa, 10-15cm of the needle point receiving surface.
Has the advantages that: the method for preparing the PVDF hollow fiber composite membrane provided by the invention has the advantages of simple process flow and low cost of preparation materials, and the prepared composite membrane has the characteristics of high temperature resistance, good flexibility, good mechanical stability, high mechanical strength, long service life, high permeability, high packing density and the like, so that the prepared composite membrane is greatly improved in filtration efficiency, higher in practicability and popularization and extremely high in market economic value.
Drawings
FIG. 1 is a simplified schematic diagram of the preparation process of the present invention;
FIG. 2 is a cross-sectional structure view of a PVDF hollow fiber composite membrane observed by a field emission electron microscope.
Detailed Description
The invention is explained in more detail below with reference to the examples and the figures:
example (b):
as shown in fig. 1, a method for preparing a PVDF hollow fiber composite membrane includes the following steps:
s1, putting PVDF powder into a vacuum drying oven at 60 ℃ for drying for 24-36h to ensure that water in the PVDF powder is completely removed;
s2, mixing the dried PVDF powder with lithium chloride powder, dimethylacetamide and propanol, then adding a proper amount of distilled water, stirring for 8 hours at the temperature of 50-60 ℃ by using a magnetic stirrer with the rotation speed of 400 plus materials of 500rmp until the mixture is uniformly stirred to form a mixed solution, wherein the mixed solution comprises 13 wt% of PVDF powder, 5 wt% of acetone, 30-37 wt% of dimethylacetamide, 1-3 wt% of lithium chloride powder and 1-1.5 wt% of distilled water;
s3, standing and defoaming the mixed solution in a vacuum drying oven to form a mixture;
s4, adding the defoamed mixture into a hollow fiber spinning machine to spin the mixture into a hollow fiber composite membrane, wherein core liquid adopted by the hollow fiber spinning machine is 1-3 wt.% of NH4Cl solution with working temperature of 15-23 deg.C, flow rate of 1.5-3ml/h, pressure of 0.2-5Mpa, and needle point acceptance surface of 10-15 cm;
s5, soaking the hollow fiber composite membrane prepared in the step S4 in distilled water for 48 hours, removing residual solvent, and putting the soaked hollow fiber composite membrane into an aqueous solution containing 30 wt% of glycerol for storage.
As shown in figure 2, the composite membrane prepared by the method has a hollow micron fiber structure, high filling density, no need of a support body, improved strength and service life, an effective aperture of 7.2nm, and a molecular weight cutoff of about 3.7 ten thousand; the membrane has strong water permeability, and can effectively reduce the filtration pressure difference and reduce the resistance; the specific surface area is large, and the filtering efficiency can be improved. In addition, the polyvinylidene fluoride is used as the material of the hollow micron fiber composite membrane, and the hollow micron fiber composite membrane has the advantages of high temperature resistance, good flexibility and good mechanical stability.
Finally, it should be noted that the above-mentioned description is only a preferred embodiment of the present invention, and those skilled in the art can make various similar representations without departing from the spirit and scope of the present invention.
Claims (5)
1. A method for preparing a PVDF hollow fiber composite membrane is characterized by comprising the following steps:
s1, putting PVDF powder into a vacuum drying oven for drying;
s2, mixing the dried PVDF powder with lithium chloride powder, dimethylacetamide and propanol, then adding a proper amount of distilled water, and uniformly stirring to form a mixed solution;
s3, standing and defoaming the mixed solution in a vacuum drying oven to form a mixture;
s4, adding the defoamed mixture into a hollow fiber spinning machine to spin a hollow fiber composite membrane;
s5, soaking the hollow fiber composite membrane prepared in the step S4 in distilled water for 48 hours, and storing the soaked hollow fiber composite membrane in an aqueous solution containing 30 wt% of glycerol.
2. The method for preparing a PVDF hollow fiber composite membrane according to claim 1, wherein: in the step S1, the PVDF powder needs to be put into a vacuum drying oven at 60 ℃ for drying for 24-36h, so as to ensure that the moisture in the PVDF powder is completely removed.
3. A method of preparing PVDF hollow fiber composite membrane according to claim 1 or 2, characterized in that: when the mixed solution is prepared in the step S2, the mixture is stirred for 8 hours at the temperature of 50-60 ℃ by using a magnetic stirrer at the rotating speed of 400-500rmp until the solution is uniformly mixed.
4. The method for preparing PVDF hollow fiber composite membrane according to claim 3, wherein: after the preparation of the mixed solution in the step S2 is completed, the mixed solution comprises, by mass, 13% of PVDF powder, 5% of acetone, 30-37% of dimethylacetamide, 1-3% of lithium chloride powder and 1-1.5% of distilled water.
5. The method for preparing a PVDF hollow fiber composite membrane according to claim 1, wherein: the core liquid adopted by the hollow fiber spinning machine in the step S4 is selected from 1-3 wt.% NH4The Cl solution has the working temperature of 15-23 ℃, the flow rate of 1.5-3ml/h, the pressure of 0.2-5Mpa and the needle point receiving surface of 10-15 cm.
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| CN202010758883.8A CN111888951A (en) | 2020-07-31 | 2020-07-31 | Method for preparing PVDF hollow fiber composite membrane |
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| CN202010758883.8A CN111888951A (en) | 2020-07-31 | 2020-07-31 | Method for preparing PVDF hollow fiber composite membrane |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101837249A (en) * | 2010-06-13 | 2010-09-22 | 苏州绿膜科技有限公司 | Composite polrvinyl chloride hollow fiber ultrafiltration membrane and preparation method thereof |
| CN106268367A (en) * | 2016-09-26 | 2017-01-04 | 天津华清健坤膜科技有限公司 | A kind of high-flux ultra-filtration membrane containing super high molecular weight PVDF and preparation method thereof |
| CN109806771A (en) * | 2019-03-01 | 2019-05-28 | 东华大学 | Nanofiber-based compound hemodialysis membrane of one kind and preparation method thereof |
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2020
- 2020-07-31 CN CN202010758883.8A patent/CN111888951A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101837249A (en) * | 2010-06-13 | 2010-09-22 | 苏州绿膜科技有限公司 | Composite polrvinyl chloride hollow fiber ultrafiltration membrane and preparation method thereof |
| CN106268367A (en) * | 2016-09-26 | 2017-01-04 | 天津华清健坤膜科技有限公司 | A kind of high-flux ultra-filtration membrane containing super high molecular weight PVDF and preparation method thereof |
| CN109806771A (en) * | 2019-03-01 | 2019-05-28 | 东华大学 | Nanofiber-based compound hemodialysis membrane of one kind and preparation method thereof |
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Application publication date: 20201106 |