CN113813799A - Preparation method of PVDF ultrafiltration membrane with polyester lining - Google Patents
Preparation method of PVDF ultrafiltration membrane with polyester lining Download PDFInfo
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- 238000000108 ultra-filtration Methods 0.000 title claims abstract description 51
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- 238000002360 preparation method Methods 0.000 title claims abstract description 29
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- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 60
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 27
- 238000005266 casting Methods 0.000 claims abstract description 21
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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
- B01D71/36—Polytetrafluoroethene
-
- 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
-
- 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
- B01D69/10—Supported membranes; Membrane supports
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention discloses a preparation method of a PVDF ultrafiltration membrane with a terylene lining, which takes a terylene braided tube as the lining, PVDF as a membrane material, DMAc as a solvent, BD-3071 as a dispersant, PMMA, PVP-k30 and glycerol as additives, wherein the addition amount of PMMA is 0.05-2.5 wt%, the addition amount of BD-3071 is 0.05-2.5 wt%, the addition amounts of PVP-k30 and glycerol are 1-12 wt%, and the PVDF ultrafiltration membrane is stirred at 65-75 ℃ for 16-20h and then is kept stand for defoaming for 12-16 h; conveying the casting solution to a spinning nozzle at the speed of 300 plus 350ml/min by using a metering pump, enabling the terylene lining to pass through the center of the spinning nozzle, uniformly coating the casting solution on the outer surface of the terylene braided tube, and enabling the flow rate of core solution pure water to be 120 plus 180 ml/min; the braided tube coated with the membrane casting solution enters a gel bath containing DMAc aqueous solution and is converted into a membrane at the temperature of 32-38 ℃; and (3) collecting the cured membrane filaments through a take-up pulley at 18-23m/min, and soaking the membrane filaments in water-glycerol mixed solutions with different proportions in stages to obtain the polyester lining enhanced PVDF ultrafiltration membrane. The ultrafiltration membrane has high compressive strength, and the adhesion between the membrane separation layer and the lining is strong, so that the ultrafiltration membrane can stably run for a long time.
Description
Technical Field
The invention relates to the technical field of polymer membrane materials, in particular to a preparation method of a PVDF ultrafiltration membrane with a terylene lining.
Background
The human survival and the social development can not be supported by water resources, the shortage of fresh water resources becomes a global problem along with the acceleration of the industrialization process and the growth of population, and the seawater desalination and the wastewater reuse are sustainable means for solving the water resource crisis. The membrane separation technology has the advantages of normal-temperature operation, no phase change, small occupied area, high efficiency, modularized design, easy combination with other processes and the like, and as a novel, efficient and green separation technology, the membrane separation technology is widely applied to the fields of petrochemical industry, biological medicine, food processing, environmental protection, metallurgy, seawater desalination, medical treatment and the like, and is particularly suitable for the urgent needs of modern industry on the aspects of energy conservation, emission reduction, efficient resource utilization and the like.
An ideal separation membrane should have high permeability, good mechanical strength and chemical stability, and the selection of membrane-forming materials and membrane-preparation processes will directly affect the above-mentioned properties of the membrane. For a membrane to be used commercially, both its mechanical strength and its permselectivity are important indicators of membrane performance. The hollow fiber membrane is a self-supporting membrane, has the advantages of large packing density, large specific surface area, easy assembly and the like, and is widely used for advanced treatment of sewage. However, hollow fiber membranes are generally low in strength, so that they are easily damaged by high-pressure water or air flow during use. There have been a lot of studies on the improvement of mechanical strength of hollow fiber membranes, and introduction of a reinforcement in the membrane has proved to be an effective method.
The reinforced controlled fiber membrane generally consists of 3 parts, namely an internal reinforcement, a membrane separation layer, and an interfacial bonding layer therebetween, which determines the bonding force between the reinforcement and the separation layer and is of great importance for the membrane performance. At present, reinforced hollow fiber membranes at home and abroad are mainly classified into long fiber reinforced hollow fiber membranes and fiber tube reinforced hollow fiber membranes, but the long fiber reinforced central control fiber membranes cannot give consideration to compressive strength and tensile strength, the fiber tube reinforced hollow fiber membranes are prepared by coating a membrane casting solution on the outer surface of a fiber tube, the strength of the reinforced hollow fiber membranes can be improved to the greatest extent while the membrane separation performance is ensured, but the preparation process is complex, the operation is difficult, and many problems are needed to be solved at present. Wherein how to improve the adhesion between the support and the membrane separation layer is directly related to the service life of the membrane.
Disclosure of Invention
Therefore, the technical problem to be solved by the invention is to provide a preparation method of a PVDF ultrafiltration membrane with a polyester lining, which adopts a polyester braided tube as the lining, PVDF as a membrane material, PMMA as a binder to enhance the binding force between the lining and the membrane material, BD-3071, PVP-k30 and glycerol as additives to regulate the microstructure and hydrophilicity of the membrane, and a high-strength modified ultrafiltration membrane is prepared in one step by a non-solvent induced phase inversion method.
The technical scheme of the invention is that a preparation method of a PVDF ultrafiltration membrane with a terylene lining comprises the steps of a, taking a terylene braided tube as the lining, PVDF as a membrane material, DMAc as a solvent, polyether modified polydimethylsiloxane (BD-3071) as a dispersant, polymethyl methacrylate (PMMA), PVP-k30 and glycerol as additives, wherein the addition amount of PMMA is 0.05-2.5 wt%, the addition amount of BD-3071 is 0.05-2.5 wt%, the addition amount of PVP-k30 is 1-12 wt%, the addition amount of glycerol is 1-12 wt%, stirring is carried out at 65-75 ℃ for 16-20h, and then standing and defoaming are carried out for 12-16 h;
b. conveying the casting solution to a spinning nozzle at the speed of 300 plus 350ml/min by using a metering pump, enabling the terylene lining to pass through the center of the spinning nozzle, uniformly coating the casting solution on the outer surface of the terylene braided tube, and enabling the flow rate of core solution pure water to be 120 plus 180 ml/min; the braided tube coated with the membrane casting solution enters a gel bath containing DMAc aqueous solution and is converted into a membrane at the temperature of 32-38 ℃;
c. and (3) collecting the cured membrane filaments through a take-up pulley at 18-23m/min, and soaking the membrane filaments in water-glycerol mixed solutions with different proportions in stages to finally obtain the polyester lining enhanced PVDF ultrafiltration membrane.
The terylene has good elasticity and is not easy to deform, the terylene has the best heat stability in the synthetic fiber, and the performance is favorable for the uniform coverage of the surface of the casting solution. The above-mentioned addition amount ratio is the content of each component in 100g of the casting solution.
The PVDF membrane is positioned at the outer interface of the braided tube and is in coaxial cylindrical relation with the braided tube.
The film of the present invention can be obtained only after sufficient exchange of the solvent and the non-solvent after the conversion into a film, i.e., a small amount of the solvent present in the film after the initial curing is replaced with water. The silk is received in order to roll up the membrane and be convenient for subsequent processing, and soaking makes solvent and non-solvent fully exchange on the one hand, and on the other hand lets glycerine enter into the membrane hole and makes the phenomenon that the membrane hole collapses because of moisture evaporation is too fast appearing in the in-process of drying the membrane. Films containing a reinforced liner, such as the polyester braided tube of the present invention, may be referred to as reinforced films.
Preferably, the water-glycerol mixed solution with different ratios in the step c refers to that the water-glycerol mixed solution is soaked in water in a ratio of 9.5-10.5:1, 6.5-7.5:3, 4.5-5.5:5 and 2-3:6-7 respectively. Soaking in 9.5-10.5:1 water-glycerol solution for 10-12 h, and then soaking in 6.5-7.5:3, 4.5-5.5:5, and 2-3:6-7 water-glycerol solution for 3-5 h. And finally, taking out the film, hanging and airing. The proportion is weight ratio, and the shrinkage of the membrane pores can be effectively prevented by soaking the membrane pores in water-glycerol solutions with different proportions.
According to the preparation method of the PVDF ultrafiltration membrane with the terylene lining, disclosed by the invention, the stirring speed is preferably 70-90 rpm.
According to the preparation method of the PVDF ultrafiltration membrane with the terylene lining, disclosed by the invention, the concentration of the DMAc aqueous solution is preferably 0.5-2 wt%.
According to the preparation method of the PVDF ultrafiltration membrane with the polyester lining, disclosed by the invention, the inner diameter of the polyester braided tube is preferably 0.6-1.0mm, the outer diameter of the polyester braided tube is preferably 1.6-2.0mm, and the pore diameter of the polyester braided tube is preferably 0.3-0.5 mm.
According to the preparation method of the PVDF ultrafiltration membrane with the polyester lining, disclosed by the invention, the addition amount of PMMA is preferably 0.1-2%.
According to the preparation method of the PVDF ultrafiltration membrane with the polyester lining, disclosed by the invention, the addition amount of BD-3071 is preferably 0.1-2%.
According to the preparation method of the PVDF ultrafiltration membrane with the polyester lining, disclosed by the invention, the addition amount of the PVP-k30 is preferably 2% -10%.
According to the preparation method of the PVDF ultrafiltration membrane with the polyester lining, disclosed by the invention, the addition amount of the glycerol is preferably 2% -10%.
According to the preparation method of the PVDF ultrafiltration membrane with the terylene lining, disclosed by the invention, the pure water flux of the prepared ultrafiltration membrane is preferably 140-160L/(m2 h); the bubble point pressure is 0.04-0.06 MPa.
The treatment capacity of the wastewater with the turbidity of 0.484NTU is 110-.
Compared with the prior art, the invention has the following positive effects:
the invention has the positive significance that the prepared ultrafiltration membrane has higher compressive strength, the adhesion effect between the membrane separation layer and the lining is stronger, and the ultrafiltration membrane can stably run for a long time. The ultrafiltration membrane prepared by taking the terylene braided tube as the lining has the advantages of simple and convenient operation, mild preparation conditions, low cost and better industrial application prospect.
Drawings
FIG. 1 is a scanning electron microscope cross-sectional view of an ultrafiltration membrane of example 1;
FIG. 2 is a scanning electron microscope surface view of an ultrafiltration membrane of example 1;
FIG. 3 is a scanning electron microscope cross-sectional view of an ultrafiltration membrane of example 1;
FIG. 4 is a scanning electron microscope cross-sectional view of an ultrafiltration membrane of example 1;
fig. 5 is a schematic diagram of the performance test of the ultrafiltration membrane of example 3.
Detailed Description
The following provides a specific embodiment of the preparation method of the PVDF ultrafiltration membrane with the terylene lining.
A preparation method of a PVDF ultrafiltration membrane with a terylene lining comprises the following steps:
the prepared ultrafiltration membrane is pre-pressed for half an hour by pure water under 0.02MPa, and the water flux of the membrane is tested by the pure water, and the calculation formula is shown as (1).
Wherein J is the flux of the membrane (L/(m)2H)), V is the volume (L) of the collected permeate, and A is the effective area (m) of the membrane2) And T is the time (h) required for collecting V volumes of permeate.
And (3) testing the interception performance of the membrane by using a BAS solution with the concentration of 20ppm as a feed liquid, carrying out sample connection detection after 30min, and calculating the method as shown in (2).
Wherein R is the rejection of the membrane, CpConcentration on the permeation side (ppm), CfIs the concentration (ppm) on the feed side.
The concentration of the organic matter solution was measured by a Total Organic Carbon (TOC) analyzer to determine the retention rate.
The membranes after BSA filtration were washed with pure water and then tested for pure water flux, and the washing recovery was calculated as shown in (3).
Wherein Jw1Is the initial pure water flux (L/(m)2·h))，Jw2Is the pure water flux (L/(m) of the membrane after cleaning2·h))。
The tensile strength of the film was measured with a tensile strength tester.
The bubble pressure gauge measures the bubble point pressure of the membrane.
The invention is prepared in the previous stage by the following steps:
(1) controlling the experimental environment: adjusting the temperature of the experimental environment to be between 15 and 35 ℃, and controlling the relative humidity of the laboratory to be 45-65%.
(2) And (3) manufacturing a membrane module: and (3) airing the membrane wires in the experimental environment until no liquid drops exist on the surface, and pouring the aired membrane wires into assemblies by respectively using polyurethane hard glue and soft glue with the hardness of 70-80D and 30-40A.
Example 1
The terylene braided tube is used as a lining, and PVDF is used as a membrane material. The inner diameter of the terylene braided tube is 0.6mm, the outer diameter is 1.6mm, and the aperture is 0.3 mm. The adding amount of PMMA is 0.05 wt%, the adding amount of BD-3071 is 1%, the adding amount of PVP-k30 is 5 wt%, the adding amount of glycerol is 4 wt%, stirring is carried out for 16h at 68 ℃, standing and defoaming are carried out for 12h, a metering pump is used for conveying the casting solution to a spinning nozzle at the speed of 310ml/min, a polyester lining passes through the center of the spinning nozzle, the casting solution is uniformly coated on the outer surface of a polyester weaving tube, and the flow rate of core solution pure water is 120 ml/min; the braided tube coated with the membrane casting solution enters a gel bath containing DMAc aqueous solution and is converted into a membrane at 35 ℃; and (3) collecting the cured membrane filaments by a filament collecting wheel at 20m/min, and soaking the membrane filaments in water-glycerol mixed solutions with different proportions in stages to finally obtain the polyester lining enhanced PVDF ultrafiltration membrane.
Soaking in water-glycerol at ratio of 9:1, 6.5:3, 5:5, and 3:6 respectively. Soaking in 9:1 water-glycerol solution for 10h, and then soaking in the latter three water-glycerol solutions for 3.5 h. And finally, taking out the film, hanging and airing.
And (3) packaging the ultrafiltration membrane filaments in the component by using the sealant, mounting the manufactured membrane component in a testing device, and testing the water flux and the organic substance interception performance of the membrane component, wherein the test result is as follows.
The separation performance of the membrane was investigated using actual wastewater as influent water, and the test results were as follows.
Example 2
The terylene braided tube is used as a lining, PVDF is used as a membrane material, the inner diameter of the terylene braided tube is 0.8mm, the outer diameter is 1.8mm, and the aperture is 0.4 mm. The adding amount of PMMA is 0.5 wt%, the adding amount of BD-3071 is 1.8%, the adding amount of PVP-k30 is 1 wt%, the adding amount of glycerol is 1 wt%, stirring for 18h at 70 ℃, standing and defoaming for 14h, conveying the casting solution to a spinning nozzle at the speed of 320ml/min by using a metering pump, allowing a polyester lining to pass through the center of the spinning nozzle, uniformly coating the casting solution on the outer surface of a polyester braided tube, and allowing core solution pure water to flow at the speed of 150 ml/min; the braided tube coated with the membrane casting solution enters a gel bath containing DMAc aqueous solution and is converted into a membrane at the temperature of 32 ℃; and (3) collecting the cured membrane filaments by a filament collecting wheel at 18m/min, and soaking the membrane filaments in water-glycerol mixed solutions with different proportions in stages to finally obtain the polyester lining enhanced PVDF ultrafiltration membrane. Soaking in water-glycerol at ratio of 9.5:1, 7:3, 5.5:5, and 3:7 respectively. Firstly soaking in 9.5:1 water-glycerol solution for 11h, and then respectively soaking in the water-glycerol solution with the last three proportions for 4 h. And finally, taking out the film, hanging and airing.
And (3) packaging the ultrafiltration membrane filaments in the component by using the sealant, mounting the manufactured membrane component in a testing device, and testing the water flux and the organic substance interception performance of the membrane component, wherein the test result is as follows.
The separation performance of the membrane was investigated using actual wastewater as influent water, and the test results were as follows.
Example 3
The terylene braided tube is used as a lining, PVDF is used as a membrane material, the inner diameter of the terylene braided tube is 1.0mm, the outer diameter is 2.0mm, and the aperture is 0.5 mm. The adding amount of PMMA is 2.3 wt%, the adding amount of BD-3071 is 0.1 wt%, the adding amount of PVP-k30 is 10 wt%, the adding amount of glycerol is 9 wt%, stirring for 19h at 72 ℃, standing and defoaming for 16h, conveying the casting solution to a spinning nozzle at the speed of 350ml/min by using a metering pump, allowing a polyester lining to pass through the center of the spinning nozzle, uniformly coating the casting solution on the outer surface of a polyester braided tube, and allowing core solution pure water to flow at the speed of 180 ml/min; the braided tube coated with the membrane casting solution enters a gel bath containing DMAc aqueous solution and is converted into a membrane at 38 ℃; and (3) collecting the cured membrane filaments by a filament collecting wheel at 23m/min, and soaking the membrane filaments in water-glycerol mixed solutions with different proportions in stages to finally obtain the polyester lining enhanced PVDF ultrafiltration membrane. Soaking in water-glycerol at ratio of 10:1, 7.5:3, 5:5, and 2.5:6 respectively. Firstly soaking in a 10:1 water-glycerol solution for 12 hours, and then respectively soaking in the water-glycerol solutions with the last three proportions for 5 hours. And finally, taking out the film, hanging and airing.
And (3) packaging the ultrafiltration membrane filaments in the component by using the sealant, mounting the manufactured membrane component in a testing device, and testing the water flux and the organic substance interception performance of the membrane component, wherein the test result is as follows.
The separation performance of the membrane was investigated using actual wastewater as influent water, and the test results were as follows.
The stability of the film was examined and the test results are shown in fig. 5.
The reinforced PVDF ultrafiltration membrane with high strength, high flux and stable performance is prepared by taking a terylene braided tube as an inner liner and adopting a non-solvent induced phase inversion method. The invention has simple process and obvious industrial practical value.
Claims (10)
1. A preparation method of a PVDF ultrafiltration membrane with a terylene lining is characterized in that: the method comprises the following steps:
a. the method comprises the following steps of taking a terylene braided tube as an inner liner, PVDF as a membrane material, DMAc as a solvent, polyether modified polydimethylsiloxane (BD-3071) as a dispersing agent, polymethyl methacrylate (PMMA), PVP-k30 and glycerol as additives, wherein the addition amount of PMMA is 0.05-2.5 wt%, the addition amount of BD-3071 is 0.05-2.5 wt%, the addition amount of PVP-k30 is 1-12 wt%, the addition amount of glycerol is 1-12 wt%, stirring for 16-20h at 65-75 ℃, standing and defoaming for 12-16 h;
b. conveying the casting solution to a spinning nozzle at the speed of 300 plus 350ml/min by using a metering pump, enabling the terylene lining to pass through the center of the spinning nozzle, uniformly coating the casting solution on the outer surface of the terylene braided tube, and enabling the flow rate of core solution pure water to be 120 plus 180 ml/min; the braided tube coated with the membrane casting solution enters a gel bath containing DMAc aqueous solution and is converted into a membrane at the temperature of 32-38 ℃;
c. and (3) collecting the cured membrane filaments through a take-up pulley at 18-23m/min, and soaking the membrane filaments in water-glycerol mixed solutions with different proportions in stages to finally obtain the polyester lining enhanced PVDF ultrafiltration membrane.
2. The preparation method of the PVDF ultrafiltration membrane with the terylene lining according to claim 1, which is characterized in that: the water-glycerol mixed solution with different proportions in the step c refers to that the water-glycerol mixed solution is soaked in water with the proportion of 9.5-10.5:1, 6.5-7.5:3, 4.5-5.5:5 and 2-3:6-7 respectively.
3. The preparation method of the PVDF ultrafiltration membrane with the terylene lining according to claim 1, which is characterized in that: the stirring speed is 70-90 rpm.
4. The preparation method of the PVDF ultrafiltration membrane with the terylene lining according to claim 1, which is characterized in that: the concentration of the aqueous DMAc solution is between 0.5 and 2 wt.%.
5. The preparation method of the PVDF ultrafiltration membrane with the terylene lining according to claim 1, which is characterized in that: the inner diameter of the terylene braided tube is 0.6-1.0mm, the outer diameter is 1.6-2.0mm, and the aperture is 0.3-0.5 mm.
6. The preparation method of the PVDF ultrafiltration membrane with the terylene lining according to claim 1, which is characterized in that: the addition amount of PMMA is 0.1-2%.
7. The preparation method of the PVDF ultrafiltration membrane with the terylene lining according to claim 1, which is characterized in that: the addition amount of the BD-3071 is 0.1-2%.
8. The preparation method of the PVDF ultrafiltration membrane with the terylene lining according to claim 1, which is characterized in that: the addition amount of the PVP-k30 is 2-10%.
9. The preparation method of the PVDF ultrafiltration membrane with the terylene lining according to claim 1, which is characterized in that: the addition amount of the glycerol is 2-10%.
10. The preparation method of the PVDF ultrafiltration membrane with the terylene lining according to claim 1, which is characterized in that: the pure water flux of the prepared ultrafiltration membrane is 140-160L/(m)2H); the bubble point pressure is 0.04-0.06 MPa.
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| CN114392651A (en) * | 2021-12-31 | 2022-04-26 | 德蓝水技术股份有限公司 | Composite ultrafiltration membrane and preparation method thereof |
Citations (12)
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