CN110479116B - Preparation method of mesoporous hydrophobic silicon modified polyvinylidene fluoride flat microfiltration membrane - Google Patents
Preparation method of mesoporous hydrophobic silicon modified polyvinylidene fluoride flat microfiltration membrane Download PDFInfo
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- CN110479116B CN110479116B CN201910694196.1A CN201910694196A CN110479116B CN 110479116 B CN110479116 B CN 110479116B CN 201910694196 A CN201910694196 A CN 201910694196A CN 110479116 B CN110479116 B CN 110479116B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/14—Ultrafiltration; Microfiltration
- B01D61/147—Microfiltration
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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
- B01D67/0079—Manufacture of membranes comprising organic and inorganic components
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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
- B01D69/06—Flat membranes
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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
- B01D71/02—Inorganic material
- B01D71/024—Oxides
- B01D71/027—Silicium oxide
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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
Abstract
The invention discloses a preparation method of a mesoporous hydrophobic silicon modified polyvinylidene fluoride flat microfiltration membrane, which utilizes the hydrophobic and oleophobic properties of mesoporous hydrophobic silicon to ensure that the surface of the polyvinylidene fluoride flat microfiltration membrane has certain hydrophobic groups, can repel the adsorption of hydrophilic pollutants and oil substances in the running process of the membrane, prevent the permeation of pollutants with low surface tension and improve the anti-pollution performance of the flat microfiltration membrane, and simultaneously, because a high-thickness and large-aperture supporting woven fabric and a pretreatment method of the woven fabric are selected, the microfiltration membrane is easy to form macropores in the membrane forming process so as to keep high flux and high anti-stripping strength.
Description
Technical Field
The invention belongs to the technical field of microfiltration membranes, and particularly relates to a preparation method of a mesoporous hydrophobic silicon modified polyvinylidene fluoride flat microfiltration membrane.
Background
In view of classifying product structures according to pore sizes, the market scale of ultrafiltration membrane and microfiltration membrane products is rapidly increased and gradually dominates in recent years. In 2016 of 2013, the composite growth rate of ultrafiltration membrane and microfiltration membrane products is up to 31.04%, the market scale is increased to 130 hundred million yuan in 2016, the specific gravity of the water treatment membrane is up to 74.29%, and the demand of the flat microfiltration membrane is huge, and the flat microfiltration membrane is mainly applied in the form of MBR and spiral-wound membranes.
Polyvinylidene fluoride (PVDF) is one of the currently preferred membrane materials because of its good chemical stability, radiation resistance, heat resistance, and ease of film formation. However, the existing PVDF membrane is easy to adsorb hydrophilic pollutants and oil stains, so that the pollution resistance is poor, the flux is difficult to maintain, and the anti-peeling strength of the membrane layer is still unsatisfactory.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method of a mesoporous hydrophobic silicon modified polyvinylidene fluoride flat microfiltration membrane.
The technical scheme of the invention is as follows:
a preparation method of a mesoporous hydrophobic silicon modified polyvinylidene fluoride flat microfiltration membrane comprises the following steps:
(1) drying the mesoporous hydrophobic silicon, the polyvinylidene fluoride and the polyester fiber non-woven fabric; the mesoporous hydrophobic silicon is porous hydrophobic nano-silica with the pore diameter of 2-50nm, and the polymerization degree of the polyvinylidene fluoride is 150000-250000;
(2) shearing the dried mesoporous hydrophobic silicon and the surfactant in an organic solvent at a high speed for 30-60min, then heating to 65-85 ℃, then sequentially adding polyvinylidene fluoride and the pore-foaming agent, and uniformly stirring;
(3) keeping the temperature of the material obtained in the step (2) at 65-85 ℃, standing or vacuumizing and defoaming until no residual bubbles exist to obtain a membrane casting solution;
(4) pretreating the dried polyester fiber non-woven fabric to enable the surface of the polyester fiber non-woven fabric to have alkaline hydrophobic groups;
(5) fixing the material obtained in the step (4) on a glass plate, then uniformly coating the casting solution on the surface of the glass plate, wherein the coating thickness is 0.1-0.4mm, and then quickly placing the glass plate in a gel bath for phase conversion to form a film;
(6) and (3) curing the material obtained in the step (5) in deionized water at room temperature for 40-50h to obtain the mesoporous hydrophobic silicon modified polyvinylidene fluoride flat micro-filtration membrane.
In a preferred embodiment of the present invention, the porogen is at least one of tween, polyethylene glycol and polyvinylpyrrolidone.
In a preferred embodiment of the present invention, the surfactant is at least one of tween, OP phosphate, alkylphenol ethoxylate, nonylphenol ethoxylate, and ammonium salt of polyoxyethylene alkylbenzene sulfonate.
In a preferred embodiment of the present invention, the organic solvent is at least one of dimethylformamide, dimethylacetamide and N-methylpyrrolidone.
In a preferred embodiment of the present invention, the step (4) is: and soaking the dried polyester fiber non-woven fabric in a pretreatment solution at room temperature for 10-30min, wherein the solvent of the pretreatment solution is dimethylformamide, the solute comprises the mesoporous hydrophobic silicon, and the pH value is 10-11.
Further preferably, the concentration of the solute in the pretreatment liquid is 2 to 5 wt%.
In a preferred embodiment of the present invention, in the casting solution, the mass percentages of the components are as follows:
in a preferred embodiment of the present invention, the porogen is at least one of tween, polyethylene glycol and polyvinylpyrrolidone, the surfactant is at least one of tween, OP phosphate, alkylphenol polyoxyethylene, nonylphenol polyoxyethylene and polyoxyethylene alkylbenzene sulfonic acid ammonium salt, and the organic solvent is at least one of dimethylformamide, dimethylacetamide and N-methylpyrrolidone.
In a preferred embodiment of the present invention, the polyester fiber nonwoven fabric has a thickness of 0.1 to 0.2mm and an average pore diameter of 15 to 25 μm.
The invention has the beneficial effects that:
1. the invention utilizes the hydrophobic and oleophobic properties of the mesoporous hydrophobic silicon to lead the surface of the polyvinylidene fluoride flat micro-filtration membrane to have certain hydrophobic groups, can repel the adsorption of hydrophilic pollutants and oil substances in the running process of the membrane, prevent the permeation of pollutants with low surface tension and improve the anti-pollution performance of the flat micro-filtration membrane, and simultaneously leads the micro-filtration membrane to be easy to form macropores in the membrane forming process and keep high flux and high anti-stripping strength due to the selection of the supporting woven fabric with high thickness and large aperture and the pretreatment method of the woven fabric.
2. The MBR component and the roll-type membrane component prepared by the invention can be well applied to the fields of low-concentration oil-polluted wastewater, low-surface-tension pollutants and the like.
Detailed Description
The technical solution of the present invention is further illustrated and described by the following detailed description.
The pretreatment in examples 1 and 2 below was: and soaking the dried polyester fiber non-woven fabric in a pretreatment solution at room temperature for 10-30min, wherein the solvent of the pretreatment solution is dimethylformamide, the solute comprises the mesoporous hydrophobic silicon, the pH value is 10-11, and the concentration of the solute is 2-5 wt%.
The mesoporous hydrophobic silicon is porous hydrophobic nano-silica with the pore diameter of 2-50nm, and the polymerization degree of the polyvinylidene fluoride is 150000-250000
Comparative example 1
Pouring 70 parts by weight of dimethylacetamide into a dissolving kettle, starting the dissolving kettle, stirring, gradually heating to 70 ℃, sequentially adding 18 parts by weight of polyvinylidene fluoride, 2 parts by weight of tween-20, 5 parts by weight of polyvinylpyrrolidone and 5 parts by weight of polyethylene glycol, and dissolving and stirring at 70 ℃ for 12 hours to prepare uniform sol. Keeping the temperature at 70 ℃ for deaeration for 12h, coating the film on polyester fiber non-woven fabric with the thickness of 0.1mm and the average pore diameter of 15 mu m by using a flat film scraper, wherein the thickness of the coating is 0.2mm, immersing the polyester fiber non-woven fabric into deionized water with the temperature of 25 ℃ for gel film formation, and testing the performance of the film after immersing the polyester fiber non-woven fabric for 48 h. The pure water flux of the membrane was 820L/m 2. multidot.h at an operating temperature of 25 ℃ and a pressure of 0.1MPa, the mechanical peel strength was 28MPa, and the flux after contamination test with 1% soybean oil and 0.5% surfactant was 65%.
Comparative example 2
Quickly stirring 5 parts by weight of mesoporous hydrophobic silicon and 70 parts by weight of dimethylacetamide under a high-speed shearing machine, pouring the mixture into a dissolving kettle, starting the dissolving kettle to stir, gradually heating to 65 ℃, and then sequentially adding 18 parts by weight of polyvinylidene fluoride, 2 parts by weight of tween-20 and 5 parts by weight of polyvinylpyrrolidone, dissolving and stirring for 12 hours at 65 ℃ to prepare uniform sol. Keeping at 65 ℃ for deaeration for 12h, coating the film on polyester fiber non-woven fabric with the thickness of 0.105mm and the average aperture of 14 mu m by using a flat film scraper, wherein the thickness of the coating is 0.2mm, immersing the polyester fiber non-woven fabric into deionized water at 25 ℃ for gel film formation, and testing the performance of the film after immersing the polyester fiber non-woven fabric for 48 h. The pure water flux of the membrane was 600L/m 2. multidot.h, the mechanical peel strength was 29MPa, and the flux recovery after contamination test with 1% soybean oil and 0.5% surfactant was 70% at an operating temperature of 25 ℃ and a pressure of 0.1 MPa.
Comparative example 3
Quickly stirring 5 parts by weight of mesoporous hydrophobic silicon and 70 parts by weight of dimethylacetamide under a high-speed shearing machine, pouring the mixture into a dissolving kettle, starting the dissolving kettle to stir, gradually heating to 65 ℃, and then sequentially adding 18 parts by weight of polyvinylidene fluoride, 2 parts by weight of tween-20 and 5 parts by weight of polyvinylpyrrolidone, dissolving and stirring at 65 ℃ for 12 hours to prepare uniform sol. Keeping at 65 ℃ for deaeration for 12h, coating the film on polyester fiber non-woven fabric with the thickness of 0.09mm and the average pore diameter of 15 mu m by using a flat film scraper, wherein the thickness of the coating is 0.2mm, immersing the polyester fiber non-woven fabric into deionized water at 25 ℃ for gel film formation, and testing the performance of the film after immersing the polyester fiber non-woven fabric for 48 h. Under the conditions of an operating temperature of 25 ℃ and a pressure of 0.1MPa, the pure water flux of the membrane is 680L/m 2h, the mechanical strength is 29MPa, and the flux recovery rate after the pollution test with 1% of soybean oil and 0.5% of surfactant is 72%.
Comparative example 4
Quickly stirring 5 parts by weight of mesoporous hydrophobic silicon and 70 parts by weight of dimethylacetamide under a high-speed shearing machine, pouring the mixture into a dissolving kettle, starting the dissolving kettle to stir, gradually heating to 65 ℃, and then sequentially adding 18 parts by weight of polyvinylidene fluoride, 2 parts by weight of tween-20 and 5 parts by weight of polyvinylpyrrolidone, dissolving and stirring for 12 hours at 65 ℃ to prepare uniform sol. Keeping at 65 ℃ for deaeration for 12h, coating the film on polyester fiber non-woven fabric with the thickness of 0.1mm and the average pore diameter of 15 mu m by using a flat film scraper, wherein the thickness of the coating is 0.2mm, immersing the polyester fiber non-woven fabric into deionized water at 25 ℃ for gel film formation, and testing the performance of the film after immersing the polyester fiber non-woven fabric for 48 h. Under the conditions of an operating temperature of 25 ℃ and a pressure of 0.1MPa, the pure water flux of the membrane was 750L/m 2. h, the mechanical strength was 29MPa, and the flux recovery after the contamination test with 1% soybean oil and 0.5% surfactant was 79%.
Example 1
Shearing and dispersing 2 wt% of mesoporous hydrophobic silicon into a dimethylformamide solvent to obtain a pretreatment solution with the concentration of 2 wt%, adjusting the pH value of the pretreatment solution to 10 by using a sodium hydroxide solvent, soaking a polyester fiber non-woven fabric with the thickness of 0.1mm and the average pore diameter of 15 mu m in the pretreatment solution for 10min, drying to obtain the pretreated polyester fiber non-woven fabric, quickly stirring 5 parts by weight of mesoporous hydrophobic silicon and 70 parts by weight of dimethylacetamide under a high-speed shearing machine, pouring the mixture into a dissolving kettle, starting the dissolving kettle to stir, gradually heating to 65 ℃, sequentially adding 18 parts by weight of polyvinylidene fluoride, 2 parts by weight of tween-20 and 5 parts by weight of polyvinylpyrrolidone, dissolving and stirring at 65 ℃ for 12h to prepare a uniform sol. Keeping the temperature at 65 ℃ for defoaming for 12h, coating the film on the pretreated polyester fiber non-woven fabric by using a flat film scraper, wherein the thickness of the coating is 0.2mm, immersing the non-woven fabric in deionized water at 25 ℃ for gel forming, and testing the performance of the film after immersing the non-woven fabric for 48 h. Under the conditions of an operating temperature of 25 ℃ and a pressure of 0.1MPa, the pure water flux of the membrane is 800L/m 2h, the mechanical strength is 36MPa, and the flux recovery rate after the pollution test with 1% of soybean oil and 0.5% of surfactant is 88%.
Example 2
Shearing and dispersing mesoporous hydrophobic silicon into a dimethylformamide solvent to obtain a pretreatment solution with the concentration of 3wt%, adjusting the pH value of the pretreatment solution to 11 by using a sodium hydroxide solvent, soaking a polyester fiber non-woven fabric with the thickness of 0.15mm and the average pore diameter of 20 mu m in the pretreatment solution for 20min, drying to obtain a pretreated polyester fiber non-woven fabric, quickly stirring 8 parts by weight of mesoporous hydrophobic silicon and 65 parts by weight of dimethylacetamide under a high-speed shearing machine, pouring into a dissolving kettle, starting the dissolving kettle to stir, gradually heating to 75 ℃, then sequentially adding 20 parts by weight of polyvinylidene fluoride, 3 parts by weight of polyvinyl alcohol, 1 part by weight of OP phosphate and 3 parts by weight of polyvinylpyrrolidone, dissolving and stirring for 12h at 75 ℃ to prepare uniform sol. Keeping the temperature at 75 ℃ for defoaming for 12h, coating the film on the pretreated polyester fiber non-woven fabric by using a flat film scraper, wherein the thickness of the coating is 0.2mm, immersing the non-woven fabric in deionized water at 25 ℃ for gel forming, and testing the performance of the film after immersing the non-woven fabric for 48 h. Under the conditions of an operating temperature of 25 ℃ and a pressure of 0.1MPa, the pure water flux of the membrane is 909L/m 2h, the mechanical strength is 38MPa, and the flux recovery after the pollution test with 1% of soybean oil and 0.5% of surfactant is 90%.
The membranes spun in comparative examples 1, 2, 3 and 4, 1 and 2 were fabricated into MBR modules, run in low oil and low surface tension contaminant wastewater, and flux recovery after cleaning were recorded.
TABLE 1 Membrane operation and flux recovery
The above description is only a preferred embodiment of the present invention, and therefore should not be taken as limiting the scope of the invention, which is defined by the appended claims.
Claims (1)
1. A preparation method of a mesoporous hydrophobic silicon modified polyvinylidene fluoride flat microfiltration membrane is characterized by comprising the following steps: the method comprises the following steps: shearing and dispersing mesoporous hydrophobic silicon into a dimethylformamide solvent to obtain a pretreatment solution with the concentration of 3wt%, adjusting the pH value of the pretreatment solution to 11 by using a sodium hydroxide solvent, soaking a polyester fiber non-woven fabric with the thickness of 0.15mm and the average pore diameter of 20 mu m in the pretreatment solution for 20min, drying to obtain a pretreated polyester fiber non-woven fabric, quickly stirring 8 parts by weight of mesoporous hydrophobic silicon and 65 parts by weight of dimethylacetamide under a high-speed shearing machine, pouring into a dissolving kettle, starting the dissolving kettle to stir, gradually heating to 75 ℃, then sequentially adding 20 parts by weight of polyvinylidene fluoride, 3 parts by weight of polyvinyl alcohol, 1 part by weight of OP phosphate and 3 parts by weight of polyvinylpyrrolidone, dissolving and stirring for 12h at 75 ℃ to prepare a uniform sol; keeping the temperature at 75 ℃ for defoaming for 12h, coating the film on the pretreated polyester fiber non-woven fabric by using a flat film scraper, wherein the thickness of the coating is 0.2mm, immersing the non-woven fabric in deionized water at 25 ℃ for gel forming, and immersing for 48h to obtain the mesoporous hydrophobic silicon modified polyvinylidene fluoride flat micro-filtration membrane.
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| CN102512971B (en) * | 2011-12-09 | 2013-10-16 | 苏州中色德源环保科技有限公司 | Method for preparing composite flat ultrafiltration membrane |
| WO2015084266A1 (en) * | 2013-12-05 | 2015-06-11 | Nanyang Technological University | A composite nanofiber membrane for membrane distillation and a method of fabrication thereof |
| US10286364B2 (en) * | 2014-05-08 | 2019-05-14 | Bettergy Corp. | Mixed matrix membranes for olefin/paraffin separation and method of making thereof |
| CN106390764B (en) * | 2015-07-28 | 2018-10-12 | 北京工业大学 | A kind of super-hydrophobic oleophobic method of modifying of perforated membrane |
| CN105107395A (en) * | 2015-09-30 | 2015-12-02 | 南京理工大学 | Preparation method of hollow mesoporous silica sphere/polyether sulfone composite ultrafiltration membrane |
| CN107174967A (en) * | 2016-03-10 | 2017-09-19 | 天津工业大学 | A kind of PVDF/SiO2Composite membrane and preparation method thereof |
| CN107349803B (en) * | 2016-05-10 | 2020-06-02 | 中国科学院宁波材料技术与工程研究所 | Super-hydrophobic polymer microporous membrane and manufacturing method thereof |
| CN106621862A (en) * | 2016-12-30 | 2017-05-10 | 北京清大国华环境股份有限公司 | Anti-dirt blockage type PVDF (polyvinylidene fluoride) modified membrane and preparation method thereof |
| CN107626211A (en) * | 2017-09-29 | 2018-01-26 | 华南理工大学 | A kind of film for possessing self-cleaning performance and preparation method thereof |
| CN108114610A (en) * | 2017-12-26 | 2018-06-05 | 天津工业大学 | A kind of preparation method of the super-hydrophobic pvdf membrane with micro-nano dual microtexture |
| CN108499363A (en) * | 2018-04-28 | 2018-09-07 | 广西民族大学 | The method of the nano-silicon dioxide modified PVDF dewatering microporous films of fabricated in situ |
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