CN107570021B - Hydrophilic polysulfone/silicon dioxide blended hollow fiber membrane and preparation method thereof - Google Patents
Hydrophilic polysulfone/silicon dioxide blended hollow fiber membrane and preparation method thereof Download PDFInfo
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- CN107570021B CN107570021B CN201711025188.5A CN201711025188A CN107570021B CN 107570021 B CN107570021 B CN 107570021B CN 201711025188 A CN201711025188 A CN 201711025188A CN 107570021 B CN107570021 B CN 107570021B
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- polysulfone
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- silica
- silicon dioxide
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 99
- 229920002492 poly(sulfone) Polymers 0.000 title claims abstract description 79
- 239000012528 membrane Substances 0.000 title claims abstract description 64
- 239000012510 hollow fiber Substances 0.000 title claims abstract description 47
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 41
- 235000012239 silicon dioxide Nutrition 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims description 18
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 28
- VYFYYTLLBUKUHU-UHFFFAOYSA-N dopamine Chemical compound NCCC1=CC=C(O)C(O)=C1 VYFYYTLLBUKUHU-UHFFFAOYSA-N 0.000 claims abstract description 24
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000005543 nano-size silicon particle Substances 0.000 claims abstract description 17
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 14
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 14
- 229960003638 dopamine Drugs 0.000 claims abstract description 12
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 10
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 10
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 238000002791 soaking Methods 0.000 claims description 15
- 238000009987 spinning Methods 0.000 claims description 11
- 238000006243 chemical reaction Methods 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000005266 casting Methods 0.000 claims description 8
- 230000001112 coagulating effect Effects 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 239000002904 solvent Substances 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 3
- 238000005507 spraying Methods 0.000 claims description 3
- 238000006116 polymerization reaction Methods 0.000 claims description 2
- 238000006277 sulfonation reaction Methods 0.000 claims description 2
- 125000000524 functional group Chemical group 0.000 abstract description 4
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 abstract description 4
- 238000000614 phase inversion technique Methods 0.000 abstract description 2
- 230000004907 flux Effects 0.000 description 7
- 230000014759 maintenance of location Effects 0.000 description 6
- 108091003079 Bovine Serum Albumin Proteins 0.000 description 5
- 229940098773 bovine serum albumin Drugs 0.000 description 5
- 229940068918 polyethylene glycol 400 Drugs 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 229920001169 thermoplastic Polymers 0.000 description 2
- 229920002725 thermoplastic elastomer Polymers 0.000 description 2
- 239000004416 thermosoftening plastic Substances 0.000 description 2
- 238000000108 ultra-filtration Methods 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 229920005597 polymer membrane Polymers 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
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- Separation Using Semi-Permeable Membranes (AREA)
- Artificial Filaments (AREA)
Abstract
The invention discloses a hydrophilic polysulfone/silicon dioxide blended hollow fiber membrane, which comprises 15-20 parts of polysulfone, 1.2-1.7 parts of sulfonated polysulfone, 33-37 parts of polyethylene glycol, 42-48 parts of N, N-dimethylacetamide and 0.5-5 parts of modified nano silicon dioxide; the modified nano silicon dioxide is modified by adopting gamma-aminopropyl triethoxysilane through supercritical carbon dioxide treatment. Aiming at the problems existing in the performance of the polysulfone hollow fiber membrane, the hydrophilic polysulfone/carbon dioxide blended hollow fiber membrane is prepared by adopting a phase inversion method. The surface of the silicon dioxide is loaded with amino functional groups by selecting gamma-aminopropyltriethoxysilane through supercritical carbon dioxide treatment, so that carbon dioxide can better exist in the polysulfone membrane, and meanwhile, the amino functional groups play a role in fixing dopamine, and the comprehensive mechanical property, hydrophilicity and pollution resistance of the polysulfone hollow fiber membrane are improved.
Description
Technical Field
The invention relates to the technical field of high polymer materials, in particular to a hydrophilic polysulfone/silicon dioxide blended hollow fiber membrane and a preparation method thereof.
Background
Polysulfone (PSF) material has the advantages of no toxicity, good compression resistance, good chemical stability, high heat resistance, wide pH adaptation range and the like, and is now the most widely used polymer membrane material in modern industry. The polysulfone hollow fiber membrane has poor hydrophilicity and pollution resistance, and is easy to be polluted in practical application, so that the membrane flux is reduced, and the service life of the membrane is shortened. For this purpose, inorganic nanoparticles, such as Al, have been introduced into the membrane material2O3，TiO2，SiO2，ZrO2And carbon nano-tubes, etc. to improve the hydrophilicity, strength, hardness, permeability, pollution resistance, etc. of the polysulfone membrane.
Disclosure of Invention
The purpose of the invention is: the hydrophilic polysulfone/silicon dioxide blended hollow fiber membrane and the preparation method thereof are provided, which obviously provide the hydrophilicity of the polysulfone membrane, improve the mechanical strength, and have excellent permeability and pollution resistance so as to overcome the defects of the prior art.
The invention is realized by the following steps: the hydrophilic polysulfone/silicon dioxide blended hollow fiber membrane comprises 15-20 parts of polysulfone, 1.2-1.7 parts of sulfonated polysulfone, 33-37 parts of polyethylene glycol, 42-48 parts of N, N-dimethylacetamide and 0.5-5 parts of modified nano silicon dioxide by mass; the modified nano silicon dioxide is modified by adopting gamma-aminopropyl triethoxysilane through supercritical carbon dioxide treatment.
The polymerization degree of the polyethylene glycol is 400-20000, and the sulfonation degree of the sulfonated polysulfone is 15-30%;
the preparation method of the hydrophilic polysulfone/silicon dioxide blended hollow fiber membrane comprises the following steps of:
1) respectively carrying out vacuum drying on polysulfone, sulfonated polysulfone and modified nano-silica for 12-24 hours at 65-75 ℃;
2) adding the dried modified nano-silica into N, N-dimethylacetamide, and uniformly dispersing the modified nano-silica in the N, N-dimethylacetamide by an ultrasonic mode;
3) then mixing the dried sulfonated polysulfone, polysulfone and polyethylene glycol, fully stirring for 10-15h at 60-80 ℃ to form a homogeneous membrane casting solution, carrying out vacuum defoaming, forming a spinning trickle flow through a spinneret plate, spraying the spinning trickle flow from the spinneret plate, immersing the spinning trickle flow into a coagulating bath after passing through an air gap, and forming a hollow fiber membrane through mass transfer exchange of a solvent N, N-dimethylacetamide and non-solvent water;
4) soaking the prepared hollow fiber membrane in distilled water for 20-24 h; and then soaking the hollow fiber membrane in an ethanol solution for 1-2h, taking out, and immediately soaking in a dopamine solution with the concentration of 0.1-10g/L for 1-24h at the soaking temperature of 25-70 ℃ to prepare the hydrophilic polysulfone/silicon dioxide blended hollow fiber membrane.
The length of the air gap between the spinneret plate and the coagulating bath is 1-20cm, the temperature of the air gap is 20-50 ℃, and the humidity is less than or equal to 50-80%.
The modified nano silicon dioxide is prepared by firstly mixing the nano silicon dioxide and gamma-aminopropyl triethoxysilane by the mass ratio of 100:1 to 20 percent; placing the mixture into a supercritical carbon dioxide reaction kettle, carrying out reaction at the temperature of 40-50 ℃, under the reaction pressure of more than or equal to 20MPa and for 1-2h, after the reaction is finished, releasing the pressure, and repeating for 3-5 times to obtain the modified nano-silicon dioxide.
The ultrasonic power of the ultrasonic mode is 50-300W, and the time is 0.5-5 h.
The method for forming the homogeneous casting solution comprises the following steps of fully stirring N, N-dimethylacetamide solution in which nano silicon dioxide is uniformly dispersed at the temperature of 60-75 ℃, uniformly mixing dried polysulfone and sulfonated polysulfone by a high-speed mixer, and mixing the polysulfone and the sulfonated polysulfone uniformly according to the mass ratio of 4: 3: 3, dividing into three parts, putting into the solution in batches, adding polyethylene glycol into the solution uninterruptedly at an interval of 1.5-2.5h each time, and fully stirring for 10-15h to form a homogeneous casting solution.
The dopamine solution is prepared by dissolving dopamine in distilled water, and adding sodium hydroxide to adjust the pH value to 7-9 to obtain 0.1-10g/L dopamine solution.
Due to the adoption of the technical scheme, compared with the prior art, the hydrophilic polysulfone/carbon dioxide blended hollow fiber membrane is prepared by adopting a phase inversion method aiming at the problems existing in the performance of the Polysulfone (PSF) hollow fiber membrane. The surface of the silicon dioxide is loaded with amino functional groups by selecting gamma-aminopropyltriethoxysilane through supercritical carbon dioxide treatment, so that carbon dioxide can better exist in the polysulfone membrane, and meanwhile, the amino functional groups play a role in fixing dopamine, and the comprehensive mechanical property, hydrophilicity and pollution resistance of the polysulfone hollow fiber membrane are improved.
Detailed Description
The present invention is further specifically described below by way of examples. In the following examples, the amounts of the components are by weight. It should be noted that the following examples are given solely for the purpose of illustration and are not to be construed as limitations on the scope of the invention, as those skilled in the art will be able to make insubstantial modifications and variations of the invention in light of the above teachings, while still remaining within the scope of the invention.
Example 1 of the invention: the hydrophilic polysulfone/silicon dioxide blended hollow fiber membrane comprises 18.5 parts of polysulfone, 1.5 parts of sulfonated polysulfone, 35.6 parts of polyethylene glycol 400, 44.4 parts of N, N-dimethylacetamide and 3 parts of modified nano silicon dioxide by mass.
The preparation method of the hydrophilic polysulfone/silicon dioxide blended hollow fiber membrane comprises the steps of putting nano silicon dioxide and gamma-aminopropyl triethoxysilane into a supercritical carbon dioxide reaction kettle according to the mass ratio of 100:10, carrying out reaction for 2 hours at the reaction temperature of 40 ℃, under the reaction pressure of more than or equal to 20MPa, and after the reaction is finished, rapidly releasing pressure, repeating for 4 times to obtain modified nano silicon dioxide treated by supercritical carbon dioxide, and adopting the modified nano silicon dioxide treated by supercritical carbon dioxide to participate in preparation; taking the following components in parts by mass:
1) respectively carrying out vacuum drying on polysulfone, sulfonated polysulfone and silicon dioxide at 70 ℃ for 24 hours;
2) adding the dried silicon dioxide into N, N-dimethylacetamide, and uniformly dispersing the silicon dioxide in the N, N-dimethylacetamide by an ultrasonic mode, wherein the ultrasonic power of the ultrasonic mode is 150W, and the time is 4 hours;
3) then mixing the dried sulfonated polysulfone, polyethylene glycol 400, thermoplastic elastomer TPE and the dried polysulfone, fully stirring for 10-15h at 65-75 ℃ to form a homogeneous membrane casting solution, carrying out vacuum defoaming, forming a spinning trickle through a spinneret plate, and immersing the spinning trickle into a coagulating bath through an air gap between the spinneret plate and the coagulating bath, wherein the temperature of the air gap between the spinneret plate and the coagulating bath is 28-32 ℃, and the humidity is less than or equal to 20%. The temperature and the humidity of the air gap are ensured, and the influence of the environment is eliminated. The temperature and the humidity of the air gap are controlled, so that the influence of the environmental temperature and the humidity on the structure and the performance of the hollow fiber membrane can be effectively solved; the temperature of the coagulation bath was 70 ℃, and a hollow fiber membrane was formed by mass transfer exchange of the solvent N, N-dimethylacetamide and non-solvent water.
4) The prepared hollow fiber membrane is soaked in distilled water for 24 hours. And then soaking the hollow fiber membrane in an ethanol solution for 2 hours, taking out the hollow fiber membrane, and immediately soaking the hollow fiber membrane in a dopamine solution with the concentration of 4g/L for 8 hours at the soaking temperature of 50 ℃ to prepare the hydrophilic polysulfone/silicon dioxide blended hollow fiber membrane.
The performance indexes of the product of the example 1 are detected as follows: 800 mu m of inner diameter and 300 mu m of wall thickness, the pure water flux is more than or equal to 130 L.m < -2 > h < -1 >, the retention rate on bovine serum albumin (67000) is more than or equal to 99 percent, and the tensile strength of the membrane wire is more than or equal to 4.5 MPa.
Example 2 of the invention: the polysulfone-thermoplastic elastomer-silicon dioxide blended hollow fiber membrane comprises, by mass, 15 parts of polysulfone, 1.7 parts of sulfonated polysulfone, 33 parts of polyethylene glycol 400, 48 parts of N, N-dimethylacetamide and 0.5 part of modified nano-silicon dioxide.
The preparation method is the same as example 1.
The performance indexes of the product of the embodiment 2 are detected as follows: the inner diameter is 600-800 mu m, the wall thickness is 200-300 mu m, the pure water flux is more than or equal to 160 L.m < -2 > h < -1 >, the retention rate on bovine serum albumin (67000) is more than or equal to 93 percent, and the tensile strength of the membrane wire is more than or equal to 3.5 MPa.
Example 3 of the invention: the polysulfone-thermoplastic elastomer-silicon dioxide blended hollow fiber membrane comprises, by mass, 20 parts of polysulfone, 1.2 parts of sulfonated polysulfone, 37 parts of polyethylene glycol 400, 42 parts of N, N-dimethylacetamide and 5 parts of modified nano-silicon dioxide.
The preparation method is the same as example 1.
The performance indexes of the product of the embodiment 3 are detected as follows: 800 mu m of inner diameter and 300 mu m of wall thickness, pure water flux is more than or equal to 110 L.m < -2 > h < -1 >, the retention rate of bovine serum albumin (67000) is more than or equal to 95 percent, and the tensile strength of the membrane wire is more than or equal to 5 MPa.
Comparative example 1
By comparing the invention patent "a method for producing a permanently hydrophilic polysulfone ultrafiltration membrane" example seven, a polysulfone ultrafiltration membrane having a solid content of 20% had a pure water flux of 130 L.m-2·h-1The bovine serum albumin retention rate is 96%, and the pure water flux of the polysulfone/graphene oxide prepared by the preparation method is more than or equal to 130 L.m.-2·h-1The retention rate of bovine serum albumin (67000) is more than or equal to 99 percent, and the retention rate is obviously superior to that of a comparative polysulfone membrane.
According to the embodiment and the comparative example, the invention proves that the comprehensive mechanical property and the pollution resistance of the polysulfone hollow fiber membrane can be improved on the premise that the polysulfone hollow fiber membrane keeps better water flux and rejection rate.
Claims (8)
1. A hydrophilic polysulfone/silicon dioxide blended hollow fiber membrane is characterized in that: calculated according to the mass portion, the material comprises 15 to 20 portions of polysulfone, 1.2 to 1.7 portions of sulfonated polysulfone, 33 to 37 portions of polyethylene glycol, 42 to 48 portions of N, N-dimethylacetamide and 0.5 to 5 portions of modified nano silicon dioxide; the modified nano silicon dioxide is modified by adopting gamma-aminopropyltriethoxysilane through supercritical carbon dioxide treatment; the preparation method comprises the following steps:
the preparation method comprises the following steps of:
1) respectively carrying out vacuum drying on polysulfone, sulfonated polysulfone and modified nano-silica for 12-24 hours at 65-75 ℃;
2) adding the dried modified nano-silica into N, N-dimethylacetamide, and uniformly dispersing the modified nano-silica in the N, N-dimethylacetamide by an ultrasonic mode;
3) adding the dried sulfonated polysulfone, polysulfone and polyethylene glycol into the solution obtained in the step 2), mixing, fully stirring for 10-15h at 60-80 ℃ to form a homogeneous membrane casting solution, carrying out vacuum defoaming, forming a spinning trickle through a spinneret plate, spraying the spinning trickle from the spinneret plate, immersing the spinning trickle into a coagulating bath after passing through an air gap, and forming a hollow fiber membrane through mass transfer exchange of a solvent N, N-dimethylacetamide and non-solvent water;
4) soaking the prepared hollow fiber membrane in distilled water for 20-24 h; and then soaking the hollow fiber membrane in an ethanol solution for 1-2h, taking out, and immediately soaking in a dopamine solution with the concentration of 0.1-10g/L for 1-24h at the soaking temperature of 25-70 ℃ to prepare the hydrophilic polysulfone/silicon dioxide blended hollow fiber membrane.
2. A hydrophilic polysulfone/silica blended hollow fiber membrane according to claim 1, characterized in that: the polymerization degree of the polyethylene glycol is 400-20000, and the sulfonation degree of the sulfonated polysulfone is 15-30%.
3. A method for preparing a hydrophilic polysulfone/silica blended hollow fiber membrane according to claim 1, wherein: the preparation method comprises the following steps of:
1) respectively carrying out vacuum drying on polysulfone, sulfonated polysulfone and modified nano-silica for 12-24 hours at 65-75 ℃;
2) adding the dried modified nano-silica into N, N-dimethylacetamide, and uniformly dispersing the modified nano-silica in the N, N-dimethylacetamide by an ultrasonic mode;
3) adding the dried sulfonated polysulfone, polysulfone and polyethylene glycol into the solution obtained in the step 2), fully stirring for 10-15h at 60-80 ℃ to form a homogeneous membrane casting solution, carrying out vacuum defoaming, forming a spinning trickle through a spinneret plate, spraying the spinning trickle from the spinneret plate, immersing the spinning trickle into a coagulating bath after passing through an air gap, and forming a hollow fiber membrane through mass transfer exchange of a solvent N, N-dimethylacetamide and non-solvent water;
4) soaking the prepared hollow fiber membrane in distilled water for 20-24 h; and then soaking the hollow fiber membrane in an ethanol solution for 1-2h, taking out, and immediately soaking in a dopamine solution with the concentration of 0.1-10g/L for 1-24h at the soaking temperature of 25-70 ℃ to prepare the hydrophilic polysulfone/silicon dioxide blended hollow fiber membrane.
4. The preparation method of the hydrophilic polysulfone/silica blended hollow fiber membrane according to claim 3, wherein: the length of the air gap between the spinneret plate and the coagulating bath is 1-20cm, the temperature of the air gap is 20-50 ℃, and the humidity is less than or equal to 50-80%.
5. The preparation method of the hydrophilic polysulfone/silica blended hollow fiber membrane according to claim 3, wherein: the modified nano-silica is prepared by putting nano-silica and gamma-aminopropyltriethoxysilane at a mass ratio of 100:1-20 into a supercritical carbon dioxide reaction kettle, reacting at 40-50 deg.C under a pressure of not less than 20MPa for 1-2h, releasing pressure, and repeating for 3-5 times to obtain the modified nano-silica.
6. The preparation method of the hydrophilic polysulfone/silica blended hollow fiber membrane according to claim 3, wherein: the ultrasonic power of the ultrasonic mode is 50-300W, and the time is 0.5-5 h.
7. The preparation method of the hydrophilic polysulfone/silica blended hollow fiber membrane according to claim 3, wherein: the method for forming the homogeneous casting solution comprises the following steps of fully stirring N, N-dimethylacetamide solution in which nano silicon dioxide is uniformly dispersed at the temperature of 60-75 ℃, uniformly mixing dried polysulfone and sulfonated polysulfone by a high-speed mixer, and mixing the polysulfone and the sulfonated polysulfone uniformly according to the mass ratio of 4: 3: 3, dividing into three parts, putting into the solution in batches, adding polyethylene glycol into the solution uninterruptedly at an interval of 1.5-2.5h each time, and fully stirring for 10-15h to form a homogeneous casting solution.
8. The preparation method of the hydrophilic polysulfone/silica blended hollow fiber membrane according to claim 3, wherein: the dopamine solution is prepared by dissolving dopamine in distilled water, and adding sodium hydroxide to adjust the pH value to 7-9 to obtain 0.1-10g/L dopamine solution.
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| CN113731199A (en) * | 2021-07-20 | 2021-12-03 | 东华大学 | Super-amphiphobic membrane and preparation method and application thereof |
| CN115287702B (en) * | 2022-07-21 | 2025-02-25 | 宁波中科氢易膜科技有限公司 | A polysulfone-ZrO2 composite diaphragm, preparation method and application |
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