CN105233710A - Preparation method of asymmetric polyether sulfone hollow fiber nanofiltration membrane - Google Patents
Preparation method of asymmetric polyether sulfone hollow fiber nanofiltration membrane Download PDFInfo
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- CN105233710A CN105233710A CN201510611726.3A CN201510611726A CN105233710A CN 105233710 A CN105233710 A CN 105233710A CN 201510611726 A CN201510611726 A CN 201510611726A CN 105233710 A CN105233710 A CN 105233710A
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- polyether sulfone
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- nanofiltration membrane
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Abstract
The invention discloses a preparation method of an asymmetric polyether sulfone hollow fiber nanofiltration membrane. According to the preparation method, beta-cyclodextrin is added for spinning of a polyether sulfone nanofiltration membrane, wherein a membrane casting solution containing polyether sulfone, beta-cyclodextrin, an organic solvent, and additives is filtered, is pressed into a spinning nozzle via nitrogen pressurization, is extruded from the spinning nozzle in a manner that a tubular liquid membrane is formed by a coagulation bath tube in the spinning nozzle with the surrounding, is dragged and stretched via air gap so as to obtain a certain radial dimension and then is subjected to coagulating bath for solidification to obtain a hollow fiber membrane, and the obtained hollow fiber membrane is washed and collected. The asymmetric polyether sulfone hollow fiber nanofiltration membrane possesses an obvious asymmetric structure, and possesses excellent retention effects on PEG 1000 with a concentration of 0.2g/L under a relatively low operation pressure (0.3 to 0.5MPa).
Description
Technical field
The invention belongs to NF membrane preparing technical field, be specifically related to a kind of preparation method of asymmetric polyether sulfone hollow fiber nanofiltration membrane.
Background technology
Nanofiltration-membrane technique occurs along with the development of reverse osmosis technology and the practical problem and reducing costs that solves industrial soft water, and is a kind of membrane separating process between counter-infiltration (RO) and ultrafiltration (UF).It is generally acknowledged that NF membrane has good removal effect to multivalent salts, to the organic molecule of molecular weight 200 ~ 1000, there is very high rejection.
Commercial nanofiltration membrane major part on market is composite membrane, and so-called composite nanometer filter is made up of ultrafiltration layer and fine and close composite bed, and while maintenance basement membrane excellent physical chemical property, composite bed determines high selectivity or the rejection of NF membrane.Have by the NF membrane be composited the advantage that pure water flux is high, rejection effect is good, but this composite nanometer filtering film preparation process is loaded down with trivial details, complex process, cost are higher.And anisotropic membrane is because preparation technology is more simple, membrane structure controllability is good, with low cost, there is good non-oxidizability and receive much concern.
Polyether sulfone is a kind of membrane material of excellent combination property, there is in its molecule the rigidity of phenyl ring simultaneously, the large conjugated system that the flexibility of ether and sulfuryl and total unit are formed, so whole molecule has suitable stability, show excellent mechanical performance, its advantage is that non-oxidizability is strong, high-temperature creep resistance is good, thermostable type is good, chemical stability is excellent, radiation hardness and intensity high, mechanical strength is high, it is ultrafiltration membrane material most widely used at present, but it is applied to nanofiltration field still based on composite membrane, about the preparation of the asymmetric nanofiltration membrane of polyether sulfone, there is not been reported.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of asymmetric polyether sulfone hollow fiber nanofiltration membrane.
Concrete technical scheme of the present invention is as follows:
A preparation method for asymmetric polyether sulfone hollow fiber nanofiltration membrane, comprises following component:
(1) each component is taken according to following percentage by weight: polyether sulfone 13 ~ 37%, beta-schardinger dextrin-1 ~ 12%, organic hydrophilic pore former 2 ~ 20%, inorganic nano-particle 1 ~ 7% and film forming solvent 24 ~ 83%; Organic hydrophilic pore former is at least one in polyvinylpyrrolidone, polyethylene glycol PEG and tween, and inorganic nano-particle is LiCl, SiO
2, TiO
2, Al
2o
3with at least one in ZrO, film forming solvent is at least one in dimethylacetylamide, dimethyl formamide and N ~ methyl pyrrolidone;
(2) above-mentioned each component is added in reaction vessel, stir 6 ~ 10h in 60 ~ 80 DEG C and dissolve, then standing and defoaming 10 ~ 16h, obtain casting solution;
(3) by the casting solution nitrogen pressurization of step (2), spinning head is pumped into through spinning measuring, be pulled through the air gap of 10 ~ 22cm, be stretched to certain radial dimension and enter 30 ~ 50 DEG C of coagulating baths and be solidified into hollow fiber nanofiltration membrane film silk, wherein the discharging speed of measuring pump is 15 ~ 25mL/min;
(4) film silk step (3) obtained, with after the speed rolling of 0.2 ~ 0.5m/s, soaks 10 ~ 24h through clear water, then is soaked in 20 ~ 30h in glycerine water solution, finally dry obtained described asymmetric polyether sulfone hollow fiber nanofiltration membrane.
In a preferred embodiment of the invention, each component is taken as following weight percent in described step (1): polyether sulfone 15 ~ 35%, beta-schardinger dextrin-1 ~ 10%, organic hydrophilic pore former 3 ~ 17%, inorganic nano-particle 1 ~ 5% and film forming solvent 33 ~ 80%.
Preferred further, described step takes each component in (1) as following weight percent: polyether sulfone 18 ~ 30%, beta-schardinger dextrin-2 ~ 9%, organic hydrophilic pore former 6 ~ 11%, inorganic nano-particle 1 ~ 3% and film forming solvent 47 ~ 73%
In a preferred embodiment of the invention, described step (2) is: add in reaction vessel by above-mentioned each component, stirs 7 ~ 9h dissolve in 65 ~ 70 DEG C, then standing and defoaming 12 ~ 14h, obtains casting solution.
In a preferred embodiment of the invention, described step (3) is: by the casting solution nitrogen pressurization of step (2), spinning head is pumped into through spinning measuring, be pulled through the air gap of 11 ~ 16cm, be stretched to certain radial dimension and enter 30 ~ 40 DEG C of coagulating baths and be solidified into hollow fiber nanofiltration membrane film silk, wherein the discharging speed of measuring pump is 17 ~ 21mL/min.
In a preferred embodiment of the invention, the coagulating bath in described step (4) is the aqueous solution of one or both mixtures in dimethylacetylamide or dimethyl formamide.
In a preferred embodiment of the invention, in described step (4), clear water soaks the time is 14 ~ 24h.
In a preferred embodiment of the invention, in described step (4), in glycerine water solution, the concentration of glycerine is 3 ~ 30%, and soak time is 24h.
In a preferred embodiment of the invention, in described step (4), the speed of rolling is 0.25 ~ 0.35m/s.
The invention has the beneficial effects as follows:
1, preparation method of the present invention adds beta-schardinger dextrin-spinning polyether sulfone filtering film, will containing by polyether sulfone, beta-schardinger dextrin-, the casting solution of organic solvent and additive composition, spinning head is pressed into after filtering by nitrogen pressurization, the form being formed tubulose liquid film by bath-fed tube in spinning head and surrounding is extruded, be pulled through the air gap, enter coagulating bath after being stretched to certain radial dimension and be solidified into hollow-fibre membrane, wait after process through washing again and collect, prepared NF membrane has obvious unsymmetric structure, under lower operating pressure (0.3 ~ 0.5MPa), good rejection effect is had to the PEG1000 that concentration is 0.2g/L.
2, preparation method of the present invention uses dry ~ wet-layer preparation hollow fiber nanofiltration membrane, and process manufacturing cycle is short, and technique is simple.
Detailed description of the invention
Below by way of detailed description of the invention, technical scheme of the present invention is further detailed and is described.
Embodiment 1
1) configuration of casting solution: add the polyether sulfone that mass percent is 18% in a kettle., the beta-schardinger dextrin-of 9%, the polyvinylpyrrolidone of 7%, the tween of 4%, the alundum (Al2O3) nano particle of 3% and the dimethyl formamide of 59%, at 65 DEG C, standing and defoaming 12h after stirring and dissolving 7h, obtains casting solution.
2) spinning, receive silk: the casting solution nitrogen pressurization after deaeration is pressed into spinning head through spinning pump with the speed of 21mL/min, behind the air gap of 11cm, enter temperature is curing molding in the dimethylacetamide solution coagulating bath of 30 DEG C, open godet roller with the speed drawing film silk of 0.26m/s, film silk is collected on godet roller.
3) post processing: after the film silk accepted is soaked 20h in Rinsing Area, immersed in the glycerine water solution of 18% and carry out post processing, is taken out after soaking 24h and is dried, obtained described asymmetric polyether sulfone hollow fiber nanofiltration membrane.
After tested, prepared asymmetric polyether sulfone hollow fiber nanofiltration membrane, under lower operating pressure (0.3 ~ 0.5MPa), is that the rejection of PEG1000 and PEG800 of 0.2g/L is respectively 99.4%, 84.5% to concentration.
Embodiment 2
1) configuration of casting solution: add the polyether sulfone that mass percent is 22% in a kettle., the beta-schardinger dextrin-of 6%, the polyvinylpyrrolidone of 6%, the polyethylene glycol of 3%, the titanium dioxide nano-particle of 2% and the dimethyl formamide of 61%, at 65 DEG C, standing and defoaming 12h after stirring and dissolving 7h, obtains casting solution.
2) spinning, receive silk: the casting solution nitrogen pressurization after deaeration is pressed into spinning head through spinning pump with the speed of 19mL/min, behind the air gap of 13cm, enter temperature is curing molding in the dimethyl formamide solution coagulating bath of 35 DEG C, open godet roller with the speed drawing film silk of 0.29m/s, film silk is collected on godet roller.
3) post processing: after the film silk accepted is soaked 18h in Rinsing Area, immersed in the glycerine water solution of 25%
Carry out post processing, taken out after soaking 24h and dry, obtain described asymmetric polyether sulfone hollow fiber nanofiltration membrane.
After tested, prepared asymmetric polyether sulfone hollow fiber nanofiltration membrane, under lower operating pressure (0.3 ~ 0.5MPa), is that the rejection of PEG1000 and PEG800 of 0.2g/L is respectively 99.7%, 84.6% to concentration.
Embodiment 3
1) configuration of casting solution: add the polyether sulfone that mass percent is 28% in a kettle., the beta-schardinger dextrin-of 4%, the polyvinylpyrrolidone of 6%, the alundum (Al2O3) nano particle of 1% and the dimethylacetylamide of 61%, at 70 DEG C, standing and defoaming 13h after stirring and dissolving 8h, obtains casting solution.
2) spinning, receive silk: the casting solution nitrogen pressurization after deaeration is pressed into spinning head through spinning pump with the speed of 18mL/min, behind the air gap of 15cm, enter temperature is curing molding in the dimethyl formamide solution coagulating bath of 40 DEG C, open godet roller with the speed drawing film silk of 0.33m/s, film silk is collected on godet roller.
3) post processing: after the film silk accepted is soaked 22h in Rinsing Area, immersed in the glycerine water solution of 25% and carry out post processing, is taken out after soaking 24h and is dried, obtained described asymmetric polyether sulfone hollow fiber nanofiltration membrane.
After tested, prepared interpolation beta-schardinger dextrin-polyether sulfone hollow fiber nanofiltration membrane, under lower operating pressure (0.3 ~ 0.5MPa), is that the rejection of PEG1000 and PEG800 of 0.2g/L is respectively 99.7%, 85.2% to concentration.
Embodiment 4
1) configuration of casting solution: add the polyether sulfone that mass percent is 30% in a kettle., the beta-schardinger dextrin-of 2%, the polyethylene glycol of 10%, the Nano particles of silicon dioxide of 1% and the dimethylacetylamide of 57%, at 70 DEG C, standing and defoaming 14h after stirring and dissolving 9h, obtains casting solution.
2) spinning, receive silk: the casting solution nitrogen pressurization after deaeration is pressed into spinning head through spinning pump with the speed of 17mL/min, behind the air gap of 16cm, enter temperature is curing molding in the dimethylacetamide solution coagulating bath of 40 DEG C, open godet roller with the speed drawing film silk of 0.35m/s, film silk is collected on godet roller.
3) post processing: after the film silk accepted is soaked 24h in Rinsing Area, immersed in the glycerine water solution of 30% and carry out post processing, is taken out after soaking 24h and is dried, obtained described asymmetric polyether sulfone hollow fiber nanofiltration membrane.
After tested, prepared asymmetric polyether sulfone hollow fiber nanofiltration membrane, under lower operating pressure (0.3 ~ 0.5MPa), is that the rejection of PEG1000 and PEG800 of 0.2g/L is respectively 99.4%, 83.9% to concentration.
Those of ordinary skill in the art are known, when the parameter of technical scheme of the present invention changes in following scope, still can obtain same as the previously described embodiments or close technique effect, still belong to protection scope of the present invention:
(1) each component is taken according to following percentage by weight: polyether sulfone 13 ~ 37%, beta-schardinger dextrin-1 ~ 12%, organic hydrophilic pore former 2 ~ 20%, inorganic nano-particle 1 ~ 7% and film forming solvent 24 ~ 83% is (preferred, polyether sulfone 15 ~ 35%, beta-schardinger dextrin-1 ~ 10%, organic hydrophilic pore former 3 ~ 17%, inorganic nano-particle 1 ~ 5% and film forming solvent 33 ~ 80%, further preferably, polyether sulfone 18 ~ 30%, beta-schardinger dextrin-2 ~ 9%, organic hydrophilic pore former 6 ~ 11%, inorganic nano-particle 1 ~ 3% and film forming solvent 47 ~ 73%); Organic hydrophilic pore former is at least one in polyvinylpyrrolidone, polyethylene glycol PEG and tween, and inorganic nano-particle is LiCl, SiO
2, TiO
2, Al
2o
3with at least one in ZrO, film forming solvent is at least one in dimethylacetylamide, dimethyl formamide and N ~ methyl pyrrolidone;
(2) above-mentioned each component is added in reaction vessel, stir 6 ~ 10h in 60 ~ 80 DEG C and dissolve, then standing and defoaming 10 ~ 16h, obtain casting solution;
(3) by the casting solution nitrogen pressurization of step (2), spinning head is pumped into through spinning measuring, be pulled through the air gap of 10 ~ 22cm, be stretched to certain radial dimension and enter 30 ~ 50 DEG C of coagulating baths (aqueous solution of one or both mixtures in dimethylacetylamide or dimethyl formamide) and be solidified into hollow fiber nanofiltration membrane film silk, wherein the discharging speed of measuring pump is 15 ~ 25mL/min;
(4) film silk step (3) obtained, with after the speed rolling of 0.2 ~ 0.5m/s, soaks 10 ~ 24h through clear water, then is soaked in 20 ~ 30h in glycerine water solution, finally dry obtained described asymmetric polyether sulfone hollow fiber nanofiltration membrane.
The above, be only preferred embodiment of the present invention, therefore can not limit scope of the invention process according to this, the equivalence change namely done according to the scope of the claims of the present invention and description with modify, all should still belong in scope that the present invention contains.
Claims (9)
1. a preparation method for asymmetric polyether sulfone hollow fiber nanofiltration membrane, is characterized in that: comprise following component:
(1) each component is taken according to following percentage by weight: polyether sulfone 13 ~ 37%, beta-schardinger dextrin-1 ~ 12%, organic hydrophilic pore former 2 ~ 20%, inorganic nano-particle 1 ~ 7% and film forming solvent 24 ~ 83%; Organic hydrophilic pore former is at least one in polyvinylpyrrolidone, polyethylene glycol PEG and tween, and inorganic nano-particle is LiCl, SiO
2, TiO
2, Al
2o
3with at least one in ZrO, film forming solvent is at least one in dimethylacetylamide, dimethyl formamide and N ~ methyl pyrrolidone;
(2) above-mentioned each component is added in reaction vessel, stir 6 ~ 10h in 60 ~ 80 DEG C and dissolve, then standing and defoaming 10 ~ 16h, obtain casting solution;
(3) by the casting solution nitrogen pressurization of step (2), spinning head is pumped into through spinning measuring, be pulled through the air gap of 10 ~ 22cm, be stretched to certain radial dimension and enter 30 ~ 50 DEG C of coagulating baths and be solidified into hollow fiber nanofiltration membrane film silk, wherein the discharging speed of measuring pump is 15 ~ 25mL/min;
(4) film silk step (3) obtained, with after the speed rolling of 0.2 ~ 0.5m/s, soaks 10 ~ 24h through clear water, then is soaked in 20 ~ 30h in glycerine water solution, finally dry obtained described asymmetric polyether sulfone hollow fiber nanofiltration membrane.
2. the preparation method of a kind of asymmetric polyether sulfone hollow fiber nanofiltration membrane as claimed in claim 1, is characterized in that: described step takes each component in (1) as following weight percent: polyether sulfone 15 ~ 35%, beta-schardinger dextrin-1 ~ 10%, organic hydrophilic pore former 3 ~ 17%, inorganic nano-particle 1 ~ 5% and film forming solvent 33 ~ 80%.
3. the preparation method of a kind of asymmetric polyether sulfone hollow fiber nanofiltration membrane as claimed in claim 2, is characterized in that: described step takes each component in (1) as following weight percent: polyether sulfone 18 ~ 30%, beta-schardinger dextrin-2 ~ 9%, organic hydrophilic pore former 6 ~ 11%, inorganic nano-particle 1 ~ 3% and film forming solvent 47 ~ 73%.
4. the preparation method of a kind of asymmetric polyether sulfone hollow fiber nanofiltration membrane as claimed in claim 1, it is characterized in that: described step (2) is: above-mentioned each component is added in reaction vessel, stir 7 ~ 9h in 65 ~ 70 DEG C to dissolve, then standing and defoaming 12 ~ 14h, obtain casting solution.
5. the preparation method of a kind of asymmetric polyether sulfone hollow fiber nanofiltration membrane as claimed in claim 1, it is characterized in that: described step (3) is: by the casting solution nitrogen pressurization of step (2), spinning head is pumped into through spinning measuring, be pulled through the air gap of 11 ~ 16cm, be stretched to certain radial dimension and enter 30 ~ 40 DEG C of coagulating baths and be solidified into hollow fiber nanofiltration membrane film silk, wherein the discharging speed of measuring pump is 17 ~ 21mL/min.
6. the preparation method of a kind of asymmetric polyether sulfone hollow fiber nanofiltration membrane as claimed in claim 1, is characterized in that: the coagulating bath in described step (4) is the aqueous solution of one or both mixtures in dimethylacetylamide or dimethyl formamide.
7. the preparation method of a kind of asymmetric polyether sulfone hollow fiber nanofiltration membrane as claimed in claim 1, is characterized in that: in described step (4), clear water soaks the time is 14 ~ 24h.
8. the preparation method of a kind of asymmetric polyether sulfone hollow fiber nanofiltration membrane as claimed in claim 1, is characterized in that: in described step (4), in glycerine water solution, the concentration of glycerine is 3 ~ 30%, and soak time is 24h.
9. the preparation method of a kind of asymmetric polyether sulfone hollow fiber nanofiltration membrane as claimed in claim 1, is characterized in that: in described step (4), the speed of rolling is 0.25 ~ 0.35m/s.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107456871A (en) * | 2017-08-02 | 2017-12-12 | 同济大学 | A kind of preparation method of the compound loose NF membrane of doughnut |
| CN107537317A (en) * | 2017-10-27 | 2018-01-05 | 贵州省材料产业技术研究院 | The preparation method of polypropylene hollow fiber NF membrane |
| CN115463550A (en) * | 2022-08-28 | 2022-12-13 | 天津汉晴环保科技有限公司 | Polyether sulfone humidifying membrane with symmetrical structure and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107456871A (en) * | 2017-08-02 | 2017-12-12 | 同济大学 | A kind of preparation method of the compound loose NF membrane of doughnut |
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| CN107537317A (en) * | 2017-10-27 | 2018-01-05 | 贵州省材料产业技术研究院 | The preparation method of polypropylene hollow fiber NF membrane |
| CN115463550A (en) * | 2022-08-28 | 2022-12-13 | 天津汉晴环保科技有限公司 | Polyether sulfone humidifying membrane with symmetrical structure and preparation method thereof |
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