CN106582308B - A kind of chitin nanocomposite ps hollow fiber uf membrane and preparation method thereof - Google Patents
A kind of chitin nanocomposite ps hollow fiber uf membrane and preparation method thereof Download PDFInfo
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- CN106582308B CN106582308B CN201611091816.5A CN201611091816A CN106582308B CN 106582308 B CN106582308 B CN 106582308B CN 201611091816 A CN201611091816 A CN 201611091816A CN 106582308 B CN106582308 B CN 106582308B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/08—Hollow fibre membranes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0002—Organic membrane manufacture
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
-
- 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
- B01D71/66—Polymers having sulfur in the main chain, with or without nitrogen, oxygen or carbon only
- B01D71/68—Polysulfones; Polyethersulfones
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/24—Mechanical properties, e.g. strength
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/36—Hydrophilic membranes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/48—Antimicrobial properties
Abstract
The invention discloses a kind of chitin nanocomposite ps hollow fiber uf membranes and preparation method thereof to be coextruded casting solution and core liquid to form tubulose liquid film through cyclic annular spinneret using immersion precipitation phase inversion process, and tubulose liquid film solidifies through coagulating bath and obtained；The casting solution is mixed by following components by mass percentage: polysulfones 12-30%, chitin nanocrystalline 0.1-7%, sulfonated polysulfone 0.5-7%, organic solvent surplus.Chitin nanocomposite ps hollow fiber uf membrane prepared by the present invention has high-intensitive and good hydrophily and antibiotic property.
Description
Technical field
The present invention relates to separation technical field of membrane, in particular to a kind of chitin nanocomposite ps hollow fiber uf membrane and
Preparation method.
Background technique
PS membrane has excellent thermal stability and chemical stability, is widely used in haemodialysis, sea water desalination and water
The fields such as processing.The composition and membrance casting condition of casting film liquid system therefore, are led to an important factor for determining polysulfones membrane structure and performance
Cross regulation casting solution concentration, composition, coagulation bath composition, temperature, the air gap and flow velocity etc., can prepare different physical structures and
The PS membrane of performance.But polysulfones is a kind of polymer material of high hydrophobicity, therefore, the hydrophily of PS membrane is poor, causes
When PS membrane is used for the separation of aqueous systems, the seperation film vulnerable to pollution, the performance and used life of film is affected.
The hydrophily for improving PS membrane becomes the important measures for improving PS membrane antifouling property, wherein using blending parent
The blending method of aqueous additive is current using most most effective hydrophilic polysulfone membrane preparation methods.For example, application No. is
201410744351.3 Chinese patent literature disclose a kind of preparation method of ps hollow fiber uf membrane, addition is poly- in casting solution
Ethylene glycol, and the mass ratio of polysulfones, polyethylene glycol and dimethyl acetamide is 20/35/45, by technique in preparation process and
The optimization of parameter, obtains ps hollow fiber uf membrane.Chinese patent CN1158273A and Japan Patent JP-A-300633/1993 etc.
Disclose the method that hydrophilic polysulfone membrane is prepared for additive with polyvinylpyrrolidone (PVP).High molecular weight or high-content
The viscosity of casting film liquid system can be improved in polyethylene glycol and polyvinylpyrrolidone, obtains the PS membrane of sponge pore structure, but also deposits
The disadvantages of film surface is of poor quality, intensity is low and film is difficult, so that its industrialized production is restricted.Therefore, preparation tool
There is high-intensitive hydrophilic polysulfone membrane to have broad application prospects.
Summary of the invention
The purpose of the present invention is to provide a kind of chitin nanocomposite ps hollow fiber uf membranes, have good machinery
Intensity and good hydrophilicity and anti-microbial property.
The present invention also provides the preparation methods of above-mentioned chitin nanocomposite ps hollow fiber uf membrane.
The technical solution adopted by the present invention to solve the technical problems is:
A kind of chitin nanocomposite ps hollow fiber uf membrane, using immersion precipitation phase inversion process, by casting solution and core
Liquid is coextruded to form tubulose liquid film, and tubulose liquid film solidifies through coagulating bath and obtained；The casting solution is by mass percentage by following
Component is mixed: polysulfones 12-30%, chitin nanocrystalline 0.1-7%, sulfonated polysulfone 0.5-7%, organic solvent surplus.
Core liquid is used to form hollow structure, while adjusting film inner surface apertures structure, improves the separating property of film.
Preferably, the casting solution is mixed by following components by mass percentage: polysulfones 14-25%, chitin are received
Rice crystalline substance 1-7%, sulfonated polysulfone 2-7%, organic solvent surplus.It is furthermore preferred that the casting solution is by mass percentage by with the following group
It point is mixed: polysulfones 14-20%, chitin nanocrystalline 2-7%, sulfonated polysulfone 3-7%, organic solvent surplus.The present invention passes through tune
The ratio for saving each raw material of casting solution, can significantly adjust membrane structure and performance.
The sulfonation degree of the sulfonated polysulfone is 10-60%, more preferably 25-50%.The present invention is by adjusting sulfonated polysulfone
Sulfonation degree improves the nanocrystalline compatibility with polysulfones of chitin.
Compared with prior art, the present invention is nanocrystalline as the reinforcing agent of PS membrane and antibacterial modified dose using chitin, together
The mechanical performance and antibiotic property of Shi Gaishan PS membrane；Between the nanocrystalline amino of sulfonic group and chitin based on sulfonated polysulfone
Electrostatic interaction improves hydrophilic first using the hydrophilic modifier of the sulfonated polysulfone dispersing agent nanocrystalline as chitin and PS membrane
The hydrophily of interface compatibility and PS membrane between the nanocrystalline and hydrophobic polysulfones of shell element, to make the chitin nanometer of preparation
Brilliant compound ps hollow fiber uf membrane has excellent mechanical strength, good hydrophilicity and anti-microbial property.It is provided by the invention
Preparation method simple process, it is easy to operate.
Preferably, the core liquid is by organic solvent: water=1:1-1:10 volume ratio mixes.Further, described
Core liquid is by organic solvent: water=1:1-1:8 volume ratio mixes, and further, the core liquid is by organic solvent: water=1:
The volume ratio of 1-1:5 mixes.
Preferably, the organic solvent is at least one of dimethyl acetamide, dimethyl sulfoxide.
Preferably, the coagulating bath is water.Play preferable solidification effect.
Preferably, the nanocrystalline diameter of the chitin is 4-35nm, length 40-600nm.More preferable chitin is received
The diameter of meter Jing is 4-20nm, length 100-500nm.The present invention improves the knot of film by adjusting the nanocrystalline length of chitin
Structure, hydrophily, antibiotic property and mechanical strength.
A kind of preparation method of chitin nanocomposite ps hollow fiber uf membrane, includes the following steps:
(1) by chitin it is nanocrystalline it is evenly dispersed in organic solvent, polysulfones and sulfonated polysulfone, stirring to shape is then added
At uniform solution, deaeration obtains casting solution；
(2) organic solvent and water are mixed and made into core liquid；
(3) casting solution and core liquid are coextruded to form tubulose liquid film by cyclic annular spinneret；
(4) tubulose liquid film enters in coagulating bath behind the air gap and solidifies, and is placed in water soaking and washing, obtains chitin
Nanocomposite ps hollow fiber uf membrane.
Defoaming method described in step (1) is preferably standing and defoaming method or vacuum defoamation method.
Preferably, the extrusion flow velocity of casting solution is 10-20 g/min in step (3).Further, the extrusion of casting solution
Flow velocity is 12-18 g/min；Further, the extrusion flow velocity of casting solution is 14-16 g/min.The present invention passes through adjusting
The flow velocity of casting solution adjusts the thickness of hollow-fibre membrane, regulates and controls membrane flux；By adjusting the flow velocity of core liquid, plays and adjust hollow fibre
Tie up the internal diameter of film and the purpose of wall thickness.
Preferably, the extrusion flow velocity of step (3) core liquid is 10-20 ml/min.Further, the extrudate flow of core liquid
Speed is 12-18 ml/min；Further, the extrusion flow velocity of core liquid is 14-16ml/min.
Preferably, the air gap is 0.1-30 cm in step (4).Preferred air gap is 1-25 cm, more preferably empty
Gas gap is 7-15 cm.The present invention plays the purpose of the structure of regulation film by the distance of control the air gap.
Preferably, using ultrasonic method or homogeneous method in step (1), organic solvent is dispersed in by chitin is nanocrystalline
In.
The invention has the advantages that and the utility model has the advantages that
1, the present invention is nanocrystalline for additive with chitin, can improve the mechanical strength and antibiotic property of PS membrane simultaneously, makes
It is standby to obtain high-intensitive antibacterial ps hollow fiber uf membrane, also, method provided by the invention is simple and easy.
2, the dispersing agent that sulfonated polysulfone is nanocrystalline for chitin is used, the sulfonic group based on sulfonated polysulfone and chitin nanometer
Electrostatic interaction between brilliant amino, can be effectively suppressed the nanocrystalline reunion of chitin, and enhance chitin it is nanocrystalline with
The compatibility of polysulfones further improves the comprehensive performance of chitin nanocomposite ps hollow fiber uf membrane.
Specific embodiment
Below by specific embodiment, technical scheme of the present invention will be further explained in detail.
In the present invention, if not refering in particular to, used raw material and equipment etc. are commercially available or commonly used in the art.
Method in following embodiments is unless otherwise instructed the conventional method of this field.
Raw material and chemical reagent used in the embodiment of the present invention are commercial product.
Embodiment 1
It is 4 nm by diameter, length, which is that the chitin of 40 nm is nanocrystalline, to be dispersed in dimethyl acetamide, is added poly-
The sulfonated polysulfone that sulfone and sulfonation degree are 20% is stirred and dissolved into uniform solution, and standing and defoaming obtains casting solution, and casting solution presses matter
Measure percentages formula are as follows: polysulfones 12%, chitin nanocrystalline 0.2%, sulfonated polysulfone 1.5%, dimethyl acetamide 86.3%；By two
Methylacetamide and water volume ratio are the mixed solution of 1:3 as core liquid.Casting solution and core liquid are passed through into immersion precipitation inversion of phases
The cyclic annular spinneret of device for spinning is extruded into tubulose liquid film simultaneously, and casting film flow velocity is 20 g/min, and core flow velocity is 20
Ml/min, tubulose liquid film, into solidify 24 hours into hollow-fibre membrane in the coagulating bath of water, pass through behind the air gap of 7 cm
After 48 h of water soaking and washing, chitin nanocomposite ps hollow fiber uf membrane is obtained.
After membrane module is made in above-mentioned chitin nanocomposite ps hollow fiber uf membrane, measuring water flux is 8000 L/
m2H, tensile strength are 10 MPa.
Embodiment 2
It is 10 nm by diameter, length, which is that the chitin of 300 nm is nanocrystalline, to be dispersed in dimethyl sulfoxide, is added poly-
The sulfonated polysulfone that sulfone and sulfonation degree are 50% is stirred and dissolved into uniform solution, and standing and defoaming obtains casting solution, and casting solution presses matter
Measure percentages formula are as follows: polysulfones 20%, chitin nanocrystalline 2%, sulfonated polysulfone 7%, dimethyl sulfoxide 71%；By dimethyl sulfoxide
With water volume ratio be 1:4 mixed solution as core liquid.Casting solution and core liquid are passed through into immersion precipitation inversion of phases device for spinning
Cyclic annular spinneret is extruded into tubulose liquid film simultaneously, and casting film flow velocity is 10 g/min, and core flow velocity is 10 ml/min, tubulose
Liquid film behind the air gap of 15 cm into water coagulating bath in solidify 24 hours at hollow-fibre membrane, through water soaking and washing
After 48 h, chitin nanocomposite ps hollow fiber uf membrane is obtained.
After membrane module is made in above-mentioned chitin nanocomposite ps hollow fiber uf membrane, measuring water flux is 9000 L/
m2H, tensile strength are 5 MPa.
Embodiment 3
It is 10 nm by diameter, length, which is that the chitin of 100 nm is nanocrystalline, is dispersed in organic solvent (dimethylacetamide
Amine and dimethyl sulfoxide press the mixed liquor of 1:1 volume ratio composition) in, polysulfones and sulfonation degree is added as 30% sulfonated polysulfone, stirs
It is dissolved into uniform solution, standing and defoaming obtains casting solution, and casting solution is formulated by mass percentage are as follows: polysulfones 30%, crust
Element nanocrystalline 4%, sulfonated polysulfone 3%, organic solvent 63%；By mixed liquor (the dimethyl second of dimethyl acetamide and dimethyl sulfoxide
Amide and dimethyl sulfoxide are mixed by 1:1 volume ratio) it is mixed for 1:3 as core liquid with water volume ratio.By casting solution and core
Liquid is extruded into tubulose liquid film by the cyclic annular spinneret of immersion precipitation inversion of phases device for spinning simultaneously, and casting film flow velocity is 10
G/min, core flow velocity be 10 ml/min, tubulose liquid film behind the air gap of 0.1 cm into water coagulating bath in solidify
At hollow-fibre membrane, after 48 h of water soaking and washing, chitin nanocomposite ps hollow fiber uf membrane is obtained within 24 hours.
After membrane module is made in above-mentioned chitin nanocomposite ps hollow fiber uf membrane, measuring water flux is 6000 L/
m2H, tensile strength are 7 MPa.
Embodiment 4
It is 15 nm by diameter, length, which is that the chitin of 350 nm is nanocrystalline, to be dispersed in dimethyl acetamide, is added
The sulfonated polysulfone that polysulfones and sulfonation degree are 25%, is stirred and dissolved into uniform solution, standing and defoaming obtains casting solution, and casting solution is pressed
Mass percent meter formula are as follows: polysulfones 15%, chitin nanocrystalline 3%, sulfonated polysulfone 0.5%, dimethyl acetamide 81.5%；By two
Methylacetamide and water volume ratio are the mixed solution of 1:1 as core liquid.Casting solution and core liquid are passed through into immersion precipitation inversion of phases
The cyclic annular spinneret of device for spinning is extruded into tubulose liquid film simultaneously, and casting film flow velocity is 15 g/min, and core flow velocity is 15
Ml/min, tubulose liquid film, into solidify 24 hours into hollow-fibre membrane in the coagulating bath of water, pass through behind the air gap of 15 cm
After 48 h of water soaking and washing, chitin nanocomposite ps hollow fiber uf membrane is obtained.
After membrane module is made in above-mentioned chitin nanocomposite ps hollow fiber uf membrane, measuring water flux is 4000 L/
m2H, tensile strength are 6 MPa.
Embodiment 5
It is 35 nm by diameter, length, which is that the chitin of 600 nm is nanocrystalline, to be dispersed in dimethyl acetamide, is added
The sulfonated polysulfone that polysulfones and sulfonation degree are 30%, is stirred and dissolved into uniform solution, standing and defoaming obtains casting solution, and casting solution is pressed
Mass percent meter formula are as follows: polysulfones 18%, chitin nanocrystalline 7%, sulfonated polysulfone 1%, dimethyl acetamide 74%；By dimethyl
Acetamide and water volume ratio are the mixed solution of 1:3 as core liquid.Casting solution and core liquid are passed through into the spinning of immersion precipitation inversion of phases
The cyclic annular spinneret of device is extruded into tubulose liquid film simultaneously, and casting film flow velocity is 15 g/min, and core flow velocity is 15 ml/
Min, tubulose liquid film behind the air gap of 30 cm into water coagulating bath in solidify 24 hours at hollow-fibre membrane, through water
After 48 h of soaking and washing, chitin nanocomposite ps hollow fiber uf membrane is obtained.
After membrane module is made in above-mentioned chitin nanocomposite ps hollow fiber uf membrane, measuring water flux is 5500 L/
m2H, tensile strength are 4 MPa.
Comparative example 1
Polysulfones and sulfonated polysulfone are dissolved in dimethyl acetamide, uniform solution is stirred into, standing and defoaming is cast
Film liquid, casting solution are formulated by mass percentage are as follows: polysulfones 14%, sulfonated polysulfone 5%, dimethyl acetamide 81%；By dimethyl second
Amide and water volume ratio are the mixed solution of 1:3 as core liquid.Casting solution and core liquid are filled by the spinning of immersion precipitation inversion of phases
The cyclic annular spinneret set while it being extruded into tubulose liquid film, casting film flow velocity is 15 g/min, and core flow velocity is 15 ml/min,
Tubulose liquid film, into solidify 24 hours into hollow-fibre membrane in the coagulating bath of water, impregnates clearly behind the air gap of 7 cm through water
After washing 48 h, ps hollow fiber uf membrane is obtained.
After membrane module is made in above-mentioned ps hollow fiber uf membrane, measuring water flux is 3000 L/m2H, tensile strength are
2.5 MPa。
Comparative example 2
Polysulfones and sulfonated polysulfone are dissolved in dimethyl acetamide, uniform solution is stirred into, standing and defoaming is cast
Film liquid, casting solution are formulated by mass percentage are as follows: polysulfones 25%, sulfonated polysulfone 3%, dimethyl acetamide 72%；；By dimethyl
Acetamide and water volume ratio are the mixed solution of 1:2 as core liquid.Casting solution and core liquid are passed through into the spinning of immersion precipitation inversion of phases
The cyclic annular spinneret of device is extruded into tubulose liquid film simultaneously, and casting film flow velocity is 10 g/min, and core flow velocity is 10 ml/
Min, tubulose liquid film behind the air gap of 25 cm into water coagulating bath in solidify 24 hours at hollow-fibre membrane, through water
After 48 h of soaking and washing, ps hollow fiber uf membrane is obtained.
After membrane module is made in above-mentioned ps hollow fiber uf membrane, measuring water flux is 3600 L/m2H, tensile strength 3
MPa。
Above-mentioned embodiment is only a preferred solution of the present invention, not the present invention is made in any form
Limitation, there are also other variations and modifications on the premise of not exceeding the technical scheme recorded in the claims.
Claims (4)
1. a kind of chitin nanocomposite ps hollow fiber uf membrane, which is characterized in that use immersion precipitation phase inversion process, will cast
Film liquid and core liquid are coextruded to form tubulose liquid film, and tubulose liquid film solidifies through coagulating bath and obtained；The casting solution is by mass percentage
Meter is mixed by following components: polysulfones 12-30%, chitin nanocrystalline 0.1-7%, sulfonated polysulfone 0.5-7%, organic solvent
Surplus；The nanocrystalline diameter of the chitin is 4-35nm, length 40-600nm；
The sulfonation degree of sulfonated polysulfone is 10-60%；
The chitin nanocomposite ps hollow fiber uf membrane is prepared through following procedure:
(1) by chitin it is nanocrystalline it is evenly dispersed polysulfones and sulfonated polysulfone is then added in organic solvent, stirring is equal to being formed
Even solution, deaeration obtain casting solution；
(2) organic solvent and water are mixed and made into core liquid；
(3) casting solution and core liquid are coextruded to form tubulose liquid film by cyclic annular spinneret；
(4) tubulose liquid film enters in coagulating bath behind the air gap and solidifies, and is placed in water soaking and washing, obtains chitin nanometer
Brilliant compound ps hollow fiber uf membrane；
The extrusion flow velocity of casting solution is 10-20g/min in step (3)；
The extrusion flow velocity of step (3) core liquid is 10-20ml/min；
The air gap is 0.1-30cm in step (4)；
Ultrasonic method or homogeneous method are used in step (1), by chitin it is nanocrystalline it is evenly dispersed in organic solvent.
2. a kind of chitin nanocomposite ps hollow fiber uf membrane according to claim 1, which is characterized in that the core
Liquid is by organic solvent: water=1:1-1:10 volume ratio mixes.
3. a kind of chitin nanocomposite ps hollow fiber uf membrane according to claim 1 or 2, which is characterized in that institute
Stating organic solvent is at least one of dimethyl acetamide, dimethyl sulfoxide.
4. a kind of chitin nanocomposite ps hollow fiber uf membrane according to claim 1 or 2, which is characterized in that institute
Stating coagulating bath is water.
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| WO2010042647A2 (en) * | 2008-10-07 | 2010-04-15 | The Research Foundation Of State University Of New York | High flux high efficiency nanofiber membranes and methods of production thereof |
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| CN105664732A (en) * | 2014-02-26 | 2016-06-15 | 宁波莲华环保科技股份有限公司 | Method for preparing organic forward osmosis membrane |
| CN105664740A (en) * | 2016-02-03 | 2016-06-15 | 沁园集团股份有限公司 | Preparation method of nanocellulose composite polysulfone hollow fiber membrane |
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| WO2010042647A2 (en) * | 2008-10-07 | 2010-04-15 | The Research Foundation Of State University Of New York | High flux high efficiency nanofiber membranes and methods of production thereof |
| CN103816811A (en) * | 2014-02-26 | 2014-05-28 | 宁波莲华环保科技股份有限公司 | Preparation method of organic forward-osmosis membrane |
| CN105664732A (en) * | 2014-02-26 | 2016-06-15 | 宁波莲华环保科技股份有限公司 | Method for preparing organic forward osmosis membrane |
| CN105457494A (en) * | 2014-09-09 | 2016-04-06 | 贵阳时代沃顿科技有限公司 | Nanostructure high-flux reverse osmosis membrane for seawater desalination and preparation method therefor |
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