CN102836645A - Polyvinylidene-fluoride hollow fibre membrane and preparation method thereof - Google Patents
Polyvinylidene-fluoride hollow fibre membrane and preparation method thereof Download PDFInfo
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- CN102836645A CN102836645A CN2012103480711A CN201210348071A CN102836645A CN 102836645 A CN102836645 A CN 102836645A CN 2012103480711 A CN2012103480711 A CN 2012103480711A CN 201210348071 A CN201210348071 A CN 201210348071A CN 102836645 A CN102836645 A CN 102836645A
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Abstract
The invention discloses a polyvinylidene-fluoride hollow fibre membrane and a preparation method thereof. Calculated according to parts by weight, the polyvinylidene-fluoride hollow fibre membrane is mainly prepared by the following components: 15 to 25 parts of polyvinylidene fluoride, 50 to 80 parts of solvent, 1 to 3 parts of surfactant, 2 to 12 parts of polymeric additive, 1 to 8 parts of inorganic additive and 1 to 12 parts of modified blend. By utilizing the simultaneous action of two modes of organic blending and inorganic adding according to the polyvinylidene-fluoride hollow fibre membrane and the preparation method thereof, the hydrophilcity of the polyvinylidene-fluoride hollow fibre membrane is obviously improved, and the pollution resistance can be obviously reinforced; and the pure water flux of the polyvinylidene-fluoride hollow fibre membrane is further enhanced by selecting and regulating the raw materials and the mixture ratio of the modified blend and the inorganic additive so as to obtain the permanently hydrophilic modified polyvinylidene-fluoride hollow fibre membrane.
Description
Technical field
The present invention relates to a kind of Kynoar hollow-fibre membrane and preparation method thereof, belong to water-treatment technology field.
Background technology
Membrane separation technique has the efficient height, energy consumption is low, technology is simple, facility compact, filtration safety, advantage such as pollution-free; Be widely used in industries such as electronics chemical industry, biological medicine, food and drink and environmental protection, but it is in water treatment field by development and application mainly.Because of it involves a wide range of knowledge and measures and big, the embrane method water technology enjoys favor in industry, be called as " water technology of 21st century ".At present, along with the development of membrane science technology, membrane separation technique has obtained application in various degree in fields such as desalinization, bitter desalination, high purity water preparation, water treatment of power plant sewage, wastewater treatment and drink water purifying processing.
Common membrane material has polysulfones, polypropylene, polyethylene, polyvinyl chloride, polyether sulfone, Kynoar etc. at present.Kynoar is a kind of crystal polymer thing; Have good chemical stability, hear resistance, radiation resistance and good physical and mechanical properties; And can under lower temperature, be dissolved in some strong polar organic solvent; Being easy to solution inversion of phases legal system film, is a kind of polymeric film material of function admirable.Kynoar is one of hydrophobic polymeric material of tool, thereby the Kynoar hollow-fibre membrane is proposed hydrophilic modification method, and it can reduce: membrane surface modification and membrane material modified two big types.The hydrophily that generally obtains through membrane surface modification can not be lasting, and its hydrophily lost efficacy along with the prolongation of film service time; And membrane material carries out hydrophilic modifying through introducing polar group, can fundamentally change the hydrophily of diffusion barrier, eliminates the deficiency on the single polymers component property, thus the desirable film product of system.
Application number is 200910231291.4 and is called in the patent application of " Kynoar hollow fiber ultrafiltration membrane and preparation method with permanent hydrophilic "; Adopt polar monomer that the PVDF raw material are carried out grafting; Thereby realize the hydrophilic modifying of film silk; But the pure water flux of the hollow-fibre membrane product that it finally obtains is lower, and antifouling property is poor, can't satisfy the needs of practical application.Application number is 201110186228.0 and is called in the patent application of " Kynoar hollow-fibre membrane and preparation method thereof "; After adopting calcium carbonate and silica to handle through modification; As reinforcing agent; Thereby realize the mechanical strength and the control of the aperture uniformity of film silk, but the hydrophilic modifying of its hollow-fibre membrane product that obtains does not belong to impermanent modification for having radiation or grafting hydrophilic group.Thereby how to seek the pure water flux height, antifouling property is strong, hydrophily is good and the Kynoar hollow-fibre membrane of permanent hydrophilic modification becomes the focus that people pay close attention to.
Summary of the invention
The objective of the invention is to; A kind of Kynoar hollow-fibre membrane and preparation method thereof is provided; The present invention acts on through utilizing organic blend and inorganic interpolation dual mode simultaneously, make the Kynoar hollow-fibre membrane hydrophily be improved significantly, antifouling property is obviously strengthened; Through the raw material of modified blends and inorganic additive and proportioning being selected and adjusted, thereby further improve the pure water flux of Kynoar hollow-fibre membrane, obtain the Kynoar hollow-fibre membrane of permanent hydrophilic modification.
The present invention constitutes like this: a kind of Kynoar hollow-fibre membrane, to calculate by weight, and it is mainly processed by following component:
1～3 part in 50～80 parts of surfactants of 15～25 parts of solvents of Kynoar
1～12 part of 1～8 part of modified blends of 2～12 parts of inorganic additives of polymeric additive.
Preferably, calculate by weight, it is mainly processed by following component:
1 part in 55 parts of surfactants of 23 parts of solvents of Kynoar
12 parts of 1 part of modified blends of 8 parts of inorganic additives of polymeric additive.
Among the present invention, described Kynoar is universal homopolymers or copolymer, and the preferred standard relative density is 1.75-1.77g/cm
3Kynoar.
Component among the present invention is nanometer particle.
Solvent described in the present invention is one or more in dimethyl formamide, dimethylacetylamide, dimethyl sulfoxide (DMSO), N-methyl pyrrolidone, the triethyl phosphate; Above-mentioned solvent is intensive polar solvent, can be more rapidly and uniformly with the spinning solution components dissolved.
Described surfactant is one or more in lauryl sodium sulfate, neopelex, sodium dodecyl aminopropionitrile, the Tweens series; Described Tweens series comprises one or more in soil temperature-20, soil temperature-40, soil temperature-60, the soil temperature-80, thereby can promote the hydrophily of hollow-fibre membrane.
Described polymeric additive is one or more in polyethylene glycol, polyvinylpyrrolidone, polyvinyl alcohol, polyoxyethylene, the methylcellulose, and polymeric additive mainly plays pore-forming, influences porosity, hydrophily and the water flux etc. of film simultaneously.
Described inorganic additive is one or more in lithium nitrate, lithium chloride, calcium chloride, calcium carbonate, calcium nitrate, silica, the kaolin; This inorganic additive requires to be nanometer particle; In casting solution, add inorganic particulate; The effect of pore former, reinforcing agent be can play, thereby hydrophily, stability, crushing resistance and the membrane flux of film improved.
Described modified blends is one or more in cellulose acetate, methyl methacrylate, vinyl acetate, polyvinyl alcohol, acrylic acid ester, maleic anhydride, the polyvinyl butyral resin.Modified blends can improve the toughness of Kynoar hollow-fibre membrane, improves the hydrophily of film simultaneously, and improves its resistance tocrocking.
The preparation method of the Kynoar hollow-fibre membrane described in the present invention; Adopt to do-the wet spinning technology preparation; Comprise: Kynoar, solvent, surfactant, polymeric additive, inorganic additive, modified blends are added in the stirred tank; 70～100 ℃ of following agitating heating blend, mixing speed is 90～120r/min, and mixing time is 1～6h; Blended liquid is left standstill 1～6h carry out the deaeration processing, and cool to 40～80 ℃, get casting solution; Casting solution is extruded through spinning nozzle with spinning core liquid under nitrogen gas pressure, after the air distance through 0～200mm, at the uniform velocity immerses in 30～60 ℃ of outer solidification liquid coagulating baths; The speed with 10～100m/min stretches in the coagulating bath outside, gets the Kynoar hollow-fibre membrane of moulding; The Kynoar hollow-fibre membrane of moulding is extracted, protects the hole post processing, get Kynoar hollow-fibre membrane finished product.
Spinning core liquid described in the present invention is the water or the dimethylacetylamide aqueous solution; Outer solidification liquid is the water or the dimethylacetylamide aqueous solution.
The used extractant of post processing described in the present invention is hydrochloric acid or sodium carbonate, thereby conveniently the organic and inorganic additive that leaves behind the pore-forming is extracted; Used guarantor hole agent is glycerine or sodium lactate aqueous solution, thereby can protect fenestra, prevents that contraction distortion of film silk and fenestra from diminishing and lost efficacy.
Compared with prior art, the present invention acts on through utilizing organic blend and inorganic interpolation dual mode simultaneously, make the Kynoar hollow-fibre membrane hydrophily be improved significantly, antifouling property is obviously strengthened; Through the raw material of modified blends and inorganic additive and proportioning being selected and adjusted, thereby further improve the pure water flux of Kynoar hollow-fibre membrane, obtained the Kynoar hollow-fibre membrane of permanent hydrophilic modification.Specifically, in the membrane material of the present invention, make through organic blend and to introduce hydrophilic radical in the material, make that the prepared hollow-fibre membrane hydrophilicity that obtains is better; Make that through inorganic interpolation the distribution in film silk aperture is narrower, the overwhelming majority concentrates on the aperture value of setting, and poroid be single skin finger-like pore structure, thereby help the lifting of water flux; In addition, organic blend and inorganic material are added makes membrane aperture be evenly distributed, and pollutant should not get into fenestra inside and pollute, and makes its antifouling property strengthen.Show that according to the mass data statistics pure water flux of the prepared Kynoar hollow-fibre membrane that obtains of the present invention reaches 25 ℃ of 1500L/ ㎡ h0.1MPa, it is 0.02～0.50um that film separates the aperture, and fracture pressure is greater than 0.3MPa.
The applicant has carried out a series of experiments and has selected component provided by the invention, proportioning and preparation technology; Assurance science, reasonable, feasible; Manufacturing enterprise can be according to the present invention Direct Production, the good Kynoar hollow-fibre membrane of preparation effect, and no longer need carry out new groping, study; In fact for doughnut membrane preparation technology in the water treatment, its key just is the selection of component, proportioning and manufacturing condition; If it is improper to select, or can not prepare effective product, or the product cost of preparing is high, do not meet market demands again; Selection of the present invention solves these problems; Simultaneously, a kind of new hollow-fibre membrane is provided again, has made the water treatment better effects if to market.
Experimental example 1: component and the research of proportioning screening test:
Conclusion: after adding modified blends in the component, the performance of the prepared hollow-fibre membrane that obtains be improved significantly; And the proportioning content of each component also has bigger influence to hollow-fibre membrane, and wherein the practical application effect of 23 parts of proportioning Kynoar, 55 parts of solvents, 1 part in surfactant, 8 parts of polymeric additives, 1 part of inorganic additive, 12 parts of resulting hollow-fibre membranes of modified blends is best.
The specific embodiment
Embodiment 1:
1 part of 60 parts of lauryl sodium sulfate of 25 parts of dimethyl formamides of Kynoar
5 parts of 1 part of cellulose acetates of 8 parts of lithium nitrates of polyethylene glycol
Above-mentioned Kynoar, dimethyl formamide, lauryl sodium sulfate, polyethylene glycol, lithium nitrate, cellulose acetate are added in the stirred tank, and 80 ℃ of following agitating heating blend, mixing speed is 100r/min, and mixing time is 3h; Blended liquid is left standstill 4h carry out the deaeration processing, and cool to 60 ℃, get casting solution; Casting solution is extruded through spinning nozzle with the aqueous solution under nitrogen gas pressure, after the air distance through 100mm, at the uniform velocity immerses in 35 ℃ of aqueous coagulation baths; The speed with 60m/min stretches in the coagulating bath outside, gets the Kynoar hollow-fibre membrane of moulding; The Kynoar hollow-fibre membrane of moulding is extracted, protects the hole post processing with glycerine with hydrochloric acid, get Kynoar hollow-fibre membrane finished product.The standard relative density of described Kynoar is 1.75-1.77g/cm
3
Embodiment 2:
3 parts of 50 parts of lauryl sodium sulfate of 17 parts of dimethyl formamides of Kynoar
10 parts of 8 parts of cellulose acetates of 12 parts of lithium nitrates of polyethylene glycol
Above-mentioned Kynoar, dimethyl formamide, lauryl sodium sulfate, polyethylene glycol, lithium nitrate, cellulose acetate are added in the stirred tank, and 100 ℃ of following agitating heating blend, mixing speed is 120r/min, and mixing time is 6h; Blended liquid is left standstill 6h carry out the deaeration processing, and cool to 80 ℃, get casting solution; Casting solution is extruded through spinning nozzle with the aqueous solution under nitrogen gas pressure, after the air distance through 200mm, at the uniform velocity immerses in 60 ℃ of dimethylacetylamide aqueous coagulation baths; The speed with 100m/min stretches in the coagulating bath outside, gets the Kynoar hollow-fibre membrane of moulding; The Kynoar hollow-fibre membrane of moulding is extracted, protects the hole post processing with sodium lactate aqueous solution with sodium carbonate, get Kynoar hollow-fibre membrane finished product.
Embodiment 3:
1 part of 80 parts of lauryl sodium sulfate of 15 parts of dimethyl formamides of Kynoar
1 part of 2 parts of cellulose acetate of 2 parts of lithium nitrates of polyethylene glycol
Above-mentioned Kynoar, dimethyl formamide, lauryl sodium sulfate, polyethylene glycol, lithium nitrate, cellulose acetate are added in the stirred tank, and 70 ℃ of following agitating heating blend, mixing speed is 90r/min, and mixing time is 1h; Blended liquid is left standstill 1h carry out the deaeration processing, and cool to 40 ℃, get casting solution; Casting solution is extruded through spinning nozzle with the dimethylacetylamide aqueous solution under nitrogen gas pressure, at the uniform velocity immerses in 30 ℃ of aqueous coagulation baths; The speed with 10m/min stretches in the coagulating bath outside, gets the Kynoar hollow-fibre membrane of moulding; The Kynoar hollow-fibre membrane of moulding is extracted, protects the hole post processing with sodium lactate aqueous solution with hydrochloric acid, get Kynoar hollow-fibre membrane finished product.
Embodiment 4:
1 part of 55 parts of lauryl sodium sulfate of 23 parts of dimethyl formamides of Kynoar
12 parts of 1 part of cellulose acetates of 8 parts of lithium nitrates of polyethylene glycol
Above-mentioned Kynoar, dimethyl formamide, lauryl sodium sulfate, polyethylene glycol, lithium nitrate, cellulose acetate are added in the stirred tank, and 80 ℃ of following agitating heating blend, mixing speed is 90r/min, and mixing time is 1h; Blended liquid is left standstill 1h carry out the deaeration processing, and cool to 76 ℃, get casting solution; Casting solution is extruded through spinning nozzle with the dimethylacetylamide aqueous solution under nitrogen gas pressure, at the uniform velocity immerses in 30 ℃ of aqueous coagulation baths; The speed with 10m/min stretches in the coagulating bath outside, gets the Kynoar hollow-fibre membrane of moulding; The Kynoar hollow-fibre membrane of moulding is extracted, protects the hole post processing with sodium lactate aqueous solution with hydrochloric acid, get Kynoar hollow-fibre membrane finished product.
According to the set of dispense of embodiment 1～embodiment 4 than and the performance of the Kynoar hollow-fibre membrane for preparing of process conditions following:
Conclusion: according to the set of dispense of embodiment 4 when technology prepare, the practical application effect of the prepared Kynoar hollow-fibre membrane that obtains is best, and the initial permeation flux of pure water is maximum, it is the most even to separate the aperture, fracture pressure is maximum.
Solvent dimethyl formamide described in the embodiment 1～4 can be used one or more replacements in dimethyl formamide, dimethylacetylamide, dimethyl sulfoxide (DMSO), N-methyl pyrrolidone, the triethyl phosphate; Described surfactant lauryl sodium sulfate can be used one or more replacements in lauryl sodium sulfate, neopelex, sodium dodecyl aminopropionitrile, the Tweens series; Described Tweens series comprises soil temperature-20; Soil temperature-40, soil temperature-60 and soil temperature-80; Described polymeric additive polyethylene glycol can be used one or more replacements in polyethylene glycol, polyvinylpyrrolidone, polyvinyl alcohol, polyoxyethylene, the methylcellulose; Described inorganic additive lithium nitrate can be used one or more replacements in lithium nitrate, lithium chloride, calcium chloride, calcium carbonate, calcium nitrate, silica, the kaolin; Described modified blends cellulose acetate can be used one or more replacements in cellulose acetate, methyl methacrylate, vinyl acetate, polyvinyl alcohol, acrylic acid ester, maleic anhydride, the polyvinyl butyral resin.
Claims (10)
1. a Kynoar hollow-fibre membrane is characterized in that, calculates by weight, and it is mainly processed by following component:
1～3 part in 50～80 parts of surfactants of 15～25 parts of solvents of Kynoar
1～12 part of 1～8 part of modified blends of 2～12 parts of inorganic additives of polymeric additive.
2. Kynoar hollow-fibre membrane according to claim 1 is characterized in that, calculates by weight, and it is mainly processed by following component:
1 part in 55 parts of surfactants of 23 parts of solvents of Kynoar
12 parts of 1 part of modified blends of 8 parts of inorganic additives of polymeric additive.
3. Kynoar hollow-fibre membrane according to claim 1 is characterized in that, described solvent is one or more in dimethyl formamide, dimethylacetylamide, dimethyl sulfoxide (DMSO), N-methyl pyrrolidone, the triethyl phosphate.
4. according to claim 1,2 or 3 described Kynoar hollow-fibre membranes; It is characterized in that described surfactant is one or more in lauryl sodium sulfate, neopelex, sodium dodecyl aminopropionitrile, soil temperature-20, soil temperature-40, soil temperature-60, the soil temperature-80.
5. Kynoar hollow-fibre membrane according to claim 4 is characterized in that, described polymeric additive is one or more in polyethylene glycol, polyvinylpyrrolidone, polyvinyl alcohol, polyoxyethylene, the methylcellulose.
6. according to claim 1 or 5 described Kynoar hollow-fibre membranes, it is characterized in that described inorganic additive is one or more in lithium nitrate, lithium chloride, calcium chloride, calcium carbonate, calcium nitrate, silica, the kaolin.
7. Kynoar hollow-fibre membrane according to claim 6; It is characterized in that described modified blends is one or more in cellulose acetate, methyl methacrylate, vinyl acetate, polyvinyl alcohol, acrylic acid ester, maleic anhydride, the polyvinyl butyral resin.
8. the preparation method of the arbitrary described Kynoar hollow-fibre membrane of claim 1～7; It is characterized in that; Comprise: Kynoar, solvent, surfactant, polymeric additive, inorganic additive, modified blends are added in the stirred tank; 70～100 ℃ of following agitating heating blend, mixing speed is 90～120r/min, and mixing time is 1～6h; Blended liquid is left standstill 1～6h carry out the deaeration processing, and cool to 40～80 ℃, get casting solution; Casting solution is extruded through spinning nozzle with spinning core liquid under nitrogen gas pressure, after the air distance through 0～200mm, at the uniform velocity immerses in 30～60 ℃ of outer solidification liquid coagulating baths; The speed with 10～100m/min stretches in the coagulating bath outside, gets the Kynoar hollow-fibre membrane of moulding; The Kynoar hollow-fibre membrane of moulding is extracted, protects the hole post processing, get Kynoar hollow-fibre membrane finished product.
9. the preparation method of Kynoar hollow-fibre membrane according to claim 8 is characterized in that, described spinning core liquid is the water or the dimethylacetylamide aqueous solution; Outer solidification liquid is the water or the dimethylacetylamide aqueous solution.
10. according to Claim 8 or the preparation method of 9 described Kynoar hollow-fibre membranes, it is characterized in that the used extractant of post processing is hydrochloric acid or sodium carbonate, used guarantor hole agent is glycerine or sodium lactate aqueous solution.
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| CN103657446A (en) * | 2013-12-17 | 2014-03-26 | 常熟丽源膜科技有限公司 | Polyvinylidene fluoride hollow-fiber membrane |
| CN103757736A (en) * | 2013-12-31 | 2014-04-30 | 马海燕 | Large-diameter melt-spun polyvinylidene fluoride monofilament and production method thereof |
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