CN102389718A - Preparation method of acetyl cellulose hollow fiber nano filter membrane - Google Patents
Preparation method of acetyl cellulose hollow fiber nano filter membrane Download PDFInfo
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- CN102389718A CN102389718A CN2011102972790A CN201110297279A CN102389718A CN 102389718 A CN102389718 A CN 102389718A CN 2011102972790 A CN2011102972790 A CN 2011102972790A CN 201110297279 A CN201110297279 A CN 201110297279A CN 102389718 A CN102389718 A CN 102389718A
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Abstract
The invention relates to a high polymer separation membrane, in particular to a preparation method of a high-performance acetyl cellulose hollow fiber nano filter membrane, which is characterized by comprising: immersing acetyl cellulose hollow fiber reverse osmosis membrane in aqueous solution of sodium hydroxide, washing with water, immersing in solution of chloroacetic acid, washing with water and obtaining the hollow fiber nano filter membrane. In the invention, by treating the acetyl cellulose hollow fiber reverse osmosis membrane with solution of sodium hydroxide and chloroacetic acid, the penetration flux and selective separation performance of the acetyl cellulose hollow fiber reverse osmosis membrane are improved greatly, and the membrane has high nano filtration separation performance. The membrane also has the characteristics of simple preparation method, readily available raw materials, and low manufacturing cost. The membrane can be used in water treatment and various kinds of special separation, and expands the use of the nano filter membrane into more fields.
Description
Technical field
The present invention relates to a kind of polymeric membrane for separation, specifically be meant a kind of preparation method of high performance cellulose acetate hollow fiber nanofiltration membrane.
Technical background
NF membrane is a kind of novel diffusion barrier of aperture between reverse osmosis membrane and milipore filter; Because how electrically charged it have on nano level membrane aperture, the film; Allow low organic matter and the multivalent ion of alite that divide, have unique separating property, higher separation accuracy through holding back higher molecular weight.Compare with other diffusion barrier, NF membrane has that membrane flux is bigger, the process infiltration forces down, selects isolating ions, operating pressure power low, system to require characteristics such as low.At present, the NF membrane technology be widely used in water softening and brackish water desalination, drink water purifying, feed separation purifying and concentrate, wastewater treatment and fields such as middle water reuse, cleaner production, obtained good economic and social benefit.
The NF membrane kind mainly contains two kinds of composite construction NF membrane and dissymmetrical structure NF membrane by the structure branch; The former deposits to suitable micropore support membrane surface, aperture with one deck ultrathin functional layer, and depositional mode mainly contains surface-coated, and interfacial polycondensation and in-situ polymerization etc. adopt the post forming method to prepare usually; The latter directly adopts the solution phase inversion, prepares through once moulding method.Compare with the dissymmetrical structure NF membrane, the composite construction NF membrane has the following advantages: (1) supporting layer and compound separating layer can be optimized respectively, thereby reach optimum performance; (2) can some membrane materials that is difficult to form dissymmetrical structure be prepared nanofiltration; (3) permeation flux and selection separating property are usually above the dissymmetrical structure NF membrane.
At present, business-like NF membrane mostly is the NF membrane of composite construction, normally on porous support membranes such as polysulfones, is prepared from through the interfacial polycondensation between polyamine and the polynary acyl chlorides.For example; Fibiger etc. are at US Patent4 in 1987, in 769,148; Earlier prepare porous support membrane through the solution phase inversion; Then on porous support membrane surface, through for to contain the aqueous phase solution of piperazine function monomer and wetting agent, and the interfacial polymerization that contains between the crosslinking agent pyromellitic trimethylsilyl chloride organic phase solution prepares the composite construction NF membrane.Cadotte etc. adopt three-step approach to prepare the composite construction NF membrane in US Patent 4,812,270 in 1989; At first prepare the supporting layer of perforated membrane as the composite construction NF membrane, then through interfacial polymerization in the compound last layer separating layer of porous film surface, through strong acid treatment technology lamination layer structure and performance are regulated and control at last, obtain the composite construction NF membrane.The water that interfacial polymerization is adopted is the aqueous solution that contains m-phenylene diamine (MPD) function monomer and wetting agent, and organic facies contains the crosslinking agent pyromellitic trimethylsilyl chloride.In addition, patent US Patent 5,152,901, US Patent 5; 693,227, US Patent 6,123,804, US Patent6; 464,873, US Patent6,536,605, US Patent 6; 878,278 grades also are to adopt two-step process, through preparing the composite construction NF membrane at the polyamine of porous film surface and the interface polymerization reaction between the polynary acyl chlorides.
But, comparing with the one-step shaping technology of dissymmetrical structure NF membrane, the post forming method preparation technology of composite construction NF membrane makes its manufacturing cost higher relatively, has seriously restricted the actual of composite construction NF membrane and has applied.In addition, the antipollution of the polyamide-based composite nanometer filtering film that generally uses at present and the poor-performing of the microbial inoculum of anti-the chlorbenside cause the service life of such film shorter, have reduced the operational efficiency of such film.
Summary of the invention
The present invention is directed to deficiency of the prior art, provide a kind of raw material be easy to get, cheap, be easy to the cellulose acetate hollow fiber nanofiltration membrane for preparing, select separating property superior.
The present invention is achieved through following technical proposals:
A kind of preparation method of cellulose acetate hollow fiber nanofiltration membrane is characterized in that, cellulose acetate doughnut reverse osmosis membrane is soaked in sodium hydrate aqueous solution; After water washing; In chloroacetic acid solution, soak again, and then use water washing, obtain hollow fiber nanofiltration membrane;
Above-mentioned cellulose acetate doughnut reverse osmosis membrane is to get with the preparation of gel spinning method; Be specially: at first cellulose diacetate and the Triafol T with drying is 1 by mass ratio: the mixed of 4-6 is even; To join with the sulfolane be primary plasticizer, be that main additive is formed mixed solution with polyethylene glycol; The quality of control cellulose acetate mixture accounts between the 30-40wt% of mixed solution quality; Sulfolane accounts for the 65-55% of mixed solution quality, and polyethylene glycol accounts for 5% of mixed solution quality; Mixed solution is warming up to 120-150 ℃, stirs after 3-6 hour cooling section discharging rapidly, material is deposited in the closed container, at room temperature deposit more than 12 hours, material to be mixed is fully lax to get final product spinning membrane system with the pellet surface after inviscid; Membrane equipment adopts extruder type spinning machine, spinning temperature between 180-230 ℃, spinning speed 250-400 rice/minute between, coagulation bath temperature is between 10-40 ℃; The hollow-fibre membrane silk of preparation can obtain the cellulose acetate doughnut reverse osmosis membrane of aperture between 0.1-1.0nm after washing and 40-90 ℃ heat treatment; The concentration of above-mentioned sodium hydrate aqueous solution is 0.01-2.0mol/L, and the control temperature is 5-50 ℃, and soak time is 1-120 minute; The mass concentration of above-mentioned chloroacetic acid solution is 0.01-10.0wt%, and temperature is 5-45 ℃, and soak time is 1-300 minute.
As preferably, the preparation method of above-mentioned cellulose acetate hollow fiber nanofiltration membrane, the aperture of described cellulose acetate doughnut reverse osmosis membrane is between 0.3-0.5nm.
As preferably, the preparation method of above-mentioned cellulose acetate hollow fiber nanofiltration membrane, the concentration of described sodium hydrate aqueous solution are 0.05-1.0mol/L, and temperature is 25-40 ℃, and soak time is 40-60 minute.
As preferably, the preparation method of above-mentioned cellulose acetate hollow fiber nanofiltration membrane, the concentration of described chloroacetic acid solution are 0.5-2.0wt%, and temperature is 25-40 ℃, and soak time is 30-100 minute.
Beneficial effect: compare with prior art; The present invention is through handling with sodium hydroxide solution and chloroacetic acid solution Dichlorodiphenyl Acetate cellulose hollow fiber reverse osmosis membrane; Make the permeation flux of cellulose acetate doughnut reverse osmosis membrane improve greatly with the selection separating property; Have good nanofiltration separation characteristic, the selection separating property and the permeance property of the high-performance cellulose acetate hollow fiber nanofiltration membrane of invention are not less than existing NF membrane.The present invention has also that the preparation method is simple, raw material is easy to get, the characteristics of low cost of manufacture.The present invention not only can be applicable to water treatment, but also can be applicable to various special separation field, is the wider field of the application extension of NF membrane.
The specific embodiment
Specify in the face of enforcement of the present invention down:
Following examples provide explanation, preparation method and their separating property of high-performance cellulose acetate hollow fiber nanofiltration membrane.Yet these embodiment only provide as explanation rather than limit the present invention.
Cellulose acetate doughnut reverse osmosis membrane preparation: adopt the gel spinning method to prepare cellulose acetate doughnut reverse osmosis membrane; In the present invention, at first fully dry cellulose diacetate (CA) and Triafol T (CTA) mixed by a certain percentage, to join with the sulfolane be primary plasticizer, be main additive with polyethylene glycol (PEG); The content of control cellulose acetate is between 30-40wt%; Be warming up to 120-150 ℃, fully stir cooling section discharging rapidly after 3-6 hour, material is deposited in the closed container; At room temperature deposit more than 12 hours, material to be mixed is fully lax to get final product spinning membrane system with the pellet surface after inviscid.Membrane equipment adopts extruder type spinning machine, spinning temperature between 180-230 ℃, spinning speed 250-400 rice/minute between, coagulation bath temperature is between 10-40 ℃.The hollow-fibre membrane silk of preparation is through fully obtaining the cellulose acetate doughnut reverse osmosis membrane of aperture between 0.1-1.0nm after washing and the heat treatment (40-90 ℃).
The preparation of cellulose acetate hollow fiber nanofiltration membrane:
Cellulose acetate doughnut reverse osmosis membrane with hygrometric state; Be immersed in earlier in the sodium hydrate aqueous solution of finite concentration and temperature and be hydrolyzed; Take out clean behind the certain hour with the clear water rinsing; And then the cellulose acetate hollow-fibre membrane after the hydrolysis is immersed in the chloroacetic acid solution of finite concentration and temperature, take out behind the certain hour and film is thoroughly washed with distilled water, can obtain the cellulose acetate hollow fiber nanofiltration membrane.Wherein, the concentration of sodium hydrate aqueous solution is 0.01-2.0mol/L, and temperature is 5-50 ℃, and soak time is 1-120 minute; The concentration of chloroacetic acid solution is 0.01-10.0wt%, and temperature is 5-45 ℃, and soak time is 1-300 minute.
The doughnut membrane separating property is estimated: solute removal efficiency and water flux are two important parameters estimating doughnut counter-infiltration/nano filter membrane separating property.Through the cross-flow permeability test, the sodium chloride removal efficiency of Dichlorodiphenyl Acetate cellulose hollow fiber film, sodium sulphate removal efficiency and water flux etc. separate performance evaluation.
Solute removal efficiency (R) is defined as: under certain operating condition, and feeding liquid solute concentration (C
f) with penetrating fluid in solute concentration (C
p) poor, again divided by the feeding liquid solute concentration.Concrete computing formula is following:
Water flux (F) is defined as: under certain operating condition, see through the volume (V) of the water of elementary membrane area (A) in the unit interval (t), its unit is l/m
2.h.Concrete computing formula is following:
The operating condition that doughnut membrane separating property mensuration adopts among the present invention is: feed liquor is sodium-chloride water solution or the aqueous sodium persulfate solution of 500mg/l, and operating pressure is 1.0MPa, and operating temperature is 25 ℃, and pH value of solution is 6.8.
Embodiment 1-3
Adopt the cellulose acetate doughnut reverse osmosis membrane in the different apertures of gel spinning prepared; Concrete parameter is following: adopt CTA (combining acid number 60-62.5%) and CA (combining acid number 50-55%) mixing vinegar acid cellulose (CTA/CA=5/1), sulfolane and PEG preparation cellulose acetate frozen glue; Be respectively concrete the composition; 38.0wt% CTA/CA+57.0wt% sulfolane+5.0wt%PEG, 35.0wt%CTA/CA+60.0wt% sulfolane+5.0wt%PEG, 33.0wt%CTA/CA+62.0wt% sulfolane+5.0wt%PEG; Between 195-200 ℃, carry out spinning, coagulating bath and heat treatment temperature are respectively 35.0 ℃ and 70.0 ℃.
Cellulose acetate doughnut reverse osmosis membrane with aforementioned preparation; Be immersed in 25 ℃ earlier, contain in the aqueous solution of 0.5mol/L NaOH 30 minutes; Take out with after the clear water washes clean; Be immersed in 25 ℃, the chloroacetic acid solution of 0.5wt% 30 minutes, the hollow-fibre membrane rinsing after will handling with pure water at last is clean again.The NF membrane of preparation is used sodium-chloride water solution and the aqueous sodium persulfate solution of 500mg/l respectively, 1.0MPa, 25 ℃, pH 6.8 times, and the solute removal efficiency and the water flux of test membrane, the result sees table 1.These several embodiment investigate cellulose acetate doughnut reverse osmosis membrane aperture to prepared hollow fiber nanofiltration membrane Effect on Performance.
Table 1 embodiment 1-3
Embodiment 4-8
Except the concentration difference of sodium hydrate aqueous solution; Adopt with embodiment 1 identical operations condition and prepare the cellulose acetate hollow fiber nanofiltration membrane; Adopt the performance of testing prepared NF membrane with embodiment 1 identical method of testing then, its result sees table 2.These several embodiment investigate concentration of sodium hydroxide solution to prepared hollow fiber nanofiltration membrane Effect on Performance.
Table 2 embodiment 4-8
Embodiment 9-13
Except the temperature difference of sodium hydrate aqueous solution; Adopt with embodiment 1 identical operations condition and prepare the cellulose acetate hollow fiber nanofiltration membrane; Adopt the performance of testing prepared NF membrane with embodiment 1 identical method of testing then, its result sees table 3.These several embodiment investigate the sodium hydroxide solution temperature to prepared hollow fiber nanofiltration membrane Effect on Performance.
Table 3 embodiment 9-13
Embodiment 14-18
Except the soak time difference of sodium hydrate aqueous solution; Adopt with embodiment 1 identical operations condition and prepare the cellulose acetate hollow fiber nanofiltration membrane; Adopt the performance of testing prepared NF membrane with embodiment 1 identical method of testing then, its result sees table 4.These several embodiment investigate the sodium hydroxide solution soak time to prepared hollow fiber nanofiltration membrane Effect on Performance.
Table 4 embodiment 14-18
Embodiment 19-23
Except the concentration difference of chloroacetic acid solution, adopt with embodiment 1 identical operations condition and prepare the cellulose acetate hollow fiber nanofiltration membrane, adopt the performance of testing prepared NF membrane with embodiment 1 identical method of testing then, its result sees table 5.These several embodiment investigate chloroacetic acid solution concentration to prepared hollow fiber nanofiltration membrane Effect on Performance.
Table 5 embodiment 19-23
Embodiment 24-28
Except the temperature difference of chloroacetic acid solution, adopt with embodiment 1 identical operations condition and prepare the cellulose acetate hollow fiber nanofiltration membrane, adopt the performance of testing prepared NF membrane with embodiment 1 identical method of testing then, its result sees table 6.These several embodiment investigate the chloroacetic acid solution temperature to prepared hollow fiber nanofiltration membrane Effect on Performance.
Table 6 embodiment 24-28
Embodiment 29-33
Except the processing time difference of chloroacetic acid solution; Adopt with embodiment 1 identical operations condition and prepare the cellulose acetate hollow fiber nanofiltration membrane; Adopt the performance of testing prepared NF membrane with embodiment 1 identical method of testing then, its result sees table 7.These several embodiment investigate the chloroacetic acid solution processing time to prepared hollow fiber nanofiltration membrane Effect on Performance.
Table 7 embodiment 29-33
Claims (4)
1. the preparation method of a cellulose acetate hollow fiber nanofiltration membrane is characterized in that, cellulose acetate doughnut reverse osmosis membrane is soaked in sodium hydrate aqueous solution; After water washing; In chloroacetic acid solution, soak again, and then use water washing, obtain hollow fiber nanofiltration membrane;
Above-mentioned cellulose acetate doughnut reverse osmosis membrane is to get with the preparation of gel spinning method; Be specially: at first cellulose diacetate and the Triafol T with drying is 1 by mass ratio: the mixed of 4-6 is even; To join with the sulfolane be primary plasticizer, be that main additive is formed mixed solution with polyethylene glycol; The quality of control cellulose acetate mixture accounts between the 30-40wt% of mixed solution quality; Sulfolane accounts for the 65-55% of mixed solution quality, and polyethylene glycol accounts for 5% of mixed solution quality; Mixed solution is warming up to 120-150 ℃, stirs after 3-6 hour cooling section discharging rapidly, material is deposited in the closed container, at room temperature deposit more than 12 hours, material to be mixed is fully lax to get final product spinning membrane system with the pellet surface after inviscid; Membrane equipment adopts extruder type spinning machine, spinning temperature between 180-230 ℃, spinning speed 250-400 rice/minute between, coagulation bath temperature is between 10-40 ℃; The hollow-fibre membrane silk of preparation can obtain the cellulose acetate doughnut reverse osmosis membrane of aperture between 0.1-1.0nm after washing and 40-90 ℃ heat treatment;
The concentration of above-mentioned sodium hydrate aqueous solution is 0.01-2.0mol/L, and the control temperature is 5-50 ℃, and soak time is 1-120 minute;
The mass concentration of above-mentioned chloroacetic acid solution is 0.01-10.0wt%, and temperature is 5-45 ℃, and soak time is 1-300 minute.
2. the preparation method of a kind of cellulose acetate hollow fiber nanofiltration membrane according to claim 1 is characterized in that, the aperture of described cellulose acetate doughnut reverse osmosis membrane is between 0.3-0.5nm.
3. the preparation method of a kind of cellulose acetate hollow fiber nanofiltration membrane according to claim 1 is characterized in that, the concentration of described sodium hydrate aqueous solution is 0.05-1.0mol/L, and temperature is 25-40 ℃, and soak time is 40-60 minute.
4. the preparation method of a kind of cellulose acetate hollow fiber nanofiltration membrane according to claim 1 is characterized in that, the concentration of described chloroacetic acid solution is 0.5-2.0wt%, and temperature is 25-40 ℃, and soak time is 30-100 minute.
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Cited By (6)
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| CN103831023A (en) * | 2014-03-14 | 2014-06-04 | 清华大学 | Preparation method of hollow cellulose acetate fiber nanofiltration membrane |
| CN105597551A (en) * | 2015-10-16 | 2016-05-25 | 福建农林大学 | Production method of regenerated cellulose nanofiltration membrane |
| CN105879697A (en) * | 2014-12-16 | 2016-08-24 | 天津工业大学 | Preparation method of environment-protective cellulose-acetate hollow fiber nanofiltration membrane |
| CN109647205A (en) * | 2018-12-27 | 2019-04-19 | 天津膜天膜科技股份有限公司 | A method of improving hollow fiber nanofiltration membrane chlorine resistance |
| CN110295406A (en) * | 2019-06-18 | 2019-10-01 | 浙江理工大学 | Porous cellulose acetate composite micro/nano tunica fibrosa, centrifugal spinning preparation method and its application at heavy metal ion adsorbed aspect |
| CN112657347A (en) * | 2020-12-16 | 2021-04-16 | 杭州科百特科技有限公司 | Regenerated cellulose ultrafiltration membrane and application and preparation method thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103831023A (en) * | 2014-03-14 | 2014-06-04 | 清华大学 | Preparation method of hollow cellulose acetate fiber nanofiltration membrane |
| CN103831023B (en) * | 2014-03-14 | 2016-08-17 | 清华大学 | A kind of preparation method of acetyl cellulose hollow fiber nano filter membrane |
| CN105879697A (en) * | 2014-12-16 | 2016-08-24 | 天津工业大学 | Preparation method of environment-protective cellulose-acetate hollow fiber nanofiltration membrane |
| CN105597551A (en) * | 2015-10-16 | 2016-05-25 | 福建农林大学 | Production method of regenerated cellulose nanofiltration membrane |
| CN105597551B (en) * | 2015-10-16 | 2019-05-10 | 福建农林大学 | A kind of preparation method of regenerated cellulose nanofiltration membrane |
| CN109647205A (en) * | 2018-12-27 | 2019-04-19 | 天津膜天膜科技股份有限公司 | A method of improving hollow fiber nanofiltration membrane chlorine resistance |
| CN110295406A (en) * | 2019-06-18 | 2019-10-01 | 浙江理工大学 | Porous cellulose acetate composite micro/nano tunica fibrosa, centrifugal spinning preparation method and its application at heavy metal ion adsorbed aspect |
| CN112657347A (en) * | 2020-12-16 | 2021-04-16 | 杭州科百特科技有限公司 | Regenerated cellulose ultrafiltration membrane and application and preparation method thereof |
| CN112657347B (en) * | 2020-12-16 | 2022-11-29 | 杭州科百特科技有限公司 | Regenerated cellulose ultrafiltration membrane and application and preparation method thereof |
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Application publication date: 20120328 |