CN105396473A - Preparation method of temperature/pH-responsive cellulose acetate membrane and application of membrane - Google Patents
Preparation method of temperature/pH-responsive cellulose acetate membrane and application of membrane Download PDFInfo
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- CN105396473A CN105396473A CN201510982664.7A CN201510982664A CN105396473A CN 105396473 A CN105396473 A CN 105396473A CN 201510982664 A CN201510982664 A CN 201510982664A CN 105396473 A CN105396473 A CN 105396473A
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- 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
- B01D71/76—Macromolecular material not specifically provided for in a single one of groups B01D71/08 - B01D71/74
- B01D71/80—Block polymers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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Abstract
The invention relates to a preparation method of a temperature/pH-responsive cellulose acetate membrane and an application of the membrane. The temperature/pH-responsive cellulose acetate membrane is prepared by modification of F127-b-PDMAEMA synthesized by F127(PEO100-PPO65-PEO100) and polymethylacrylic acid-N,N-dimethylamino ethyl ester (PDMAEMA). According to the prepared temperature/pH-responsive cellulose acetate membrane, pore size of the membrane can be adjusted by changing temperature and pH of the system. Adjustable range of temperature is 10-80 DEG C, and adjustable range of pH is 2-14. Within the temperature and pH ranges, maximum water-flux variation of the modified membrane is 100 L/m<2>h. The prepared temperature/pH-responsive cellulose acetate membrane has strong hydrophilicity and strong anti-pollution capacity, is environmentally friendly and low-cost, and is suitable for large-scale production.
Description
Technical field
The present invention relates to modified block polymer F127-b-PDMAEMA and the temperature prepared by immersion precipitation phase inversion process, the pH response CAM of the synthesis of regeneration activator ATRP (ARGETATRP) method.And test the pore size of this film under different temperatures, pH, specific targets are the water flux under different temperatures, pH condition.
Background technology
Membrane separation process is a kind of new separation technology grown up over nearly 20 years, has the advantage such as outstanding transmitting selective and low energy consumption.Membrane technology, due to the advantage such as practical, efficient, energy-conservation, technique is simple and adjustable, is widely used, creates very high economic benefit in modern Economy Development and people's daily life.
Along with the progress of science and technology and the mankind are to the understanding of autonomous mechanism, people more and more favor in intelligence, have mechanism from main response and equipment, therefore for the common film with separating effect, people can not meet, and people wish to obtain a kind of film that can change performance according to the difference of system factor.Therefore carry out functionalization and intellectuality to membrane material, develop and the film responded can be stimulated to external world to become inexorable trend, this film is called as intelligent film material or environmental response type film material.The structure of intelligent membrane material, effective aperture, the flux of film and the performance of film can change along with the change of environmental stimuli as optical, electrical, temperature, pH, chemical factor etc., thisly not only take into account conventional film material advantage but also the feature responded can be stimulated to external world, impel smart membrane material to become a kind of novel functional membrane material.Smart membrane has broad application prospects in the field such as analysis detection, separating-purifying, insoluble drug release, artificial organs of material.
In order to the needs of problems of the mankind to response film can be solved, need to carry out modification to traditional film.Synthesis has the modified material of response, and by itself and the blended system of the membrane material method of modifying for the easiest a kind of film of Modified Membrane.F127-b-PDMAEMA is a kind of amphipathic polymer, and wherein F127 is the PEO synthesized by polyethylene oxide and polyoxy propane
100-PPO
65-PEO
100amphipathic nature polyalcohol.PEO has hydrophily, can improve the hydrophilicity of film; PPO has hydrophobicity, can be cross-linked with film basic material well, improves the fastness of modified material in film.PDMAEMA is polymethylacrylic acid N, N-dimethylaminoethyl, it is the material of a kind of temperature, pH response, itself and F127 are prepared modified block polymer F127-b-PDMAEMA by the copolymerization of regeneration activating Transfer Radical Polymerization, the hydrophilicity of film and the fastness of modified material can not only be improved, film can also be made to have temperature, pH response.Again because cellulose acetate has aboundresources, hydrophily is high and filming performance is good advantage, the CAM of therefore preparation F127-b-PDMAEMA modification has good prospect.
Summary of the invention:
Technical problem: the object of the invention is to solve the problems such as traditional cellulose acetate membrane aperture is single, non-responsiveness, hydrophily are poor, contamination resistance is weak, provides a kind of temperature, the preparation method of CAM of pH response and the application of this film.
Summary of the invention: for solving the problems of the technologies described above, the invention provides the preparation method of CAM of a kind of temperature, pH value response, modified block polymer F127-b-PDMAEMA is prepared, by the CAM that itself and cellulose acetate are responded by immersion precipitation phase inversion process preparation temperature and pH by regeneration activating Transfer Radical Polymerization; And by the temperature of regulation system and the pore size of pH test membrane; This preparation method comprises the following steps:
Step 1: synthesis initator F127-Br: getting F127, acylbromide and triethylamine that mol ratio is 1:2:2-1:100:100, take carrene as solvent, and stirring reaction 2-48h obtains product initator F127-Br after process;
Step 2: synthesis F127-b-PDMAEMA: initator F127-Br, monomer DMAEMA, Catalysts Cu Br
2, part five methyl diethylentriamine PMDETA, add in reactor according to the mol ratio of 1:50-200:001-1:001-1, add solvent methanol, treat to dissolve completely, air in removing reactor, then adds in above-mentioned reactor by the reducing agent dissolved, and device seals, stirring reaction 2-48h at 20-80 DEG C, removal of impurities, obtains F127-b-PDMAEMA;
Step 3: the CAM of preparation temperature, pH response: the cellulose acetate getting F127-b-PDMAEMA and 4-10g of 0.1g-1g, is dissolved in 20-70gDMF, deaeration, film forming;
Step 4: the Modified Membrane of preparation is applied to different temperature and pH system.
Preferably, there is temperature, the film of pH response is the CAM of F127-b-PDMAEMA modification.
Present invention also offers a kind of be made up of said method temperature, pH response the application of CAM, the pore size of CAM and the size of water flux is changed by the temperature, the pH that change system, temperature adjustable extent is 10-80 DEG C, pH adjustable extent is 2-14.
Beneficial effect:
The present invention compared with prior art, has the following advantages:
1. the cheaper starting materials of the inventive method, reaction condition is gentle, production cost is low, is applicable to large-scale production
2. temperature prepared by the present invention, pH response CAM hydrophily is strong, contamination resistance strong, by the fenestra size changing system temperature, pH changes Modified Membrane.
Detailed description of the invention
The preparation method of the CAM of a kind of temperature provided by the invention, pH value response, modified block polymer F127-b-PDMAEMA is prepared, by the CAM that itself and cellulose acetate are responded by immersion precipitation phase inversion process preparation temperature and pH by regeneration activating Transfer Radical Polymerization; And by the temperature of regulation system and the pore size of pH test membrane; This preparation method comprises the following steps:
Step 1: synthesis initator F127-Br: getting F127, acylbromide and triethylamine that mol ratio is 1:2:2-1:100:100, take carrene as solvent, and stirring reaction 2-48h obtains product initator F127-Br after process;
Step 2: synthesis F127-b-PDMAEMA: initator F127-Br, monomer DMAEMA, Catalysts Cu Br
2, part five methyl diethylentriamine PMDETA, add in reactor according to the mol ratio of 1:50-200:001-1:001-1, add solvent methanol, treat to dissolve completely, air in removing reactor, then adds in above-mentioned reactor by the reducing agent dissolved, and device seals, stirring reaction 2-48h at 20-80 DEG C, removal of impurities, obtains F127-b-PDMAEMA;
Step 3: the CAM of preparation temperature, pH response: the cellulose acetate getting F127-b-PDMAEMA and 4-10g of 0.1g-1g, is dissolved in 20-70gDMF, deaeration, film forming;
Step 4: the Modified Membrane of preparation is applied to different temperature and pH system.
There is temperature, the film of pH response is the CAM of F127-b-PDMAEMA modification.
Present invention also offers the application of CAM of temperature that a kind of said method makes, pH response, the pore size of CAM and the size of water flux is changed by the temperature, the pH that change system, temperature adjustable extent is 10-80 DEG C, pH adjustable extent is 2-14.
The invention solves the problems such as general cellulose acetate membrane aperture is single, non-responsiveness.Described temperature, pH response CAM are with by F127 (PEO
100-PPO
65-PEO
100) and polymethylacrylic acid-N, N-dimethylaminoethyl (PDMAEMA) the F127-b-PDMAEMA modification of synthesizing prepare.Temperature prepared by the present invention, pH response CAM can regulate the pore size of film by change system temperature and pH, the adjustable range of temperature is 10
-80 DEG C, the adjustable extent of pH is 2-14.Within the scope of this temperature and pH, the maximum variable quantity of water flux of Modified Membrane is 100L/m
2h.And made temperature, pH response CAM have, and hydrophily is strong, contamination resistance strong, environmental friendliness, cost are low, is beneficial to large-scale production.
Embodiment 1: get 6gF127 and 0.3g acylbromide, at room temperature react 24h, obtains initator F127-Br, then removes the F127-Br6g synthesized, monomer DMAEMA15g, CuBr
2be 0.001g with part PMDETA, be dissolved in the methanol solution of 60g, inject the aqueous ascorbic acid of 3g in the condition bet of nitrogen bubble, at 60 DEG C, react 48h.Obtain the F127-b-PDMAEMA that molecular weight is 36500g/mol.Take the F127-b-PDMAEMA that 0.1g molecular weight is 36500g/mol, 5.9gCA is dissolved in the DMF of 40g, 60 DEG C of mechanical agitation are to dissolving completely, vacuumizing and defoaming 3h, above-mentioned casting solution is poured on smooth glass plate, scrapes with smooth ruler, place 10 seconds in atmosphere, then be immersed in coagulating bath (deionized water) gently, forming film with phase transformation method.Water flux test is carried out soak 24h in water after.First film precompressed 1h under 0.15MPa, under 0.1MPa, then test the pure water flux of 25 DEG C, 35 DEG C, 45 DEG C, 55 DEG C, 65 DEG C, 75 DEG C, water flux is respectively 60L/m
2h, 62L/m
2h, 65L/m
2h, 70L/m
2h, 75L/m
2h, 77L/m
2h, water flux increases 19L/m
2h; Then under 0.1MPa, test again pure water flux when pH is respectively 2,4,6,8,10,12,14, water flux is respectively 60L/m
2h, 63L/m
2h, 65L/m
2h, 70L/m
2h, 74L/m
2h, 77L/m
2h, 80L/m
2h.Water flux increases 20L/m
2h, film surface water contact angle is 74 °.
Embodiment 2: get 6gF127 and 0.3g acylbromide, at room temperature react 24h, obtains initator F127-Br, then removes the F127-Br6g synthesized, monomer DMAEMA15g, CuBr
2be 0.001g with part PMDETA, be dissolved in the methanol solution of 60g, inject the aqueous ascorbic acid of 3g in the condition bet of nitrogen bubble, at 60 DEG C, react 24h.Obtain the F127-b-PDMAEMA that molecular weight is 30000g/mol.Take the F127-b-PDMAEMA that 0.1g molecular weight is 30000g/mol, 5.8gCA is dissolved in the DMF of 40g, 60 DEG C of mechanical agitation are to dissolving completely, vacuumizing and defoaming 3h, above-mentioned casting solution is poured on smooth glass plate, scrapes with smooth ruler, place 10 seconds in atmosphere, then be immersed in coagulating bath (deionized water) gently, forming film with phase transformation method.Water flux test is carried out soak 24h in water after.First film precompressed 1h under 0.15MPa, under 0.1MPa, then test the pure water flux of 25 DEG C, 35 DEG C, 45 DEG C, 55 DEG C, 65 DEG C, 75 DEG C, water flux is respectively 57L/m
2h, 60L/m
2h, 65L/m
2h, 68L/m
2h, 70L/m
2h, 71L/m
2h, water flux increases 14L/m
2h; Then under 0.1MPa, test again pure water flux when pH is respectively 2,4,6,8,10,12,14, water flux is respectively 56L/m
2h, 59L/m
2h, 62L/m
2h, 67L/m
2h, 70L/m
2h, 72L/m
2h, 73L/m
2h.Water flux increases 17L/m
2h, film surface water contact angle is 78 °.
Embodiment 3: get 6gF127 and 0.3g acylbromide, at room temperature react 24h, obtains initator F127-Br, then removes the F127-Br6g synthesized, monomer DMAEMA15g, CuBr
2be 0.001g with part PMDETA, be dissolved in the methanol solution of 60g, inject the aqueous ascorbic acid of 3g in the condition bet of nitrogen bubble, at 60 DEG C, react 48h.Obtain the F127-b-PDMAEMA that molecular weight is 36500g/mol.Take the F127-b-PDMAEMA that 0.2g molecular weight is 36500g/mol, 5.7gCA is dissolved in the DMF of 40g, 60 DEG C of mechanical agitation are to dissolving completely, vacuumizing and defoaming 3h, above-mentioned casting solution is poured on smooth glass plate, scrapes with smooth ruler, place 10 seconds in atmosphere, then be immersed in coagulating bath (deionized water) gently, forming film with phase transformation method.Water flux test is carried out soak 24h in water after.First film precompressed 1h under 0.15MPa, under 0.1MPa, then test the pure water flux of 25 DEG C, 35 DEG C, 45 DEG C, 55 DEG C, 65 DEG C, 75 DEG C, water flux is respectively 90L/m
2h, 95L/m
2h, 120L/m
2h, 130L/m
2h, 135L/m
2h, 136L/m
2h, water flux increases 46L/m
2h; Then under 0.1MPa, test again pure water flux when pH is respectively 2,4,6,8,10,12,14, water flux is respectively 90L/m
2h, 94L/m
2h, 119L/m
2h, 132L/m
2h, 133L/m
2h, 139L/m
2h, 142L/m
2h.Water flux increases 52L/m
2h, film surface water contact angle is 63 °.
Embodiment 4: get 6gF127 and 0.3g acylbromide, at room temperature react 24h, obtains initator F127-Br, then removes the F127-Br6g synthesized, monomer DMAEMA15g, CuBr
2be 0.001g with part PMDETA, be dissolved in the methanol solution of 60g, inject the aqueous ascorbic acid of 3g in the condition bet of nitrogen bubble, at 60 DEG C, react 48h, obtain the F127-b-PDMAEMA that molecular weight is 36500g/mol.Take the F127-b-PDMAEMA that 0.3g molecular weight is 36500g/mol, 5.6gCA is dissolved in the DMF of 40g, 60 DEG C of mechanical agitation are to dissolving completely, vacuumizing and defoaming 3h, above-mentioned casting solution is poured on smooth glass plate, scrapes with smooth ruler, place 10 seconds in atmosphere, then be immersed in coagulating bath (deionized water) gently, forming film with phase transformation method.Water flux test is carried out soak 24h in water after.First film precompressed 1h under 0.15MPa, under 0.1MPa, then test the pure water flux of 25 DEG C, 35 DEG C, 45 DEG C, 55 DEG C, 65 DEG C, 75 DEG C, water flux is respectively 100L/m
2h, 110L/m
2h, 135L/m
2h, 150L/m
2h, 155L/m
2h, 160L/m
2h, water flux increases 60L/m
2h; Then under 0.1MPa, test again pure water flux when pH is respectively 2,4,6,8,10,12,14, water flux is respectively 100L/m
2h, 110L/m
2h, 119L/m
2h, 145L/m
2h, 150L/m
2h, 153L/m
2h, 154L/m
2h.Water flux increases 54L/m
2h, film surface water contact angle is 60 °.
Embodiment 5:
Get 6gF127 and 0.3g acylbromide, at room temperature react 24h, obtain initator F127-Br, then remove the F127-Br6g synthesized, monomer DMAEMA15g, CuBr
2be 0.001g with part PMDETA, be dissolved in the methanol solution of 60g, inject the aqueous ascorbic acid of 3g in the condition bet of nitrogen bubble, under the condition of 60 DEG C, react 48h.Obtain the F127-b-PDMAEMA that molecular weight is 36500g/mol.Take the F127-b-PDMAEMA that 0.7g molecular weight is 36500g/mol, 5.5gCA is dissolved in the DMF of 40g, 60 DEG C of mechanical agitation are to dissolving completely, vacuumizing and defoaming 3h, above-mentioned casting solution is poured on smooth glass plate, scrapes with smooth ruler, place 10 seconds in atmosphere, then be immersed in coagulating bath (deionized water) gently, forming film with phase transformation method.Water flux test is carried out soak 24h in water after.First film precompressed 1h under 0.15MPa, under 0.1MPa, then test the pure water flux of 25 DEG C, 35 DEG C, 45 DEG C, 55 DEG C, 65 DEG C, 75 DEG C, water flux is respectively 200L/m
2h, 215L/m
2h, 245L/m
2h, 260L/m
2h, 265L/m
2h, 270L/m
2h, water flux increases 70L/m
2h; Then under 0.1MPa, test again pure water flux when pH is respectively 2,4,6,8,10,12,14, water flux is respectively 202L/m
2h, 216L/m
2h, 227L/m
2h, 257L/m
2h, 266L/m
2h, 271L/m
2h.Water flux increases 69L/m
2h, film surface water contact angle is 49 °.
Claims (3)
1. the preparation method of the CAM of a temperature, pH value response, it is characterized in that: prepare modified block polymer F127-b-PDMAEMA by regeneration activating Transfer Radical Polymerization, by the CAM that itself and cellulose acetate are responded by immersion precipitation phase inversion process preparation temperature and pH; And by the temperature of regulation system and the pore size of pH test membrane; This preparation method comprises the following steps:
Step 1: synthesis initator F127-Br: getting F127, acylbromide and triethylamine that mol ratio is 1:2:2-1:100:100, take carrene as solvent, and stirring reaction 2-48h obtains product initator F127-Br after process;
Step 2: synthesis F127-b-PDMAEMA: initator F127-Br, monomer DMAEMA, Catalysts Cu Br
2, part five methyl diethylentriamine PMDETA, add in reactor according to the mol ratio of 1:50-200:001-1:001-1, add solvent methanol, treat to dissolve completely, air in removing reactor, then adds in above-mentioned reactor by the reducing agent dissolved, and device seals, stirring reaction 2-48h at 20-80 DEG C, removal of impurities, obtains F127-b-PDMAEMA;
Step 3: the CAM of preparation temperature, pH response: the cellulose acetate getting F127-b-PDMAEMA and 4-10g of 0.1g-1g, is dissolved in 20-70gDMF, deaeration, film forming;
Step 4: the Modified Membrane of preparation is applied to different temperature and pH system.
2. the preparation method of the CAM of temperature according to claim 1, pH value response, is characterized in that: have temperature, the film of pH response is the CAM of F127-b-PDMAEMA modification.
3. the application of the temperature that method is made according to claim 1 or 2, the CAM of pH response, it is characterized in that: change the pore size of CAM and the size of water flux by the temperature, the pH that change system, temperature adjustable extent is 10-80 DEG C, pH adjustable extent is 2-14.
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| CN107051235A (en) * | 2017-01-25 | 2017-08-18 | 东南大学 | A kind of preparation method and application of hydrophilic polyethersulfone milipore filter |
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Cited By (5)
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| CN106731909A (en) * | 2017-01-25 | 2017-05-31 | 东南大学 | A kind of water-oil separating poly (ether-sulfone) ultrafiltration membrane based on ATRP method and preparation method and application |
| CN107051235A (en) * | 2017-01-25 | 2017-08-18 | 东南大学 | A kind of preparation method and application of hydrophilic polyethersulfone milipore filter |
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Application publication date: 20160316 |