CN103537200B - A kind of Cellulose acetate forward osmotic membrane and preparation method thereof - Google Patents
A kind of Cellulose acetate forward osmotic membrane and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of Cellulose acetate forward osmotic membrane and preparation method thereof。This preparation adds the proportional arrangement raw material of the acetone of 20-40ml, the Isosorbide-5-Nitrae-dioxane of 50-70ml, 7-10ml methanol according to every 3-5g cellulose acetate, and adds the lactic acid of pore creating material 5-10ml or the zinc chloride of 0.8-28g；By raw material mix homogeneously, stirring at normal temperatures makes cellulose acetate be completely dissolved, and stands more than casting solution 12h；Sodium hydroxide solution immersion treatment；Being immersed in casting solution 30-60s, lift is once dipped into afterwards in deionized water and carries out inversion of phases 2-6h, obtains Cellulose acetate forward osmotic membrane, and middle basement membrane is polysulfone membrane, forms the cellulose acetate membrane in attachment in basement membrane both sides；Preparation method technique of the present invention is simple, and the forward osmosis membrane prepared can effectively stop solute to enter porous support layer, has good chemical stability, higher salt-stopping rate and membrane flux。
Description
Technical field
One forward osmosis membrane of the present invention, particularly relates to a kind of Cellulose acetate forward osmotic membrane and preparation method thereof, belongs to polymeric membrane for separation technical field。
Background technology
The consumption of quickly growth and the Fossil fuel of population makes water and the energy become most important two spike-type cultivars in the world。Water shortage and energy crisis annoying many areas in the world, it was reported that lack clean healthy drinking water more than 1,200,000,000 people in the world。Membrane separation technique normal-temperature operation, without phase transformation, be up-and-coming regenerating drinking water technology。
The positive infiltration technology that development in recent years is got up is a kind of technology utilizing penetration theory to carry out membrance separation, what the osmotic pressure difference utilizing film both sides solution made hydrone spontaneous passes through semipermeable membrane, from the material liquid that water chemistry gesture is higher penetrate into water chemistry gesture relatively low draw liquid, can be used for directly from sea water, extracting fresh water。Currently the only commercial forward osmosis membrane is the three cellulose acetate membrane (CTA) of HTI company of the U.S., and it is made up of active dense layer and polyester support, has higher membrane flux and salt-stopping rate。
In theory, just permeating and can realize the membrane flux bigger than reverse osmosis with the liquid that draws that osmotic pressure is significantly high, but research finds that actual membrane flux is much smaller than theoretical value, this is owing to commercial reverse osmosis membrane has serious dissymmetrical structure, very serious interior concentration polarization phenomenon is there is in active layer structure very fine and close causing in positive process of osmosis, cause effectively driving pressure to be substantially reduced, thus substantially reducing membrane flux。Owing to interior concentration polarization is present in fenestra, only alleviate by improving membrane structure and film properties, and the interior concentration polarization basic reason that forward osmosis membrane flux declines to a great extent just, often make membrane flux reduce by 80%。
Currently for interior concentration polarization phenomenon, effective precautions has increase supporting layer aperture, adopts hydroaropic substance prepare supporting layer or prepare double activated layer。Polysulfones ultrafiltration supports counterdie and has finger, advantageously reduces interior concentration polarization phenomenon, and modified hydrophilic polysulfone membrane more can improve membrane flux。Utilize hydrophilic cellulose acetate (CA) to prepare active layer, adopt the Cellulose acetate forward osmotic membrane that lactic acid prepares as pore creating material to have significantly high salt-stopping rate and membrane flux。
Current patent of invention has various different film-forming solute and solvent, additive etc. have been some explorations contrast experiment, the film-forming method adopted is all use scraper knifing, masking solute has CA, CTA, acetylbutyrylcellulose etc., and their comparison is complicated。Multiple additives and film-forming solute solvent have all been done discussion test by such as patent No. CN201210453553.3, its obtained film with deionized water as material liquid, the sodium chloride of 1mol/L is all not as high as obtained flux when drawing liquid experiment, and most high energy reaches 13.12L/m2.h, and the back-mixing flux of salt can reach 3.32g/m2.h。Patent No. CN201210137147.6 adopts the raw material of hypertoxicity, as polyamine solution and polynary solution of acid chloride react molding, with pure water as material liquid, the sodium chloride solution of 1mol/L is as when drawing liquid, and the membrane flux of obtained hollow-fibre membrane only reaches 5.97L/m2.h。Patent No. CN201310092067.8 first prepares hydrophilic carboxylated polysulphones hyperfiltration membrane to polysulfones is modified, on this ultrafilter membrane, in-situ polymerization generates polyamide forward osmosis membrane again, the method still adopts poisonous reagent m-diaminobenzene. and pyromellitic trimethylsilyl chloride as Material synthesis polyamide forward osmosis membrane, it is unfavorable for environmental protection, and using the sodium chloride of 2g/L as material liquid, the glucose of 2mol/L is as drawing under the experiment condition of liquid, and membrane flux is 13.9L/m2.h, salt-stopping rate only reaches 96.12%。Ultra-thin pair of cortex forward osmosis membrane obtained by patent No. CN201210578252.3 it adopt environmentally friendly Triafol T, cellulose diacetate as membrane-forming agent, 100um is reached at the thickness scraping out with scraper, when using 0.1mol/L sodium chloride as material liquid, 4mol/L glucose is as when drawing liquid experiment condition, and membrane flux is 12.8L/m2.h, salt-stopping rate reaches 96.8%。
Summary of the invention
An object of the present invention is to provide a kind of positive good hydrophilic property, and membrane flux is high, and salt-stopping rate is good, the Cellulose acetate forward osmotic membrane of good mechanical property。It is another object of the present invention to the preparation method that described Cellulose acetate forward osmotic membrane to be provided。
Masking solute used by profit of the present invention is the simple molecular weight cellulose acetate at 40000-50000, solvent is 1, the mixed solvent that 4-dioxane and acetone mix by a certain percentage, additive is single methanol, pore creating material have chosen different materials, according to a certain percentage after the uniform froth breaking of mixed dissolution, have employed simple dipping membrane formation, film forming thickness is uniform, obtained forward osmosis membrane is in positive permeability test when adopting identical material liquid and drawing liquid, and getable membrane flux reaches 17.17L/m2.h, salt-stopping rate reaches more than 99.999%, is highly suitable as the forward osmosis membrane required for desalinization。And the forward osmosis membrane film forming later stage obtained in the present invention is according to suitable post processing, as membrane flux more can be significantly improved with the nonionic surfactant of variable concentrations when soaking。
The object of the invention is achieved through the following technical solutions:
The preparation method of a kind of Cellulose acetate forward osmotic membrane, comprises the steps:
1) preparation raw material: add the proportions raw material of the acetone of 20-40mL, the Isosorbide-5-Nitrae-dioxane of 50-70mL, 7-10mL methanol according to every 3-5g cellulose acetate, and add the lactic acid of pore creating material 5-10mL or the zinc chloride of 0.8-28g；
2) by raw material mix homogeneously, stirring at normal temperatures makes cellulose acetate be completely dissolved, and obtains casting solution, stands more than casting solution 12h, to complete froth breaking；
3) by the sodium hydroxide solution immersion treatment 30-70min that polysulfone membrane mass concentration is 8%-12% of porous, remove the impurity that adsorbs of surface, then with after deionized water cleaning, drying as supporting layer, stand-by；
4) by step 3) in the supporting layer that obtains of pretreatment soak 30-60s in casting solution in step 2, lift is once dipped into afterwards in deionized water and carries out inversion of phases 2-6h, obtain the Cellulose acetate forward osmotic membrane of uniform pore diameter, middle basement membrane is polysulfone membrane, it it is porous support layer, the cellulose acetate membrane in attachment is formed, for active layer in basement membrane both sides；
5) by step 4) obtain forward osmosis membrane and put in the water-bath of 40-90 degree and carry out heat treatment, it is placed on cryopreservation in the sodium sulfite solution that mass concentration is 0.3%-0.8% after cleaning。
For realizing goal of the invention further, active layer cellulose acetate molecular weight of the present invention is preferably 40000-50000。Described stirring is preferably mechanical agitation。The described inversion of phases time is 3-5h。The described heat treated time is preferably 5-60min。
A kind of Cellulose acetate forward osmotic membrane, has above-mentioned preparation method to prepare。
Relative to prior art, present invention have the advantage that
1) in the inventive method, the Cellulose acetate forward osmotic membrane of preparation is with cellulose acetate for main matter, and cellulose acetate has good hydrophilic and film property, and specific surface area is big, adsorbance is low, having and cut salt effect preferably, compared with prior art, salt-stopping rate is significantly increased。
2) Cellulose acetate forward osmotic membrane prepared by the inventive method has hydrophilic supporting layer and two layers of hydrophilic active layer, and the membrane flux that can reach in experimentation has 17L/m2.h, salt-stopping rate has all reached more than 99.99%, and it is 13L/m that other forward osmosis membrane can reach membrane flux2.h, salt-stopping rate is 97%, and both compare Cellulose acetate forward osmotic membrane prepared by the inventive method and have the features such as membrane flux height, salt-stopping rate be good, preferably resolve interior concentration polarization problem, can be used for desalinization, the field such as sewage disposal and food processing。
3) the hydrophilic polysulfone membrane of the present invention is provided that a supporting layer well, and heat stability is high, hydrolysis, and can have very strong adhesion between cellulose acetate, without affecting membrane flux。
4) present invention lactic acid or zinc chloride are as pore creating material, and molecular weight is little, can guarantee that it has significantly high section salt effect。
Detailed description of the invention
For being more fully understood that the present invention, below in conjunction with embodiment, the present invention is further illustrated, but embodiments of the present invention are not limit so。
Embodiment 1.
Step 1: preparation raw material: 3.0g cellulose acetate, cellulose acetate molecular weight is the Isosorbide-5-Nitrae-dioxane of 40320g/mol, 52.5mL, the acetone of 22mL, the methanol of 8.2mL, the lactic acid of 6.6mL；
Step 2: weighed for step 1 solid and liquid are joined mix homogeneously in round-bottomed flask, and mechanical agitation makes cellulose acetate be completely dissolved at normal temperatures, obtains cellulose acetate casting solution, stands more than casting solution 12h and makes its complete froth breaking；
Step 3: by the sodium hydroxide solution immersion treatment 30min that polysulfone membrane mass concentration is 10% of the porous that model is JQE-3631-130326 that Shenzhen Jiaquan Membrane Filtration Equipment Co., Ltd. produces, remove the impurity that surface is adsorbed, then with stand-by after deionized water clean dry；
Step 4: polysulfone membrane supporting layer pretreatment in step 3 obtained soaks 60s in casting solution in step 2, and lift is once dipped into afterwards in deionized water and carries out inversion of phases 6h；By Electronic Speculum it can be seen that film is divided into three layers, centre to be the supporting layer of porous, both sides are the cellulose acetate active layer formed；
Step 5: the film obtained in step 4 is put 60 degree of heat treatment 10min in a water bath, obtains the Cellulose acetate forward osmotic membrane of uniform pore diameter。
This forward osmosis membrane using mass fraction be 3.5% sodium chloride solution as drawing liquid, deionized water is tested as material liquid。
The test result of forward osmosis membrane is membrane flux 13.1L/m2.h, salt-stopping rate is 99.999%。Compared with prior art, when membrane flux is suitable, salt-stopping rate is significantly increased this test result。
Embodiment 2.
Step 1: preparation raw material: 3.3g cellulose acetate, cellulose acetate molecular weight is the Isosorbide-5-Nitrae-dioxane of 40320g/mol, 52.5mL, the acetone of 22mL, the methanol of 8.2mL, the lactic acid of 6.6mL；
Step 2: weighed for step 1 solid and liquid are joined mix homogeneously in round-bottomed flask, and mechanical agitation makes cellulose acetate be completely dissolved at normal temperatures, obtains cellulose acetate casting solution, stands more than casting solution 12h and makes its complete froth breaking；
Step 3: by the polysulfone membrane of porous by the sodium hydroxide solution immersion treatment of 10%, remove the impurity that surface is adsorbed, then with stand-by after deionized water clean dry；
Step 4: supporting layer pretreatment in step 3 obtained soaks 60s in casting solution in step 2, and lift is once dipped into afterwards in deionized water and carries out inversion of phases 6h；
Step 5: the film obtained in step 4 is put 60 degree of heat treatment 10min in a water bath, obtains the Cellulose acetate forward osmotic membrane of uniform pore diameter。
This forward osmosis membrane using mass fraction be 3.5% sodium chloride solution as drawing liquid, deionized water is tested as material liquid。
The test result of forward osmosis membrane is membrane flux 17.17L/m2.h, salt-stopping rate is 99.998%。Test result indicate that, when other conditions are identical, the amount properly increasing cellulose acetate can increase the membrane flux of forward osmosis membrane, and salt-stopping rate is substantially unchanged。Compared with prior art, salt-stopping rate is significantly increased this test result。
Embodiment 3.
Step 1: preparation raw material: 3.3g cellulose acetate, cellulose acetate molecular weight is the Isosorbide-5-Nitrae-dioxane of 40320g/mol, 52.5mL, the acetone of 22mL, the methanol of 8.2mL, the lactic acid of 6.6mL；
Step 2: weighed for step 1 solid and liquid are joined mix homogeneously in round-bottomed flask, and mechanical agitation makes cellulose acetate be completely dissolved at normal temperatures, obtains cellulose acetate casting solution, stands more than casting solution 12h and makes its complete froth breaking；
Step 3: by the polysulfone membrane of porous by the sodium hydroxide solution immersion treatment of 10%, remove the impurity that surface is adsorbed, then with stand-by after deionized water clean dry；
Step 4: supporting layer pretreatment in step 3 obtained soaks 60s in casting solution in step 2, and lift is once dipped into afterwards in deionized water and carries out inversion of phases 6h；
Step 5: the film obtained in step 4 is put 60 degree of heat treatment 20min in a water bath, obtains the Cellulose acetate forward osmotic membrane of uniform pore diameter。
This forward osmosis membrane using mass fraction be 3.5% sodium chloride solution as drawing liquid, deionized water is tested as material liquid。
The test result of forward osmosis membrane is membrane flux 14.65L/m2.h, salt-stopping rate is 99.998%。Test result shows, when other conditions are identical, properly increase heat treatment time and the membrane flux of forward osmosis membrane can be made to reduce, and salt-stopping rate is substantially unchanged。Compared with prior art, salt-stopping rate is significantly increased this test result。
Embodiment 4.
Step 1: preparation raw material: 3.3g cellulose acetate, cellulose acetate molecular weight is the Isosorbide-5-Nitrae-dioxane of 40320g/mol, 52.5mL, the acetone of 22mL, the methanol of 8.2mL, the lactic acid of 6.6mL；
Step 2: weighed for step 1 solid and liquid are joined mix homogeneously in round-bottomed flask, and mechanical agitation makes cellulose acetate be completely dissolved at normal temperatures, obtains cellulose acetate casting solution, stands more than casting solution 12h and makes its complete froth breaking；
Step 3: by the polysulfone membrane of porous by the sodium hydroxide solution immersion treatment of 10%, remove the impurity that surface is adsorbed, then with stand-by after deionized water clean dry；
Step 4: supporting layer pretreatment in step 3 obtained soaks 60s in casting solution in step 2, and lift is once dipped into afterwards in deionized water and carries out inversion of phases 6h；
Step 5: the film obtained in step 4 is put 70 degree of heat treatment 10min in a water bath, obtains the Cellulose acetate forward osmotic membrane of uniform pore diameter。
This forward osmosis membrane using mass fraction be 3.5% sodium chloride solution as drawing liquid, deionized water is tested as material liquid。
The test result of forward osmosis membrane is membrane flux 7.5L/m2.h, salt-stopping rate is 99.995%。Test result indicate that, when other conditions are identical, properly increasing heat treatment temperature and the membrane flux of forward osmosis membrane can be made substantially to reduce, salt-stopping rate is substantially unchanged。Compared with prior art, salt-stopping rate is significantly increased this test result。
Embodiment 5
Step 1: preparation raw material: 3.3g cellulose acetate, cellulose acetate molecular weight is the Isosorbide-5-Nitrae-dioxane of 40320g/mol, 52.5mL, the acetone of 22mL, the methanol of 8.2mL, the zinc chloride of 3.0g；
Step 2: weighed for step 1 solid and liquid are joined mix homogeneously in round-bottomed flask, and mechanical agitation makes cellulose acetate be completely dissolved at normal temperatures, obtains cellulose acetate casting solution, stands more than casting solution 12h and makes its complete froth breaking；
Step 3: by the polysulfone membrane of porous by the sodium hydroxide solution immersion treatment of 10%, remove the impurity that surface is adsorbed, then with stand-by after deionized water clean dry；
Step 4: supporting layer pretreatment in step 3 obtained soaks 60s in casting solution in step 2, and lift is once dipped into afterwards in deionized water and carries out inversion of phases 6h；
Step 5: the film obtained in step 4 is put 60 degree of heat treatment 20min in a water bath, obtains the Cellulose acetate forward osmotic membrane of uniform pore diameter。
This forward osmosis membrane using mass fraction be 3.5% sodium chloride solution as drawing liquid, deionized water is tested as material liquid。
The test result of forward osmosis membrane is membrane flux 9.7L/m2.h, salt-stopping rate is 99.997%。Test result indicate that, when other conditions are identical, replacing lactic acid also to have certain membrane flux as the forward osmosis membrane prepared by pore creating material with zinc chloride, salt-stopping rate is higher, and compared with prior art, salt-stopping rate is significantly increased。
Embodiment 6.
Step 1: preparation raw material: 3.3g cellulose acetate, cellulose acetate molecular weight is the Isosorbide-5-Nitrae-dioxane of 40320g/mol, 52.5mL, the acetone of 22mL, the methanol of 8.2mL, the zinc chloride of 4.0g；
Step 2: weighed for step 1 solid and liquid are joined mix homogeneously in round-bottomed flask, and mechanical agitation makes cellulose acetate be completely dissolved at normal temperatures, obtains cellulose acetate casting solution, stands more than casting solution 12h and makes its complete froth breaking；
Step 3: by the polysulfone membrane of porous by the sodium hydroxide solution immersion treatment of 10%, remove the impurity that surface is adsorbed, then with stand-by after deionized water clean dry；
Step 4: supporting layer pretreatment in step 3 obtained soaks 60s in casting solution in step 2, and lift is once dipped into afterwards in deionized water and carries out inversion of phases 6h；
Step 5: the film obtained in step 4 is put 60 degree of heat treatment 20min in a water bath, obtains the Cellulose acetate forward osmotic membrane of uniform pore diameter。
This forward osmosis membrane using mass fraction be 3.5% sodium chloride solution as drawing liquid, deionized water is tested as material liquid。
The test result of forward osmosis membrane is membrane flux 14.6L/m2.h, salt-stopping rate is 99.999%。Test result indicate that, when other conditions are identical, the amount properly increasing pore creating material zinc chloride can improve membrane flux and the salt-stopping rate of forward osmosis membrane；Compared with prior art, salt-stopping rate is significantly increased this test result。
Claims (4)
1. the preparation method of a Cellulose acetate forward osmotic membrane, it is characterised in that comprise the steps:
1) preparation raw material: add the proportions raw material of the acetone of 20-40mL, the Isosorbide-5-Nitrae-dioxane of 50-70mL, 7-10mL methanol according to every 3-5g cellulose acetate, and add the lactic acid of pore creating material 5-10mL or the zinc chloride of 0.8-28g；
2) by raw material mix homogeneously, stirring at normal temperatures makes cellulose acetate be completely dissolved, and obtains casting solution, stands more than casting solution 12h, to complete froth breaking；
3) by the sodium hydroxide solution immersion treatment 30-70min that polysulfone membrane mass concentration is 8%-12% of porous, remove the impurity that adsorbs of surface, then with after deionized water cleaning, drying as supporting layer, stand-by；
4) by step 3) in the supporting layer that obtains of pretreatment be immersed in step 2) in casting solution in 30-60s, lift is once dipped into afterwards in deionized water and carries out inversion of phases 2-6h, obtain the Cellulose acetate forward osmotic membrane of uniform pore diameter, middle basement membrane is polysulfone membrane, it it is porous support layer, the cellulose acetate membrane in attachment is formed, for active layer in basement membrane both sides；Described active layer cellulose acetate molecular weight is 40000-50000；
5) by step 4) obtain forward osmosis membrane and put in the water-bath of 40-90 degree and carry out heat treatment, it is placed on cryopreservation in the sodium sulfite solution that mass concentration is 0.3%-0.8% after cleaning；The described heat treated time is 5-60min。
2. the preparation method of a kind of Cellulose acetate forward osmotic membrane according to claim 1, it is characterised in that: described stirring is mechanical agitation。
3. the preparation method of a kind of Cellulose acetate forward osmotic membrane according to claim 1, it is characterised in that: the described inversion of phases time is 3-5h。
4. a Cellulose acetate forward osmotic membrane, it is characterised in that its preparation method described in any one of claim 1-3 prepares。
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| CN103785301B (en) * | 2014-02-13 | 2016-08-17 | 中国科学院上海高等研究院 | A kind of Cellulose acetate forward osmotic membrane material and preparation method thereof |
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| CN107021588A (en) * | 2017-06-20 | 2017-08-08 | 湖南文理学院 | A kind of sponge urban construction osmos tube |
| CN109304089B (en) * | 2017-07-28 | 2020-10-02 | 中国科学院宁波材料技术与工程研究所 | Composite cellulose acetate forward osmosis membrane and preparation method and application thereof |
| CN112090290A (en) * | 2020-07-31 | 2020-12-18 | 浙江工业大学 | Hollow nanocapsule modified forward osmosis membrane and preparation method and application thereof |
| CN113491962B (en) * | 2021-09-09 | 2022-02-22 | 北京宝盛通国际电气工程技术有限公司 | Forward osmosis membrane and method for producing same |
| CN114028946A (en) * | 2021-10-25 | 2022-02-11 | 浙江工业大学 | Nano composite cellulose acetate forward osmosis membrane and preparation method thereof |
| CN116392972B (en) * | 2023-06-06 | 2023-08-08 | 华电水务装备(天津)有限公司 | Forward osmosis membrane applied to emergency water treatment, preparation method and application |
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