CN103537200A - Cellulose acetate forward osmotic membrane and preparation method thereof - Google Patents
Cellulose acetate forward osmotic membrane and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a cellulose acetate forward osmotic membrane and a preparation method of the cellulose acetate forward osmotic membrane. The preparation method comprises the following steps: preparing raw materials according to a ratio of adding 20ml-40ml of acetone, 50ml-70ml of 1,4-dioxane and 7ml-10ml of methanol into 3g-5g of cellulose acetate; adding a pore former, namely 5ml-10ml of lactic acid or 0.8g-28g of zinc chloride; uniformly mixing the raw materials and completely dissolving the cellulose acetate under room-temperature agitation; standing a membrane casting solution for more than 12 hours; immersing and treating by a sodium hydroxide solution; immersing a mixture into the membrane casting solution for 30-60 seconds; and pulling for one time and immersing into de-ionized water for carrying out phase inversion for 2-6 hours so as to obtain the cellulose acetate forward osmotic membrane, wherein a middle base membrane is a polysulfone membrane and attached cellulose acetate membranes are formed on the two sides of the base membrane. The preparation method is simple in process and the prepared forward osmotic membrane can effectively prevent solutes from entering a porous supporting layer; the cellulose acetate forward osmotic membrane has good chemical stability and high salt rejection rate and membrane flux.
Description
Technical field
A kind of forward osmosis membrane of the present invention, particularly relates to a kind of cellulose acetate forward osmosis membrane and preparation method thereof, belongs to polymeric membrane for separation technical field.
Background technology
The rapid growth of population and the consumption of fossil fuel make water and the energy become most important two kinds of resources in the world.Water shortage and energy crisis are perplexing many areas in the world, it is reported and surpass in the world the drinking water that 1,200,000,000 people lack clean health.Membrane separation technique normal-temperature operation, without phase transformation, be up-and-coming regeneration drinking water technology.
The positive infiltration technology that development in recent years is got up is a kind of technology of utilizing penetration theory to carry out film separation, utilize the osmotic pressure difference of film both sides solution make hydrone spontaneous pass through pellicle, from the higher material liquid of water chemistry gesture, be penetrated into lower the drawing liquid of water chemistry gesture, can be used for directly from seawater, extracting fresh water.The three cellulose acetate membrane (CTA) that unique commercial forward osmosis membrane is U.S. HTI company at present, it consists of active compacted zone and polyester support, has higher membrane flux and salt-stopping rate.
In theory, just permeating and can realize the membrane flux larger than counter-infiltration with the very high liquid that draws of osmotic pressure, yet research finds that actual membrane flux is much smaller than theoretical value, this is because commercial reverse osmosis membrane has serious dissymmetrical structure, active layer structure is very fine and close causes existing in positive process of osmosis very serious interior concentration polarization phenomenon, cause effective driving pressure significantly to reduce, thereby obviously reduce membrane flux.Because interior concentration polarization is present in fenestra, only have by improving membrane structure and film properties is alleviated, and the interior concentration polarization basic reason that forward osmosis membrane flux declines to a great extent just often makes membrane flux reduce by 80%.
For interior concentration polarization phenomenon, effectively precautions has the supporting layer aperture of increase, adopts hydroaropic substance to prepare supporting layer or prepare double activated layer at present.Polysulfones ultrafiltration is supported counterdie and is had finger, is conducive to reduce interior concentration polarization phenomenon, and the hydrophily PS membrane after modification more can improve membrane flux.Utilize hydrophilic cellulose acetate (CA) to prepare active layer, the cellulose acetate forward osmosis membrane that adopts lactic acid to make as pore creating material has very high salt-stopping rate and membrane flux.
In current patent of invention, have various film forming solute and solvent, additive etc. have been done to some exploration contrast experiments, the film-forming method adopting is all to use scraper knifing, masking solute has CA, CTA, acetylbutyrylcellulose etc., and their comparison is complicated.For example patent No. CN201210453553.3 has done discussion test to multiple additives and film forming solvents, its resulting film is using deionized water as material liquid, the sodium chloride of 1mol/L is not very high as drawing liquid resulting flux of when experiment, and high energy reaches 13.12L/m
2.h, and the back-mixing flux of salt can reach 3.32g/m
2.h.In patent No. CN201210137147.6, adopt the raw material of hypertoxicity, as polyamine solution and polynary solution of acid chloride reaction molding, with pure water as material liquid, the sodium chloride solution of 1mol/L is when drawing liquid, the membrane flux of prepared hollow-fibre membrane only reaches 5.97L/m
2.h.In patent No. CN201310092067.8, first to polysulfones, hydrophilic carboxylated polysulphone super-filter membrane is prepared in modification, on this milipore filter, in-situ polymerization generates polyamide forward osmosis membrane again, the method still adopts poisonous reagent m-phenylene diamine (MPD) and pyromellitic trimethylsilyl chloride as raw material synthesizing polyamides forward osmosis membrane, be unfavorable for environmental protection, and usining 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/m
2.h, salt-stopping rate only reaches 96.12%.The prepared ultra-thin pair of cortex forward osmosis membrane of patent No. CN201210578252.3 it adopt environmentally friendly Triafol T, cellulose diacetate as membrane-forming agent, at the thickness of scraping out with scraper, reach 100um, when usining 0.1mol/L sodium chloride as material liquid, 4mol/L glucose is when drawing liquid experiment condition, and membrane flux is 12.8L/m
2.h, salt-stopping rate reaches 96.8%.
Summary of the invention
One of 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 osmosis membrane of good mechanical property.Another object of the present invention is the preparation method that described cellulose acetate forward osmosis membrane will be provided.
The present invention's profit masking solute used is that simple molecular weight is at the cellulose acetate of 40000-50000, solvent is 1, the mixed solvent that 4-dioxane and acetone mix by a certain percentage, additive is single methyl alcohol, pore creating material has been chosen different materials, according to a certain percentage after the even froth breaking of mixed dissolution, adopted simple infusion process film forming, film forming thickness is even, resulting forward osmosis membrane is in positive permeability test when adopting identical material liquid and drawing liquid, and getable membrane flux reaches 17.17L/m
2.h, salt-stopping rate reaches more than 99.999%, is suitable as very much the needed forward osmosis membrane of desalinization.And if in the present invention the prepared forward osmosis membrane film forming later stage adopt suitable post processing, while soaking as non-ionic surface active agent with variable concentrations, more can obviously improve membrane flux.
The object of the invention is achieved through the following technical solutions:
A preparation method for cellulose acetate forward osmosis membrane, comprises the steps:
1) preparation raw material: add the acetone of 20-40ml, the proportional arrangement raw material of Isosorbide-5-Nitrae-dioxane of 50-70ml, 7-10ml methyl alcohol 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) raw material is mixed, stir cellulose acetate is dissolved completely at normal temperatures, obtain casting solution, more than standing casting solution 12h, to complete froth breaking;
3) the sodium hydroxide solution immersion treatment 30-70min that is 8%-12% by the PS membrane of porous by mass concentration, removes the impurity that adsorbs of surface, then uses after deionized water cleaning, drying as supporting layer, stand-by;
4) supporting layer pretreatment in step 3) being obtained is immersed in 30-60s in the casting solution in step 2, lift to be once dipped into afterwards and in deionized water, carry out inversion of phases 2-6h, obtain the uniform cellulose acetate forward osmosis membrane in aperture, middle basement membrane is PS membrane, it is porous support layer, in basement membrane both sides, forming the CAM adhering to, is active layer;
5) step 4) is obtained to forward osmosis membrane and put into the water-bath of 40-90 degree and heat-treat, after cleaning, be placed on low temperature in the solution of sodium bisulfite that mass concentration is 0.3%-0.8% and preserve.
For further realizing goal of the invention, 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 forward osmosis membrane, has above-mentioned preparation method to make.
With respect to prior art, tool of the present invention has the following advantages:
1) the cellulose acetate forward osmosis membrane of preparing in the inventive method be take cellulose acetate as main matter, and cellulose acetate has good hydrophily and film forming, and specific area is large, adsorbance is low, can have and cut preferably salt effect, compared with prior art, salt-stopping rate is significantly increased.
2) the cellulose acetate forward osmosis membrane that prepared by the inventive method has hydrophily supporting layer and two layers of hydrophilic active layer, and the membrane flux that can reach in experimentation has 17L/m
2.h, salt-stopping rate has all reached more than 99.99%, and other forward osmosis membrane can reach membrane flux, is 13L/m
2.h, salt-stopping rate is 97%, and both compare cellulose acetate forward osmosis membrane prepared by the inventive method and have the features such as membrane flux is high, salt-stopping rate is good, preferably resolve interior concentration polarization problem, can be used for desalinization, the fields such as sewage disposal and food processing.
3) the hydrophilic PS membrane of the present invention can provide a supporting layer well, and heat endurance is high, hydrolysis, and can have very strong adhesion between cellulose acetate, can not affect membrane flux yet.
4) the present invention is with lactic acid or zinc chloride as pore creating material, and molecular weight is little, can guarantee that it has the very high salt effect of cutting.
The specific embodiment
For understanding better 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 40320g/mol, Isosorbide-5-Nitrae-dioxane of 52.5ml, the acetone of 22ml, the methyl alcohol of 8.2ml, the lactic acid of 6.6ml;
Step 2: the solid that step 1 is weighed and liquid join in round-bottomed flask and mixes, mechanical agitation is dissolved cellulose acetate completely at normal temperatures, obtains cellulose acetate casting solution, and standing casting solution 12h makes its complete froth breaking above;
Step 3: the sodium hydroxide solution immersion treatment 30min that the PS membrane of the porous that the model that Jia, Shenzhen City spring membrane filtration equipment Co., Ltd is produced is JQE-3631-130326 is 10% by mass concentration, remove the impurity that adsorbs of surface, then use after deionized water clean dry stand-by;
Step 4: the PS membrane supporting layer that pretreatment in step 3 is obtained is immersed in 60s in the casting solution in step 2, lifts to be once dipped into afterwards and in deionized water, carries out inversion of phases 6h; By Electronic Speculum, can see that film is divided into three layers, centre is the supporting layer of porous, the cellulose acetate active layer of both sides for forming;
Step 5: the film obtaining in step 4 is placed on to 60 degree heat treatment 10min in water-bath, obtains the uniform cellulose acetate forward osmosis membrane in aperture.
This forward osmosis membrane is usingd sodium chloride solution that mass fraction is 3.5% as drawing liquid, and deionized water is tested as material liquid.
The test result of forward osmosis membrane is membrane flux 13.1L/m
2.h, salt-stopping rate is 99.999%.Compared with prior art, in the situation that 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 40320g/mol, Isosorbide-5-Nitrae-dioxane of 52.5ml, the acetone of 22ml, the methyl alcohol of 8.2ml, the lactic acid of 6.6ml;
Step 2: the solid that step 1 is weighed and liquid join in round-bottomed flask and mixes, mechanical agitation is dissolved cellulose acetate completely at normal temperatures, obtains cellulose acetate casting solution, and standing casting solution 12h makes its complete froth breaking above;
Step 3: by 10% sodium hydroxide solution immersion treatment for the PS membrane of porous, remove the impurity that adsorb on surface, then use after deionized water clean dry stand-by;
Step 4: the supporting layer that pretreatment in step 3 is obtained is immersed in 60s in the casting solution in step 2, lifts to be once dipped into afterwards and in deionized water, carries out inversion of phases 6h;
Step 5: the film obtaining in step 4 is placed on to 60 degree heat treatment 10min in water-bath, obtains the uniform cellulose acetate forward osmosis membrane in aperture.
This forward osmosis membrane is usingd sodium chloride solution that mass fraction is 3.5% as drawing liquid, and deionized water is tested as material liquid.
The test result of forward osmosis membrane is membrane flux 17.17L/m
2.h, salt-stopping rate is 99.998%.Experimental result shows, when other conditions are identical, the amount that suitably improves 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 40320g/mol, Isosorbide-5-Nitrae-dioxane of 52.5ml, the acetone of 22ml, the methyl alcohol of 8.2ml, the lactic acid of 6.6ml;
Step 2: the solid that step 1 is weighed and liquid join in round-bottomed flask and mixes, mechanical agitation is dissolved cellulose acetate completely at normal temperatures, obtains cellulose acetate casting solution, and standing casting solution 12h makes its complete froth breaking above;
Step 3: by 10% sodium hydroxide solution immersion treatment for the PS membrane of porous, remove the impurity that adsorb on surface, then use after deionized water clean dry stand-by;
Step 4: the supporting layer that pretreatment in step 3 is obtained is immersed in 60s in the casting solution in step 2, lifts to be once dipped into afterwards and in deionized water, carries out inversion of phases 6h;
Step 5: the film obtaining in step 4 is placed on to 60 degree heat treatment 20min in water-bath, obtains the uniform cellulose acetate forward osmosis membrane in aperture.
This forward osmosis membrane is usingd sodium chloride solution that mass fraction is 3.5% as drawing liquid, and deionized water is tested as material liquid.
The test result of forward osmosis membrane is membrane flux 14.65L/m
2.h, salt-stopping rate is 99.998%.Test result shows, when other conditions are identical, suitably improve heat treatment time and can make the membrane flux of forward osmosis membrane reduce, and salt-stopping rate are 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 40320g/mol, Isosorbide-5-Nitrae-dioxane of 52.5ml, the acetone of 22ml, the methyl alcohol of 8.2ml, the lactic acid of 6.6ml;
Step 2: the solid that step 1 is weighed and liquid join in round-bottomed flask and mixes, mechanical agitation is dissolved cellulose acetate completely at normal temperatures, obtains cellulose acetate casting solution, and standing casting solution 12h makes its complete froth breaking above;
Step 3: by 10% sodium hydroxide solution immersion treatment for the PS membrane of porous, remove the impurity that adsorb on surface, then use after deionized water clean dry stand-by;
Step 4: the supporting layer that pretreatment in step 3 is obtained is immersed in 60s in the casting solution in step 2, lifts to be once dipped into afterwards and in deionized water, carries out inversion of phases 6h;
Step 5: the film obtaining in step 4 is placed on to 70 degree heat treatment 10min in water-bath, obtains the uniform cellulose acetate forward osmosis membrane in aperture.
This forward osmosis membrane is usingd sodium chloride solution that mass fraction is 3.5% as drawing liquid, and deionized water is tested as material liquid.
The test result of forward osmosis membrane is membrane flux 7.5L/m
2.h, salt-stopping rate is 99.995%.Experimental result shows, when other conditions are identical, suitably improve heat treatment temperature and can make the membrane flux of forward osmosis membrane obviously reduce, and 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 40320g/mol, Isosorbide-5-Nitrae-dioxane of 52.5ml, the acetone of 22ml, the methyl alcohol of 8.2ml, the zinc chloride of 3.0g;
Step 2: the solid that step 1 is weighed and liquid join in round-bottomed flask and mixes, mechanical agitation is dissolved cellulose acetate completely at normal temperatures, obtains cellulose acetate casting solution, and standing casting solution 12h makes its complete froth breaking above;
Step 3: by 10% sodium hydroxide solution immersion treatment for the PS membrane of porous, remove the impurity that adsorb on surface, then use after deionized water clean dry stand-by;
Step 4: the supporting layer that pretreatment in step 3 is obtained is immersed in 60s in the casting solution in step 2, lifts to be once dipped into afterwards and in deionized water, carries out inversion of phases 6h;
Step 5: the film obtaining in step 4 is placed on to 60 degree heat treatment 20min in water-bath, obtains the uniform cellulose acetate forward osmosis membrane in aperture.
This forward osmosis membrane is usingd sodium chloride solution that mass fraction is 3.5% as drawing liquid, and deionized water is tested as material liquid.
The test result of forward osmosis membrane is membrane flux 9.7L/m
2.h, salt-stopping rate is 99.997%.Experimental result shows, when other conditions are identical, with zinc chloride, replaces lactic acid also to have certain membrane flux as the prepared forward osmosis membrane of pore creating material, and 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 40320g/mol, Isosorbide-5-Nitrae-dioxane of 52.5ml, the acetone of 22ml, the methyl alcohol of 8.2ml, the zinc chloride of 4.0g;
Step 2: the solid that step 1 is weighed and liquid join in round-bottomed flask and mixes, mechanical agitation is dissolved cellulose acetate completely at normal temperatures, obtains cellulose acetate casting solution, and standing casting solution 12h makes its complete froth breaking above;
Step 3: by 10% sodium hydroxide solution immersion treatment for the PS membrane of porous, remove the impurity that adsorb on surface, then use after deionized water clean dry stand-by;
Step 4: the supporting layer that pretreatment in step 3 is obtained is immersed in 60s in the casting solution in step 2, lifts to be once dipped into afterwards and in deionized water, carries out inversion of phases 6h;
Step 5: the film obtaining in step 4 is placed on to 60 degree heat treatment 20min in water-bath, obtains the uniform cellulose acetate forward osmosis membrane in aperture.
This forward osmosis membrane is usingd sodium chloride solution that mass fraction is 3.5% as drawing liquid, and deionized water is tested as material liquid.
The test result of forward osmosis membrane is membrane flux 14.6L/m
2.h, salt-stopping rate is 99.999%.Experimental result shows, when other conditions are identical, the amount that suitably improves 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 (6)
1. a preparation method for cellulose acetate forward osmosis membrane, is characterized in that comprising the steps:
1) preparation raw material: add the acetone of 20-40ml, the proportional arrangement raw material of Isosorbide-5-Nitrae-dioxane of 50-70ml, 7-10ml methyl alcohol 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) raw material is mixed, stir cellulose acetate is dissolved completely at normal temperatures, obtain casting solution, more than standing casting solution 12h, to complete froth breaking;
3) the sodium hydroxide solution immersion treatment 30-70min that is 8%-12% by the PS membrane of porous by mass concentration, removes the impurity that adsorbs of surface, then uses after deionized water cleaning, drying as supporting layer, stand-by;
4) supporting layer pretreatment in step 3) being obtained is immersed in 30-60s in the casting solution in step 2, lift to be once dipped into afterwards and in deionized water, carry out inversion of phases 2-6h, obtain the uniform cellulose acetate forward osmosis membrane in aperture, middle basement membrane is PS membrane, it is porous support layer, in basement membrane both sides, forming the CAM adhering to, is active layer;
5) step 4) is obtained to forward osmosis membrane and put into the water-bath of 40-90 degree and heat-treat, after cleaning, be placed on low temperature in the solution of sodium bisulfite that mass concentration is 0.3%-0.8% and preserve.
2. the preparation method of cellulose acetate forward osmosis membrane according to claim 1, is characterized in that: described active layer cellulose acetate molecular weight is 40000-50000.
3. the preparation method of a kind of cellulose acetate forward osmosis membrane according to claim 1, is characterized in that: described stirring is mechanical agitation.
4. the preparation method of a kind of cellulose acetate forward osmosis membrane according to claim 1, is characterized in that: the described inversion of phases time is 3-5h.
5. the preparation method of a kind of cellulose acetate forward osmosis membrane according to claim 1, is characterized in that: the described heat treated time is 5-60min.
6. a cellulose acetate forward osmosis membrane, is characterized in that it is made by preparation method described in claim 1-5 any one.
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| CN103785301A (en) * | 2014-02-13 | 2014-05-14 | 中国科学院上海高等研究院 | Cellulose acetate forward osmosis film material and preparation method thereof |
| CN103861472A (en) * | 2014-03-28 | 2014-06-18 | 东华大学 | Preparation method of amino-modified graphene oxide composite positive permeable film |
| CN106917263A (en) * | 2017-03-24 | 2017-07-04 | 马鞍山中创环保科技有限公司 | A kind of method for preparing heavy metal ion exchange fiber using discarded acetate fiber |
| CN107021588A (en) * | 2017-06-20 | 2017-08-08 | 湖南文理学院 | A kind of sponge urban construction osmos tube |
| CN107789988A (en) * | 2016-08-31 | 2018-03-13 | 山东东岳高分子材料有限公司 | Hollow fiber composite membrane of ultra-thin active layer and preparation method thereof |
| CN109304089A (en) * | 2017-07-28 | 2019-02-05 | 中国科学院宁波材料技术与工程研究所 | A kind of multiple cellulose acetate forward osmosis membrane and the 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 |
| CN113491962A (en) * | 2021-09-09 | 2021-10-12 | 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 |
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| WO2023035556A1 (en) * | 2021-09-09 | 2023-03-16 | 北京宝盛通国际电气工程技术有限公司 | Forward osmosis membrane and preparation method therefor |
| 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 |
| CN116392972A (en) * | 2023-06-06 | 2023-07-07 | 华电水务装备(天津)有限公司 | Forward osmosis membrane applied to emergency water treatment, preparation method and application |
| 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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