CN105561808A - Preparation method for cellulose acetate forward osmosis membrane - Google Patents
Preparation method for cellulose acetate forward osmosis membrane Download PDFInfo
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- CN105561808A CN105561808A CN201610080870.3A CN201610080870A CN105561808A CN 105561808 A CN105561808 A CN 105561808A CN 201610080870 A CN201610080870 A CN 201610080870A CN 105561808 A CN105561808 A CN 105561808A
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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
- B01D71/08—Polysaccharides
- B01D71/12—Cellulose derivatives
- B01D71/14—Esters of organic acids
- B01D71/16—Cellulose acetate
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0002—Organic membrane manufacture
- B01D67/0009—Organic membrane manufacture by phase separation, sol-gel transition, evaporation or solvent quenching
- B01D67/0011—Casting solutions therefor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/10—Supported membranes; Membrane supports
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/02—Details relating to pores or porosity of the membranes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/04—Characteristic thickness
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/24—Mechanical properties, e.g. strength
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Abstract
The invention relates to a preparation method for a cellulose acetate forward osmosis membrane, and belongs to the technical field of membrane separation. The preparation method comprises the steps that dried cellulose acetate powder is dissolved in mixed organic solvent, and the mixture is put into a water bath to be mechanically stirred to form a uniform solution; the solution is put into a vacuum environment for standing and defoaming to form a membrane casting solution; the membrane casting solution is poured on a clean glass board and uniformly applied on the glass board with a scraper; the surface of the membrane casting solution is covered with a polyester screen immediately, and the membrane casting solution is quickly transferred into a baking oven for volatilization; the glass board with the membrane casting solution is put into a flowing deionized water gel bath; a regenerative membrane piece is stripped from the glass board and then put into a water bath at the temperature of 50 DEG C-90 DEG C, and the cellulose acetate forward osmosis membrane is obtained. The preparation method is simple in technology and easy to operate, and the prepared membrane is excellent in mechanical performance and high in water flux and has the higher salt intercepting rate and the lower inner concentration polarization phenomenon.
Description
Technical field
The present invention relates to a kind of preparation method of Cellulose acetate forward osmotic membrane, belong to technical field of membrane separation.
Background technology
Water resource is the most critical resource of human being's production life.Nowadays, ecological environment is seriously damaged, and water pollution is serious, and the protection of water resource and the improvement of water pollutions become the problem that modern society pays close attention to most.Membrane Separation for Water Treatment is one of important water technology.Traditional ultrafiltration, nanofiltration and reverse osmosis technology take hydraulic pressuring difference as the membrane separating process of driving force, and high to equipment requirement, energy consumption is large.(F0) technology of just permeating is a kind of new membrane isolation technics that development in recent years is got up.Just permeating is a spontaneous process, and what film both sides were respectively the material liquid of low concentration and high concentration draws liquid, and the water in material liquid draws liquid side due to spontaneous the entering through film of permeable pressure head, thus realizes being separated of water and pollutant.Different from traditional pressure-driven membrane process, just permeating with the permeable pressure head of film both sides for driving force, having low energy consumption, low stain, the feature of high-recovery, is therefore a kind of isolation technics of environmental protection.F0 is in wastewater treatment, and agricultural irrigation, food processing, medicine, desalinization, space industry all has a wide range of applications.
At present, the forward osmosis membrane of Unique Product is the three cellulose acetate membrane of HTI company of the U.S., has higher water flux.The factor of restriction F0 technology extensive use is that film exists higher interior concentration polarization phenomenon, and this is by the structures shape of film.Desirable forward osmosis membrane has following features: 1. the separating layer of densification; 2. separating layer has higher hydrophily; 3. supporting layer is as far as possible thin, has higher porosity; 4. higher mechanical strength; 5. there is resistance to chemical attack.In addition, membrane material is also the key of positive infiltration technology, and the material at present for forward osmosis membrane research mainly contains cellulose acetate (CA) and derivative thereof, polyamide (PA), polyether sulfone (PES), polybenzimidazoles (PBI) etc.
Cellulose acetate is a kind of natural macromolecular material obtained after hydroxyl acetic acid esterified in cellulose, and esterification degree is about 37-42%, and fusing point is about 230-300 DEG C, nontoxic.As porous film material, have selective height, permeable amount is large, processes the features such as simple.Cellulose acetate is adopted to have many documents and patent report as the material of preparing of F0 film.
It is solvent with ionic liquid that CN104069746A describes a kind of, cellulose dissolution is prepared casting solution, is prepared the method for cellulose forward osmosis membrane by phase inversion; It is basement membrane with PS membrane that CN103537200A describes a kind of, and by once soaking, lifting the method preparing forward osmosis membrane going to deionized water coagulating bath, obtained film is both sides is cellulose acetate active layers, and centre is the forward osmosis membrane of polysulfones basement membrane; Su etc. (SuJincaietal, 2010) have prepared acetyl cellulose hollow fiber nano filter membrane for positive permeability test, show that this film has higher NaCl rejection, but pure water flux are lower.At present, the research about Cellulose acetate forward osmotic membrane is a lot, but mostly adopts more complicated casting solution system, and preparation process is complicated, and that makes is low without support membrane intensity, or thicker supporting course causes serious interior concentration polarization phenomenon.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, providing a kind of simple to operate, the preparation method of the Cellulose acetate forward osmotic membrane that water flux is high.
The technical scheme that the present invention solves the problems of the technologies described above is as follows:
A preparation method for Cellulose acetate forward osmotic membrane, the method realizes as follows
1) joined by the cellulose acetate of the drying of 15-25 weight portion in the organic solvent of 75-85 weight portion, in the water bath of 30-55 DEG C, mechanical agitation makes cellulose acetate dissolves completely, evenly;
2) by Homogeneous phase mixing liquid obtained above more than standing and defoaming 12h in the vacuum environment of 30-55 DEG C, casting solution is obtained;
3) being poured on the cleaned glass plate of 15-30 DEG C by the casting solution after standing and defoaming, is that casting solution is coated into the uniform casting film liquid layer of thickness by 100-250 μm of scraper with thickness;
4) by smooth for clean polyester webs cover to be positioned in the baking oven of 20-80 DEG C after on casting film liquid layer volatilize between 10-90s;
5) then go in the deionized water coagulation bath of flowing by above-mentioned casting solution, deionized water coagulation bath temperature controls between 0-25 DEG C, and gel time controls between 6-24h, obtains newborn cellulose acetate diaphragm;
6) be placed in deionized water heat-treat departing from obtained newborn cellulose acetate diaphragm from glass plate, deionized water temperature controls between 50-90 DEG C, and heat treatment time controls, between 10-60min, to obtain Cellulose acetate forward osmotic membrane.
Further, in process prepared by the present invention, in indoor environment, temperature controls at 15-30 DEG C, and relative humidity controls at 30-75%;
Further, described cellulose acetate is cellulose diacetate, and weight average molecular weight is 3-10 ten thousand;
Further, described organic solvent is acetone, DMF, DMA, one or both in 1-METHYLPYRROLIDONE;
Preferably, described polyester mesh number is 100-200 order.
The present invention adopts the cellulose acetate of low toxic and environment-friendly to be raw material, prepares better simply casting solution system, with polyester webs as backing material, adopts phase inversion to prepare Cellulose acetate forward osmotic membrane.This method film-forming process is simple, easy to operate, is easy to realize suitability for industrialized production; Meanwhile, obtained film has higher water flux and salt-stopping rate, and mechanical strength is higher, is with a wide range of applications.
Adopt Cellulose acetate forward osmotic membrane prepared by the present invention, thickness is about 80-210 μm, hot strength up to 38.67N, porosity 65-73%.
Detailed description of the invention
Be described principle of the present invention and feature below, example, only for explaining the present invention, is not intended to limit scope of the present invention.
Embodiment 1
Take the cellulose acetate powder of 15g drying, add 85gNMP (1-METHYLPYRROLIDONE), be placed in the water-bath of 45 DEG C, mechanical agitation is to forming uniform solution; This solution is placed in the vacuum environment standing and defoaming 18h of 45 DEG C, forms casting solution; Being poured over by casting solution on the clean glass plate of 20 DEG C, is that casting solution applies on a glass by the scraper of 250 μm uniformly with thickness; Immediately 200 object polyester webs are covered casting solution surface, go to rapidly in the baking oven of 40 DEG C the 70s that volatilizees; Glass plate with casting solution is placed in the deionized water coagulation bath 6h of 5 DEG C of flowings; The diaphragm of new life and glass plate are peeled off, is placed in the water-bath 30min of 90 DEG C, obtains Cellulose acetate forward osmotic membrane.
The forward osmosis membrane thickness that this embodiment obtains is 213 μm, and porosity is 72.1%.This forward osmosis membrane, is tested as material liquid using deionized water for drawing agent with 1mol/LNaCl solution, stabilization time 30min, the testing time is 2h, carries out relevant parameter calculating according to data in the testing time.As calculated, this forward osmosis membrane flux is 12.6Lm-2h-1, and accumulation of salt in the surface soil permeation flux is 26.1gm-2h-1, and salt-stopping rate is 96.3%.Compared with prior art, when membrane flux is suitable, salt-stopping rate is higher for this test result.
Embodiment 2
Take the cellulose acetate powder of 15g drying, be dissolved in the mixed solvent be made up of 10g acetone and 75gNMP, be placed in the water-bath of 30 DEG C, mechanical agitation is to forming uniform solution; This solution is placed in the vacuum environment standing and defoaming 12h of 30 DEG C, forms casting solution; Being poured over by casting solution on the clean glass plate of 25 DEG C, is that casting solution applies on a glass by the scraper of 250 μm uniformly with thickness; Immediately 200 object polyester webs are covered casting solution surface, go to rapidly in the baking oven of 50 DEG C the 60s that volatilizees; Glass plate with casting solution is placed in the deionized water coagulation bath 6h of 5 DEG C of flowings; The diaphragm of new life and glass plate are peeled off, is placed in the water-bath 10min of 90 DEG C, obtains Cellulose acetate forward osmotic membrane.
The forward osmosis membrane thickness that this embodiment obtains is 217 μm, and porosity is 72.6%.This forward osmosis membrane, is tested as material liquid using deionized water for drawing agent with 1mol/LNaCl solution, stabilization time 30min, the testing time is 2h, carries out relevant parameter calculating according to data in the testing time.As calculated, this forward osmosis membrane flux is 13.4Lm-2h-1, and accumulation of salt in the surface soil permeation flux is 29.9gm-2h-1, and salt-stopping rate is 96.0%.
Embodiment 3
Take the cellulose acetate powder of 17g drying, be dissolved in the mixed solvent be made up of 10g acetone and 73gNMP, be placed in the water-bath of 45 DEG C, mechanical agitation is to forming uniform solution; This solution is placed in the vacuum environment standing and defoaming 18h of 45 DEG C, forms casting solution; Being poured over by casting solution on the clean glass plate of 15 DEG C, is that casting solution applies on a glass by the scraper of 200 μm uniformly with thickness; Immediately 150 object polyester webs are covered casting solution surface, go to rapidly in the baking oven of 20 DEG C the 90s that volatilizees; Glass plate with casting solution is placed in the deionized water coagulation bath 12h of 0 DEG C of flowing; The diaphragm of new life and glass plate are peeled off, is placed in the water-bath 20min of 80 DEG C, obtains Cellulose acetate forward osmotic membrane.
The forward osmosis membrane thickness that this embodiment obtains is 176 μm, and porosity is 71.7%.This forward osmosis membrane, is tested as material liquid using deionized water for drawing agent with 1mol/LNaCl solution, stabilization time 30min, the testing time is 2h, carries out relevant parameter calculating according to data in the testing time.As calculated, this forward osmosis membrane flux is 11.2Lm-2h-1, and accumulation of salt in the surface soil permeation flux is 21.3gm-2h-1, and salt-stopping rate is 96.6%.
Embodiment 4
Take the cellulose acetate powder of 17g drying, be dissolved in the mixed solvent be made up of 15g acetone and 68gNMP, be placed in the water-bath of 45 DEG C, mechanical agitation is to forming uniform solution; This solution is placed in the vacuum environment standing and defoaming 18h of 45 DEG C, forms casting solution; Being poured over by casting solution on the clean glass plate of 25 DEG C, is that casting solution applies on a glass by the scraper of 200 μm uniformly with thickness; Immediately 150 object polyester webs are covered casting solution surface, go to rapidly in the baking oven of 70 DEG C the 30s that volatilizees; Glass plate with casting solution is placed in the deionized water coagulation bath 12h of 5 DEG C of flowings; The diaphragm of new life and glass plate are peeled off, is placed in the water-bath 10min of 90 DEG C, obtains Cellulose acetate forward osmotic membrane.
The forward osmosis membrane thickness that this embodiment obtains is 185 μm, and porosity is 70.3%.This forward osmosis membrane, is tested as material liquid using deionized water for drawing agent with 1mol/LNaCl solution, stabilization time 30min, the testing time is 2h, carries out relevant parameter calculating according to data in the testing time.As calculated, this forward osmosis membrane flux is 7.9Lm-2h-1, and accumulation of salt in the surface soil permeation flux is 10.3gm-2h-1, and salt-stopping rate is 97.7%.
Embodiment 5
Take the cellulose acetate powder of 17g drying, be dissolved in the mixed solvent be made up of 20g acetone and 63gNMP, be placed in the water-bath of 45 DEG C, mechanical agitation is to forming uniform solution; This solution is placed in the vacuum environment standing and defoaming 18h of 45 DEG C, forms casting solution; Being poured over by casting solution on the clean glass plate of 30 DEG C, is that casting solution applies on a glass by the scraper of 200 μm uniformly with thickness; Immediately 150 object polyester webs are covered casting solution surface, go to rapidly in the baking oven of 40 DEG C the 70s that volatilizees; Glass plate with casting solution is placed in the deionized water coagulation bath 12h of 5 DEG C of flowings; The diaphragm of new life and glass plate are peeled off, is placed in the water-bath 20min of 80 DEG C, obtains Cellulose acetate forward osmotic membrane.
The forward osmosis membrane thickness that this embodiment obtains is 182 μm, and porosity is 69.8%.This forward osmosis membrane, is tested as material liquid using deionized water for drawing agent with 1mol/LNaCl solution, stabilization time 30min, the testing time is 2h, carries out relevant parameter calculating according to data in the testing time.As calculated, this forward osmosis membrane flux is 9.7Lm-2h-1, and accumulation of salt in the surface soil permeation flux is 17.4gm-2h-1, and salt-stopping rate is 96.8%.
Embodiment 6
Take the cellulose acetate powder of 20g drying, be dissolved in the mixed solvent be made up of 5g acetone and 75gNMP, be placed in the water-bath of 55 DEG C, mechanical agitation is to forming uniform solution; This solution is placed in the vacuum environment standing and defoaming 24h of 55 DEG C, forms casting solution; Being poured over by casting solution on the clean glass plate of 25 DEG C, is that casting solution applies on a glass by the scraper of 150 μm uniformly with thickness; Immediately 100 object polyester webs are covered casting solution surface, go to rapidly in the baking oven of 25 DEG C the 90s that volatilizees; Glass plate with casting solution is placed in the deionized water coagulation bath 18h of 10 DEG C of flowings; The diaphragm of new life and glass plate are peeled off, is placed in the water-bath 40min of 70 DEG C, obtains Cellulose acetate forward osmotic membrane.
The forward osmosis membrane thickness that this embodiment obtains is 115 μm, and porosity is 68.9%.This forward osmosis membrane, is tested as material liquid using deionized water for drawing agent with 1mol/LNaCl solution, stabilization time 30min, the testing time is 2h, carries out relevant parameter calculating according to data in the testing time.As calculated, this forward osmosis membrane flux is 12.2Lm-2h-1, and accumulation of salt in the surface soil permeation flux is 15.9gm-2h-1, and salt-stopping rate is 97.7%.
Embodiment 7
Take the cellulose acetate powder of 20g drying, be dissolved in the mixed solvent be made up of 10g acetone and 70gDMF (DMF), be placed in the water-bath of 55 DEG C, mechanical agitation is to forming uniform solution; This solution is placed in the vacuum environment standing and defoaming 20h of 55 DEG C, forms casting solution; Being poured over by casting solution on the clean glass plate of 20 DEG C, is that casting solution applies on a glass by the scraper of 150 μm uniformly with thickness; Immediately 100 object polyester webs are covered casting solution surface, go to rapidly in the baking oven of 80 DEG C the 10s that volatilizees; Glass plate with casting solution is placed in the deionized water coagulation bath 18h of 20 DEG C of flowings; The diaphragm of new life and glass plate are peeled off, is placed in the water-bath 40min of 70 DEG C, obtains Cellulose acetate forward osmotic membrane.
The forward osmosis membrane thickness that this embodiment obtains is 119 μm, and porosity is 67.4%.This forward osmosis membrane, is tested as material liquid using deionized water for drawing agent with 1mol/LNaCl solution, stabilization time 30min, the testing time is 2h, carries out relevant parameter calculating according to data in the testing time.As calculated, this forward osmosis membrane flux is 9.1Lm-2h-1, and accumulation of salt in the surface soil permeation flux is 40.8gm-2h-1, and salt-stopping rate is 92.0%.
Embodiment 8
Take the cellulose acetate powder of 25g drying, be dissolved in the mixed solvent be made up of 75gDMAc (DMA), be placed in the water-bath of 55 DEG C, mechanical agitation is to forming uniform solution; This solution is placed in the vacuum environment standing and defoaming 24h of 55 DEG C, forms casting solution; Being poured over by casting solution on the clean glass plate of 20 DEG C, is that casting solution applies on a glass by the scraper of 100 μm uniformly with thickness; Immediately 100 object polyester webs are covered casting solution surface, go to rapidly in the baking oven of 50 DEG C the 60s that volatilizees; Glass plate with casting solution is placed in the deionized water coagulation bath 24h of 25 DEG C of flowings; The diaphragm of new life and glass plate are peeled off, is placed in the water-bath 60min of 50 DEG C, obtains Cellulose acetate forward osmotic membrane.
The forward osmosis membrane thickness that this embodiment obtains is 82 μm, and porosity is 65.7%.This forward osmosis membrane, is tested as material liquid using deionized water for drawing agent with 1mol/LNaCl solution, stabilization time 30min, the testing time is 2h, carries out relevant parameter calculating according to data in the testing time.As calculated, this forward osmosis membrane flux is 14.8Lm-2h-1, and accumulation of salt in the surface soil permeation flux is 109.8gm-2h-1, and salt-stopping rate is 86.7%.
The above; be only the present invention's preferably detailed description of the invention, but protection scope of the present invention is not limited thereto, is anyly familiar with those skilled in the art in the technical scope that the present invention discloses; the change that can expect easily or replacement, all should be encompassed within protection scope of the present invention.
Claims (5)
1. a preparation method for Cellulose acetate forward osmotic membrane, is characterized in that, the method realizes as follows:
1) joined by the cellulose acetate of the drying of 15-25 weight portion in the organic solvent of 75-85 weight portion, in the water bath of 30-55 DEG C, mechanical agitation makes cellulose acetate dissolves completely, evenly;
2) by Homogeneous phase mixing liquid obtained above more than standing and defoaming 12h in the vacuum environment of 30-55 DEG C, casting solution is obtained;
3) being poured on the cleaned glass plate of 15-30 DEG C by the casting solution after standing and defoaming, is that casting solution is coated into the uniform casting film liquid layer of thickness by 100-250 μm of scraper with thickness;
4) by smooth for clean polyester webs cover to be positioned in the baking oven of 20-80 DEG C after on casting film liquid layer volatilize between 10-90s:
5) then go in the deionized water coagulation bath of flowing by above-mentioned casting solution, deionized water coagulation bath temperature controls between 0-25 DEG C, and gel time controls between 6-24h, obtains newborn cellulose acetate diaphragm:
6) be placed in deionized water heat-treat departing from obtained newborn cellulose acetate diaphragm from glass plate, deionized water temperature controls between 50-90 DEG C, and heat treatment time controls, between 10-60min, to obtain Cellulose acetate forward osmotic membrane.
2. Cellulose acetate forward osmotic membrane preparation method according to claim 1, is characterized in that, in the indoor environment in the process of preparation, temperature controls at 15-30 DEG C, and relative humidity controls at 30-75%.
3. Cellulose acetate forward osmotic membrane preparation method according to claim 1, is characterized in that, step 1) described in cellulose acetate be cellulose diacetate, weight average molecular weight is 3-10 ten thousand.
4. Cellulose acetate forward osmotic membrane preparation method according to claim 1, is characterized in that, step 1) described in organic solvent be acetone, DMF, DMA, one or both in 1-METHYLPYRROLIDONE.
5. Cellulose acetate forward osmotic membrane preparation method according to claim 1, is characterized in that, step 4) in polyester mesh number be 100-200 order.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106046403A (en) * | 2016-05-31 | 2016-10-26 | 江苏师范大学 | Preparation method of composite proton exchange membrane based on hydrophilic porous supporting body |
| CN107855007A (en) * | 2017-07-13 | 2018-03-30 | 枫科(北京)膜技术有限公司 | A kind of asymmetric forward osmosis membrane and preparation method thereof |
| CN112452152A (en) * | 2020-11-17 | 2021-03-09 | 江苏通用环保集团有限公司 | Mineralized modified cellulose composite forward osmosis membrane material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104437117A (en) * | 2014-11-27 | 2015-03-25 | 新疆德蓝股份有限公司 | Preparation method of cellulose acetate forward osmosis membrane for bitter water desalting |
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2016
- 2016-02-04 CN CN201610080870.3A patent/CN105561808A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104437117A (en) * | 2014-11-27 | 2015-03-25 | 新疆德蓝股份有限公司 | Preparation method of cellulose acetate forward osmosis membrane for bitter water desalting |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106046403A (en) * | 2016-05-31 | 2016-10-26 | 江苏师范大学 | Preparation method of composite proton exchange membrane based on hydrophilic porous supporting body |
| CN106046403B (en) * | 2016-05-31 | 2019-01-11 | 江苏师范大学 | The preparation method of compound proton exchange membrane based on hydrophilic porous supporter |
| CN107855007A (en) * | 2017-07-13 | 2018-03-30 | 枫科(北京)膜技术有限公司 | A kind of asymmetric forward osmosis membrane and preparation method thereof |
| CN112452152A (en) * | 2020-11-17 | 2021-03-09 | 江苏通用环保集团有限公司 | Mineralized modified cellulose composite forward osmosis membrane material and preparation method thereof |
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