CN102139189B - Method for preparing seawater desalting electro-filtration ionic membrane - Google Patents
Method for preparing seawater desalting electro-filtration ionic membrane Download PDFInfo
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- CN102139189B CN102139189B CN2011100268562A CN201110026856A CN102139189B CN 102139189 B CN102139189 B CN 102139189B CN 2011100268562 A CN2011100268562 A CN 2011100268562A CN 201110026856 A CN201110026856 A CN 201110026856A CN 102139189 B CN102139189 B CN 102139189B
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A20/00—Water conservation; Efficient water supply; Efficient water use
- Y02A20/124—Water desalination
- Y02A20/131—Reverse-osmosis
Abstract
The invention relates to a method for preparing a seawater desalting electro-filtration ionic membrane, which is characterized by comprising the following steps of: cooling and knifing mixed solution of a polymer and a solvent, then adding cross linker and conductive filler to perform cross linking reaction, and preparing the membrane. The preparation method is simple, is easily controlled, and can realize continuous production; compared with the prior art, actual test proves that the tensile strength of the seawater desalting electro-filtration ionic membrane prepared by adopting the method for preparing the seawater desalting electro-filtration ionic membrane can reach 13.2MPa, and the electric conductivity can be 10.4omega.cm; and the method has the remarkable advantages that the operation process is simple and convenient, the cost is low, the prepared membrane has good performance and the like.
Description
Technical field
The invention belongs to desalinization membrane technology field, the preparation method of specifically a kind of long service life, the simple desalinization electrofiltration of operating procedure ionic membrane.
Background technology
As everyone knows; Different films has different microstructures and function; Need prepare with diverse ways, membrane preparation method is the core research topic in film field always, successfully is used for seawater desalination from nineteen sixty Loeb and Sourirajan invention cellulose acetate anisotropic membrane; In decades, membrane technology has obtained flourish.At present, domestic and international main film manufacturer is like U.S. Dow Chem company, Hydranautics company, Koch company; Japan Nitto Denko company, Toray company; Korea S Saehan company, spring company of CHINA COLLECTED TongYuan etc. have developed the multi-series membrane module.Existing film preparation technology has fusion drawn, solution deposition, thermic to be separated three kinds.Using is the thermic phase disengagement method comparatively widely.Industrialized at present film majority is processed by materials such as polypropylene, polyethylene, polytetrafluoroethylene (PTFE), aromatic polyamide, polysulfones; They have good heat endurance and chemical resistance; But poor because of these material hydrophilies, be prone to cause solute absorption and fenestra to stop up, make that separating effect descends in the film separating process; And because its wettability not, the higher barometric gradient of needs just can make water infiltrate fenestra when water treatment is used.On the other hand, traditional hydrophilic film, for example film such as cellulose acetate because mechanical strength, heat endurance and chemical resistance are relatively poor, also has certain limitation in the use.Along with developing rapidly and extensively utilization of membrane technology, the research of charged membrane is more and more general.The charged membrane material has polarity group, and after solution contacted, the film surface was charged, attracts the different charge species of polarity, because high relative molecular mass and the surface charge held back, its average permeation flux is much larger than charged membrane not.Existing charged membrane is still pressure-driven; Utilize its separating property to realize relative separation to ion to special ion; Though there is faint electric field in the charged membrane course of work; Problems such as membrane process fouling, microbial contamination can not be effectively solved but electric-field intensity is too little, still various chemical agents need be added.Therefore, a kind of preparation method that can lean on electrically driven (operated) desalinization electrofiltration ionic membrane need be provided.
Summary of the invention
The objective of the invention is to propose to have certain mechanical strength and excellent conducting performance, be not easy to pollute the preparation method of deterioration, long service life, the simple desalinization electrofiltration of operating procedure ionic membrane.
A kind of preparation method of desalinization electrofiltration ionic membrane, be with polymer and solvent in reactor, be heated with stirring to 50 ℃-90 ℃; After treating to be dissolved into homogeneous phase fully, crosslinking agent and conductive filler are added in the above-mentioned solution, keep above temperature to stir 10min; With mix products cooling cooling knifing; Cross-linking reaction 1-4h makes the electrofiltration ionic membrane under 100 ℃ of temperature at last, and wherein, the rate of charge of polymer, solvent, crosslinking agent, conductive filler is controlled as follows: polymer and solvent quality are than scope 1:4-40; Polymer and conductive filler quality be than scope 1:0.2-0.8, and solvent and crosslinking agent quality are than scope 200-800:1.
Polymer is the ethenol copolymer with hydroxyl among the present invention; Crosslinking agent is the organic acid that esterification can take place; Conductive filler is to have electric conductivity, thermal conductivity, corrosion resistant metal or inorganic non-metallic powder; Solvent is deionized water, dimethyl sulfoxide (DMSO) or xylenes.
Among the present invention, can polymer, solvent, crosslinking agent, conductive filler be added simultaneously in the feeding method.
The present invention waters film with the mixed solution cooling of polymer and conductive filler; Make through cross-linking reaction have excellent hydrophilic, the electrofiltration ionic membrane of electric conductivity and mechanical strength; Preparation method proposed by the invention is simple and convenient, and cost is low, and the film properties that makes is good.
Description of drawings
Accompanying drawing 1 is the dissolution time situation sketch map of polyvinyl alcohol of the present invention.
Accompanying drawing 2 is the sketch mapes that concern of polyvinyl alcohol of the present invention and deionized water volume.
Accompanying drawing 3 is film formation time situation sketch mapes of polyvinyl alcohol of the present invention.
Accompanying drawing 4 is consumption of oxalic acid of the present invention sketch mapes that influence to electrofiltration ionic membrane thickness.
Accompanying drawing 5 is the graphite-filled amount of the present invention sketch mapes that influence to electrofiltration ionic membrane thickness.
Reference numeral: polyvinyl alcohol content X1; Dissolution time Y1; Polyvinyl alcohol content X2; Polyvinyl alcohol and deionized water volume Y2; The volume 1 of polyvinyl alcohol; The volume 2 of deionized water; Polyvinyl alcohol content X3; Film formation time Y3; Ethanedioic acid consumption X4; Electrofiltration ionic membrane thickness Y4; The ethanedioic acid consumption was to the influence curve 3 of electrofiltration ionic membrane thickness when polyvinyl alcohol was 6.7wt% adding 1g graphite; The ethanedioic acid consumption was to the influence curve 4 of electrofiltration ionic membrane thickness when polyvinyl alcohol was 6.7wt% adding 2g graphite; The ethanedioic acid consumption was to the influence curve 5 of electrofiltration ionic membrane thickness when polyvinyl alcohol 6.7wt% was adding 3g graphite; The ethanedioic acid consumption was to the influence curve 6 of electrofiltration ionic membrane thickness when polyvinyl alcohol was 6.7wt% adding 4g graphite; Graphite-filled amount X5; Electrofiltration ionic membrane thickness Y5.
The specific embodiment:
Below in conjunction with accompanying drawing and embodiment the present invention is further described:
The preparation method of a kind of desalinization electrofiltration ionic membrane that the present invention proposes, be with polymer and solvent in reactor, be heated with stirring to 50 ℃-90 ℃; After treating to be dissolved into homogeneous phase fully; Crosslinking agent and conductive filler are added in the above-mentioned solution, keep above temperature to stir 10min, with mix products cooling cooling knifing; Cross-linking reaction 1-4h under 100 ℃ of temperature at last; Wherein, the rate of charge of polymer, solvent, crosslinking agent, conductive filler is controlled as follows: polymer and solvent quality be than scope 1:4-40, and polymer and conductive filler quality are than scope 1:0.2-0.8; Solvent and crosslinking agent quality are than scope 200-800:1, and wherein polymer is the ethenol copolymer with hydroxyl; Crosslinking agent is the organic acid that esterification can take place; Conductive filler is to have electric conductivity, thermal conductivity, corrosion resistant metal or inorganic non-metallic powder; Solvent is deionized water, dimethyl sulfoxide (DMSO) or xylenes.
Wherein, Shown in accompanying drawing; Among the preparation method of desalinization electrofiltration ionic membrane, relate to the dissolving situation of polyvinyl alcohol, comprise the relation (as shown in Figure 2) of the concentration of polyvinyl alcohol and the relation of its dissolution time (as shown in Figure 1), different quality mark polyvinyl alcohol and deionized water volume; Relate to the film forming situation of polyvinyl alcohol, the film formation time (as shown in Figure 3), ethanedioic acid consumption that comprises the variable concentrations polyvinyl alcohol is to the influence (as shown in Figure 4) of film forming thickness, the graphite-filled amount influence (as shown in Figure 5) to film forming thickness.
Weighing polyvinyl alcohol 5g and solvent deionized water 75mL are disposed in the beaker, and sealing is to solution stirring heating 5h; Heating-up temperature keeps 70 ℃, and mixing speed is 1000r/min, after treating to be dissolved into homogeneous phase fully; Accurately take by weighing the 0.1g ethanedioic acid and add in the above-mentioned solution, continue heated and stirred 10min, accurately take by weighing the 2g graphite powder then and add in the above-mentioned solution; Continue agitating heating 20min, use the knifing brush to dip in and get the polyvinyl alcohol graphite mixed solution knifing on glass plate that configures, leave standstill 20min; The glass plate that will have knifing is dried 1h under 100 ℃ of temperature, make the electrofiltration ionic membrane.
Test result: the hot strength of the desalinization electrofiltration ionic membrane of gained is 9.1MPa, and resistivity is 14.0 Ω cm.
Weighing polyvinyl alcohol 5g and solvent deionized water 75mL are disposed in the beaker, and sealing is to solution stirring heating 5h; Heating-up temperature keeps 70 ℃, and mixing speed is 1000r/min, after treating to be dissolved into homogeneous phase fully; Accurately take by weighing the 0.1g ethanedioic acid and add in the above-mentioned solution, continue heated and stirred 10min, accurately take by weighing the 4g graphite powder then and add in the above-mentioned solution; Continue agitating heating 20min, use the knifing brush to dip in and get the polyvinyl alcohol graphite mixed solution knifing on glass plate that configures, leave standstill 20min; The glass plate that will have knifing is dried 3h under 100 ℃ of temperature, make the electrofiltration ionic membrane.
Test result: the hot strength of the desalinization electrofiltration ionic membrane of gained is 8.4MPa, and resistivity is 10.4 Ω cm.
Embodiment 3
Weighing polyvinyl alcohol 5g and solvent deionized water 75mL are disposed in the beaker, and sealing is to solution stirring heating 5h; Heating-up temperature keeps 70 ℃, and mixing speed is 1000r/min, after treating to be dissolved into homogeneous phase fully; Accurately take by weighing the 0.05g ethanedioic acid and add in the above-mentioned solution, continue heated and stirred 10min, accurately take by weighing the 1g graphite powder then and add in the above-mentioned solution; Continue agitating heating 20min, use the knifing brush to dip in and get the polyvinyl alcohol graphite mixed solution knifing on glass plate that configures, leave standstill 20min; The glass plate that will have knifing is dried 1h under 100 ℃ of temperature, make the electrofiltration ionic membrane.
Test result: the hot strength of the desalinization electrofiltration ionic membrane of gained is 13.2MPa, and resistivity is 16.4 Ω cm.
All can implement according to the said scope of above-mentioned instance content of the present invention, make respond well electrofiltration ionic membrane, the present invention not only is confined to above-mentioned instance.
The present invention compared with prior art; A kind of preparation method of desalinization electrofiltration ionic membrane is provided; Through actual test proof; Adopt the tensile strength of the desalinization electrofiltration ionic membrane of this method preparation can reach 13.2MPa, electrical conductivity can be low to moderate 10.4 Ω cm, and the present invention has that operating procedure is easy, cost is low, make significant advantages such as film properties is good.
Claims (5)
1. the preparation method of a desalinization electrofiltration ionic membrane is characterized in that polymer and solvent are placed reactor, is heated with stirring to 50 ℃-90 ℃; After treating to be dissolved into homogeneous phase fully, crosslinking agent and conductive filler are added in the above-mentioned solution, said conductive filler is for having electric conductivity, thermal conductivity, corrosion resistant metal or inorganic non-metallic powder; Keep above temperature to stir 10min; With mix products cooling cooling knifing, cross-linking reaction 1-4h makes the electrofiltration ionic membrane under 100 ℃ of temperature at last, wherein; The control of the rate of charge of polymer, solvent, crosslinking agent, conductive filler is as follows: polymer and solvent quality are than scope 1:4-40; Polymer and conductive filler quality be than scope 1:0.2-0.8, and solvent and crosslinking agent quality are than scope 200-800:1, and said polymer is the ethenol copolymer with hydroxyl.
2. the preparation method of a kind of desalinization electrofiltration ionic membrane according to claim 1 is characterized in that crosslinking agent is an ethanedioic acid.
3. the preparation method of a kind of desalinization electrofiltration ionic membrane according to claim 1 is characterized in that said conductive filler is a kind of of copper, graphite, CNT, carbon gel.
4. the preparation method of a kind of desalinization electrofiltration ionic membrane according to claim 1, one or more that it is characterized in that said solvent deionized water, dimethyl sulfoxide (DMSO), xylenes are mixed and made into.
5. the preparation method of a kind of desalinization electrofiltration ionic membrane according to claim 1 is characterized in that it is 10-20 ℃ that mix products is cooled to temperature range, carries out knifing again, cross-linking reaction makes the electrofiltration ionic membrane.
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Effective date of registration: 20170110 Address after: 264200 Weihai, Huancui, sheep sheep town, Phoenix Road, No. -985-7 Patentee after: Weihai Gerun Environmental Protection Technology Co.,Ltd. Address before: 264200 Weihai high tech Zone, Shandong Cultural West Road, No. 2 Patentee before: HARBIN INSTITUTE OF TECHNOLOGY (WEIHAI) |
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Denomination of invention: Preparation of electro filtration ion membrane for seawater desalination Effective date of registration: 20220728 Granted publication date: 20121226 Pledgee: Weihai City Commercial Bank Co.,Ltd. Park sub branch Pledgor: Weihai Gerun Environmental Protection Technology Co.,Ltd. Registration number: Y2022980011367 |