CN103816811B - A kind of preparation method of organic forward osmosis membrane - Google Patents
A kind of preparation method of organic forward osmosis membrane Download PDFInfo
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- CN103816811B CN103816811B CN201410065806.9A CN201410065806A CN103816811B CN 103816811 B CN103816811 B CN 103816811B CN 201410065806 A CN201410065806 A CN 201410065806A CN 103816811 B CN103816811 B CN 103816811B
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Abstract
The invention discloses the preparation method of a kind of organic forward osmosis membrane, all added with nano particle in its preparation method, concrete preparation be divided into proportioning, stir, stand, several steps such as coating.Organic forward osmosis membrane that the present invention makes not only significantly improves the hydrophily of film, decreases interior concentration polarization, improves permeation flux, remains high rejection, dramatically increase anti-microbial property and due to nanometer particle size, also enhance film strength, more practical.
Description
Technical field
The utility model relates to the preparation method of a kind of permeable membrane, particularly relates to the system of a kind of organic forward osmosis membrane
Preparation Method, belongs to technical field of membrane separation.
Background technology
FO (Forward Osmosis) technology is a kind of osmotic drive membrane process, has low energy consumption, low dirt
The features such as dye, high recovery, in desalinization, waste water processes, and the energy generates electricity, food processing, drug concentration
Real or potential application prospect is had in field.But, owing to lacking efficient FO membrane material, greatly
The development of restriction FO technology.The membrane material being currently used for FO process all has unsymmetric structure, by thin selection
, during FO, all there is outer concentration polarization and interior concentration polarization, especially in separating layer and porous support layer composition
It is interior concentration polarization, causes the actual water flux of FO film to be far smaller than theoretical water flux.Under normal circumstances, outer dense
Difference polarization occurs in the interface of film Yu solution, can be alleviated by increasing the hydrodynamics such as flow velocity；In
Concentration polarization is phenomenon specific to FO process, and orientation according to film during FO, solute is many at film
Accumulation or dilution in the supporting layer of hole, formed and concentrate and the interior concentration polarization of dilution, greatly reduce film both sides
Osmotic pressure,effective poor.Interior concentration polarization occurs in porous support layer, it is difficult to by change external condition
Alleviate.Research shows interior concentration polarization and film open support Rotating fields (porosity, hole flexibility, thickness
Degree) and the physicochemical properties (hydrophilic and hydrophobic, selectivity) of membrane material itself have the biggest relation.?
Support layer thickness is the least, and porosity is the highest, and hole flexibility is the least, and hydrophily is the best, then membrane structure parameter is then got over
Little, interior concentration polarization is the least.
Its hydrophily of organic forward osmosis membrane that existing method makes is poor, and interior concentration polarization is big, permeation flux
Little, rejection is low and antibiotic property is poor, film strength is the highest, Practical Performance is bad.
Summary of the invention
In order to solve the weak point in the problems referred to above, the invention provides the preparation of a kind of organic forward osmosis membrane
Method.
For solving above technical problem, the technical solution used in the present invention is: the system of a kind of organic forward osmosis membrane
Preparation Method, its preparation method is:
By volume percentages, employing Triafol T is as polymer, by 13.1% Triafol T
Nanocrystalline with the chitin of 0.9% join the Isosorbide-5-Nitrae-dioxane by 57.8%, the acetone of 19.6% and 8.6%
Methyl alcohol composition mixed solvent in, at a temperature of 60 DEG C stir 9 hours dissolve formed content be 0.9%
The nanocrystalline casting solution of chitin；Stand more than 24h and make its complete deaeration；Casting solution is stirred through
It is coated on base material after standing and defoaming, and uses scraper to scrape formation bottom membrane on base material uniformly, by base material
On bed die layer stand 30 seconds in atmosphere, then bottom membrane is put in coagulation bath through inversion of phases gel become tool
Have the film of dense layer surface, and film be heat-treated 5 minutes in 50 DEG C of water-baths, after cleaning, obtain organic just
Permeable membrane being placed in 1% solution of sodium bisulfite saves backup；
Or by weight, weigh 20g polysulfone polymer, it is dissolved in 80g by DMA and poly-second
In the mixed solvent of glycol 400 composition, the ratio of DMA and PEG400 is 72: 8,
It is made into the polysulfones solution that polymer concentration is 20%；1g organic carbon nanometer is added in the polysulfones solution prepared
Pipe, at the casting solution of the organic carbon nanotube that ultrasonic middle dispersion is made into containing 1wt% for 30 minutes, stirs casting solution
Mix uniformly, be coated on base material after standing and defoaming, and use scraper to scrape formation counterdie on base material uniformly
Layer, puts into gel film forming in coagulation bath by bed die layer, uses m-phenylene diamine (MPD) and pyromellitic trimethylsilyl chloride in formation
Carry out interface polymerization reaction on film, react 3 minutes at 110 DEG C；By prepared film after interface polymerization reaction
Clean by deionized water, remove remaining organic solvent, thus prepare organic forward osmosis membrane；
Base material is selected from one or a combination set of polyester screen, non-woven fabrics, cotton, glass plate, curtain coating plate.
All added with nano particle in the preparation of three kinds of methods；Nano particle is nanocrystalline selected from chitin, nanometer has
Machine silicon, organic carbon nanotube, pyrene derivatives nano particle or a combination thereof.
In film liquid, the content of polymer is calculated as 10-18wt% or 10-20wt% or 10-by the gross weight of casting solution
22wt%；In described casting solution, the content of nano particle is calculated as 0.04-20wt% or 0.05 by casting solution gross weight
-10wt% or 0.1-5wt%.
The thickness of bottom membrane is 60-200 μm.
Organic forward osmosis membrane that the present invention makes not only significantly improves the hydrophily of film, decreases interior concentration polarization
Change, improve permeation flux, remain high rejection, dramatically increase anti-microbial property and due to nanometer particle size,
Also enhance film strength, more practical.
Detailed description of the invention
Being described in further detail the present invention below in conjunction with embodiment, the preparation process of organic forward osmosis membrane is such as
Under:
Preparation method:
Embodiment 1:
Employing Triafol T is as polymer, by 13.1% (V%) Triafol T and 0.9%
(V%) chitin is nanocrystalline joins the Isosorbide-5-Nitrae-dioxane by 57.8% (V%), 19.6% (V%)
Acetone and 8.6% (V%) methyl alcohol composition mixed solvent in, at a temperature of 60 DEG C stir 9 hours
Dissolve that to form content be the nanocrystalline casting solution of the chitin of 0.9% (V%)；Standing more than 24h makes it complete
Deaeration；Casting solution is stirred and is coated on base material after standing and defoaming, and use scraper to scrape uniformly
Form bottom membrane on base material, the bed die layer on base material is stood 30 seconds in atmosphere, then bottom membrane is put into
Coagulation bath (composition of coagulation bath is deionized water) becomes to have the film of dense layer surface through inversion of phases gel, and
Film is heat-treated 5 minutes in 50 DEG C of water-baths, after cleaning, be placed on 1% solution of sodium bisulfite preserves standby
With.
The flux of organic forward osmosis membrane prepared by the present embodiment is 19L m-2·h-1, rejection is more than 90%.
Prepared organic forward osmosis membrane carries out micro-life at identical conditions with the film of not plus nano organic filler
Thing pollutes and intensity experiment.On film surface plus e. coli microorganisms, microscope is used to see after 24h
Examine the microorganism adhesion condition on film surface, find that the film adding nanometer organic filler does not adds without microorganism attachment
The substantial amounts of microorganism of film surface attachment, indicate and add the film of nanometer organic filler and have the most antibacterial
Property, antibiotic rate is more than 90%.Film is tested on universal testing machine hot strength, by organic forward osmosis membrane with
The film of plus nano organic filler does not contrasts at identical conditions, finds that organic forward osmosis membrane hot strength improves
30%.
Embodiment 2:
Weigh 20g polysulfone polymer, be dissolved in 80g and be made up of DMA and PEG400
Mixed solvent in (the two ratio is 72: 8), be made into the polysulfones solution that polymer concentration is 20%；To preparing
Polysulfones solution in add 1g organic carbon nanotube, ultrasonic middle dispersion within 30 minutes, be made into containing 1wt% organic
The casting solution of CNT, stirs casting solution, is coated on base material after standing and defoaming, and use
Formation bottom membrane on base material scraped uniformly by scraper, bed die layer is put into gel film forming in coagulation bath, between employing
Phenylenediamine and pyromellitic trimethylsilyl chloride carry out interface polymerization reaction on the film formed, and react 3 points at 110 DEG C
Clock；After interface polymerization reaction, prepared film deionized water is cleaned, remove remaining organic solvent, from
And prepare organic forward osmosis membrane.
The water flux of organic forward osmosis membrane prepared by the present embodiment is 17L m-2·h-1, rejection 90% with
On.
Prepared film is carried out microorganism and pollutes experiment, on film surface plus e. coli microorganisms, pass through
Use microscope to observe the microorganism adhesion condition on film surface after 24h, find that its surface is adhered to without microorganism,
Showing that this film has obvious anti-microbial property, antibiotic rate is more than 90%.Film is tested on universal testing machine and draws
Stretch intensity, the film of organic forward osmosis membrane with not plus nano organic filler is contrasted at identical conditions, find
Organic forward osmosis membrane hot strength improves 25%.
Base material is selected from one or a combination set of polyester screen, non-woven fabrics, cotton, glass plate, curtain coating plate.
Nano particle is nanocrystalline selected from chitin, nano-organosilicon, organic carbon nanotube, pyrene derivatives nanometer
Particle or a combination thereof.
In casting solution, the content of polymer is calculated as 10-18wt% or 10-20wt% or 10-by the gross weight of casting solution
22wt%；In casting solution, the content of nano particle is calculated as 0.04-20wt% or 0.05-by casting solution gross weight
10wt% or 0.1-5wt%.
The thickness of bottom membrane is 60-180 μm or 60-200 μm.
Claims (4)
1. the preparation method of an organic forward osmosis membrane, it is characterised in that: its preparation method is:
By volume percentages, employing Triafol T is as polymer, by 13.1% Triafol T
Nanocrystalline with the chitin of 0.9% join the Isosorbide-5-Nitrae-dioxane by 57.8%, the acetone of 19.6% and 8.6%
Methyl alcohol composition mixed solvent in, at a temperature of 60 DEG C stir 9 hours dissolve formed content be 0.9%
The nanocrystalline casting solution of chitin；Stand more than 24h and make its complete deaeration；Casting solution is stirred through
It is coated on base material after standing and defoaming, and uses scraper to scrape formation bottom membrane on base material uniformly, by base material
On bed die layer stand 30 seconds in atmosphere, then bottom membrane is put in coagulation bath through inversion of phases gel become tool
Have the film of dense layer surface, and film be heat-treated 5 minutes in 50 DEG C of water-baths, after cleaning, obtain organic just
Permeable membrane being placed in 1% solution of sodium bisulfite saves backup.
The preparation method of organic forward osmosis membrane the most according to claim 1, it is characterised in that: described base
Material is selected from one or a combination set of polyester screen, non-woven fabrics, cotton, glass plate, curtain coating plate.
The preparation method of organic forward osmosis membrane the most according to claim 1, it is characterised in that: described side
All added with nano particle in the preparation of method；Described nano particle is selected from nano-organosilicon, pyrene derivatives nanoparticle
Son or a combination thereof.
The preparation method of organic forward osmosis membrane the most according to claim 1, it is characterised in that: the described end
The thickness of film layer is 60-200 μm.
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| CN201410065806.9A CN103816811B (en) | 2014-02-26 | 2014-02-26 | A kind of preparation method of organic forward osmosis membrane |
| CN201610237369.3A CN105664732B (en) | 2014-02-26 | 2014-02-26 | A kind of preparation method of organic forward osmosis membrane |
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Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104174299B (en) * | 2014-07-30 | 2017-06-23 | 中国海洋大学 | High flux forward osmosis membrane based on ultra-thin supporting layer and preparation method thereof |
| CN104147943A (en) * | 2014-08-15 | 2014-11-19 | 武汉大学 | Preparation method and application of high-molecular forward osmosis membrane |
| CN104174304B (en) * | 2014-09-12 | 2016-06-29 | 天津工业大学 | A kind of preparation method of anti-pollution PVDF separation film |
| 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 |
| CN105289318A (en) * | 2015-11-18 | 2016-02-03 | 新疆德蓝股份有限公司 | Hollow fiber composite nanofiltration membrane and preparation method thereof |
| CN106582308B (en) * | 2016-12-01 | 2019-07-05 | 沁园集团股份有限公司 | A kind of chitin nanocomposite ps hollow fiber uf membrane and preparation method thereof |
| CN108452685A (en) * | 2018-02-13 | 2018-08-28 | 温州莲华环保科技有限公司 | A kind of compound forward osmosis membrane of high-performance and preparation method thereof |
| CN109289541A (en) * | 2018-11-07 | 2019-02-01 | 温州莲华环保科技有限公司 | A kind of preparation method of organic forward osmosis membrane |
| 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 |
| CN113491961B (en) * | 2021-09-09 | 2022-02-01 | 北京宝盛通国际电气工程技术有限公司 | Forward osmosis membrane and preparation method thereof |
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Effective date of registration: 20230714 Address after: No. 9 Xuecuo Lane, Gantang Town, Fu'an City, Ningde City, Fujian Province, 355009 Patentee after: Xue Lixin Address before: 315499 Floor 3, Incubation Building, No. 4, Science and Technology Entrepreneurship Center, Yeshan Road, Chengdong New District, Yuyao City, Zhejiang Province Patentee before: NINGBO LIANHUA ENVIRONMENTAL SCIENCE AND TECHNOLOGY Co.,Ltd. |
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