CN105214516B - The preparation method of high flux, the Electrospun nano-fibers milipore filter of high rejection - Google Patents
The preparation method of high flux, the Electrospun nano-fibers milipore filter of high rejection Download PDFInfo
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Abstract
The present invention is a kind of high flux, the preparation method of the Electrospun nano-fibers milipore filter of high rejection; bamboo fibre is used for coating liquid raw material; polyethyleneglycol diacrylate is crosslinking agent; ammonium persulfate is initiator and polyethylene glycol is protective agent, and it is that top layer protective layer, enhancement type nanometer cellulose layer handle filter membrane for third layer, non-woven fabrics as the second layer, electrostatic spinning layer for the composite water of the common four-layer structure of bottom using polyethylene glycol layer to use electrostatic spinning technique and spin coating cladding process to be prepared into a kind of.Not only aperture is small for nanofibre hyperfiltration membrane made from the inventive method, stability is high, and usage cycles length, resistance tocrocking are good, also has the advantages that flux height, rejection effect are good.
Description
Technical field
The present invention relates to a kind of milipore filter, a kind of high flux, the Electrospun nano-fibers of high rejection are particularly disclosed
The preparation method of milipore filter, obtained nanofibre hyperfiltration membrane aperture is small, stability is high, usage cycles length, resistance tocrocking are good, is
A kind of NEW TYPE OF COMPOSITE milipore filter.Product made from the inventive method is applied to the fields such as medicine, environmental protection, food.
Background technology
Bamboo fibre is a kind of cellulose fibre for extracting from the bamboo of growth naturally, be after cotton, fiber crops, hair, silk it
The fifth-largest natural fiber afterwards.Bamboo fibre is mainly used in the bamboo fibre fabric of craftwork manufacture, with bacteria growing inhibiting, cleans people
Body surrounding air, the function such as keep off infection.In addition to traditional application, how to be prepared into nano-cellulose and develop
Advanced nano composite material, uses it for the fields such as environmental protection, medicine, food and the energy, as grinding for competitively carrying out both at home and abroad
Study carefully problem.
Electrostatic spinning has been widely used for the system of nano fibrous membrane as a kind of effective technology for preparing nano material
It is standby.By changing the concentration, viscosity, flow velocity of spinning solution, institute's making alive can obtain the regulatable nanofiber of diameter.Pass through
The nano fibrous membrane that this method is obtained has open-celled structure good, high porosity, the advantages of specific surface area is big, and these are excellent
Performance correspondence, which is used in the fields such as environmental improvement, chemical petroleum, medicine food, has fine prospect.Electrospun nano-fibers film is outstanding
It is in feed separation, and the field such as sewage disposal provides efficient filter medium.
Surface cladding process is that a kind of constraints is few, the selection space of the easy to operate and type of skill and material it is very big into
Functional coating liquid can be uniformly coated on substrate surface by film method, this method, and to follow-up technical finesse, including
There is provided further possibility for phase separation, crosslinking, natural film forming, function modified etc..
The work principle of filter of milipore filter is to carrying out mechanical screening by the particles of solute size of film surface.Traditional ultrafiltration
Film has that porosity is low, pore structure closing causes that flux is small, the low shortcoming of rejection, and the film prepared by electrostatic spinning technique
Have the advantages that ultra-high throughput, modified space are big, be even thousands of times of the hundred times of traditional ultrafiltration membrane flux.Therefore with Static Spinning
Silk has high value in actual applications for the milipore filter that means are obtained, but in order to improve rejection, by electrostatic spinning
Tunica fibrosa is that substrate obtains defect of the milipore filter still with its original flux of reduction.
The content of the invention
The purpose of the present invention is to be to overcome existing water process ultrafiltration membrane flux is low, rejection is poor, resistance tocrocking is poor etc. to lack
Point is there is provided the preparation method of a kind of high flux, the Electrospun nano-fibers milipore filter of high rejection, and obtained nanofiber surpasses
Filter membrane has the advantages that flux is high, rejection effect is good, resistance tocrocking is good, stable chemical performance.
What the present invention was realized in：A kind of preparation of high flux, the Electrospun nano-fibers milipore filter of high rejection
Method, uses bamboo fibre for coating liquid raw material, and polyethyleneglycol diacrylate is crosslinking agent, and ammonium persulfate is initiator and poly-
Ethylene glycol is protective agent, and it is top layer protection with polyethylene glycol layer to use electrostatic spinning technique and spin coating cladding process to be prepared into a kind of
Layer, enhancement type nanometer cellulose layer be the second layer, electrostatic spinning layer be third layer, common four-layer structure that non-woven fabrics is bottom answers
The water-treated filter membrane of mould assembly.The major function layer of the structure of the milipore filter is by the acid treated coated with nano of electrostatic spinning layer
Cellulose gel, then the enhancement type nanometer cellulose layer formed after drying and electrostatic spinning layer composite bed.
The acid solution that the acid treatment is used for one or more of arbitrary proportions in hydrochloric acid, sulfuric acid, acetic acid, oxalic acid mixing
Thing, pH value is 2~6.
The molecular weight of described polyethyleneglycol diacrylate is the propylene of polyethylene glycol two in 200~2000, preparation process
Mass fraction of the acid esters in nano-cellulose mixed solution is 0.01~1%, and ammonium persulfate initiator is mixed in nano-cellulose
Mass fraction in solution is 0.001~0.01%.
The drying of the enhancement type nanometer cellulose layer, initiation temperature are 50~100 DEG C, and the time is 10~60 minutes.
Described is 6000~20000 as the polyethylene glycol layer molecular weight of top layer protective layer.
High flux, the Electrospun nano-fibers milipore filter of high rejection made from the inventive method are a kind of comprising four layers
The composite water processing filter membrane of structure：It is followed successively by nonwoven fabric base bottom and high-throughout Nanowire is obtained by method of electrostatic spinning
Tie up film layer；The film layer is carried out after acidleach profit, utilizes the nano-cellulose using bamboo fibre as raw material under certain pH environment in film
Layer surface formation gel, while the crosslinking agent added is to the further crosslinking of gel layer, obtains the stable enhancing of performance after solidification
Type nano-cellulose layer, finally uses polyethylene glycol（PEG）Film surface is protected.
The inventive method mainly including the preparation of bamboo pulp nano-cellulose, the application of electrostatic spinning technique, painting method with
And nano-cellulose, into the condition of gel, specific preparation process is as follows：
（1）Prepare bamboo pulp nano-cellulose suspension：
The first step：By the bamboo fibre powder of 1~10 parts by weight be soaked in the mass fractions of 20~200 parts by weight for 5~
In 30% sodium hydroxide solution, temperature control stirs 1~3 hour at 30~80 DEG C, uses vavuum pump suction filtration, the bamboo obtained by washing
Pulp fibres obtain the bamboo pulp fiber powder of alkali process to neutrality after vacuum drying.Second step：In 2~70 DEG C of bath temperature conditions
Under, the fiber dust of the alkali process obtained by the first step is added to and fills TEMPO（2,2,6,6- tetramethyl piperidine -1- oxygen are free
Base）In the reactor of catalyst system and catalyzing, using the real-time monitoring of pH meters, sodium hydroxide solution or ice second of the mass fraction for 3% is added dropwise
Acid for adjusting pH value, to the constant rear addition absolute ethyl alcohol terminating reaction of pH value, the bamboo pulp nanofiber stablized after centrifugation
Plain suspension.
（2）Prepared polymer electrostatic spinning solution：
By the high molecular polymer magnetic agitation dissolving of spinning in a solvent, the spinning that mass fraction is 5~10% is obtained
Liquid.
（3）Electrostatic spinning：
By step（2）The polymer solution configured loads spinning head, and spinning is carried out under certain temperature humidity, is received
Rice tunica fibrosa.
（4）By step（3）The nano fibrous membrane pH value prepared is infiltrated for 2~6 acid solution, and remained on surface is removed afterwards
Acid solution.
（5）Preparation of nano cellulose coating solution：
By step（1）Nano-cellulose, 0.01~1% polyethylene glycol dipropyl of the mass fraction of preparation for 0.01~0.1%
Olefin(e) acid ester, 0.001~0.01% ammonium persulfate mixed liquor are coated with sol evenning machine, and being positioned over baking oven after standing 10~30 seconds enters
Row cross-linking reaction, temperature is 50~100 DEG C, and the time is 10~60 minutes, obtains nano-cellulose layer and is covered in spinning film layer.
（6）Polyethylene glycol（PGE）Coating：
Molecular weight is coated for 6000~20000 PEG with sol evenning machine, it is carried out in the case where temperature is 40~70 DEG C
Cross-linking reaction, forms the polyethylene glycol layer as protective layer.
The beneficial effects of the invention are as follows：Not only aperture is small for nanofibre hyperfiltration membrane made from the inventive method, stability is high,
And usage cycles length, resistance tocrocking are good, also have the advantages that flux height, rejection effect are good, be a kind of new MULTILAYER COMPOSITE
Milipore filter.
Embodiment
A kind of high flux of the present invention, the preparation method of the Electrospun nano-fibers milipore filter of high rejection, it is fine using bamboo
Tie up as coating liquid raw material, polyethyleneglycol diacrylate is crosslinking agent, and ammonium persulfate is initiator and polyethylene glycol is protection
Agent, uses electrostatic spinning technique and spin coating cladding process to be prepared into one kind with polyethylene glycol layer for top layer protective layer, enhancement type nanometer
Cellulose layer be the second layer, electrostatic spinning layer be third layer, the composite water for the common four-layer structure that non-woven fabrics is bottom treat
Filter membrane.Described is 6000~20000 as the polyethylene glycol layer molecular weight of top layer protective layer.The structure of the milipore filter it is main
Functional layer is by the acid treated coated with nano cellulose gel of electrostatic spinning layer, then the enhancement type nanometer formed after drying
The composite bed of cellulose layer and electrostatic spinning layer.The acid solution that the acid treatment is used is one in hydrochloric acid, sulfuric acid, acetic acid, oxalic acid
The mixture of kind or several arbitrary proportions, pH value is 2~6.The molecular weight of described polyethyleneglycol diacrylate be 200~
2000, mass fraction of the polyethyleneglycol diacrylate in nano-cellulose mixed solution is 0.01~1% in preparation process,
Mass fraction of the ammonium persulfate initiator in nano-cellulose mixed solution is 0.001~0.01%.The enhancement type nanometer is fine
The drying of the plain layer of dimension, initiation temperature are 50~100 DEG C, and the time is 10~60 minutes.
With reference to specific embodiment, the present invention is further elaborated.
Bamboo pulp fiber used in following examples is commercial goods, originates from Sichuan, and all reagents can be in traditional Chinese medicines collection
The purchase of chemical reagent Co., Ltd of group is obtained, and the pH meter used is the thunder magnetic that Shanghai INESA Scientific Instrument Co., Ltd. produces
PHS-25 types, digital display ultrasound homogenous disperse machine is Shanghai Sheng Xi ultrasonic instruments Co., Ltd DS-1510DTH types.
Embodiment 1：
（1）Under 60 DEG C of bath temperatures, 10.0g bamboo fibres powder is being soaked in the hydrogen-oxygen that 120g mass fractions are 10%
Change in sodium solution, stirred 1.5 hours with 400rpm mixing speed, use vavuum pump suction filtration, the bamboo pulp fiber obtained by washing is into
Property, bamboo pulp fiber powder is dried in vacuo, vacuum is 0.1MPa, drying temperature is 70 DEG C.
（2）Under 20 DEG C of temperature conditionss, weigh the alkali-treated fiber dusts of 5g be added to fill TEMPO 0.001g,
In the stirred tank of NaClO 15g and NaBr the 0.01g aqueous solution, speed of agitator is 700rpm, and 3% sodium hydroxide regulation body is added dropwise
Be pH values 11.0, using the real-time monitoring of pH meters, to pH value it is constant when, 5ml absolute ethyl alcohol terminating reactions are added, by turning
After fast 1000rpm centrifugations, supernatant is removed, bamboo pulp nano-cellulose sediment is obtained.
（3）Nano-cellulose made from 0.1g is dispersed in 100g deionized waters, while adding 0.4g polyethylene glycol two
Acrylate and 0.1g ammonium persulfates obtain final coating liquid.
（4）Weigh 10g polyacrylonitrile（PAN）It is dissolved in 90g N,N-dimethylformamides（DMF）, obtain transparent and homogeneous
Spinning solution, add it in shower nozzle, carry out electrostatic spinning, receptions substrate be polyester non-woven fabric, electrostatic spinning it is basic
Parameter is：Voltage 15kV, spout aperture 0.5mm, spinning solution flow velocity 0.002mm/s, spinning head to receive roller distance be
20cm, spinning environment temperature is 35 DEG C, and ambient relative humidity is 20%, obtains PAN microfiltration membranes.
（5）By step（4）Obtained PAN microfiltration membranes are infiltrated with pH for 4 hydrochloric acid solution, are positioned over and are scraped on film device, will
Step（3）The nano-cellulose coating liquid of 0.1% prepared is added in the gap of scraper and film surface, setting scraper and film surface
Distance be 50 μm, scraper translational speed is set to 1cm/s, starts motor, makes scraper to the nano-cellulose coating liquid of film surface
Uniformly scratched, after blade coating terminates, be dried 30 minutes, temperature is 60 DEG C.Obtain high hydrophilic fibrous layer, gather
Propylene nitrile layer and nonwoven fabric base bottom sandwich diaphragm.
（6）By the polyethylene glycol that molecular weight is 6000（PEG）Using step（5）Three layers to gained of described film mode
Composite film surface is coated, and coating is baked to after terminating, and drying temperature is 60 DEG C, and drying time is 30 minutes.Final
To PEG protective layers, high hydrophilic fibrous layer, four layers of composite membrane of polypropylene nitrile layer and nonwoven fabric base bottom.
The composite membrane prepared under 0.2MPa constant pressure, filtering test, the composite membrane are carried out using PEG6000
Pure water flux be 70L/m2H, rejection is 97%.
Embodiment 2：
（1）Under 70 DEG C of bath temperatures, 15.0g bamboo fibres powder is being soaked in the hydrogen-oxygen that 100g mass fractions are 20%
Change in sodium solution, stirred 1.5 hours with 400rpm mixing speed, use vavuum pump suction filtration, the bamboo pulp fiber obtained by washing is into
Property, bamboo pulp fiber powder is dried in vacuo, vacuum is 0.1MPa, drying temperature is 70 DEG C.
（2）Under 20 DEG C of temperature conditionss, weigh the alkali-treated fiber dusts of 5g be added to fill TEMPO 0.001g,
In the stirred tank of NaClO 15g and NaBr the 0.01g aqueous solution, speed of agitator is 700rpm, and 3% sodium hydroxide regulation body is added dropwise
Be pH values 11.0, using the real-time monitoring of pH meters, to pH value it is constant when, 5ml absolute ethyl alcohol terminating reactions are added, by turning
After fast 1000rpm centrifugations, supernatant is removed, bamboo pulp nano-cellulose sediment is obtained.
（3）Nano-cellulose made from 0.5g is dispersed in 100g deionized waters, while adding 0.2g polyethylene glycol two
Acrylate and 0.05g ammonium persulfates obtain final coating liquid.
（4）Weigh 10g polyacrylonitrile（PAN）It is dissolved in 90g N,N-dimethylformamides（DMF）, obtain transparent and homogeneous
Spinning solution, add it in shower nozzle, carry out electrostatic spinning, receptions substrate be polyester non-woven fabric, electrostatic spinning it is basic
Parameter is：Voltage 10kV, spout aperture 1.0mm, spinning solution flow velocity 0.002mm/s, spinning head to receive roller distance be
20cm, spinning environment temperature is 25 DEG C, and ambient relative humidity is 30%, obtains PAN microfiltration membranes.
（5）By step（4）Obtained PAN microfiltration membranes are infiltrated with pH for 5 hydrochloric acid solution, are positioned over and are scraped on film device, will
Step（3）The nano-cellulose coating liquid of 0.5% prepared is added in the gap of scraper and film surface, setting scraper and film surface
Distance be 50 μm, scraper translational speed is set to 1cm/s, starts motor, makes scraper to the nano-cellulose coating liquid of film surface
Uniformly scratched, after blade coating terminates, be dried 30 minutes, temperature is 60 DEG C.Obtain high hydrophilic fibrous layer, gather
Propylene nitrile layer and nonwoven fabric base bottom sandwich diaphragm.
（6）By the polyethylene glycol that molecular weight is 10000（PEG）Using step（5）Described film mode is to the three of gained
Layer composite film surface is coated, and coating is baked to after terminating, and drying temperature is 60 DEG C, and drying time is 30 minutes.Finally
Obtain PEG protective layers, high hydrophilic fibrous layer, four layers of composite membrane of polypropylene nitrile layer and nonwoven fabric base bottom.
The composite membrane prepared under 0.2MPa constant pressure, filtering test, the composite membrane are carried out using PEG6000
Pure water flux be 65L/m2H, rejection is 98%.
Claims (4)
1. a kind of preparation method of the Electrospun nano-fibers milipore filter of high flux, high rejection, it is characterised in that：Described
Electrospun nano-fibers milipore filter is to use electrostatic spinning technique and spin coating cladding process to be prepared into one kind to be with polyethylene glycol layer
Top layer protective layer, enhancement type nanometer cellulose layer be the second layer, electrostatic spinning layer be third layer, totally four layers that non-woven fabrics is bottom
The composite water processing filter membrane of structure, the major function layer of the Electrospun nano-fibers milipore filter is by electrostatic spinning layer
Acid treated coated with nano cellulose coating liquid simultaneously forms gel, then the enhancement type nanometer cellulose layer formed after drying
With the composite bed of electrostatic spinning layer, the acid solution that the acid treatment is used is the one or more in hydrochloric acid, sulfuric acid, acetic acid, oxalic acid
The mixture of arbitrary proportion, pH value is 2~6, and described nano-cellulose is the nano-cellulose using bamboo fibre as raw material, described
Nano-cellulose coating liquid be using nano-cellulose and polyethyleneglycol diacrylate of the mass fraction as 0.01~0.1%, mistake
The nano-cellulose mixed solution that ammonium sulfate is formulated, described enhancement type nanometer cellulose layer is to use bamboo fibre for nanometer
Cellulose coating liquid raw material, polyethyleneglycol diacrylate are that crosslinking agent, ammonium persulfate are described top layer made from initiator
Protective layer is that film surface is protected by protective agent of polyethylene glycol, is formed on described enhancement type nanometer cellulose layer surface
Protective layer.
2. the preparation method of the Electrospun nano-fibers milipore filter of high flux, high rejection according to claim 1,
It is characterized in that：The molecular weight of described polyethyleneglycol diacrylate is polyethylene glycol dipropyl in 200~2000, preparation process
Mass fraction of the olefin(e) acid ester in nano-cellulose mixed solution is 0.01~1%, and ammonium persulfate initiator is mixed in nano-cellulose
It is 0.001~0.01% to close the mass fraction in solution.
3. the preparation side of the Electrospun nano-fibers milipore filter of high flux, high rejection according to claim 1 or 2
Method, it is characterised in that：The drying of the enhancement type nanometer cellulose layer, initiation temperature are 50~100 DEG C, and the time is 10~60 points
Clock.
4. the preparation method of the Electrospun nano-fibers milipore filter of high flux, high rejection according to claim 1,
It is characterized in that：Described is 6000~20000 as the polyethylene glycol layer molecular weight of top layer protective layer.
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Effective date of registration: 20230302 Address after: Room 4065, Floor 4, Building 22, No. 85, Mingnan Road, Zhongshan Street, Songjiang District, Shanghai, 2016 Patentee after: Shanghai Zhanheng Environmental Protection Technology Co.,Ltd. Address before: 9B 2F, No. 100, Haike Road, Zhangjiang High-tech Park, Pudong New Area, Shanghai, October 2012 Patentee before: SHANGHAI JIESHENGYUAN TECH CO.,LTD. |