CN102418237A - Preparation method for electrostatic blended sugar-containing polyacrylonitrile (PAN) nano-fiber membrane - Google Patents

Preparation method for electrostatic blended sugar-containing polyacrylonitrile (PAN) nano-fiber membrane Download PDF

Info

Publication number
CN102418237A
CN102418237A CN2011102317205A CN201110231720A CN102418237A CN 102418237 A CN102418237 A CN 102418237A CN 2011102317205 A CN2011102317205 A CN 2011102317205A CN 201110231720 A CN201110231720 A CN 201110231720A CN 102418237 A CN102418237 A CN 102418237A
Authority
CN
China
Prior art keywords
pan
glucose
preparation
electrostatic
ethene fat
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN2011102317205A
Other languages
Chinese (zh)
Inventor
朱利民
李艳
权静
武晋娴
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Donghua University
Original Assignee
Donghua University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Donghua University filed Critical Donghua University
Priority to CN2011102317205A priority Critical patent/CN102418237A/en
Publication of CN102418237A publication Critical patent/CN102418237A/en
Pending legal-status Critical Current

Links

Images

Landscapes

  • Artificial Filaments (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)

Abstract

The invention relates to a preparation method for an electrostatic blended sugar-containing polyacrylonitrile (PAN) nano-fiber membrane, which comprises the steps of: 1) dissolving diacid divinyl esters and glucose into anhydrous pyridine and synthesizing glucose vinyl esters by using an enzymatic synthesis technique; adding ammonium persulfate into the glucose vinyl esters, using H2O as solvent and conducting polymerization under the protection of nitrogen to obtain glucose vinyl ester homopolymers; 2) adding dimethyl formamide (DMF) solution of the PAN into the glucose vinyl ester homopolymers to obtain PAN/glucose vinyl ester homopolymer spinning solution; and 3) conducting electrostatic spinning to the PAN/glucose vinyl ester homopolymer spinning solution to obtain a PAN/glucose vinyl ester superfine nano-fiber membrane, and finally drying. The preparation method provided by the invention has the advantages that the operation is simple, the product is easy to obtain and the method is economic and environmental-friendly; and the membrane material provided by the invention contains rich reactive hydrophilic active functional groups and has a potential of being used for subsequent relevant experimental analysis.

Description

A kind of electrostatic blended spinning contains the preparation method of sugared polyacrylonitrile nano tunica fibrosa
Technical field
The invention belongs to the preparation field of nano fibrous membrane, particularly a kind of electrostatic blended spinning contains the preparation method of sugared polyacrylonitrile nano tunica fibrosa.
Background technology
Electrostatic spinning is that a kind of charged Polymer Solution or melt of utilizing flows in electrostatic field and the technology of distortion preparation nanometer to the submicron-scale polymer fiber.With respect to the polymer fiber of conventional method preparation, the fiber that electro-spinning is equipped with has great specific area, and fiber surface has specific forms such as aperture.These characteristics make this fiber at aspects such as filtration, organizational project, hypersensitization sensors very big potential application foreground arranged.Characteristics such as electrostatic spinning also has simply, convenience, cheapness, thus people evoked to its great interest of furtheing investigate.
Polyacrylonitrile (PAN) is one type of commodity polymeric material, good, the anti-common solvent of its fibre forming property, not facile hydrolysis, anti-oxidant, chemically stable, and have excellent anti-bacterium aggressivity.Utilize electrostatic spinning technique, can prepare the PAN nanofiber simply and easily; The formed nano fibrous membrane of the unordered accumulation of PAN nanofiber then has high specific area and porosity, has mechanical strength preferably simultaneously, and its fibre morphology can also be regulated and control through preparation condition.These characteristics make this material demonstrate potential application foreground in fields such as bioengineering, composite, isolated by filtration, sensor and photoelectric devices.
Because its surperficial relative inertness and hydrophily are relatively poor; When separating as the aqueous solution; Especially for bio-medical field and other during with environment that biomolecule contacts, the polyacrylonitrile microporous barrier can with biomolecule generation non-specific interaction, cause protein, blood platelet etc. in a large amount of absorption in film surface; Cause film to pollute, have a strong impact on the military service stability of film.Therefore, be necessary the polyacrylonitrile microporous barrier is carried out surface modification, improve the hydrophily of film on the one hand, improve the contamination resistance of film, increase the service life; Give film on the other hand with new function, widen its range of application.
Summary of the invention
Technical problem to be solved by this invention provides the preparation method that a kind of electrostatic blended spinning contains sugared polyacrylonitrile nano tunica fibrosa; This method is simple to operate, product is prone to handle and economic environmental protection; This nano fibrous membrane has overcome the intrinsic defective of polyacrylonitrile; But contain abundant reactive hydrophilic activated functional groups, improved the non-specific adsorption of material surface and improved the biocompatibility of material surface.
A kind of electrostatic blended spinning of the present invention contains the preparation method of sugared polyacrylonitrile nano tunica fibrosa, comprising:
(1) diacid divinyl ester and glucose were dissolved in the anhydrous pyridine in 1: 1 in molar ratio~4: 1, utilize enzymatic synthetic technology synthesis of glucose ethene fat; In above-mentioned glucose ethene fat, add ammonium persulfate as initator, add H again 2O makes solvent, and stirring reaction 3-5h under 55-60 ℃ of nitrogen protection obtains glucose ethene fat homopolymers after the polymerisation end then;
(2) PAN is dissolved in DMF and obtains the PAN solution that concentration is 0.05~0.07g/ml, add above-mentioned glucose ethene fat homopolymers then, be stirred to dissolving fully, leave standstill then, get PAN/ glucose ethene fat homopolymers spinning solution;
(3) above-mentioned PAN/ glucose ethene fat homopolymers spinning solution is carried out electrostatic spinning and get PAN/ glucose ethene fat superfine nano tunica fibrosa, final drying promptly gets and contains sugared polyacrylonitrile nano tunica fibrosa.
Enzymatic synthetic technology described in the step (1) is: diacid divinyl ester and glucose were dissolved in 50~100mL anhydrous pyridine in 1: 1 in molar ratio~4: 1; Add 0.5~1.5g alkali protease; Putting into 40~60 ℃ of constant-temperature shaking culture casees reacted 3~5 days; Rotating speed is 210rpm, synthesis of glucose ethene fat;
Glucose ethene fat described in the step (1), its crude product separate with silica gel column chromatography purifies, and eluant, eluent is an ethyl acetate, and solvent is that volume ratio is ethyl acetate/methanol/water of 17: 3: 1, uses I 2Colour developing.
It is 0.2~2% that ammonium persulfate described in the step (1) accounts for glucose ethene lipid amount mark.
Adding H described in the step (1) 2After O made solvent, the concentration of glucose ethene fat was 2-3mol/L.
After polymerisation described in the step (1) finishes, with product through acetone precipitation and remove the glucose ethene fat that does not have reaction.
The mass fraction of glucose ethene fat homopolymers is 10%~90% in the PAN/ glucose ethene fat homopolymers spinning solution described in the step (2).
The mass fraction of glucose ethene fat homopolymers is 50%, 55%, 60%, 65% or 70% in the PAN/ glucose ethene fat homopolymers spinning solution described in the step (2).
The technological parameter of the electrostatic spinning described in the step (3) is: the syringe specification is 5ml; The syringe needle internal diameter is 0.4~0.7mm, ejection flow velocity 0.8~2ml/h, electrostatic pressure 10~18kv; Receiving screen adopts the reception of aluminium foil ground connection; Accepting distance is 10~20cm, adopts orthogonal method (change a certain parameter, fix other parameter) adjusting spinning parameter to carry out electricity and spin.
The diameter of the PAN/ glucose ethene fat superfine nano tunica fibrosa of gained is almost constant along with the increase of glucose ethene fat homopolymers mass fraction in the step (3), is 80~250nm.
Drying described in the step (3) is for putting into 40~60 ℃ of freeze-day with constant temperature 24~48h of vacuum drying chamber.
Sugar is a kind of in the biomolecule, extensively is present in the organism, and be the polyhydroxyl compound, have extremely strong hydrophily, therefore, the surface of introducing material to sugar is with the biocompatibility that effectively improves material surface.Therefore, sugar-containing polymer often is used to improve the non-specific adsorption of the material such as hydrophily and CKIs matter of material at material surface.
The present invention obtains diameter and aperture at nano level membrane material PAN/ glucose ethene fat superfine nano tunica fibrosa with polyacrylonitrile and glucose ethene lipid blend.This membrane material has overcome the intrinsic defective of polyacrylonitrile, but contains abundant reactive hydrophilic activated functional groups, has improved the non-specific adsorption of material surface and has improved the biocompatibility of material surface, has to use it and do the potentiality that follow-up related experiment is analyzed.
The present invention is main spinning material with PAN; And mix the good synthesis of glucose ethene fat homopolymers of surfaces for biocompatibility; Through adjustment solvent and relevant spinning condition parameter, successful realization blending, for the research and development of novel nano bioactive materials are offered reference.
Beneficial effect
(1) the present invention adopts the aqueous phase precipitation polymerization to prepare glucose ethene fat homopolymers, and the preparation method is simple to operate, product is prone to handle and economic environmental protection.
(2) membrane material of the present invention has overcome the intrinsic defective of polyacrylonitrile; But contain abundant reactive hydrophilic activated functional groups; Improved the non-specific adsorption of material surface and improved the biocompatibility of material surface, had and use it and do the potentiality that follow-up related experiment is analyzed.
Description of drawings
Fig. 1 is the stereoscan photograph that contains sugared polyacrylonitrile nano tunica fibrosa of Comparative Examples 1, embodiment 1-5 gained; Wherein the stereoscan photograph that contains sugared polyacrylonitrile nano tunica fibrosa of Comparative Examples 1, embodiment 1-5 is respectively (a) and (b) (c), (d), (e) and (f) (spinning voltage is 15kv; Receiving range is 15cm, and the injection flow velocity is 1.5ml/h);
Fig. 2 is the diameter that contains sugared polyacrylonitrile nano tunica fibrosa of Comparative Examples 1, embodiment 1-5 gained and the graph of a relation of glucose ethene fat homopolymers concentration; Wherein the mass fraction of glucose ethene fat homopolymers is respectively 0 (a), 50% (b), 55% (c), 60% (d), 65% (e) in the PAN/ glucose ethene fat homopolymers spinning solution, (electrostatic pressure is 15kv to 70% (f); Receiving range is 15cm, and the injection flow velocity is 1.5ml/h);
Fig. 3 is different monomers and hybrid films FT-IR resolution chart (a. glucose ethene fat; B. glucose ethene fat homopolymers; C.PAN/ glucose ethene fat homopolymers nano fibrous membrane; D.PAN)
The specific embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in the restriction scope of the present invention.Should be understood that in addition those skilled in the art can do various changes or modification to the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Embodiment 1
(1) with diacid divinyl ester and glucose according to a certain percentage (4: 1, mol ratio) be dissolved in the anhydrous pyridine, utilize enzymatic synthetic technology synthesis of glucose ethene fat.After reaction finished, crude product separates with silica gel column chromatography purified, and eluant, eluent is an ethyl acetate, solvent be ethyl acetate/methanol/water (17: 3: 1, v/v/v), develop the color with I2.Above-mentioned glycolipid is put in the micro-polymerization pipe, as initator, adds H with ammonium persulfate (APS) (accounting for glucose ethene lipid amount mark is 1.0) 2O makes solvent, and (monomer concentration is 2.5mol/LH 2O), sealing vacuumizes the logical nitrogen in back, repeated multiple times with oil pump.System is placed stirring reaction 3h under 55~60 ℃ of nitrogen protections.
(2) PAN of certain mass is dissolved in DMF and obtains the PAN solution that concentration is 0.06g/ml; Add the homopolymerization of glucose ethene fat then, make its shared mass fraction be respectively 50%, stirred for several hour is to dissolving fully, leaves standstill bubble to be stirred fully form the homogeneous spinning solution.
(3) extract PAN/ glucose ethene fat homopolymers with syringe, be fixed on the electrostatic spinning apparatus, control ejection flow velocity 1.5ml/h; Electrostatic pressure 15kv; Receiving screen adopts the reception of aluminium foil ground connection, and the distance of syringe needle and receiving screen is 10~20cm, adopts orthogonal method (to change a certain parameter; Fix other parameter) the different spinning parameters of adjusting carry out electricity and spin, and must diameter be the PAN/ glucose ethene fat homopolymers superfine nano tunica fibrosa of 80~250nm; Put into 60~80 ℃ of freeze-day with constant temperature 36h of vacuum drying chamber, process the regeneration nano composite membrane, its electromicroscopic photograph is shown in Fig. 1 (b), and diameter Distribution is shown in Fig. 2 (b).
Embodiment 2
(1) with diacid divinyl ester and glucose according to a certain percentage (3: 1, mol ratio) be dissolved in the anhydrous pyridine, utilize enzymatic synthetic technology synthesis of glucose ethene fat.After reaction finished, crude product separates with silica gel column chromatography purified, and eluant, eluent is an ethyl acetate, solvent be ethyl acetate/methanol/water (17: 3: 1, v/v/v), use I 2Colour developing.Above-mentioned glycolipid is put in the micro-polymerization pipe, as initator, adds H with ammonium persulfate (APS) (accounting for glucose ethene lipid amount mark is 1.0) 2O makes solvent, and (monomer concentration is 2.5mol/L H 2O), sealing vacuumizes the logical nitrogen in back, repeated multiple times with oil pump.System is placed stirring reaction 5h under 55~60 ℃ of nitrogen protections.
(2) PAN of certain mass is dissolved in DMF and obtains the PAN solution that concentration is 0.06g/ml; Add the homopolymerization of glucose ethene fat then, make its shared mass fraction be respectively 55%, stirred for several hour is to dissolving fully, leaves standstill bubble to be stirred fully form the homogeneous spinning solution.
(3) extract PAN/ glucose ethene fat homopolymers with syringe, be fixed on the electrostatic spinning apparatus, control ejection flow velocity 1.5ml/h; Electrostatic pressure 15kv; Receiving screen adopts the reception of aluminium foil ground connection, and the distance of syringe needle and receiving screen is 10~20cm, adopts orthogonal method (to change a certain parameter; Fix other parameter) the different spinning parameters of adjusting carry out electricity and spin, and must diameter be the PAN/ glucose ethene fat homopolymers superfine nano tunica fibrosa of 80-250nm; Put into 60~80 ℃ of freeze-day with constant temperature 24h of vacuum drying chamber, process the regeneration nano composite membrane, its electromicroscopic photograph is shown in Fig. 1 (c), and diameter Distribution is shown in Fig. 2 (c).
Embodiment 3
(1) with diacid divinyl ester and glucose according to a certain percentage (2: 1, mol ratio) be dissolved in the anhydrous pyridine, utilize enzymatic synthetic technology synthesis of glucose ethene fat.After reaction finished, crude product separates with silica gel column chromatography purified, and eluant, eluent is an ethyl acetate, solvent be ethyl acetate/methanol/water (17: 3: 1, v/v/v), use I 2Colour developing.Above-mentioned glycolipid is put in the micro-polymerization pipe, as initator, adds H with ammonium persulfate (APS) (accounting for glucose ethene lipid amount mark is 1.0) 2O makes solvent, and (monomer concentration is 2.5mol/L H 2O), sealing vacuumizes the logical nitrogen in back, repeated multiple times with oil pump.System is placed stirring reaction 4h under 55~60 ℃ of nitrogen protections.
(2) PAN of certain mass is dissolved in DMF and obtains the PAN solution that concentration is 0.06g/ml; Add the homopolymerization of glucose ethene fat then, make its shared mass fraction be respectively 60%, stirred for several hour is to dissolving fully, leaves standstill bubble to be stirred fully form the homogeneous spinning solution.
(3) extract PAN/ glucose ethene fat homopolymers with syringe, be fixed on the electrostatic spinning apparatus, control ejection flow velocity 1.5ml/h; Electrostatic pressure 15kv; Receiving screen adopts the reception of aluminium foil ground connection, and the distance of syringe needle and receiving screen is 10~20cm, adopts orthogonal method (to change a certain parameter; Fix other parameter) the different spinning parameters of adjusting carry out electricity and spin, and must diameter be the PAN/ glucose ethene fat homopolymers superfine nano tunica fibrosa of 80~250nm; Put into 60~80 ℃ of freeze-day with constant temperature 30h of vacuum drying chamber, process the regeneration nano composite membrane, its electromicroscopic photograph is shown in Fig. 1 (d), and diameter Distribution is shown in Fig. 2 (d).
Embodiment 4
(1) with diacid divinyl ester and glucose according to a certain percentage (4: 1, mol ratio) be dissolved in the anhydrous pyridine, utilize enzymatic synthetic technology synthesis of glucose ethene fat.After reaction finished, crude product separates with silica gel column chromatography purified, and eluant, eluent is an ethyl acetate, solvent be ethyl acetate/methanol/water (17: 3: 1, v/v/v), use I 2Colour developing.Above-mentioned glycolipid is put in the micro-polymerization pipe, as initator, adds H with ammonium persulfate (APS) (accounting for glucose ethene lipid amount mark is 1.0) 2O makes solvent, and (monomer concentration is 2.5mol/L H 2O), sealing vacuumizes the logical nitrogen in back, repeated multiple times with oil pump.System is placed stirring reaction 3h under 55~60 ℃ of nitrogen protections.
(2) PAN of certain mass is dissolved in DMF and obtains the PAN solution that concentration is 0.06g/ml; Add the homopolymerization of glucose ethene fat then, make its shared mass fraction be respectively 65%, stirred for several hour is to dissolving fully, leaves standstill bubble to be stirred fully form the homogeneous spinning solution.
(3) extract PAN/ glucose ethene fat homopolymers with syringe, be fixed on the electrostatic spinning apparatus, control ejection flow velocity 1.5ml/h; Electrostatic pressure 15kv; Receiving screen adopts the reception of aluminium foil ground connection, and the distance of syringe needle and receiving screen is 10~20cm, adopts orthogonal method (to change a certain parameter; Fix other parameter) the different spinning parameters of adjusting carry out electricity and spin, and must diameter be the PAN/ glucose ethene fat homopolymers superfine nano tunica fibrosa of 80~250nm; Put into 60~80 ℃ of freeze-day with constant temperature 40h of vacuum drying chamber, process the regeneration nano composite membrane, its electromicroscopic photograph is shown in Fig. 1 (e), and diameter Distribution is shown in Fig. 2 (e).
Embodiment 5
(1) with diacid divinyl ester and glucose according to a certain percentage (4: 1, mol ratio) be dissolved in the anhydrous pyridine, utilize enzymatic synthetic technology synthesis of glucose ethene fat.After reaction finished, crude product separates with silica gel column chromatography purified, and eluant, eluent is an ethyl acetate, solvent be ethyl acetate/methanol/water (17: 3: 1, v/v/v), use I 2Colour developing.Above-mentioned glycolipid is put in the micro-polymerization pipe, as initator, adds H with ammonium persulfate (APS) (accounting for glucose ethene lipid amount mark is 1.0) 2O makes solvent, and (monomer concentration is 2.5mol/L H 2O, sealing vacuumizes the logical nitrogen in back, repeated multiple times with oil pump.System is placed stirring reaction 5h under 55~60 ℃ of nitrogen protections.
(2) PAN of certain mass is dissolved in DMF and obtains the PAN solution that concentration is 0.06g/ml; Add glucose ethene fat homopolymers then, make its shared mass fraction be respectively 70%, stirred for several hour is to dissolving fully, leaves standstill bubble to be stirred fully form the homogeneous spinning solution.
(3) extract PAN/ glucose ethene fat homopolymers with syringe, be fixed on the electrostatic spinning apparatus, control ejection flow velocity 1.5ml/h; Electrostatic pressure 15kv; Receiving screen adopts the reception of aluminium foil ground connection, and the distance of syringe needle and receiving screen is 10~20cm, adopts orthogonal method (to change a certain parameter; Fix other parameter) the different spinning parameters of adjusting carry out electricity and spin, and must diameter be the PAN/ glucose ethene fat homopolymers superfine nano tunica fibrosa of 80~250nm; Put into 60~80 ℃ of freeze-day with constant temperature 48h of vacuum drying chamber, process the regeneration nano composite membrane, its electromicroscopic photograph is shown in Fig. 1 (f), and diameter Distribution is shown in Fig. 2 (f).
Embodiment 6
Glucose ethene fat, glucose ethene fat homopolymers, blending nano fibrous membrane, the PAN of gained among the embodiment 1 are characterized with FI-IR, and its result is as shown in Figure 3 respectively.Can find out the two key (1647cm in the glucose ethene fat by Fig. 3 (a) and 3 (b) -1) disappear.Can find out that from Fig. 3 (b), 3 (c) and 3 (d) (characteristic peak combines the characteristic of 3 (b), 3 (d) to the blending nano fibrous membrane among 3 (c).
Comparative Examples 1
(1) diacid divinyl ester and glucose are dissolved in the anhydrous pyridine by (4: 1, mol ratio), utilize enzymatic synthetic technology synthesis of glucose ethene fat.After reaction finished, crude product separates with silica gel column chromatography purified, and eluant, eluent is an ethyl acetate, solvent be ethyl acetate/methanol/water (17: 3: 1, v/v/v), use I 2Colour developing.Above-mentioned glycolipid is put in the micro-polymerization pipe, as initator, adds H with ammonium persulfate (APS) (accounting for glucose ethene lipid amount mark is 1.0) 2O makes solvent, and (monomer concentration is 2.5mol/L H 2O), sealing vacuumizes the logical nitrogen in back, repeated multiple times with oil pump.System is placed stirring reaction 3h under 55~60 ℃ of nitrogen protections.
(2) PAN with certain mass is dissolved among the DMF.Stirred for several hour is to dissolving fully, leaves standstill bubble to be stirred fully form the homogeneous spinning solution, and obtaining concentration is the PAN solution of 6%g/ml.
(3) extract PAN/ glucose ethene fat homopolymers with syringe, be fixed on the electrostatic spinning apparatus, control ejection flow velocity 1.0~1.5ml/h; Electrostatic pressure 10~18kv; Receiving screen adopts the reception of aluminium foil ground connection, and the distance of syringe needle and receiving screen is 10~20cm, adopts orthogonal method (to change a certain parameter; Fix other parameter) the different spinning parameters of adjusting carry out electricity and spin, and must diameter be the PAN/ glucose ethene fat superfine nano tunica fibrosa of 80~250nm; Put into 60~80 ℃ of freeze-day with constant temperature 36h of vacuum drying chamber, process the regeneration nano composite membrane, its electromicroscopic photograph is shown in Fig. 1 (a), and diameter Distribution is shown in Fig. 2 (a).

Claims (10)

1. an electrostatic blended spinning contains the preparation method of sugared polyacrylonitrile nano tunica fibrosa, comprising:
(1) diacid divinyl ester and glucose were dissolved in the anhydrous pyridine in 1: 1 in molar ratio~4: 1, utilize enzymatic synthetic technology synthesis of glucose ethene fat; In above-mentioned glucose ethene fat, add ammonium persulfate as initator, add H again 2O makes solvent, and stirring reaction 3-5h under 55~60 ℃ of nitrogen protections obtains glucose ethene fat homopolymers after the polymerisation end then;
(2) polyacrylonitrile (PAN) is dissolved in DMF and obtains the PAN solution that concentration is 0.05~0.07g/ml, add above-mentioned glucose ethene fat homopolymers then, be stirred to dissolving fully, leave standstill then, get PAN/ glucose ethene fat homopolymers spinning solution;
(3) above-mentioned PAN/ glucose ethene fat homopolymers spinning solution is carried out electrostatic spinning and get PAN/ glucose ethene fat superfine nano tunica fibrosa, final drying promptly gets and contains sugared polyacrylonitrile nano tunica fibrosa.
2. a kind of electrostatic blended spinning according to claim 1 contains the preparation method of sugared polyacrylonitrile nano tunica fibrosa; It is characterized in that: the glucose ethene fat described in the step (1); Its crude product separates with silica gel column chromatography purifies; Eluant, eluent is an ethyl acetate, and solvent is that volume ratio is ethyl acetate/methanol/water of 17: 3: 1, uses I 2Colour developing.
3. a kind of electrostatic blended spinning according to claim 1 contains the preparation method of sugared polyacrylonitrile nano tunica fibrosa, it is characterized in that: it is 02~2% that the ammonium persulfate described in the step (1) accounts for glucose ethene lipid amount mark.
4. a kind of electrostatic blended spinning according to claim 1 contains the preparation method of sugared polyacrylonitrile nano tunica fibrosa, it is characterized in that: the adding H described in the step (1) 2After O made solvent, the concentration of glucose ethene fat was 2-3mol/L.
5. a kind of electrostatic blended spinning according to claim 1 contains the preparation method of sugared polyacrylonitrile nano tunica fibrosa, it is characterized in that: after the polymerisation described in the step (1) finishes, product is removed the glucose ethene fat that does not have reaction simultaneously through acetone precipitation.
6. a kind of electrostatic blended spinning according to claim 1 contains the preparation method of sugared polyacrylonitrile nano tunica fibrosa, it is characterized in that: the mass fraction of glucose ethene fat homopolymers is 10%~90% in the PAN/ glucose ethene fat homopolymers spinning solution described in the step (2).
7. a kind of electrostatic blended spinning according to claim 1 contains the preparation method of sugared polyacrylonitrile nano tunica fibrosa, it is characterized in that: the mass fraction of glucose ethene fat homopolymers is 50%, 55%, 60%, 65% or 70% in the PAN/ glucose ethene fat homopolymers spinning solution described in the step (2).
8. a kind of electrostatic blended spinning according to claim 1 contains the preparation method of sugared polyacrylonitrile nano tunica fibrosa; It is characterized in that: the technological parameter of the electrostatic spinning described in the step (3) is: the syringe specification is 5ml, and the syringe needle internal diameter is 0.4~0.7mm, ejection flow velocity 0.8~2ml/h; Electrostatic pressure 10~18kv; Receiving screen employing aluminium foil ground connection receives, and accepting distance is 10~20cm, adopts orthogonal method adjusting spinning parameter to carry out electricity and spins.
9. a kind of electrostatic blended spinning according to claim 1 contains the preparation method of sugared polyacrylonitrile nano tunica fibrosa, it is characterized in that: the diameter of the PAN/ glucose ethene fat superfine nano tunica fibrosa of gained is 80~250nm in the step (3).
10. a kind of electrostatic blended spinning according to claim 1 contains the preparation method of sugared polyacrylonitrile nano tunica fibrosa, it is characterized in that: the drying described in the step (3) is for putting into 40~60 ℃ of freeze-day with constant temperature 24~48h of vacuum drying chamber.
CN2011102317205A 2011-08-12 2011-08-12 Preparation method for electrostatic blended sugar-containing polyacrylonitrile (PAN) nano-fiber membrane Pending CN102418237A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN2011102317205A CN102418237A (en) 2011-08-12 2011-08-12 Preparation method for electrostatic blended sugar-containing polyacrylonitrile (PAN) nano-fiber membrane

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN2011102317205A CN102418237A (en) 2011-08-12 2011-08-12 Preparation method for electrostatic blended sugar-containing polyacrylonitrile (PAN) nano-fiber membrane

Publications (1)

Publication Number Publication Date
CN102418237A true CN102418237A (en) 2012-04-18

Family

ID=45942872

Family Applications (1)

Application Number Title Priority Date Filing Date
CN2011102317205A Pending CN102418237A (en) 2011-08-12 2011-08-12 Preparation method for electrostatic blended sugar-containing polyacrylonitrile (PAN) nano-fiber membrane

Country Status (1)

Country Link
CN (1) CN102418237A (en)

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102758268A (en) * 2012-05-11 2012-10-31 东华大学 Preparation method of double-hydrophilic thermal-sensitive nanofiber membrane
CN102776599A (en) * 2012-07-10 2012-11-14 东华大学 Preparation method of electrospun multi-wall carbon nanotube (MWCNT)/glycopolymer nanofiber membrane
CN102808233A (en) * 2012-07-26 2012-12-05 东华大学 Method for preparing electrostatic spinning mannose ester/ acrylonitrile copolymer nano fiber membrane
CN102828346A (en) * 2012-07-26 2012-12-19 东华大学 Method for preparing galactose homopolymer/polyacrylonitrile composite nanofiber membrane
CN102899735A (en) * 2012-07-10 2013-01-30 东华大学 Static spinning glycopolymer and acrylonitrile copolymer nano fiber film preparation method
CN103194857A (en) * 2013-04-12 2013-07-10 东华大学 Preparation method of electrostatic spinning glucose ether/acrylonitrile copolymer nanofiber membrane
CN104947226A (en) * 2015-07-13 2015-09-30 山东大学 Method for preparing PAN/POMs composite fiber membrane through electrostatic spinning
CN105155139A (en) * 2015-06-11 2015-12-16 浪莎针织有限公司 Preparation method for electrostatic spinning glucose ester/acrylonitrile copolymer nanofiber membrane and application thereof

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
《The 5th International Conference on Bioinformatics and Biomedical Engineering》 20110512 Yan Li et als "Chemo-enzymatic synthesis of nanofiber membrane with glucose by electrospinning" , *
YAN LI ET ALS: ""Chemo-enzymatic synthesis of nanofiber membrane with glucose by electrospinning"", 《THE 5TH INTERNATIONAL CONFERENCE ON BIOINFORMATICS AND BIOMEDICAL ENGINEERING》 *

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102758268A (en) * 2012-05-11 2012-10-31 东华大学 Preparation method of double-hydrophilic thermal-sensitive nanofiber membrane
CN102758268B (en) * 2012-05-11 2014-07-02 东华大学 Preparation method of double-hydrophilic thermal-sensitive nanofiber membrane
CN102776599A (en) * 2012-07-10 2012-11-14 东华大学 Preparation method of electrospun multi-wall carbon nanotube (MWCNT)/glycopolymer nanofiber membrane
CN102899735A (en) * 2012-07-10 2013-01-30 东华大学 Static spinning glycopolymer and acrylonitrile copolymer nano fiber film preparation method
CN102776599B (en) * 2012-07-10 2014-02-26 东华大学 Preparation method of electrospun multi-wall carbon nanotube (MWCNT)/glycopolymer nanofiber membrane
CN102899735B (en) * 2012-07-10 2014-07-02 东华大学 Static spinning glycopolymer and acrylonitrile copolymer nano fiber film preparation method
CN102808233A (en) * 2012-07-26 2012-12-05 东华大学 Method for preparing electrostatic spinning mannose ester/ acrylonitrile copolymer nano fiber membrane
CN102828346A (en) * 2012-07-26 2012-12-19 东华大学 Method for preparing galactose homopolymer/polyacrylonitrile composite nanofiber membrane
CN103194857A (en) * 2013-04-12 2013-07-10 东华大学 Preparation method of electrostatic spinning glucose ether/acrylonitrile copolymer nanofiber membrane
CN105155139A (en) * 2015-06-11 2015-12-16 浪莎针织有限公司 Preparation method for electrostatic spinning glucose ester/acrylonitrile copolymer nanofiber membrane and application thereof
CN104947226A (en) * 2015-07-13 2015-09-30 山东大学 Method for preparing PAN/POMs composite fiber membrane through electrostatic spinning

Similar Documents

Publication Publication Date Title
CN102418237A (en) Preparation method for electrostatic blended sugar-containing polyacrylonitrile (PAN) nano-fiber membrane
CN103422194B (en) A kind of strong-hydrophobicity porous carbon nanofiber and preparation method thereof
CN103898676A (en) Cellulose acetate/ titanium dioxide composite nanofiber adsorption film and preparation method thereof
CN103173933B (en) A kind of preparation method of glucose vinyl acetate/N-isopropylacrylamide copolymer nano tunica fibrosa
CN102758268B (en) Preparation method of double-hydrophilic thermal-sensitive nanofiber membrane
CN103074733B (en) A kind of electro-spinning is for the method for Thermo-sensitive galactolipin vinyl acetate nano drug-carrying tunica fibrosa
CN1908039A (en) Process for preparing chitosan nano fiber film with stable state
CN104437124B (en) A kind of self-cleaning type polyvinylidene fluoride microporous film and preparation method thereof
CN101481855A (en) Preparation of silicon dioxide / polyvinylidene fluoride composite nano fiber film
AU2012362513A1 (en) Fiber composition comprising 1,3-glucan and a method of preparing same
CN103895293A (en) Nanofiber membrane fabric with modified self-cleaning carbon nano tube and preparation method
CN113026210A (en) Preparation method of starch nanofiber membrane and starch nanofiber membrane
CN102828346A (en) Method for preparing galactose homopolymer/polyacrylonitrile composite nanofiber membrane
CN109338497A (en) A kind of preparation method of hydrophily degradable poly butyrolactam superfine fibre
CN103173934B (en) A kind of preparation method of galactolipin vinyl acetate/N-isopropylacrylamide copolymer nano tunica fibrosa
CN106146694A (en) A kind of polyaniline nano-composite material and its preparation method and application
CN109528167B (en) Preparation method of lignin-based flexible piezoresistive sensor
CN103073682B (en) Method for preparing temperature sensitive galactose vinyl ester nano particles by electric spray method
CN113122938A (en) Preparation method and application of MOFs-containing chitosan/polyvinyl alcohol nanofiber membrane
CN105040277A (en) Nano-cellulose/cellulose triacetate composite nano-fiber membrane capable of adsorbing and desorbing proteins
CN105040157B (en) A kind of preparation of wooden liquefied substance electrostatic spinning liquid and spinning process
CN103614860A (en) Method for preparing glucose azelaic acid divinyl ester/N-isopropylacrylamide copolymer nanofiber membrane
CN103194857A (en) Preparation method of electrostatic spinning glucose ether/acrylonitrile copolymer nanofiber membrane
CN109678992B (en) Folic acid functionalized modified polyvinyl alcohol medicinal polymer material for soluble microneedle and preparation method thereof
CN104264372B (en) Method for preparing PNIPAAm (poly(N-isopropylacrylamide)) and EC (ethyecellulose) blended nano-fiber membrane by electrostatic spinning

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C12 Rejection of a patent application after its publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20120418