CN105063894A - Method for preparing perfluor liquid injection type transparent flexible anti-icing thin film through electrostatic spinning - Google Patents
Method for preparing perfluor liquid injection type transparent flexible anti-icing thin film through electrostatic spinning Download PDFInfo
- Publication number
- CN105063894A CN105063894A CN201510487033.8A CN201510487033A CN105063894A CN 105063894 A CN105063894 A CN 105063894A CN 201510487033 A CN201510487033 A CN 201510487033A CN 105063894 A CN105063894 A CN 105063894A
- Authority
- CN
- China
- Prior art keywords
- film
- electrostatic spinning
- electrospinning
- thin film
- transparent flexible
- 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.)
- Granted
Links
Landscapes
- Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
- Nonwoven Fabrics (AREA)
- Laminated Bodies (AREA)
Abstract
The invention provides a method for preparing a perfluor liquid injection type transparent flexible anti-icing thin film through electrostatic spinning and belongs to the field of interface chemistry. An electrospinning film is prepared on the surface of aluminum foil through the electrospinning technology; the electrospinning film on the surface of the aluminum foil is transferred to the surface of a propping material through alcohol soaking, hot pressing and drying processes, and a porous electrostatic spinning nanofiber film is prepared; perfluor liquid is added to the surface of the porous electrostatic spinning nanofiber membrane dropwise, and the perfluor liquid injection type transparent flexible anti-icing thin film is obtained. The visible light transmittance of the prepared transparent flexible anti-icing thin film is more than 80%, the contact angles between water drops and the surface of the flexible anti-icing thin film are 113 degrees, and the rolling angles are 3 degrees. Most of the regions of the surface of the transparent flexible anti-icing thin film are frostless after 60 min under the condition of the -5 DEG C temperature and the 50% humidity, and the drop setting time is obviously prolonged compared with a traditional hydrophobic film.
Description
Technical field
The invention belongs to surface chemistry field, specifically, refer to a kind of at backing material surface preparation porous Electrospun nano-fibers film, then inject perfluor liquid, prepare the method for the anti-ina thin film of the pouring-in transparent flexible of perfluor liquid.
Background technology
Mostly the anti-icing material of tradition is to build micro nano structure to form super hydrophobic surface by hydro-thermal method, electron beam lithography etc., but traditional super hydrophobic surface anti-icing effect under high pressure or super-humid conditions is remarkable, surface micronano coarse structure destructible or promotion ice crystal nucleation.And the pouring-in porous surface of perfluor liquid efficiently solves the drawback that traditional super hydrophobic surface exists.But the pouring-in porous surface of traditional perfluor liquid can not possess higher clarity and flexibility simultaneously, and conventional method need do further chemical treatment (as fluorination treatment) to anti-icing surface, add anti-icing cost, greatly limit the practical application of these methods.
Summary of the invention
The invention provides a kind of method utilizing electrostatic spinning to prepare the anti-ina thin film of the pouring-in transparent flexible of perfluor liquid.Be intended to solve the pouring-in porous surface of traditional perfluor liquid and can not possess higher clarity and flexible problem simultaneously, thus provide better material for anti-icing field.The present invention utilizes electrostatic spinning technique, having the electrospun polymer fibers rete of micro-nano porous structure, providing good base material for preparing the pouring-in porous surface of perfluor liquid further in the preparation of backing material surface.Product prepared by the present invention can directly apply to the surface need carrying out anti-icing process, avoids conventional method and treats anti-icing surface and do further chemically treated necessity.This method is low to requirement for experiment condition, and Repeatability reaches 100%.
The invention provides a kind of method utilizing electrostatic spinning to prepare the anti-ina thin film of the pouring-in transparent flexible of perfluor liquid, specifically comprise following step:
Step one: prepare electrostatic spinning precursor liquid;
After polymer vacuumize, join in solvent, heating is stirred to polymer and dissolves completely, obtains electrostatic spinning precursor liquid, leaves standstill, for subsequent use.
Described polymer is Kynoar (PVDF) or Kynoar-hexafluoropropene (PVDF-HFP) copolymer.In described PVDF-HFP copolymer, the mol ratio of PVDF and HFP is 1:1.
Described solvent is the mixture of dimethyl formamide (DMF), acetone or dimethylacetylamide and acetone.In the mixture of described dimethylacetylamide and acetone, the mass ratio of acetone and dimethylacetylamide is 7:3.
The mass ratio of described polymer and described solvent meets 3:17 ~ 1:9.
Described vacuum drying condition is: temperature is 50 DEG C, and the time is 24h.
Described heating whipping temp is 20 ~ 80 DEG C, and mixing time is more than 8h.
Step 2: electrostatic spinning prepares electrospinning film;
Choosing aluminium foil is dash receiver, is loaded in syringe by the electrostatic spinning precursor liquid in step one, and is placed on micro-injection pump by syringe, carry out electrostatic spinning, obtain electrospinning film.
The technological parameter that described electrostatic spinning prepares electrospinning film is: electrospinning syringe needle internal diameter is 0.2 ~ 0.8mm, the flow-control of electrostatic spinning precursor liquid is 0.1 ~ 2.0mL/h, electrospinning device is 10 ~ 25kV to the voltage that electrostatic spinning precursor liquid applies, spinning head is 10 ~ 25cm to the vertical range of dash receiver, and the electrostatic spinning time is 30 ~ 90min.
Step 3: backing material surface preparation porous Electrospun nano-fibers film;
Described backing material is polyethylene terephthalate (PET) film, polyvinyl chloride (PVC) film, PVC tape, polypropylene (PP) film or Biaxially oriented polypropylene (BOPP) adhesive tape.
Step 4: porous Electrospun nano-fibers film surface imp lantation perfluor liquid;
Draw perfluor liquid with suction pipe, dripped to the porous Electrospun nano-fibers film surface that step 3 is obtained, unnecessary perfluor liquid is removed by gravity, spin coater or stream of nitrogen gas method, the obtained anti-ina thin film of the pouring-in transparent flexible of perfluor liquid.
Described perfluor liquid is PFPE (PFPE), PFO (PO), perfluor triamylamine or FC-770 fluoridize liquid.
The invention has the advantages that:
1, the method utilizing electrostatic spinning to prepare the anti-ina thin film of the pouring-in transparent flexible of perfluor liquid provided by the invention is simple to operate, cost is low, at the porous Electrospun nano-fibers film of flexible support material surface preparation, there is micro-nano porous structure, thus enable tunica fibrosa surface fix perfluor liquid well, serve good anti-ice action.
2, the pouring-in porous surface of perfluor liquid that prepared by the present invention possesses higher transparency and flexibility.
3, the anti-ina thin film of the pouring-in transparent flexible of perfluor liquid that prepared by the present invention still can keep good anti-icing effect under high pressure super-humid conditions, avoids the deficiency that the super-hydrophobic anti-icing material of tradition easily lost efficacy under high pressure super-humid conditions.
4, the anti-ina thin film of the pouring-in transparent flexible of perfluor liquid that prepared by the present invention can directly apply to the surface need carrying out anti-icing process, avoids conventional method and need treat anti-icing surface and do further chemically treated necessity.
5, the method manufacturing cycle utilizing electrostatic spinning to prepare the anti-ina thin film of the pouring-in transparent flexible of perfluor liquid provided by the invention is short, can realize large-scale production.
Accompanying drawing explanation
Figure 1A is the pictorial diagram of the anti-ina thin film of K100-PVDF-PET prepared by the present invention;
Figure 1B is the anti-ina thin film of K100-PVDF-PET pictorial diagram in the bent state prepared by the present invention;
Fig. 2 is the nanofiber loose structure SEM phenogram of the anti-icing film surface of K100-PVDF-PET prepared by the present invention;
Fig. 3 A, 3B are respectively contact angle, the roll angle picture of the anti-icing film surface of K100-PVDF-PET that water droplet is prepared in the present invention;
Fig. 4 A, 4B are respectively BOPP transparent hydrophobic film and the anti-ina thin film of K100-PVDF-PET at-5 DEG C, the comparison diagram of 0min under 50% humidity;
Fig. 5 A, 5B are respectively BOPP transparent hydrophobic film and the anti-ina thin film of K100-PVDF-PET at-5 DEG C, the frosting comparison diagram of 15min under 50% humidity;
Fig. 6 A, 6B are respectively BOPP transparent hydrophobic film and the anti-ina thin film of K100-PVDF-PET at-5 DEG C, the frosting comparison diagram of 30min under 50% humidity;
Fig. 7 A, 7B are respectively BOPP transparent hydrophobic film and the anti-ina thin film of K100-PVDF-PET at-5 DEG C, the frosting comparison diagram of 45min under 50% humidity;
Fig. 8 A, 8B are respectively BOPP transparent hydrophobic film and the anti-ina thin film of K100-PVDF-PET at-5 DEG C, the frosting comparison diagram of 60min under 50% humidity.
Detailed description of the invention
Below in conjunction with drawings and Examples, the present invention is described in further details.
The invention provides a kind of method utilizing electrostatic spinning to prepare the anti-ina thin film of the pouring-in transparent flexible of perfluor liquid, specifically comprise following step:
Step one: prepare electrostatic spinning precursor liquid;
After polymer vacuumize, join in solvent, add thermal agitation until polymer dissolves completely, obtain electrostatic spinning precursor liquid, leave standstill, until the bubble in electrostatic spinning precursor liquid disappears completely.
Described polymer is PVDF or PVDF-HFP copolymer.In described PVDF-HFP copolymer, the mol ratio of PVDF and HFP is 1:1.
Described solvent is the mixture of DMF, acetone or dimethylacetylamide and acetone.In the mixture of described dimethylacetylamide and acetone, the mass ratio of acetone and dimethylacetylamide is 7:3.
The mass ratio of described polymer and described solvent meets 3:17 ~ 1:9.
Described vacuum drying condition is: temperature is 50 DEG C, and the time is 24h.
The described condition adding thermal agitation is: temperature is 20 ~ 80 DEG C, more than mixing time 8h.More preferably temperature 80 DEG C, mixing time 8h.
Step 2: electrostatic spinning prepares electrospinning film;
Choosing aluminium foil is dash receiver, electrostatic spinning precursor liquid in step one is loaded in the syringe of 20mL, and syringe is placed on micro-injection pump, electrospinning syringe needle internal diameter is 0.2 ~ 0.8mm, the flow-control of electrostatic spinning precursor liquid is 0.1 ~ 2.0mL/h, and electrospinning device is 10 ~ 25kV to the voltage that electrostatic spinning precursor liquid applies, and spinning head is 10 ~ 25cm to the vertical range of dash receiver, the electrostatic spinning time is 30 ~ 90min, obtains electrospinning film.
Preferred electrostatic spinning precursor liquid flow is 1.0 ~ 2.0mL/h, and electrospinning device is 20 ~ 25kV to the voltage that electrostatic spinning precursor liquid applies, and spinning head is 15cm to the vertical range of dash receiver, and the electrostatic spinning time is 50 ~ 60min.
Step 3: backing material surface preparation porous Electrospun nano-fibers film;
According to the relation of the fusing point of backing material and the fusing point of selected polymer, a point the following two kinds mode is prepared:
(A) as described in backing material fusing point higher than as described in melting point polymer;
Aluminium foil with electrospinning film is immersed in the alcohol of mass fraction 10 ~ 50% after 10 ~ 30s along electrospinning film edge side, aluminium foil is taken out; Had by aluminium foil electrospinning film one side to be attached to backing material surface along electrospinning film edge, then taken off by aluminium foil, electrospinning film transfers to backing material surface; After surface is placed in the dry 24h of vacuum drying chamber with the backing material of electrospinning film, take out, be clipped between common color printing paper, with hot press hot pressing 1 ~ 2s, hot pressing pressure is 1MPa, obtains porous Electrospun nano-fibers film, for subsequent use.
(B) as described in backing material fusing point lower than as described in melting point polymer;
Be clipped in by aluminium foil with electrospinning film between common color printing paper, with hot press hot pressing 1 ~ 2s, hot pressing pressure is 1MPa; Aluminium foil with electrospinning film is immersed in the alcohol of mass fraction 10 ~ 50% after 10 ~ 30s along electrospinning film edge side, takes out; Had by aluminium foil electrospinning film one side to be attached to backing material surface along electrospinning film edge, then taken off by aluminium foil, electrospinning film transfers to backing material surface; After surface is placed in the dry 24h of vacuum drying chamber with the backing material of electrospinning film, takes out, obtain porous Electrospun nano-fibers film, for subsequent use.
Described backing material is PET film, PVC film, PVC tape, PP film or BOPP adhesive tape.
The temperature of described vacuum drying chamber is 40 ~ 50 DEG C.Described hot pressing temperature is 150 ~ 180 DEG C.
Step 4: porous Electrospun nano-fibers film surface imp lantation perfluor liquid;
Draw perfluor liquid with suction pipe, dripped to the porous Electrospun nano-fibers film surface that step 3 is obtained, leave standstill 30min, perfluor liquid can spontaneous impregnating porous Electrospun nano-fibers film under capillary action.Unnecessary perfluor liquid is removed by gravity, spin coater or stream of nitrogen gas method, the obtained anti-ina thin film of the pouring-in transparent flexible of perfluor liquid.
Described perfluor liquid is PFPE (PFPE), PFO (PO), perfluor triamylamine or FC-770 fluoridize liquid.
The anti-ina thin film of the pouring-in transparent flexible of perfluor liquid that said method prepares, possesses transparent and flexible characteristic simultaneously, directly can be applied in and treat that anti-icing surface is for anti-icing, under temperature-5, humidity 50% condition, and frost-free in the 60min time.
Provide specific embodiment below.
embodiment 1:the preparation of the anti-ina thin film of K100-PVDF-PET transparent flexible, concrete steps are:
Step one: prepare electrostatic spinning precursor liquid;
Take 15gPVDF powder, 50 DEG C of vacuumize 24h, be dissolved in 85gDMF by dried PVDF powder, heating, stirs 8h at 80 DEG C, obtains electrostatic spinning precursor liquid, leaves standstill, until bubble disappears completely in electrostatic spinning precursor liquid.
Step 2: electrostatic spinning prepares electrospinning film;
Choosing aluminium foil is dash receiver, and loaded by the electrostatic spinning precursor liquid in step one in the syringe of 20mL, and be placed on micro-injection pump by syringe, the flow-control of electrostatic spinning precursor liquid is 2.0mL/h.Electrospinning syringe needle internal diameter is 0.2mm, and electrospinning device is 25kV to the voltage that electrostatic spinning precursor liquid applies, and spinning head is 15cm to the vertical range of dash receiver, and the electrostatic spinning time is 50min, obtains electrospinning film.
Step 3: backing material surface preparation porous Electrospun nano-fibers film;
Choosing PET film is backing material, the aluminium foil with electrospinning film is immersed in 20s in the alcohol of mass fraction 50% along electrospinning film edge side, is taken out by aluminium foil; Had by aluminium foil electrospinning film one side to be attached to PET film surface along electrospinning film edge, then taken off by aluminium foil, electrospinning film transfers to PET film surface; After PET film simultaneously with electrospinning film is placed in the dry 24h of vacuum drying chamber of 50 DEG C, takes out, be clipped between common color printing paper, with hot press hot pressing 2s, hot pressing pressure is 1MPa, and hot pressing temperature is 172 DEG C, obtains PVDF-PET porous Electrospun nano-fibers film.
Step 4: porous Electrospun nano-fibers film surface imp lantation perfluor liquid;
Drawing model with suction pipe is
pFPE, dripped to PVDF-PET porous Electrospun nano-fibers film surface prepared by step 3, leave standstill 30min, PFPE can spontaneous infiltration PVDF-PET porous Electrospun nano-fibers film under capillary action, unnecessary PFPE is removed by gravity, the obtained anti-ina thin film of K100-PVDF-PET transparent flexible.
Figure 1A is the pictorial diagram of the anti-ina thin film of K100-PVDF-PET transparent flexible of preparation, relatively PFPE injects the light transmittance of front and back PVDF-PET film, can find out, inject the light transmittance of PVDF-PET film after PFPE to significantly improve, the anti-icing thin film of K100-PVDF-PET transparent flexible for more than 80% visible light transmissivity.Figure 1B is the anti-ina thin film of K100-PVDF-PET transparent flexible pictorial diagram in the bent state prepared by the present invention, can find out, the anti-ina thin film of K100-PVDF-PET transparent flexible can realize the degree of crook identical with backing material, and the anti-ina thin film of K100-PVDF-PET transparent flexible prepared by visible the present invention possesses higher transparency and good flexibility simultaneously.
Adopt environmental scanning electronic microscope to carry out microscopic appearance observation to the anti-ina thin film of K100-PVDF-PET transparent flexible, as shown in Figure 2, PVDF nanofiber diameter is between 100 ~ 600nm.
Contact angle instrument (with cold bench) is adopted to carry out water droplet contact angle test to the anti-ina thin film of K100-PVDF-PET transparent flexible, test result is as shown in Fig. 3 A, 3B, can find out that water droplet (5 μ L) is 113 ° at the contact angle of the anti-icing film surface of K100-PVDF-PET transparent flexible, roll angle is 3 °.
Cold bench is adopted to carry out frosting test to the anti-ina thin film of K100-PVDF-PET transparent flexible, Fig. 4 A-8A have recorded BOPP transparent hydrophobic film at-5 DEG C, Frost formation process under 50% damp condition, can find out, when 30min there is a large amount of frosting in BOPP transparent hydrophobic film surface, basic all frostings during 60min; Fig. 4 B-8B have recorded the anti-ina thin film of K100-PVDF-PET transparent flexible at-5 DEG C, Frost formation process under 50% damp condition, and can find out, the anti-icing thin film of K100-PVDF-PET transparent flexible is for good anti-icing effect.At-5 DEG C, the anti-ina thin film of K100-PVDF-PET transparent flexible does not have frost to be formed in the most region of 60min and 50% damp condition lower surface, the K100-PVDF-PET transparent flexible anti-icing film surface droplets agglomerate time comparatively BOPP transparent hydrophobic film have obvious prolongation.
embodiment 2:the preparation of the anti-ina thin film of PO-PVDF-BOPP transparent flexible, concrete steps are:
Step one: prepare electrostatic spinning precursor liquid;
Take 15gPVDF powder, 50 DEG C of vacuumize 24h, be dissolved in 85gDMF by dried PVDF powder, heating, stirs 8h at 80 DEG C, obtains electrostatic spinning precursor liquid, leaves standstill, until bubble disappears completely in electrostatic spinning precursor liquid.
Step 2: electrostatic spinning prepares electrospinning film;
Choosing aluminium foil is dash receiver, and loaded by the electrostatic spinning precursor liquid in step one in the syringe of 20mL, and be placed on micro-injection pump by syringe, the flow-control of electrostatic spinning precursor liquid is 2.0mL/h.Electrospinning syringe needle internal diameter is 0.2mm, and electrospinning device is 25kV to the voltage that electrostatic spinning precursor liquid applies, and spinning head is 15cm to the vertical range of dash receiver, and the electrostatic spinning time is 50min, obtains electrospinning film.
Step 3: backing material surface preparation porous Electrospun nano-fibers film;
Choosing BOPP adhesive tape is backing material, is clipped in by the aluminium foil with electrospinning film between common color printing paper, and with hot press hot pressing 2s, hot pressing pressure is 1MPa, and hot pressing temperature is 172 DEG C; Aluminium foil with electrospinning film is immersed in 20s in the alcohol of mass fraction 50% along electrospinning film edge side, takes out; Had by aluminium foil electrospinning film one side to be attached on the glue face of BOPP adhesive tape along electrospinning film edge, then taken off by aluminium foil, electrospinning film transfers to BOPP tape surface; After surface is placed in the dry 24h of vacuum drying chamber of 40 DEG C with the BOPP adhesive tape of electrospinning film, takes out, obtain PVDF-BOPP porous Electrospun nano-fibers film.
Step 4: porous Electrospun nano-fibers film surface imp lantation perfluor liquid;
PFO is drawn with suction pipe, and dripped to PVDF-BOPP porous Electrospun nano-fibers film surface prepared by step 3, leave standstill 30min, PFO can spontaneous infiltration PVDF-BOPP porous Electrospun nano-fibers film under capillary action, the spin coater of unnecessary PFO 2000r/min is removed, the obtained anti-ina thin film of PO-PVDF-BOPP transparent flexible.
The described anti-ina thin film of PO-PVDF-BOPP transparent flexible possesses transparent and flexible characteristic, visible light transmissivity 80% simultaneously, flexible suitable with backing material, directly can be applied in and treat that anti-icing surface is for anti-icing.
embodiment 3:the preparation of the anti-ina thin film of K100-PH-PET transparent flexible, concrete steps are:
Step one: configuration electrostatic spinning precursor liquid;
Take 10gPVDF-HFP copolymer, after 50 DEG C of vacuumize 24h, dried PVDF-HFP copolymer is dissolved in 90g dimethylacetylamide and acetone mixture, 8h is stirred at 80 DEG C, obtain electrostatic spinning precursor liquid, leave standstill, until bubble disappears completely in electrostatic spinning precursor liquid.
Step 2: electrostatic spinning prepares electrospinning film;
Choosing aluminium foil is dash receiver, and loaded by the electrostatic spinning precursor liquid in step one in the syringe of 20mL, and be placed on micro-injection pump by syringe, the flow-control of electrostatic spinning precursor liquid is 1.0mL/h.Electrospinning syringe needle internal diameter is 0.8mm, and electrospinning device is 20kV to the voltage that electrostatic spinning precursor liquid applies, and spinning head is 15cm to the vertical range of dash receiver, and the electrostatic spinning time is 60min, obtains electrospinning film.
Step 3: backing material surface preparation porous Electrospun nano-fibers film;
Aluminium foil with electrospinning film is immersed in 20s in the alcohol of mass fraction 50% along electrospinning film edge side, aluminium foil is taken out; Had by aluminium foil electrospinning film one side to be attached to PET film surface along electrospinning film edge, then taken off by aluminium foil, electrospinning film transfers to PET film surface.After PET film simultaneously with electrospinning film is placed in the dry 24h of vacuum drying chamber of 50 DEG C, take out, be clipped between common color printing paper, with hot press hot pressing 2s, hot pressing pressure is 1MPa, hot pressing temperature is 150 DEG C, obtained PVDF-HFP-PET (PH-PET) porous Electrospun nano-fibers film.
Step 4: porous Electrospun nano-fibers film surface imp lantation perfluor liquid;
Drawing model with suction pipe is
pFPE, and dripped to PH-PET porous Electrospun nano-fibers film surface prepared by step 3, leave standstill 30min, PFPE can spontaneous infiltration PH-PET porous Electrospun nano-fibers film under capillary action, unnecessary PFPE stream of nitrogen gas method is removed, the obtained anti-ina thin film of K100-PH-PET transparent flexible.
The described anti-ina thin film of K100-PH-PET transparent flexible possesses transparent and flexible characteristic, visible light transmissivity more than 80% simultaneously, flexible suitable with backing material, directly can be applied in and treat that anti-icing surface is for anti-icing.
Claims (8)
1. utilize electrostatic spinning to prepare a method for the anti-ina thin film of the pouring-in transparent flexible of perfluor liquid, it is characterized in that: comprise the following steps,
Step one: prepare electrostatic spinning precursor liquid;
By polymer vacuumize, join in solvent, heating is stirred to polymer and dissolves completely, obtains electrostatic spinning precursor liquid, leaves standstill, for subsequent use; Described vacuum drying condition is temperature 50 C, and the vacuumize time is 24h; The mass ratio of described polymer and described solvent meets 3:17 ~ 1:9; The described condition adding thermal agitation is temperature 20 ~ 80 DEG C, and heating mixing time is more than 8h;
Step 2: electrostatic spinning prepares electrospinning film;
Choosing aluminium foil is dash receiver, is loaded in syringe by the electrostatic spinning precursor liquid in step one, and is placed on micro-injection pump, carry out electrostatic spinning, obtain electrospinning film;
Step 3: backing material surface preparation porous Electrospun nano-fibers film;
According to the relation of the fusing point of backing material and the fusing point of selected polymer, a point the following two kinds mode is prepared:
(A) if the fusing point of described backing material is higher than the fusing point of described polymer;
The aluminium foil posting electrospinning film is immersed in the alcohol of mass fraction 10 ~ 50% after 10 ~ 30s along electrospinning film edge side, aluminium foil is taken out; Had by aluminium foil electrospinning film one side to be attached to backing material surface along electrospinning film edge, then taken off by aluminium foil, electrospinning film transfers to backing material surface; After surface is placed in the dry 24h of vacuum drying chamber with the backing material of electrospinning film, takes out, be clipped between common color printing paper, with hot press hot pressing 1 ~ 2s, obtain porous Electrospun nano-fibers film; Described hot pressing pressure is 1MPa, and hot pressing temperature is 150 ~ 180 DEG C; The baking temperature of described vacuum drying chamber is 40 ~ 50 DEG C;
(B) if the fusing point of described backing material is lower than the fusing point of described polymer;
Aluminium foil with electrospinning film is clipped between common color printing paper, with hot press hot pressing 1 ~ 2s; Aluminium foil with electrospinning film is immersed in 10 ~ 30s in the alcohol of mass fraction 10 ~ 50% along electrospinning film edge side, takes out; Had by aluminium foil electrospinning film one side to be attached to backing material surface along electrospinning film edge, then taken off by aluminium foil, electrospinning film transfers to backing material surface; After surface is placed in the dry 24h of vacuum drying chamber with the backing material of electrospinning film, takes out, obtain porous Electrospun nano-fibers film; Described hot pressing pressure is 1MPa, and hot pressing temperature is 150 ~ 180 DEG C; The temperature of described vacuum drying chamber is 40 ~ 50 DEG C;
Step 4: porous Electrospun nano-fibers film surface imp lantation perfluor liquid;
Draw perfluor liquid with suction pipe, dripped to the porous Electrospun nano-fibers film surface that step 3 is obtained, leave standstill 30min, unnecessary perfluor liquid is removed by gravity, spin coater or stream of nitrogen gas method, the obtained anti-ina thin film of the pouring-in transparent flexible of perfluor liquid.
2. a kind of method utilizing electrostatic spinning to prepare the anti-ina thin film of the pouring-in transparent flexible of perfluor liquid according to claim 1, it is characterized in that: described polymer is Kynoar PVDF or Kynoar-hexafluoropropene PVDF-HFP copolymer, and in described PVDF-HFP copolymer, the mol ratio of PVDF and HFP is 1:1; Described solvent is the mixture of dimethyl formamide, acetone or dimethylacetylamide and acetone, and in described dimethylacetylamide and the mixture of acetone, the mass ratio of acetone and dimethylacetylamide is 7:3.
3. a kind of method utilizing electrostatic spinning to prepare the anti-ina thin film of the pouring-in transparent flexible of perfluor liquid according to claim 1, it is characterized in that: in step 2, the technological parameter of electrostatic spinning is: electrospinning syringe needle internal diameter is 0.2 ~ 0.8mm, the flow-control of electrostatic spinning precursor liquid is 0.1 ~ 2.0mL/h, electrospinning device is 10 ~ 25kV to the voltage that electrostatic spinning precursor liquid applies, spinning head is 10 ~ 25cm to the vertical range of dash receiver, and the electrostatic spinning time is 30 ~ 90min.
4. a kind of method utilizing electrostatic spinning to prepare the anti-ina thin film of the pouring-in transparent flexible of perfluor liquid according to claim 1 or 3, it is characterized in that: in step 2, the technological parameter of electrostatic spinning is: electrospinning syringe needle internal diameter is 0.2 ~ 0.8mm, the flow-control of electrostatic spinning precursor liquid is 1.0 ~ 2.0mL/h, electrospinning device is 20 ~ 25kV to the voltage that electrostatic spinning precursor liquid applies, spinning head is 15cm to the vertical range of dash receiver, and the electrostatic spinning time is 50 ~ 60min.
5. a kind of method utilizing electrostatic spinning to prepare the anti-ina thin film of the pouring-in transparent flexible of perfluor liquid according to claim 1, is characterized in that: described backing material is polyethylene terephthalate film, polychloroethylene film, polyvinyl chloride rubber belt, polypropylene screen or Biaxially oriented polypropylene adhesive tape.
6. a kind of method utilizing electrostatic spinning to prepare the anti-ina thin film of the pouring-in transparent flexible of perfluor liquid according to claim 1, is characterized in that: described perfluor liquid is PFPE, PFO, perfluor triamylamine or FC-770 fluoridize liquid.
7. the anti-ina thin film of the pouring-in transparent flexible of perfluor liquid, is characterized in that: the visible light transmissivity of the anti-ina thin film of the pouring-in transparent flexible of described perfluor liquid reaches more than 80%; Water droplet is 113 ° at the contact angle of the anti-icing film surface of the pouring-in transparent flexible of described perfluor liquid, and roll angle is 3 °.
8. an application for the anti-ina thin film of the pouring-in transparent flexible of perfluor liquid, is characterized in that: be directly applied in and treat that anti-icing surface is for anti-icing, under temperature-5, humidity 50% condition, and frost-free in the 60min time.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510487033.8A CN105063894B (en) | 2015-08-10 | 2015-08-10 | Method for preparing perfluor liquid injection type transparent flexible anti-icing thin film through electrostatic spinning |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510487033.8A CN105063894B (en) | 2015-08-10 | 2015-08-10 | Method for preparing perfluor liquid injection type transparent flexible anti-icing thin film through electrostatic spinning |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105063894A true CN105063894A (en) | 2015-11-18 |
| CN105063894B CN105063894B (en) | 2017-04-19 |
Family
ID=54493382
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510487033.8A Active CN105063894B (en) | 2015-08-10 | 2015-08-10 | Method for preparing perfluor liquid injection type transparent flexible anti-icing thin film through electrostatic spinning |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105063894B (en) |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105347690A (en) * | 2015-12-28 | 2016-02-24 | 中国科学院兰州化学物理研究所 | Transparent coating material with repairable super hydrophobic property and preparation method therefor |
| CN106283390A (en) * | 2016-11-10 | 2017-01-04 | 北京航空航天大学 | A kind of anti-icing double-layer fabric cortina and preparation method thereof |
| CN107488940A (en) * | 2017-09-13 | 2017-12-19 | 安徽农业大学 | A kind of method that electrostatic spinning prepares the degradable biological plasma membrane of PLA Tea Polyphenols |
| CN109750417A (en) * | 2019-01-31 | 2019-05-14 | 青岛大学 | Electrospinning treatment process in situ for paper relics protection |
| CN110603355A (en) * | 2017-03-10 | 2019-12-20 | 索邦大学 | Composite membrane and method for manufacturing such a membrane |
| CN111394891A (en) * | 2020-03-25 | 2020-07-10 | 武汉理工大学 | Preparation method of chitosan oligosaccharide and polyester composite material |
| CN112430900A (en) * | 2020-11-26 | 2021-03-02 | 吉林大学 | Anti-frost light-transmitting electrostatic spinning film and preparation method and application thereof |
| CN112467391A (en) * | 2020-11-16 | 2021-03-09 | 北京航空航天大学 | Inhale and pass through integrative controllable electromagnetic protection material |
| CN117783220A (en) * | 2023-12-21 | 2024-03-29 | 南京邮电大学 | Gas sensor and processing method thereof |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008291371A (en) * | 2007-05-22 | 2008-12-04 | Toyobo Co Ltd | Nanofiber sheet |
| CN102268783A (en) * | 2011-06-20 | 2011-12-07 | 东华大学 | Method for preparing polyvinylidene fluoride (PVDF) porous nanofiber membrane with high ion migration number |
| CN102587040A (en) * | 2012-02-17 | 2012-07-18 | 浙江大东南集团有限公司 | Preparation method of nanofiber membrane for lithium ion battery diaphragm |
| CN102704190A (en) * | 2011-12-29 | 2012-10-03 | 浙江大学 | Method for preparing polyvinylidene fluoride and titanium dioxide (PVDF/TiO2) compounded nanofiber membrane |
| CN103668781A (en) * | 2013-12-17 | 2014-03-26 | 常熟丽源膜科技有限公司 | Preparation method for PVDF porous nanofiber membrane |
| CN104389106A (en) * | 2014-11-12 | 2015-03-04 | 无锡中科光远生物材料有限公司 | Polytetrafluoroethylene superfine fiber film and preparation method thereof |
| JP2016079541A (en) * | 2014-10-21 | 2016-05-16 | キヤノン株式会社 | Polymer nanofiber sheet and method for producing the same |
-
2015
- 2015-08-10 CN CN201510487033.8A patent/CN105063894B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008291371A (en) * | 2007-05-22 | 2008-12-04 | Toyobo Co Ltd | Nanofiber sheet |
| CN102268783A (en) * | 2011-06-20 | 2011-12-07 | 东华大学 | Method for preparing polyvinylidene fluoride (PVDF) porous nanofiber membrane with high ion migration number |
| CN102704190A (en) * | 2011-12-29 | 2012-10-03 | 浙江大学 | Method for preparing polyvinylidene fluoride and titanium dioxide (PVDF/TiO2) compounded nanofiber membrane |
| CN102587040A (en) * | 2012-02-17 | 2012-07-18 | 浙江大东南集团有限公司 | Preparation method of nanofiber membrane for lithium ion battery diaphragm |
| CN103668781A (en) * | 2013-12-17 | 2014-03-26 | 常熟丽源膜科技有限公司 | Preparation method for PVDF porous nanofiber membrane |
| JP2016079541A (en) * | 2014-10-21 | 2016-05-16 | キヤノン株式会社 | Polymer nanofiber sheet and method for producing the same |
| CN104389106A (en) * | 2014-11-12 | 2015-03-04 | 无锡中科光远生物材料有限公司 | Polytetrafluoroethylene superfine fiber film and preparation method thereof |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105347690A (en) * | 2015-12-28 | 2016-02-24 | 中国科学院兰州化学物理研究所 | Transparent coating material with repairable super hydrophobic property and preparation method therefor |
| CN106283390A (en) * | 2016-11-10 | 2017-01-04 | 北京航空航天大学 | A kind of anti-icing double-layer fabric cortina and preparation method thereof |
| CN110603355A (en) * | 2017-03-10 | 2019-12-20 | 索邦大学 | Composite membrane and method for manufacturing such a membrane |
| CN107488940A (en) * | 2017-09-13 | 2017-12-19 | 安徽农业大学 | A kind of method that electrostatic spinning prepares the degradable biological plasma membrane of PLA Tea Polyphenols |
| CN109750417A (en) * | 2019-01-31 | 2019-05-14 | 青岛大学 | Electrospinning treatment process in situ for paper relics protection |
| CN111394891A (en) * | 2020-03-25 | 2020-07-10 | 武汉理工大学 | Preparation method of chitosan oligosaccharide and polyester composite material |
| CN112467391A (en) * | 2020-11-16 | 2021-03-09 | 北京航空航天大学 | Inhale and pass through integrative controllable electromagnetic protection material |
| CN112467391B (en) * | 2020-11-16 | 2021-12-31 | 北京航空航天大学 | Inhale and pass through integrative controllable electromagnetic protection material |
| CN112430900A (en) * | 2020-11-26 | 2021-03-02 | 吉林大学 | Anti-frost light-transmitting electrostatic spinning film and preparation method and application thereof |
| CN117783220A (en) * | 2023-12-21 | 2024-03-29 | 南京邮电大学 | Gas sensor and processing method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105063894B (en) | 2017-04-19 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105063894A (en) | Method for preparing perfluor liquid injection type transparent flexible anti-icing thin film through electrostatic spinning | |
| CN110468461B (en) | Polyamide aerogel fiber, preparation method and application thereof | |
| CN103386257B (en) | A kind of preparation method of the nanofiber composite hyperfiltration membrane based on electrostatic spinning technique | |
| CN105801918B (en) | A kind of cellulose/graphene oxide composite membrane and preparation method thereof | |
| CN102627780A (en) | Method for preparing submicron polyimide self-supporting film by adopting spin-coating method | |
| CN103409940A (en) | Preparation method of dopamine composite nano-fiber affinity membrane for adsorbing La3+ | |
| CN103131040B (en) | Hollow microsphere of polymer having non-permeable surface, and its preparation method | |
| CN102600737A (en) | Method for modifying electrostatic spinning film filtering materials | |
| CN110079876A (en) | A kind of preparation method and application of high oil-absorbing nanofiber aeroge | |
| CN104777019A (en) | Preparation method of cubic boron nitride micro-powder scanning electron microscopy sample | |
| CN105898981A (en) | Stretchable electrode based on conductive fabric and preparation method thereof | |
| CN105568555A (en) | Preparation method of air filtering graphene fiber membrane | |
| CN104250861B (en) | A kind of electrospinning process prepared containing azelon | |
| CN103537206A (en) | Preparation and application of polyimide-imidazole micro-capsule hybrid membrane | |
| CN104562268B (en) | There is phase-change energy-storage fibre of isolation chamber and preparation method thereof | |
| CN100531873C (en) | Application of composite distillation film | |
| CN106784295A (en) | A kind of multi-pore channel IPMC electro-active materials based on foam metal and preparation method thereof | |
| CN103337597B (en) | Silicon oxide nanofiber and polymer composite transparent film and its preparation method and application | |
| CN104888626A (en) | Preparation method of degradable polylactic acid microporous membrane | |
| CN106283390B (en) | A kind of anti-icing double-layer fabric cortina and preparation method thereof | |
| Liu et al. | Properties of hydrophilic chitosan/polysulfone nanofibrous filtration membrane | |
| CN105540618A (en) | Sodium bicarbonate, preparation method thereof and application of sodium bicarbonate in foam materials | |
| CN109622079B (en) | Preparation method of strip-shaped liquid marble | |
| CN108609608A (en) | A method of it prepares with excellent toughness carbon nanocapsule thin film | |
| CN109457391A (en) | A kind of PcH/ZIF nano fibrous membrane and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |