CN104032381A - Method for preparing hyperbranched polyethylene fiber and hyperbranched polyethylene fiber and carbon nano tube complex fiber through electrostatic spinning - Google Patents
Method for preparing hyperbranched polyethylene fiber and hyperbranched polyethylene fiber and carbon nano tube complex fiber through electrostatic spinning Download PDFInfo
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- CN104032381A CN104032381A CN201410250304.3A CN201410250304A CN104032381A CN 104032381 A CN104032381 A CN 104032381A CN 201410250304 A CN201410250304 A CN 201410250304A CN 104032381 A CN104032381 A CN 104032381A
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Abstract
The invention discloses a method for preparing hyperbranched polyethylene fiber and hyperbranched polyethylene fiber and carbon nano tube complex fiber through electrostatic spinning. The method comprises the following steps: adding hyperbranched polyethylene and an organic solvent into a flask, stirring, heating and dissolving the mixture, cooling the mixture to normal temperature, extracting a solution by an injector to be subjected to the electrostatic spinning; adding hyperbranched polyethylene and the carbon nano tube into the flask; adding the organic solvent into the mixture of hyperbranched polyethylene fiber and the carbon nano tube, stirring, heated and dissolving the mixture of hyperbranched polyethylene, the carbon nano tube and the organic solvent, and then carrying out ultrasonic dispersion; continuously adding hyperbranched polyethylene into the flask, heating, dissolving and then carrying out ultrasonic dispersion; then performing electrostatic spinning after hyperbranched polyethylene is cooled to normal temperature. The method takes advantage of good solubleness of high branching degree polyethylene at normal temperature, and prepares hyperbranched polyethylene fiber through electrostatic spinning at normal temperature, and material is endowed with various excellent performances; the method takes advantage of good dispersibility to carbon nano tube by hyperbranched polyethylene in the solution, prepares the hyperbranched polyethylene solution containing stable dispersed carbon nano tube, and obtains hyperbranched polyethylene complex fiber containing carbon nano tube through electrostatic spinning.
Description
Technical field
The present invention relates to the preparation method of a kind of hyperbranched fiber and composite fibre thereof, particularly a kind of electrostatic spinning is prepared hyperbranched polyethylene fiber and the method with carbon nano tube composite fibre thereof.
Background technology
Polyolefin method of electrostatic spinning is a kind of continuous, efficient, the general method of preparing polymer fiber, can prepare diameter from nanoscale to micron-sized polymer fiber, and therefore electrostatic spinning is prepared polymer fiber and is widely studied.Although electrostatic spinning has been obtained significant progress preparing aspect polymer fiber, but because conventional polyethylene degree of crystallinity is higher, be difficult to dissolve at normal temperatures, cannot carry out solution electrostatic spinning to it at normal temperatures, so it is slow that electrostatic spinning is prepared the progress of polyethylene fiber, generally carry out electrostatic spinning by high-temperature fusion or pyrosol and prepare polyethylene fiber.And the hyperbranched polyethylene of being prepared by rear transition Ni and Pd catalyst has the very high degree of branching, under normal temperature, in the organic solvents such as oxolane, there is good dissolubility, and hyperbranched polyethylene has good film forming, ropiness energy, be applicable to very much preparing polyethylene fiber by electrostatic spinning.
Multi-walled carbon nano-tubes becomes the nano-filled material of preparing advanced polymer composites with its unique character.By with polyblend, it can give material multiple good performance, comprises mechanical performance, thermal conductance, electrical conductance and the rheological property etc. of enhancing.Prepare multiple the polymer composite fibrous of CNT (CNT) that contain by electrostatic spinning, comprised polystyrene/CNT, Merlon/CNT etc.
Summary of the invention
In order to solve the problem existing in background technology, the present invention proposes a kind of electrostatic spinning and prepares hyperbranched polyethylene fiber and the method with carbon nano tube composite fibre thereof.
The object of the invention is to realize by following technical scheme:
One, a kind of electrostatic spinning is prepared the method for hyperbranched polyethylene fiber:
Hyperbranched polyethylene and organic solvent are added in flask, under agitation heating for dissolving obtain solution, the concentration of hyperbranched polyethylene is 3wt%-10wt%, treat that it is cooled to normal temperature, then extract solution from obtain solution with syringe, and the syringe that hyperbranched polyethylene solution is housed is fixed on the specimen holder of electrospinning device, positive source is connected with syringe needle, power cathode is connected with collector, start sampling pump and open high voltage source and carry out electrostatic spinning, after electrostatic spinning finishes, close high voltage source, sampling pump and collector, stop spray silk.
It is 10～30 minutes that described electrostatic spinning carries out duration.
Described collector is cylinder collector.
Described hyperbranched polyethylene is prepared by diimine nickel complex system catalyzed ethylene polymerization.
Described organic solvent is oxolane, chloroform or toluene.
The operating voltage of described electrostatic spinning is at 7-20 kilovolt.
The spinning head of described electrostatic spinning is 10-20 centimetre to the distance of collector.
Described CNT is multi-walled carbon nano-tubes.
To make charging rate be 0.5～0.9ml/h to the speed that pushes away of described sampling pump.
Two, a kind of electrostatic spinning is prepared the method for hyperbranched polyethylene and carbon nano tube composite fibre:
Hyperbranched polyethylene and CNT are added in flask by the mass ratio of 10:1, add organic solvent agitating heating to dissolve 1h, then ultrasonic dispersion 1h, then continue to add hyperbranched polyethylene, the mass ratio that makes hyperbranched polyethylene total amount and CNT is 100:1～20:1, the concentration of hyperbranched polyethylene total amount is 3wt%-10wt%, continues ultrasonic dispersion 1h after heating for dissolving 2h, carries out electrostatic spinning after being then cooled to normal temperature; First extract solution with syringe, and the syringe that hyperbranched polyethylene and carbon nano-tube solution are housed is fixed on the specimen holder of electrospinning device, positive source is connected with syringe needle, power cathode is connected with collector, start sampling pump and open high voltage source and start electrostatic spinning, after electrostatic spinning finishes, close high voltage source, sampling pump and cylinder collector, stop spray silk.
It is 10～30 minutes that described electrostatic spinning carries out duration.
Described collector is cylinder collector.
Described hyperbranched polyethylene is prepared by diimine nickel complex system catalyzed ethylene polymerization.
Described organic solvent is oxolane, chloroform or toluene.
The operating voltage of described electrostatic spinning is at 7-20 kilovolt.
The spinning head of described electrostatic spinning is 10-20 centimetre to the distance of collector.
Described CNT is multi-walled carbon nano-tubes.
To make charging rate be 0.5～0.9ml/h to the speed that pushes away of described sampling pump.
The invention has the beneficial effects as follows:
1, this method is utilized high-branched polyethylene good dissolubility at normal temperatures, prepares hyperbranched polyethylene fiber at normal temperatures by electrostatic spinning.Impact by research solution parameter, electrostatic spinning parameter etc. on polyethylene fiber pattern, utilize CNT to become the nano-filled material of preparing advanced polymer composites with its unique character, by itself and polyblend, give material multiple good performance.
2, the present invention utilizes hyperbranched polyethylene dispersiveness good to CNT in solution, prepare the hyperbranched polyethylene solution that contains stable dispersion CNT, and prepared by electrostatic spinning the hyperbranched polyethylene composite fibre that contains CNT.
Brief description of the drawings
Fig. 1 is the SEM figure of gained fiber after the electrostatic spinning of the embodiment of the present invention 1.
Fig. 2 is the SEM figure of gained fiber after the electrostatic spinning of the embodiment of the present invention 2.
Fig. 3 is the SEM figure of gained fiber after the electrostatic spinning of the embodiment of the present invention 3.
Fig. 4 is the SEM figure of gained fiber after the electrostatic spinning of the embodiment of the present invention 4.
Fig. 5 is the SEM figure of gained fiber after the electrostatic spinning of the embodiment of the present invention 5.
Fig. 6 is the SEM figure of gained fiber after the electrostatic spinning of the embodiment of the present invention 6.
Fig. 7 is the SEM figure that after the electrostatic spinning of the embodiment of the present invention 7, gained contains MWCNT composite fibre.
Fig. 8 is the SEM figure that after the electrostatic spinning of the embodiment of the present invention 8, gained contains MWCNT composite fibre.
Fig. 9 is the SEM figure that after the electrostatic spinning of the embodiment of the present invention 9, gained contains MWCNT composite fibre.
Figure 10 is the SEM figure that after the electrostatic spinning of the embodiment of the present invention 10, gained contains MWCNT composite fibre.
Detailed description of the invention
Below in conjunction with drawings and the specific embodiments, the present invention is described in further detail.
The present invention includes following steps:
Hyperbranched polyethylene and organic solvent are added in flask, under agitation heating for dissolving obtain solution, the concentration of hyperbranched polyethylene is 3wt%-10wt%, treat that it is cooled to normal temperature, then extract solution from obtain solution with syringe, and the syringe that hyperbranched polyethylene solution is housed is fixed on the specimen holder of electrospinning device, positive source is connected with syringe needle, power cathode is connected with collector, set the speed that pushes away of operating voltage and sampling pump, start sampling pump and open high voltage source and carry out electrostatic spinning, after finishing, electrostatic spinning closes high voltage source, sampling pump and collector, stop spray silk.
Hyperbranched polyethylene and CNT are added in flask by the mass ratio of 10:1, add organic solvent agitating heating to dissolve 1h, then ultrasonic dispersion 1h, then continue to add hyperbranched polyethylene, the mass ratio that makes hyperbranched polyethylene total amount and CNT is 100:1～20:1, the concentration of hyperbranched polyethylene total amount is 3wt%-10wt%, continues ultrasonic dispersion 1h after heating for dissolving 2h, carries out electrostatic spinning after being then cooled to normal temperature.
First extract solution with syringe, and the syringe that hyperbranched polyethylene and carbon nano-tube solution are housed is fixed on the specimen holder of electrospinning device, positive source is connected with syringe needle, power cathode is connected with collector, set the speed that pushes away of operating voltage and sampling pump, start sampling pump and open high voltage source and start electrostatic spinning, after electrostatic spinning finishes, closing high voltage source, sampling pump and cylinder collector, stopping spray silk.
It is 10～30 minutes that described electrostatic spinning carries out duration.
Described collector is cylinder collector.
Described hyperbranched polyethylene is prepared by diimine nickel complex system catalyzed ethylene polymerization.
Described organic solvent is oxolane, chloroform or toluene.
The operating voltage of described electrostatic spinning is at 7-20 kilovolt.
The spinning head of described electrostatic spinning is 10-20 centimetre to the distance of collector, and spinning head tip is 10-20 centimetre to the vertical range of collector port.
Described CNT is multi-walled carbon nano-tubes (MWCNT).
To make charging rate be 0.7～1.0ml/h to the speed that pushes away of described sampling pump.
Embodiments of the invention are as follows:
Embodiment 1:
Employing oxolane is organic solvent, the hyperbranched polyethylene being prepared by diimine nickel complex system catalyzed ethylene polymerization and oxolane are added in flask, the solution that under agitation heating for dissolving preparation hyperbranched polyethylene concentration is 5wt%, treat that it is cooled to normal temperature, then extract solution from obtain solution with syringe, and the syringe that hyperbranched polyethylene solution is housed is fixed on the specimen holder of electrospinning device, aluminium-foil paper is looped around on cylinder collector, it is that the rotating speed of 0.76ml/h and cylinder collector is 4m/min that the fltting speed that sampling pump is set makes charging rate, positive source is connected with syringe needle, power cathode is connected with cylindrical collector, open gathering-device and micro-sampling pump, then open high voltage source and start electrostatic spinning, it is that 7kv is (in order to ensure that polymer fiber arrives cylinder receiver smoothly that operating voltage is set, cathode voltage is made as-2kv, cathode voltage is made as 5kv, and will be just, the voltage difference of negative pole is designated as the operating voltage of electrostatic spinning), spinning head is 15 centimetres to the distance of collector, spray silk was closed high voltage source after 30 minutes, sampling pump and cylinder collector, stop spray silk.
The hyperbranched polyethylene fiber pattern of electrostatic spinning gained shows as Fig. 1, and the hyperbranched polyethylene fiber of formation is semi-cylindrical, and relatively homogeneous of the hyperbranched polyethylene fiber thickness preparing, its diameter distributes greatly between 1-3 μ m.
Embodiment 2:
Employing oxolane is organic solvent, the hyperbranched polyethylene being prepared by diimine nickel complex system catalyzed ethylene polymerization and oxolane are added in flask, the solution that under agitation heating for dissolving preparation hyperbranched polyethylene concentration is 5wt%, treat that it is cooled to normal temperature, then extract solution from obtain solution with syringe, and the syringe that hyperbranched polyethylene solution is housed is fixed on the specimen holder of electrospinning device, aluminium-foil paper is looped around on cylinder collector, the fltting speed of sampling pump and the rotating speed of cylinder collector are set, it is that the rotating speed of 0.76ml/h and cylinder collector is 4m/min that the fltting speed that sampling pump is set makes charging rate, positive source is connected with syringe needle, power cathode is connected with cylindrical collector, open gathering-device and micro-sampling pump, then open high voltage source and start electrostatic spinning, it is that 9kv is (in order to ensure that polymer fiber arrives cylinder receiver smoothly that operating voltage is set, cathode voltage is made as-2kv, cathode voltage is made as 7kv, and will be just, the voltage difference of negative pole is designated as the operating voltage of electrostatic spinning), spinning head is 15 centimetres to the distance of collector, spray silk was closed high voltage source after 30 minutes, sampling pump and cylinder collector, stop spray silk.
Electrostatic spinning gained branching, crosslinked hyperbranched polyethylene fiber pattern show as Fig. 2.
Embodiment 3:
Employing oxolane is organic solvent, the hyperbranched polyethylene being prepared by diimine nickel complex system catalyzed ethylene polymerization and oxolane are added in flask, the solution that under agitation heating for dissolving preparation hyperbranched polyethylene concentration is 5wt%, treat that it is cooled to normal temperature, then extract solution from obtain solution with syringe, and the syringe that hyperbranched polyethylene solution is housed is fixed on the specimen holder of electrospinning device, aluminium-foil paper is looped around on cylinder collector, the fltting speed of sampling pump and the rotating speed of cylinder collector are set, it is that the rotating speed of 0.76ml/h and cylinder collector is 4m/min that the fltting speed that sampling pump is set makes charging rate, positive source is connected with syringe needle, power cathode is connected with cylindrical collector, open gathering-device and micro-sampling pump, then open high voltage source and start electrostatic spinning, it is that 12kv is (in order to ensure that polymer fiber arrives cylinder receiver smoothly that operating voltage is set, cathode voltage is made as-2kv, cathode voltage is made as 10kv, and will be just, the voltage difference of negative pole is designated as the operating voltage of electrostatic spinning), spinning head is 15 centimetres to the distance of collector, spray silk was closed high voltage source after 30 minutes, sampling pump and cylinder collector, stop spray silk.
The more curling hyperbranched polyethylene fiber pattern of electrostatic spinning gained shows as Fig. 3.
The concrete electrostatic spinning condition of embodiment 1-3 is summarized in table 1.The implementation process of embodiment 4-6 is identical with embodiment 1, and its concrete electrostatic spinning condition is summarized in table 2, and its gained hyperbranched polyethylene fiber pattern is respectively as Fig. 4～Fig. 6 shows.
The electrostatic spinning implementation condition of table 1 embodiment 1-3
The electrostatic spinning implementation condition of table 2 embodiment 4-6
Embodiment 7:
Hyperbranched polyethylene and multi-walled carbon nano-tubes (MWCNT) are added in flask by the mass ratio of 10:1, add oxolane agitating heating to dissolve 1h, then ultrasonic dispersion 1h, then continue to add hyperbranched polyethylene, the mass ratio that makes hyperbranched polyethylene total amount and multi-walled carbon nano-tubes (MWCNT) is 50:1, the concentration of hyperbranched polyethylene total amount is 3.6wt%, continues ultrasonic dispersion 1h after heating for dissolving 2h, carries out electrostatic spinning after being then cooled to normal temperature.
The polyethylene solution that is dispersed with MWCNT is carried out to electrostatic spinning, first extract solution with syringe, and the syringe that hyperbranched polyethylene and carbon nano-tube solution are housed is fixed on the specimen holder of electrospinning device, positive source is connected with syringe needle, power cathode is connected with collector, setting operating voltage is 9kv, setting the speed that pushes away of sampling pump, to make charging rate be 0.76ml/h, start sampling pump and open high voltage source and start electrostatic spinning, electrostatic spinning carries out 30 minutes, after finishing, electrostatic spinning closes high voltage source, sampling pump and cylinder collector, stop spray silk.
The polyethylene fiber that contains MWCNT preparing as shown in Figure 7.
Embodiment 8:
Hyperbranched polyethylene and multi-walled carbon nano-tubes (MWCNT) are added in flask by the mass ratio of 10:1, add oxolane agitating heating to dissolve 1h, then ultrasonic dispersion 1h, then continue to add hyperbranched polyethylene, the mass ratio that makes hyperbranched polyethylene total amount and multi-walled carbon nano-tubes (MWCNT) is 50:1, the concentration of hyperbranched polyethylene total amount is 3.6wt%, continues ultrasonic dispersion 1h after heating for dissolving 2h, carries out electrostatic spinning after being then cooled to normal temperature.
The polyethylene solution that is dispersed with MWCNT is carried out to electrostatic spinning, first extract solution with syringe, and the syringe that hyperbranched polyethylene and carbon nano-tube solution are housed is fixed on the specimen holder of electrospinning device, positive source is connected with syringe needle, power cathode is connected with collector, setting operating voltage is 12kv, setting the speed that pushes away of sampling pump, to make charging rate be 0.76ml/h, start sampling pump and open high voltage source and start electrostatic spinning, electrostatic spinning carries out 30 minutes, after finishing, electrostatic spinning closes high voltage source, sampling pump and cylinder collector, stop spray silk.
The polyethylene fiber that contains MWCNT preparing as shown in Figure 8.
Embodiment 9:
Hyperbranched polyethylene and multi-walled carbon nano-tubes (MWCNT) are added in flask by the mass ratio of 10:1, add oxolane agitating heating to dissolve 1h, then ultrasonic dispersion 1h, then continue to add hyperbranched polyethylene, the mass ratio that makes hyperbranched polyethylene total amount and multi-walled carbon nano-tubes (MWCNT) is 25:1, the concentration of hyperbranched polyethylene total amount is 3.6wt%, continues ultrasonic dispersion 1h after heating for dissolving 2h, carries out electrostatic spinning after being then cooled to normal temperature.
The polyethylene solution that is dispersed with MWCNT is carried out to electrostatic spinning, first extract solution with syringe, and the syringe that hyperbranched polyethylene and carbon nano-tube solution are housed is fixed on the specimen holder of electrospinning device, positive source is connected with syringe needle, power cathode is connected with collector, setting operating voltage is 9kv, setting the speed that pushes away of sampling pump, to make charging rate be 0.76ml/h, start sampling pump and open high voltage source and start electrostatic spinning, electrostatic spinning carries out 30 minutes, after finishing, electrostatic spinning closes high voltage source, sampling pump and cylinder collector, stop spray silk.
The polyethylene fiber that contains MWCNT preparing as shown in Figure 9.
Embodiment 10:
Hyperbranched polyethylene and multi-walled carbon nano-tubes (MWCNT) are added in flask by the mass ratio of 10:1, add oxolane agitating heating to dissolve 1h, then ultrasonic dispersion 1h, then continue to add hyperbranched polyethylene, the mass ratio that makes hyperbranched polyethylene total amount and multi-walled carbon nano-tubes (MWCNT) is 25:1, the concentration of hyperbranched polyethylene total amount is 3.6wt%, continues ultrasonic dispersion 1h after heating for dissolving 2h, carries out electrostatic spinning after being then cooled to normal temperature.
The polyethylene solution that is dispersed with MWCNT is carried out to electrostatic spinning, first extract solution with syringe, and the syringe that hyperbranched polyethylene and carbon nano-tube solution are housed is fixed on the specimen holder of electrospinning device, positive source is connected with syringe needle, power cathode is connected with collector, setting operating voltage is 15kv, setting the speed that pushes away of sampling pump, to make charging rate be 0.95ml/h, start sampling pump and open high voltage source and start electrostatic spinning, electrostatic spinning carries out 30 minutes, after finishing, electrostatic spinning closes high voltage source, sampling pump and cylinder collector, stop spray silk.
The polyethylene fiber that contains MWCNT preparing as shown in figure 10.
The concrete electrostatic spinning condition of embodiment 7-10 is summarized in table 3.
Table 3 electrostatic spinning is prepared the condition of polyethylene/carbon nano tube composite fibre
Because research shows, hyperbranched polyethylene has good peptizaiton in organic solvent to CNT, therefore can prepare and obtain the hyperbranched polyethylene solution that contains stable dispersion CNT, then prepare the HBPE/CNT composite fibre with special performance by electrostatic spinning.Therefore in the inventive method, select hyperbranched polyethylene, by heating, polyethylene is dissolved in solvent completely, be mixed with the solution that concentration is 3wt%-10wt%.
According to former report, by heating and ultrasonic dispersion, the polyethylene solution that preparation contains MWCNT, leaves standstill 2 hours, and without MWCNT precipitation generation, what show to obtain is stable solution.
Distinguishing feature of the present invention is that the solution electrostatic spinning by implementing under normal temperature has been prepared hyperbranched polyethylene fiber and hyperbranched polyethylene/carbon nano tube composite fibre.The composite fibre of having prepared the polymer fiber of different-shape and having contained CNT by adjusting the parameters such as solution concentration, voltage.
Electrostatic spinning condition (embodiment 1～3) when different voltage is summarized in table 1, and the pattern of gained fiber as shown in FIG. 1 to 3.Fig. 1 is the SEM figure of embodiment 1 gained fiber, and right figure B ' is the partial enlarged drawing of left figure B.Fig. 2 is the SEM figure of embodiment 2 gained fibers, and right figure D ' is the partial enlarged drawing of left figure D.Fig. 3 is the SEM figure of embodiment 3 gained fibers, and right figure E ' is the partial enlarged drawing of left figure E.
In figure, can find out, when 9kv, electrostatic spinning obtain except most polyethylene fiber, also have a small amount of pearl polyethylene.When 12kv, what electrostatic spinning obtained is fiber bending, lack of alignment, and its diameter distributes and is about 1-4 μ m.
Electrostatic spinning condition (embodiment 4～6) when different solutions concentration is summarized in table 1, and the pattern of gained fiber is as shown in Fig. 4～Fig. 6.Fig. 4 is the SEM figure of embodiment 4 gained fibers, and right figure B ' is the partial enlarged drawing of left figure B.Fig. 5 is the SEM figure of embodiment 5 gained fibers, and right figure F ' is the partial enlarged drawing of left figure F.Fig. 6 is the SEM figure of embodiment 6 gained fibers, and right figure I ' is the partial enlarged drawing of left figure I.
Tri-solution concentrations of 3wt%, 4wt% and 5wt% electrostatic spinning of polyethylene solution at present in embodiment, actual conditions is summarized in table 2.Concentration is that polyethylene fiber that the solution electrostatic spinning of 3wt% obtains can be divided into crude fibre (diameter 2-3 μ m) and fine fibre (m) two parts of diameter <1 μ.Gained crude fibre length is shorter, exists a large amount of fine fibres to make it to interconnect and reticulate between crude fibre.When 4wt% and 5wt% concentration, electrostatic spinning can obtain being evident as cancellated polyethylene fiber, and its diameter is distributed between 1-4 μ m mostly.
The solution of HBPE/MWCNT=50:1 under different voltage electrostatic spinning gained fiber pattern as shown in Figure 7 and Figure 8, actual conditions is summarized in table 3.Fig. 7 is the SEM figure of embodiment 7 gained fibers, and right Fig. 5 A ' is the partial enlarged drawing of left Fig. 5 A.Fig. 8 is the SEM figure of embodiment 8 gained fibers, and right Fig. 5 B ' is the partial enlarged drawing of left Fig. 5 B.All there is black splotch obvious, not of uniform size on the polyethylene composite fibre surface obtaining under two voltages.Due to the MWCNT that contains a great deal of for the polyethylene solution of electrostatic spinning, therefore black region should be MWCNT accumulation regions.The existence of MWCNT accumulation regions may be in polyethylene solution, to disperse inhomogeneously due to MWCNT, and voltage is distributed with certain influence in fiber to MWCNT.
The solution of HBPE/MWCNT=25:1 under different voltage electrostatic spinning gained fiber pattern as shown in Figure 9 and Figure 10, actual conditions is summarized in table 3.Fig. 9 is the SEM figure of embodiment 9 gained fibers, and right Fig. 6 B ' is the partial enlarged drawing of left Fig. 6 B.Figure 10 is the SEM figure of embodiment 10 gained fibers, and right Fig. 6 C ' is the partial enlarged drawing of left Fig. 6 C.Under two voltages, all obtain the hyperbranched polyethylene composite fibre that contains MWCNT.
As can be seen here, the present invention utilizes electrostatic spinning technique to prepare to have the hyperbranched polyethylene fiber of unique morphology, the potential application of further having expanded hyperbranched polyethylene.Utilize electrostatic spinning to prepare the hyperbranched polyethylene composite fibre that contains multi-walled carbon nano-tubes, for hyperbranched polyethylene fiber has been given new performance.
Claims (10)
1. an electrostatic spinning is prepared the method for hyperbranched polyethylene fiber, it is characterized in that: hyperbranched polyethylene and organic solvent are added in flask, under agitation heating for dissolving obtain solution, the concentration of hyperbranched polyethylene is 3wt%-10wt%, treat that it is cooled to normal temperature, then extract solution from obtain solution with syringe, and the syringe that hyperbranched polyethylene solution is housed is fixed on the specimen holder of electrospinning device, positive source is connected with syringe needle, power cathode is connected with collector, start sampling pump and open high voltage source and carry out electrostatic spinning, after finishing, electrostatic spinning closes high voltage source, sampling pump and collector, stop spray silk.
2. an electrostatic spinning is prepared the method for hyperbranched polyethylene and carbon nano tube composite fibre, it is characterized in that: hyperbranched polyethylene and CNT are added in flask by the mass ratio of 10:1, add organic solvent agitating heating to dissolve 1h, then ultrasonic dispersion 1h, then continue to add hyperbranched polyethylene, the mass ratio that makes hyperbranched polyethylene total amount and CNT is 100:1～20:1, the concentration of hyperbranched polyethylene total amount is 3wt%-10wt%, continue ultrasonic dispersion 1h after heating for dissolving 2h, carry out electrostatic spinning after being then cooled to normal temperature;
First extract solution with syringe, and the syringe that hyperbranched polyethylene and carbon nano-tube solution are housed is fixed on the specimen holder of electrospinning device, positive source is connected with syringe needle, power cathode is connected with collector, start sampling pump and open high voltage source and start electrostatic spinning, after electrostatic spinning finishes, close high voltage source, sampling pump and cylinder collector, stop spray silk.
3. method according to claim 1 and 2, is characterized in that: it is 10～30 minutes that described electrostatic spinning carries out duration.
4. method according to claim 1 and 2, is characterized in that: described collector is cylinder collector.
5. method according to claim 1 and 2, is characterized in that: described hyperbranched polyethylene is prepared by diimine nickel complex system catalyzed ethylene polymerization.
6. method according to claim 1 and 2, is characterized in that: described organic solvent is oxolane, chloroform or toluene.
7. method according to claim 1 and 2, is characterized in that: the operating voltage of described electrostatic spinning is at 7-20 kilovolt.
8. method according to claim 1 and 2, is characterized in that: the spinning head of described electrostatic spinning is 10-20 centimetre to the distance of collector.
9. method according to claim 1 and 2, is characterized in that: described CNT is multi-walled carbon nano-tubes.
10. method according to claim 1 and 2, is characterized in that: to make charging rate be 0.5 ~ 0.9 ml/h to the speed that pushes away of described sampling pump.
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