CN102061091B - Method for preparing nylon nano-fiber/polyolefin hybrid shish-kebab - Google Patents
Method for preparing nylon nano-fiber/polyolefin hybrid shish-kebab Download PDFInfo
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- CN102061091B CN102061091B CN2010105899311A CN201010589931A CN102061091B CN 102061091 B CN102061091 B CN 102061091B CN 2010105899311 A CN2010105899311 A CN 2010105899311A CN 201010589931 A CN201010589931 A CN 201010589931A CN 102061091 B CN102061091 B CN 102061091B
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Abstract
The invention discloses a method for preparing a nylon nano-fiber/polyolefin hybrid shish-kebab. The method comprises the following steps: nylon 66 is dissolved in solvent to prepare a nylon solution; the prepared nylon solution is electrospun by using a static spinning device to prepare nano-grade nylon fiber, and the nano-grade nylon fiber is loaded on cover glass; a raw material polyolefin is dissolved in organic solvent under a constant temperature condition to prepare a polyolefin solution; the cover glass on which the electrospun nano-grade nylon fiber is loaded is put in the prepared polyolefin solution to perform constant temperature crystallization; the cover glass is cleaned with pure dimethylbenzene after constant temperature crystallization, and is dried to prepare the nylon nano-fiber/polyolefin hybrid shish-kebab loaded on the cover glass. By the method, massive feature-controllable nylon nano-fiber/polyolefin hybrid shish-kebag structures can be prepared, so that the mechanical performance of the polyolefin composite material can be remarkably improved.
Description
Technical field
The present invention relates to a kind of preparation method of polymer hybrid shish-kebab, particularly relate to the preparation method of a kind of nylon nano fiber/polyolefine hydridization shish-kebab.
Background technology
At present, prepare the technological increasingly mature of nano grade polymer fiber, and nano level polymer fiber is owing to have a very large major diameter returnability when, and the mechanical property of material and thermal property etc. are all had the raising effect through electrostatic spinning.The large-scale production of nanofiber in industry provides possibility for expanding its application in industry.Nylon all is applied in the daily life as a kind of good spinning material all the time.Equally, for emerging electrostatic spinning technique, the electrostatic spinning technique of nylon 66 is also very ripe.Contain carboxamido-group in the nylon 66 on the one hand, its electroconductibility is more better relatively in superpolymer; And nylon 66 can be dissolved in formic acid at normal temperatures, and the electroconductibility of prepared nylon 66 solution is better, can use electrospinning device so more easily and prepare nano level fiber.
Polyolefine is as general-purpose plastics, and is more and more universal in daily life and production.But polyolefinic intensity is not high to have limited its application in some high-end fields.Thereby how research obtains high performance polyolefine material has reality and important meaning.
Big quantity research shows, can significantly improve its intensity when forming shish-kebab structure in the polyolefine.Relevant document shows that shish-kebab is under the effect that has shearing force, to form.Under the effect of shearing force, molecular weight is orientated, and the structure that forms uncrimping chain is shish, the growth of on uncrimping chain, growing nonparasitically upon another plant of the molecular chain around the uncrimping chain then, formation wafer, promptly so-called kebab structure.Keller thinks that the molecular mass of the molecular chain that forms uncrimping chain (shish) will surpass a critical molecular mass (M*), and molecular mass is lower than the molecular chain formation kebab structure of M*.At present, people just are orientated polyolefin melt through in the course of processing, introducing shearing force, thereby obtain shish-kebab structure (shish-kebab).Yet, be limited through the shish-kebab structure quantity of introducing this method acquisition of shearing force, and be difficult to realize, be difficult in the industry and apply.
In recent years, matrix material is widely applied to various fields as a kind of brand-new material that is easy to prepare and can significantly improves product properties.For example, filamentary materials such as spun glass are used to polyolefinic enhancing modified, but owing to reasons such as interface compatibility are relatively poor, the raising effect of polyolefine intensity is limited; And when polyolefin modified,, want usually earlier carry out modification to spun glass in order to improve the cohesiveness between polyolefine and spun glass interface in glass fiber applications.Spun glass is carried out modification generally adopt chemical method or physics method, might destroy the character of spun glass itself like this, thereby reduce the intensity of spun glass.Carbon nanotube, thomel, nanometer silicon dioxide particle etc. also are used to modified polyolefin, mainly are to utilize the property of nano material to reach the purpose that improves the strength of materials.And bibliographical information is arranged, when thomel, carbon nanotube and whisker modified Vilaterm that some are inorganic, produced the crystalline structure similar with shish-kebab.Lee cultivates talent seminar with its called after nano hybridization shish-kebab (nano-hybrid shish-kebab).Yet these are inorganic, diameter is in nano level filler and has also become technical barrier with it with bonding between polymer interface in the dispersion of polymkeric substance.When reaching good dispersiveness, can reduce its intensity again usually through modification.In polyolefin substrate, add polymer fiber, as: polyethylene terephthalate (PET) fiber, polyamide (PA) series fiber (PA6, PA66, PA610 etc.) can form the transcrystallization layer usually.Material property is improved.At present, along with the development of electrostatic spinning technique, can obtain the nanofiber of a large amount of cheapnesss, consider the excellent properties of nanofiber, nanofiber will cause investigator's concern to polyolefinic enhancement.
Summary of the invention
The objective of the invention is: in order to overcome the problems referred to above, the present invention provides a kind of nylon nano fiber/polyolefine assorted
Change the preparation method of shish-kebab.Can prepare the controlled nylon nano fiber of pattern/polyolefine hydridization shish-kebab structure through preparation method of the present invention, like this since, can significantly improve the mechanical property of composite polyolefine material.
In order to address the above problem, the technical scheme that the present invention adopts is:
The present invention provides the preparation method of a kind of nylon nano fiber/polyolefine hydridization shish-kebab, and said preparation method may further comprise the steps:
A, nylon 66 is dissolved in the organic solvent formic acid at 40～80 ℃, is mixed with mass percentage concentration after the dissolving and is 10～25% nylon solution;
B, the nylon solution that step a is prepared utilize electrostatic spinning apparatus; In temperature is that 10～50 ℃, humidity are that 0～50%RH, voltage are that 10～50kV, receiving range are that 10～35cm, receiving trap are the deckglass that is placed on the aluminium sheet; Prepare the nano level nylon fiber after electricity spins, gained nano level nylon fiber loads on the deckglass;
C, take by weighing polyolefine and under 120～135 ℃ of constant temperatures, be dissolved in the organic solvent, be mixed with mass percentage concentration after the dissolving and be 0.01～0.25% polyolefin solution;
The deckglass that d, the load that step b is processed have electricity to spin the nano level nylon fiber is put into the polyolefin solution that step c is mixed with, constant temperature 2～10min under 120～135 ℃ of conditions; Behind the constant temperature its temperature is reduced under 85～120 ℃ of conditions thermostatical crystallization 3～60min;
E, the deckglass behind the steps d thermostatical crystallization is taken out; Utilize pure YLENE to wash; At room temperature dry after the washing, promptly be prepared into nylon nano fiber/polyolefine hydridization shish-kebab after the drying, the nylon nano fiber of processing/polyolefine hydridization shish-kebab loads on the deckglass.
According to the preparation method of above-mentioned nylon nano fiber/polyolefine hydridization shish-kebab, the model of nylon described in the step a 66 is nylon 66 EPR27; Said nylon 66 is dissolved in the organic solvent formic acid under 50～70 ℃ of conditions; Be mixed with mass percentage concentration after 66 dissolvings of said nylon and be 10～20% nylon solution.
According to the preparation method of above-mentioned nylon nano fiber/polyolefine hydridization shish-kebab, temperature described in the step b is that 17～35 ℃, humidity are that 0～30%RH, voltage are that 20～30KV, receiving range are 20～30cm.
According to the preparation method of above-mentioned nylon nano fiber/polyolefine hydridization shish-kebab, the diameter of the nano level nylon fiber that makes after electricity spins described in the step b is 90～180nm.
According to the preparation method of above-mentioned nylon nano fiber/polyolefine hydridization shish-kebab, polyolefine described in the step c is Vilaterm or Vestolen PP 7052; Said organic solvent is YLENE or dichlorobenzene.
According to the preparation method of above-mentioned nylon nano fiber/polyolefine hydridization shish-kebab, in the steps d under 120～135 ℃ of conditions constant temperature 2～5min; Behind the constant temperature its temperature is reduced under 85～120 ℃ of conditions thermostatical crystallization 10～40min.
Preparing method according to above-mentioned nylon nano fiber/polyolefine hydridization shish-kebab utilizes pure YLENE to wash described in the step e, its washing times is 2～3 times; At room temperature dry after the said washing, be 1～10 hour time of drying.
According to the preparation method of above-mentioned nylon nano fiber/polyolefine hydridization shish-kebab, be 3～8 hours said time of drying.
Positive beneficial effect of the present invention:
1, can prepare the controlled nylon nano fiber of a large amount of patterns/polyolefinic hydridization shish-kebab structure (seeing accompanying drawing 2 and Fig. 3 for details) through the inventive method.Thus, can significantly improve the mechanical property of composite polyolefine material, especially can significantly improve the intensity of composite polyolefine material, thereby solve the not high problem of ubiquitous intensity in the polyolefine.
2, preparing method's technology of the present invention is simple; Need not introduce shearing force; Can prepare the hydridization shish-kebab structure (seeing accompanying drawing 2 and accompanying drawing 3 for details) of nylon nano fiber/composite polyolefine material, make the nylon nano fiber/composite polyolefine material of its preparation have higher mechanical property.
3, the nano level nylon fiber of the method prepared one-tenth of the present invention through electrostatic spinning, the nano level nylon fiber that this working method is produced is with low cost, and can mass production; Utilize polyolefin polymer and nylon fiber polymkeric substance to be in preparing method's process of the present invention and had certain consistency between polymkeric substance and the interface; Can prepare nylon nano fiber/polyolefinic matrix material in a large number; And the mechanical property of this matrix material is higher, particularly has higher intensity.
Four, description of drawings:
The nano level nylon fiber sem photograph of Fig. 1 the present invention preparation
One of sem photograph of Fig. 2 product nylon nano fiber of the present invention/polyolefine hydridization shish-kebab
Two of the sem photograph of Fig. 3 product nylon nano fiber of the present invention/polyolefine hydridization shish-kebab
The nano level nylon fiber diameter Distribution figure of Fig. 4 the present invention preparation
Five, embodiment:
Following examples have been merely and have further specified the present invention, do not limit content of the present invention.
Embodiment 1: the preparation method of a kind of nylon nano fiber/polyolefine hydridization shish-kebab
The preparation method of nylon nano fiber of the present invention/polyolefine hydridization shish-kebab, this preparing method's detailed step is following:
A, nylon 66 EPR27 are dissolved in the organic solvent formic acid under 70 ℃ of conditions, are mixed with mass percentage concentration after the dissolving and are 15% nylon solution;
B, the nylon solution that step a is prepared utilize electrostatic spinning apparatus; At spinning temperature is that 30 ℃, spinning humidity are that 0RH, voltage are that 25KV, receiving range are that 25cm, receiving trap are to carry out electricity under the deckglass condition that is placed on the aluminium sheet to spin; Prepare the nano level nylon fiber after electricity spins, gained nano level nylon fiber loads on the deckglass;
C, take by weighing material polyethylene and under 120 ℃ of constant temperatures, be dissolved in the organic solvent YLENE, be mixed with mass percentage concentration after the dissolving and be 0.12% polyethylene solution;
D, the load that step b electricity is spun into have the deckglass of nano level nylon fiber to put into the polyethylene solution that step c is mixed with, constant temperature 2min under 120 ℃ of conditions; Behind the constant temperature its temperature is reduced under 105 ℃ of conditions thermostatical crystallization 30min;
E, the deckglass behind the steps d thermostatical crystallization is taken out; Utilize pure YLENE washing 2～3 times; After the washing at room temperature dry 5 hours, promptly prepare nylon nano fiber/polyolefine hydridization shish-kebab after the drying, the nylon nano fiber of processing/polyolefine hydridization shish-kebab loads on the deckglass.
Embodiment 2: basic identical with embodiment 1, difference is:
The preparation method of nylon nano fiber of the present invention/polyolefine hydridization shish-kebab, this preparation method and embodiment 1 difference are:
Among the step a: nylon 66 EPR27 are dissolved in the organic solvent formic acid under 50 ℃ of conditions, are mixed with mass percentage concentration after the dissolving and are 10% nylon solution;
Among the step b: spinning temperature is that 35 ℃, spinning humidity are that 10RH, voltage are that 20KV, receiving range are 20cm;
Among the step c: take by weighing the raw material Vestolen PP 7052 and under 135 ℃ of constant temperatures, be dissolved in the organic solvent YLENE, be mixed with mass percentage concentration after the dissolving and be 0.2% Vestolen PP 7052 solution;
In the steps d: constant temperature 4min under 135 ℃ of conditions; Behind the constant temperature its temperature is reduced under 110 ℃ of conditions thermostatical crystallization 15min;
Among the step e: after the washing at room temperature dry 3 hours.
Embodiment 3: basic identical with embodiment 1, difference is:
The preparation method of nylon nano fiber of the present invention/polyolefine hydridization shish-kebab, this preparation method and embodiment 1 difference are:
Among the step a: nylon 66 EPR27 are dissolved in the organic solvent formic acid under 60 ℃ of conditions, are mixed with mass percentage concentration after the dissolving and are 20% nylon solution;
Among the step b: spinning temperature is that 25 ℃, spinning humidity are that 20RH, voltage are that 30KV, receiving range are 30cm;
Among the step c: take by weighing material polyethylene and under 130 ℃ of constant temperatures, be dissolved in the organic solvent YLENE, be mixed with mass percentage concentration after the dissolving and be 0.15% polyethylene solution;
In the steps d: constant temperature 5min under 130 ℃ of conditions; Behind the constant temperature its temperature is reduced under 95 ℃ of conditions thermostatical crystallization 10min;
Among the step e: after the washing at room temperature dry 8 hours.
Embodiment 4: basic identical with embodiment 1, difference is:
The preparation method of nylon nano fiber of the present invention/polyolefine hydridization shish-kebab, this preparation method and embodiment 1 difference are:
Among the step a: nylon 66 EPR27 are dissolved in the organic solvent formic acid under 40 ℃ of conditions, are mixed with mass percentage concentration after the dissolving and are 25% nylon solution;
Among the step b: spinning temperature is that 20 ℃, spinning humidity are that 15RH, voltage are that 15KV, receiving range are 10cm;
Among the step c: take by weighing material polyethylene and under 135 ℃ of constant temperatures, be dissolved in the organic solvent YLENE, be mixed with mass percentage concentration after the dissolving and be 0.10% polyethylene solution;
In the steps d: constant temperature 10min under 135 ℃ of conditions; Behind the constant temperature its temperature is reduced under 90 ℃ of conditions thermostatical crystallization 20min;
Among the step e: after the washing at room temperature dry 10 hours.
Embodiment 5: basic identical with embodiment 1, difference is:
The preparation method of nylon nano fiber of the present invention/polyolefine hydridization shish-kebab, this preparation method and embodiment 1 difference are:
Among the step a: nylon 66 EPR27 are dissolved in the organic solvent formic acid under 80 ℃ of conditions, are mixed with mass percentage concentration after the dissolving and are 18% nylon solution;
Among the step b: spinning temperature is that 40 ℃, spinning humidity are that 25RH, voltage are that 50KV, receiving range are 35cm;
Among the step c: take by weighing material polyethylene and under 120 ℃ of constant temperatures, be dissolved in the organic solvent YLENE, be mixed with mass percentage concentration after the dissolving and be 0. 01% polyethylene solution;
In the steps d: constant temperature 3min under 120 ℃ of conditions; Behind the constant temperature its temperature is reduced under 85 ℃ of conditions thermostatical crystallization 60min;
Among the step e: after the washing at room temperature dry 4 hours.
Embodiment 6: basic identical with embodiment 1, difference is:
The preparation method of nylon nano fiber of the present invention/polyolefine hydridization shish-kebab, this preparation method and embodiment 1 difference are:
Among the step a: nylon 66 EPR27 are dissolved in the organic solvent formic acid under 65 ℃ of conditions, are mixed with mass percentage concentration after the dissolving and are 13% nylon solution;
Among the step b: spinning temperature is that 50 ℃, spinning humidity are that 35RH, voltage are that 35KV, receiving range are 32cm;
Among the step c: take by weighing material polyethylene and under 120 ℃ of constant temperatures, be dissolved in the organic solvent YLENE, be mixed with mass percentage concentration after the dissolving and be 0.2% polyethylene solution;
In the steps d: constant temperature 6min under 120 ℃ of conditions; Behind the constant temperature its temperature is reduced under 105 ℃ of conditions thermostatical crystallization 10min;
Among the step e: after the washing at room temperature dry 7 hours.
Embodiment 7: basic identical with embodiment 2, difference is:
The preparation method of nylon nano fiber of the present invention/polyolefine hydridization shish-kebab, this preparation method and embodiment 2 differences are:
Among the step a: nylon 66 EPR27 are dissolved in the organic solvent formic acid under 55 ℃ of conditions, are mixed with mass percentage concentration after the dissolving and are 22% nylon solution;
Among the step b: spinning temperature is that 30 ℃, spinning humidity are that 5RH, voltage are that 28KV, receiving range are 27cm
Among the step c: take by weighing the raw material Vestolen PP 7052 and under 130 ℃ of constant temperatures, be dissolved in the organic solvent dichlorobenzene, be mixed with mass percentage concentration after the dissolving and be 0.25% Vestolen PP 7052 solution;
In the steps d: constant temperature 5min under 130 ℃ of conditions; Behind the constant temperature its temperature is reduced under 100 ℃ of conditions thermostatical crystallization 30min;
Among the step e: after the washing at room temperature dry 6 hours.
Embodiment 8: basic identical with embodiment 1, difference is:
The preparation method of nylon nano fiber of the present invention/polyolefine hydridization shish-kebab, this preparation method and embodiment 1 difference are:
Among the step a: nylon 66 EPR27 are dissolved in the organic solvent formic acid under 70 ℃ of conditions, are mixed with mass percentage concentration after the dissolving and are 16% nylon solution;
Among the step b: spinning temperature is that 28 ℃, spinning humidity are that 0RH, voltage are that 23KV, receiving range are 22cm;
Among the step c: take by weighing material polyethylene and under 120 ℃ of constant temperatures, be dissolved in the organic solvent dichlorobenzene, be mixed with mass percentage concentration after the dissolving and be 0.15% polyethylene solution;
In the steps d: constant temperature 3min under 120 ℃ of conditions; Behind the constant temperature its temperature is reduced under 95 ℃ of conditions thermostatical crystallization 40min;
Among the step e: after the washing at room temperature dry 4 hours.
Claims (2)
1. the preparation method of nylon nano fiber/polyolefine hydridization shish-kebab is characterized in that said preparation method may further comprise the steps:
A, nylon 66 is dissolved in the organic solvent formic acid at 40～80 ℃, is mixed with mass percentage concentration after the dissolving and is 10～25% nylon solution;
B, the nylon solution that step a is prepared utilize electrostatic spinning apparatus; In temperature is that 10～50 ℃, humidity are that 0～50%RH, voltage are that 10～50kV, receiving range are that 10～35cm, receiving trap are the deckglass that is placed on the aluminium sheet; Prepare the nano level nylon fiber after electricity spins, gained nano level nylon fiber loads on the deckglass;
C, take by weighing polyolefine and under 120～135 ℃ of constant temperatures, be dissolved in the organic solvent, be mixed with mass percentage concentration after the dissolving and be 0.01～0.25% polyolefin solution; Said polyolefine is Vilaterm or Vestolen PP 7052, and said organic solvent is YLENE or dichlorobenzene;
The deckglass that d, the load that step b is processed have electricity to spin the nano level nylon fiber is put into the polyolefin solution that step c is mixed with, constant temperature 2～10min under 120～135 ℃ of conditions; Behind the constant temperature its temperature is reduced under 85～120 ℃ of conditions thermostatical crystallization 3～60min;
E, the deckglass behind the steps d thermostatical crystallization is taken out; Utilize pure YLENE to wash; At room temperature dry after the washing, promptly be prepared into nylon nano fiber/polyolefine hydridization shish-kebab after the drying, the nylon nano fiber of processing/polyolefine hydridization shish-kebab loads on the deckglass.
2. the preparation method of nylon nano fiber according to claim 1/polyolefine hydridization shish-kebab is characterized in that: the model of nylon described in the step a 66 is nylon 66 EPR27; Said nylon 66 is dissolved in the organic solvent formic acid under 50～70 ℃ of conditions; Be mixed with mass percentage concentration after 66 dissolvings of said nylon and be 10～20% nylon solution.
3, the preparation method of nylon nano fiber according to claim 1/polyolefine hydridization shish-kebab is characterized in that: temperature described in the step b is that 17～35 ℃, humidity are that 0～30%RH, voltage are that 20～30KV, receiving range are 20～30cm.
4, the preparation method of nylon nano fiber according to claim 1/polyolefine hydridization shish-kebab is characterized in that: the diameter of the nano level nylon fiber that makes after electricity spins described in the step b is 90～180nm.
5, the preparation method of nylon nano fiber according to claim 1/polyolefine hydridization shish-kebab is characterized in that: in the steps d under 120～135 ℃ of conditions constant temperature 2～5min; Behind the constant temperature its temperature is reduced under 85～120 ℃ of conditions thermostatical crystallization 10～40min.
6, the preparation method of nylon nano fiber according to claim 1/polyolefine hydridization shish-kebab is characterized in that: utilize pure YLENE to wash described in the step e, its washing times is 2～3 times; At room temperature dry after the said washing, be 1～10 hour time of drying.
7, the preparation method of nylon nano fiber according to claim 6/polyolefine hydridization shish-kebab, it is characterized in that: be 3～8 hours said time of drying.
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| WO2005034144A1 (en) * | 2003-09-29 | 2005-04-14 | General Electric Company | Conductive thermoplastic compositions, methods of manufacture and articles derived from such compositions |
| CN1657554A (en) * | 2005-01-27 | 2005-08-24 | 武汉理工大学 | Crystalline modified method for transfering phase polymer in magnetic-force-electro-coupling effect |
| CN101100536A (en) * | 2007-07-02 | 2008-01-09 | 四川大学 | Polymer alloy products containing intercrystalline bridge texture and processing method thereof |
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