CN107938011A - A kind of method for preparing GNS/PP composite fibres - Google Patents
A kind of method for preparing GNS/PP composite fibres Download PDFInfo
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- CN107938011A CN107938011A CN201711273254.0A CN201711273254A CN107938011A CN 107938011 A CN107938011 A CN 107938011A CN 201711273254 A CN201711273254 A CN 201711273254A CN 107938011 A CN107938011 A CN 107938011A
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- gns
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- graphene
- spinning
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Classifications
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
- D01F6/46—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polyolefins
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/09—Addition of substances to the spinning solution or to the melt for making electroconductive or anti-static filaments
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
- D01F1/103—Agents inhibiting growth of microorganisms
Abstract
The present invention provides a kind of method for preparing GNS/PP composite fibres, and step is as follows：Prepare the compound preparation liquids of GNS；Feeding；Screw rod mixing；Spinning.Pass through rotary flash distillation, and the mixing in screw rod again, add dispersivenesses of the GNS in PP, spinneret is directly entered after mixing and carries out spinning, it can accomplish scattered compound plus spinning integration, eliminate the intermediate steps for first obtaining graphene/PP composite master batch, save production cost and time.Gained fiber has good antibacterial property, antistatic performance and far infrared transmission performance.
Description
Technical field
The invention belongs to graphene composite material field, and in particular to a kind of method for preparing GNS/PP composite fibres.
Background technology
Graphene (GNS) is because possessing numerous excellent performances, and the graphene worker of all circles is trying to explore stone at present
The downstream application of black alkene, wherein GNS is compound with high molecular material, it is always research hotspot.In numerous composite materials, fiber
The market of material is huge, still, during GNS/ macromolecular fibres are prepared, deposits the problems such as difficult scattered always.
In ZL 201210549357.6, first graphene oxide is mixed with cellulose spin dope, then through Wet-spinning
Silk prepares graphene/cellulose composite fiber.Both of which is solution, and does not have dispersing apparatus in stoste conservation tank, certainly will
Waste liquid can be caused more and disperse non-uniform influence, environmental pressure is added and cause fibre property unstable.
In ZL 201610124616.9, now graphene is mixed with female (PA) grain of polyamide fibre, after double-screw extruding pelletizing,
Graphene modified nylon fiber is obtained after melt spinning.This method is very simple, but because Graphene powder volume density is too small, with PA
Master batch mixing is not easy, and at the same time, twin-screw simply plays the role of extrusion and mixing, is easily caused without further mixing
It is compound uneven, so as to influence the stability of fiber.Secondly, the step of adding to obtain GNS/PA master batches in preparation process, need
Additional power consumption.
In addition, according to some researchs, in order to improve dispersiveness of the graphene in macromolecule, in the mistake of Polymer Synthesizing
Graphene is added in journey.Really, this method can significantly improve dispersiveness, but for manufacturer, this process
Extremely difficult realization, because during Polymer Synthesizing, is related to specifically equipment and condition, adds the production cost of enterprise.
The content of the invention
Extra Granulation Equipments is not required it is an object of the invention to provide a kind of, disperses compound plus spinning integration, ring
Border pollution is small, and method is applicable in the strong method for preparing GNS/PP composite fibres.
The technical solution adopted by the present invention to solve the technical problems is：A kind of method for preparing GNS/PP composite fibres,
Comprise the following steps：
1) preparation of graphene preparation liquid
Suitable solvent is selected, by a certain amount of graphene dispersion in a solvent, high speed shear is uniformly dispersed to obtain graphene
Preparation liquid；
2) feeding
The graphene preparation liquid prepared and PP (polypropylene) master batch are poured into storage tank with certain proportion, set in storage tank
Mixing speed so that graphene is uniformly mixed with PP, then pass through transfer passage, be sent into screw rod mixing, melting mixing；
3) screw rod mixing
Uniformly cover the PP master batches of graphene and enter screw rod mixing by transfer passage, according to the ratio of graphene and PP,
Mixing time and screw speed are set；
4) spinning
Selection spinning process as needed, is made short fine or long filiform GNS/PP composite fibres.
Specifically, the solvent in the step 1) is ethanol, acetone, NMP, DMAc, DMF, polyacrylate, polychlorostyrene acid
It is one or two kinds of in ester, ethylene-vinyl acetate copolymer, paraffin oil.
Specifically, the concentration of graphene is 1-15mg/ml in the GNS preparation liquids in the step 1), and high speed shear is disperseed
Speed 100-800rpm.
Specifically, the mass ratio of GNS and PP is 0.1-5% in the step 2).
Specifically, storage tank mixing speed is arranged to 50-250rpm, incorporation time 30-90min in the step 2).
Specifically, flash distillation and slewing are equipped with the step 2) in transfer passage, flash temperature is at 50-300 DEG C, rotation
Rotary speed is in 50-300rpm.
Specifically, screw speed is 150-350rpm, mixing time 30-60min in the step 3).
Specifically, the spinning process in the step 4) is one kind in melt-spun, wet spinning, dry-spinning, Static Spinning.
Specifically, the GNS/PP composite fibre antibacterial indexes ＞ 95%, antistatic performance ＞ C prepared in the step 4)
Level, far infrared transmission performance ＞ 88%.
The invention has the advantages that：The present invention is mixed through graphene preparation liquid with master batch, then by rotary flash distillation,
The mixing in screw rod again, adds dispersivenesses of the GNS in PP, and spinneret is directly entered after mixing and carries out spinning, can be accomplished
Scattered compound plus spinning integration, eliminate first prepare graphene/PP composite master batch the step for, it is not necessary to extra granulation
Equipment, saves cost.In one embodiment, the fibre antibacterial prepared after testing is 98%, A grade of antistatic performance, far
Infrared emittance 91%.This method is simple, convenient, and environmental pollution is small, and method is applicable in by force, is adapted to extensive composite fibre
Prepare, can be mass-produced and prepare graphene/PP fibers, the production of other composite fibres can also be generalized to.
Embodiment
It is the specific embodiment of the present invention below, technical scheme is described further, but the present invention
Protection domain is not limited to these embodiments.It is every to be included in the present invention without departing substantially from the change of present inventive concept or equivalent substitute
Protection domain within.
Embodiment 1
The accurate GNS powders for weighing certain mass, are dispersed in ethanol with the mixed solution of acetone 1: 1, cutting at a high speed
Cutting dissipates, rate of dispersion 600rpm, it is ensured that the concentration of GNS preparation liquids is 5mg/ml.
It is 0.1% according to GNS and PP master batches mass ratio, PP and preparation liquid is poured into fluid reservoir respectively.Set in fluid reservoir
Mixing velocity 150rpm, mix 30min.Graphene preparation liquid and PP mixtures are transported to screw rod area by conveying device.
Flash distillation and slewing are equipped with transfer passage, flash temperature is at 50 DEG C, and rotary speed is in 300rpm.
Achieve the purpose that to remove solvent by the flash distillation in conveying device.Mixture enters screw rod area, sets screw rod close
Refining condition：200rpm, mixing 45min.
Select wet spinning.Gained fiber is by detection, C grades of antistatic performance, antibacterial index 98%, far infrared transmission
Rate 89%.
Embodiment 2
The accurate GNS powders for weighing certain mass, are dispersed in paraffin oil, high speed shear is disperseed, rate of dispersion
300rpm, it is ensured that the concentration of GNS preparation liquids is 15mg/ml.
It is 1% according to GNS and PP master batches mass ratio, PP and preparation liquid is poured into fluid reservoir respectively.Set in fluid reservoir
Mixing velocity 180rpm, mixes 60min.Graphene preparation liquid and PP mixtures are transported to screw rod area by conveying device.It is defeated
Send and flash distillation and slewing are equipped with passage, flash temperature is at 135 DEG C, and rotary speed is in 200rpm.
Achieve the purpose that to remove solvent by the flash distillation in conveying device.Mixture enters screw rod area, sets screw rod close
Refining condition：300rpm, mixing 30min.
Select melt spinning.Gained fiber is by detection, B grades of antistatic performance, antibacterial index 98.7%, far infrared hair
Penetrate rate 91%.
Embodiment 3
The accurate GNS powders for weighing certain mass, are dispersed in polyacrylate, ethylene-vinyl acetate copolymer 1: 1
Mixed solution in, high speed shear is disperseed, rate of dispersion 250rpm, it is ensured that the concentration of GNS preparation liquids is 10mg/ml.
It is 5% according to GNS and PP master batches mass ratio, PP and preparation liquid is poured into fluid reservoir respectively.Set in fluid reservoir
Mixing velocity 250rpm, mixes 60min.GNS preparation liquids and PP mixtures are transported to screw rod area by conveying device.Conveying is logical
Flash distillation and slewing are equipped with road, flash temperature is at 120 DEG C, and rotary speed is in 220rpm.
Achieve the purpose that to remove solvent by the flash distillation in conveying device.Mixture enters screw rod area, sets screw rod close
Refining condition：350rpm, mixing 60min.
Select electrostatic spinning.Gained fiber is by detection, A grades of antistatic performance, antibacterial index 98%, far infrared transmission
Rate 91%.
Embodiment 4
The accurate GNS powders for weighing certain mass, are dispersed in DMF, DMAc1: in 1 mixed solution, high speed shear
It is scattered, rate of dispersion 800rpm, it is ensured that the concentration of GNS preparation liquids is 1mg/ml.
It is 3% according to GNS and PP master batches mass ratio, PP and preparation liquid is poured into fluid reservoir respectively.Set in fluid reservoir
Mixing velocity 50rpm, mixes 90min.GNS preparation liquids and PP mixtures are transported to screw rod area by conveying device.Conveying is logical
Flash distillation and slewing are equipped with road, flash temperature is at 300 DEG C, and rotary speed is in 50rpm.
Achieve the purpose that to remove solvent by the flash distillation in conveying device.Mixture enters screw rod area, sets screw rod close
Refining condition：150rpm, mixing 50min.
Select dry-spinning spinning.Gained fiber is by detection, B grades of antistatic performance, antibacterial index 98.2%, far infrared hair
Penetrate rate 90%.
Embodiment 5
The accurate GNS powders for weighing certain mass, are dispersed in the mixed solution of NMP, polychlorostyrene acid esters 1: 1, at a high speed
Shearing is scattered, rate of dispersion 500rpm, it is ensured that the concentration of GNS preparation liquids is 10mg/ml.
It is 2% according to GNS and PP master batches mass ratio, PP and preparation liquid is poured into fluid reservoir respectively.Set in fluid reservoir
Mixing velocity 200rpm, mixes 50min.GNS preparation liquids and PP mixtures are transported to screw rod area by conveying device.Conveying is logical
Flash distillation and slewing are equipped with road, flash temperature is at 200 DEG C, and rotary speed is in 100rpm.
Achieve the purpose that to remove solvent by the flash distillation in conveying device.Mixture enters screw rod area, sets screw rod close
Refining condition：250rpm, mixing 45min.
Select electrostatic spinning.Gained fiber is by detection, B grades of antistatic performance, antibacterial index 98%, far infrared transmission
Rate 91%.
Claims (9)
- A kind of 1. method for preparing GNS/PP composite fibres, it is characterised in that comprise the following steps：1) preparation of graphene preparation liquidSuitable solvent is selected, by a certain amount of graphene dispersion in a solvent, high speed shear is uniformly dispersed to obtain graphene preparation Liquid；2) feedingThe graphene preparation liquid prepared and PP master batches are poured into storage tank with certain proportion, the mixing speed in storage tank is set, So that graphene is uniformly mixed with PP, then by transfer passage, screw rod mixing, melting mixing are sent into；3) screw rod mixingThe PP master batches for uniformly covering graphene enter screw rod mixing by transfer passage, according to the ratio of graphene and PP, set Mixing time and screw speed；4) spinningSelection spinning process as needed, is made short fine or long filiform GNS/PP composite fibres.
- 2. the method according to claim 1 for preparing GNS/PP composite fibres, it is characterised in that molten in the step 1) Agent is ethanol, in acetone, NMP, DMAc, DMF, polyacrylate, polychlorostyrene acid esters, ethylene-vinyl acetate copolymer, paraffin oil It is one or two kinds of.
- 3. the method according to claim 1 for preparing GNS/PP composite fibres, it is characterised in that in the step 1) The concentration of graphene is 1-15mg/ml, high speed shear rate of dispersion 100-800rpm in GNS preparation liquids.
- 4. the method according to claim 1 for preparing GNS/PP composite fibres, it is characterised in that GNS in the step 2) Mass ratio with PP is 0.1-5%.
- 5. the method according to claim 1 for preparing GNS/PP composite fibres, it is characterised in that storage tank in the step 2) Mixing speed is arranged to 50-250rpm, incorporation time 30-90min.
- 6. the method according to claim 1 for preparing GNS/PP composite fibres, it is characterised in that conveying in the step 2) Flash distillation and slewing are equipped with passage, flash temperature is at 50-300 DEG C, and rotary speed is in 50-300rpm.
- 7. the method according to claim 1 for preparing GNS/PP composite fibres, it is characterised in that screw rod in the step 3) Rotating speed is 150-350rpm, mixing time 30-60min.
- 8. the method according to claim 1 for preparing GNS/PP composite fibres, it is characterised in that the spinning in the step 4) Silk method is one kind in melt-spun, wet spinning, dry-spinning, Static Spinning.
- 9. the method according to claim 1 for preparing GNS/PP composite fibres, it is characterised in that prepared in the step 4) GNS/PP composite fibre antibacterial indexes ＞ 95%, C grades of antistatic performance ＞, far infrared transmission performance ＞ 88%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711273254.0A CN107938011A (en) | 2017-12-06 | 2017-12-06 | A kind of method for preparing GNS/PP composite fibres |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711273254.0A CN107938011A (en) | 2017-12-06 | 2017-12-06 | A kind of method for preparing GNS/PP composite fibres |
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| CN107938011A true CN107938011A (en) | 2018-04-20 |
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| CN201711273254.0A Pending CN107938011A (en) | 2017-12-06 | 2017-12-06 | A kind of method for preparing GNS/PP composite fibres |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110055610A (en) * | 2019-04-10 | 2019-07-26 | 陕西金瑞烯科技发展有限公司 | A kind of preparation method of graphene polypropylene fiber |
| CN114990787A (en) * | 2022-07-04 | 2022-09-02 | 厦门当盛新材料有限公司 | Flash evaporation non-woven fabric and preparation method thereof |
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| US20170182474A1 (en) * | 2015-12-28 | 2017-06-29 | Aruna Zhamu | Integral 3D graphene-carbon hybrid foam and devices containing same |
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| US20170182474A1 (en) * | 2015-12-28 | 2017-06-29 | Aruna Zhamu | Integral 3D graphene-carbon hybrid foam and devices containing same |
| CN106591981A (en) * | 2017-02-21 | 2017-04-26 | 青岛信泰科技有限公司 | Production device of compound graphene high-strength high-mold polyethylene fiber and preparation method thereof |
| CN107287682A (en) * | 2017-07-07 | 2017-10-24 | 山东圣泉新材料股份有限公司 | A kind of stone needle composite fibre of graphene-containing and its preparation method and application |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110055610A (en) * | 2019-04-10 | 2019-07-26 | 陕西金瑞烯科技发展有限公司 | A kind of preparation method of graphene polypropylene fiber |
| CN114990787A (en) * | 2022-07-04 | 2022-09-02 | 厦门当盛新材料有限公司 | Flash evaporation non-woven fabric and preparation method thereof |
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Application publication date: 20180420 |
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