CN103184651A - Preparation method of bacteria cellulose fiber-based carbon nanofiber knitted fabric - Google Patents
Preparation method of bacteria cellulose fiber-based carbon nanofiber knitted fabric Download PDFInfo
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- CN103184651A CN103184651A CN201110455904XA CN201110455904A CN103184651A CN 103184651 A CN103184651 A CN 103184651A CN 201110455904X A CN201110455904X A CN 201110455904XA CN 201110455904 A CN201110455904 A CN 201110455904A CN 103184651 A CN103184651 A CN 103184651A
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Abstract
The invention relates to a bacteria cellulose fiber-based carbon nanofiber knitted fabric, which is made through the following steps: adopting spinning and knitting technology to prepare a carbon nanofiber knitted fabric with a superfine bacteria cellulose fiber subjected to refining and carding treatment by the needling, and carrying out pyrolysis carbonization and graphitization. The preparation method has the benefits that the raw material source is wide; the price is low; the processing method is environment-friendly, safe, simple and efficient; the bacteria cellulose fiber-based carbon nanofiber knitted fabric gained after processing has wide application fields; and the potential economic benefit is huge.
Description
Technical field
This patent relates to a kind of preparation method of carbon nano-fiber knitted cloth, particularly a kind of preparation method of bacteria cellulose fibre base nano carbon fibre knitted cloth.
Technical background
In 19 end of the centurys, people are when research hydrocarbons thermal cracking and carbon monoxide disproportionated reaction, and just having been found that at catalyst surface has superfine little fibrous material to occur, and this fibrous material is exactly carbon nano-fiber (GNFs or CNFs).Carbon nano-fiber is the nanofiber that is curled and formed by the multilayer graphite flake, do not have tangible hollow structure, diameter is generally between 10-500 nm, between CNT (carbon nano-tube) and gas-phase growth of carbon fibre, thereby the structure of carbon nano-fiber and the transition state that performance is in gas-phase growth of carbon fibre and CNT (carbon nano-tube) have been determined, not only have the characteristic that gas-phase growth of carbon fibre has, and very similar to CNT (carbon nano-tube) at aspects such as structure, performance and application.The preparation method of carbon nano-fiber has multiple, but major part still is in laboratory stage.Difference because of preparation method and technology, carbon nano-fiber can present different shapes, by adopting different parameters in course of reaction, not only can control the diameter of carbon nano-fiber, can also obtain the nanofiber of different-shape, as whisker shape, helical form, tubulose, cellular etc.
Carbon nano-fiber is as a kind of novel material with carbon element, and excellent physics, mechanical property and chemical stability are arranged, the suction ripple, conduction, heat conduction and the thermal stability that compare favourably as low-density, high ratio modulus, high specific strength, high-specific surface area, with graphite.In recent years, the research about carbon nano-fiber has caused people's interest widely.Diversified nano-sized carbon crystallization, needle-like, bar-shaped, tubbiness etc. emerge in an endless stream.Carbon nanometer technology purposes is extremely extensive, obtains in fields such as Aeronautics and Astronautics, military affairs, the energy, automobile, food, light industry, weaving, IT, medical science to use.Along with to carbon nano-fiber research deepen continuously and the potential high-tech area of carbon nano-fiber is used widely, limitation has appearred in carbon nanomaterial in actual applications, and people begin the sight of research is further turned to the preparation of carbon nano-fabric from the preparation of carbon nano-fiber fiber.
As nanofiber is implanted fabric face, can form the stable gas membrane of one deck, make two thin property interfaces fabric, reach both waterproof, again can be grease proofing, antifouling; With the senior protective clothing that nanofiber is made, its fabric porous and film is arranged air is seen through, but minuteness particle be kept out the wind and be filtered to the tool respiratory can also, and aerosol is had block, can prevent chemical and biological weapons and noxious material.Successful spun the CNT ultra high strength fiber to the nanotechnology research in branch school, Texas ,Usa university Dallas, and it is more solid than steel wire or spider silk, can conduct electricity simultaneously, and scientist has woven the CNT cloth with this nano wire.This new development of carbon nanomaterial makes people utilize CNT to spin in the near future and weaves cotton cloth, and cutting sews the clothes that can be through on one's body.The research group of Bao Man has also developed carbon nano-tube fibre and has been made into cloth making step: at first, millions of small CNTs and polyvinyl alcohol are evenly mixed, make gel; Then, through weaving and baking operation, this gel is spun into soft CNT long fiber; Then, again the fiber of making is put into the container that fills poly-vinyl alcohol solution, make carbon nano-tube/poly vinyl alcohol (SWCNT/PVA) composite fibre that diameter is about 50 μ m, wherein contain 60% CNT approximately; At last, they attempt this fiber is made into cloth.The method that University of Texas utilized and stretch, twisted CNT " forest " and compound absorption powder processes carbon nano-tube yarn.Nanocomp scientific ﹠ technical corporation is with traditional wool processing technology processing carbon nano tube " forest ", produce carbon nanometer yarn and be applied to bulletproof jacket, artificial-muscle, ultracapacitor, super high intensity lamps, superelevation inductor, and the various products such as absorption of microwave, electric wave.But the limitation of the process technology of CNT " forest " has restricted development and the popularization of this method.The exploitation of carbon nanomaterial and application have become the scientific research hot topic.But the problem that faces at present is to lack the large-scale production that can bring economic benefit.Realize that industrialization production carbon nano-fiber knitted fabric becomes very necessary.
Bacterial cellulose wet-coating is a kind of byproduct of food industries, the chemical purity height, the source is wide, and price is low, has meticulous space network structure, its fibre diameter is between 10-100 nm, and chemical purity is very high, does not need follow-up removal of impurities, the present invention is raw material with the bacteria cellulose superfine fibre, adopt spinning, knitting, be woven into the bacteria cellulose micro-fiber knitted fabric, after pyrolysis carbonization and graphitization, prepare the woven cloth of carbon nano-fiber.The bacteria cellulose micro-fiber knitted fabric that this method is produced adopts the weaving processing technology, and weaving processes that cost is lower comparatively speaking, potential huge economic benefit.
Summary of the invention
The present invention relates to a kind of preparation method of bacteria cellulose fibre base nano carbon fibre knitted cloth.
For achieving the above object, the technical solution used in the present invention is as follows:
The preparation method of bacteria cellulose fibre base nano carbon fibre knitted cloth of the present invention comprises the steps:
(1) will bleach bacterial cellulose wet-coating after handling and place between a pair of gripping roller or grip roller and feed between the plate, feed with 10 mm ~ 100 m/ minutes speed;
(2) puncture at a high speed, isolate and combing effect through licker-in surface acupuncture from the cellulose membrane of exporting between the roller, bacterial cellulose wet-coating is become bacteria cellulose fibre;
(3) the bacteria cellulose superfine fibre is handled through the filter press press filtration, prepared the bacteria cellulose superfine fibre bar of 15% ~ 50000% moisture content; Superfine fibre diameter 10 ~ 500nm, superfine fibre length 200nm ~ 100mm;
(4) above bacteria cellulose superfine fibre bar is handled through shredding, combing, one-tenth net, slivering, spinning processing technology through ribbon, form bacteria cellulose superfine fibre yarn, through being prepared into the bacteria cellulose micro-fiber knitted fabric through volume, weft-knitted processing technology;
(5) above bacteria cellulose micro-fiber knitted fabric is handled through liquid nitrogen;
(6) above bacteria cellulose micro-fiber knitted fabric is put into the freeze drier freeze-drying;
(7) treat in the bacterial fibers knitted cloth to prepare the macro morphology when keeping hygrometric state, the porous bacteria cellulose fabric knitted cloth of constancy of volume behind the moisture-free;
(8) the bacteria cellulose knitted cloth after the freeze drying is positioned in the horse expense stove, sets certain heating curve, under 600 ℃ ~ 1500 ℃ condition, carrying out carbonization respectively under the protective atmosphere of straight argon, thereby preparing the carbon nano-fiber knitted cloth;
(9) the carbon fiber knitted cloth after the carbonization is placed in the high temperature graphitization stove, under 2200 ℃ ~ 2800 ℃ temperature, is carrying out graphitization respectively under the protective atmosphere of straight argon.
Described bacteria cellulose film is the bacterial cellulose wet-coating of bleaching after handling, and bacterial cellulose wet-coating is the former film of bacteria cellulose that utilizes acetobacter xylinum to obtain for the whole bag of tricks of main bacteria seed, and this former film obtains bacterial cellulose wet-coating after the NaOH solution-treated.
Described gripping roller diameter is 20 ~ 3000mm.
Described licker-in comprises central shaft, be with cylinder on the central shaft, the outer wall of cylinder is provided with needle-like combing acupuncture, diameter of cylinder is 300 ~ 600mm, acupuncture length 0.1 ~ 5cm, acupuncture bar portion diameter is 0.001 ~ 3mm, acupuncture tip diameter is 1 ~ 100um, needle puncture tip minister's degree is 1 ~ 10mm, 2 ~ 1000/cm of needling density
2
Above bacteria cellulose superfine fibre is handled through the liquid nitrogen submergence.
At present, the preparation method of carbon nano-fiber has multiple, but major part still is in laboratory stage.Based on the huge potential using value of carbon nano-fiber, realize that industrialization production carbon nano-fiber becomes very necessary.Electrostatic spinning is present unique method that can prepare polymer nanofiber directly, continuously, but its operation more complicated, cost is than higher.If directly carbonization has the high molecular polymer of nanofibrous structures, then can simplify preparation process and reduce cost.Bacteria cellulose is a kind of natural macromolecular material, has meticulous space network structure, its fibre diameter is between 10-100 nm, and chemical purity is very high, does not need follow-up removal of impurities, bacteria cellulose is a kind of byproduct of food industries in addition, the source is wide, and price is low, and it is present that the present invention prepares carbon nano-fiber with the bacteria cellulose fibre base as the matrix of carbonization, the preparation method of carbon nano-fiber has multiple, but major part still is in laboratory stage.Based on the huge potential using value of carbon nano-fiber, realize that industrialization production carbon nano-fiber becomes very necessary.Electrostatic spinning is present unique method that can prepare polymer nanofiber directly, continuously, but its operation more complicated, cost is than higher.If directly carbonization has the high molecular polymer of nanofibrous structures, then can simplify preparation process and reduce cost.Bacteria cellulose is a kind of natural macromolecular material, has meticulous space network structure, its fibre diameter is between 10-100 nm, and chemical purity is very high, do not need follow-up removal of impurities, bacteria cellulose is a kind of byproduct of food industries in addition, the source is wide, price is low, the present invention prepares the carbon nano-fiber yarn with the bacteria cellulose fibre base as the matrix of carbonization, and raw material sources are wide, price is low, processing method environmental protection, safety, simple, efficient, the bacteria cellulose base nano carbon fibre yarn Application Areas that processing obtains is extensive, potential huge economic benefit.
Knitted fabric is to form coil by yarn by the regular motion of knitting needle, the mutual fabric that overlaps and form of going here and there between coil and the coil.The knitted fabric quality is soft, and good wrinkle resistance and permeability are arranged, and has bigger extensibility and elasticity.Be widely used in the tubular fiber material, as filtration, oil transportation, gas transmission high-voltage tube.The carbon fiber strength height, rigidity is big, can't use traditional knitting processing technology and prepare extensibility, elasticity, permeability material.Processing technology of the present invention can realize the processing of carbon fiber knitted fabric, the knitted fabric carbon fibre material of obtained performance excellence.
The specific embodiment
Below in conjunction with specific embodiment, further set forth the present invention.
Embodiment 1
It is between the gripping roller of 20mm that bacterial cellulose wet-coating after the bleaching processing is placed a pair of diameter, feeds according to certain speed (10 mm/ minutes); Puncture at a high speed, isolate and combing effect through needle-like, polishing wheel surface needle-like combing acupuncture superhard, that the elastic stainless steel silk constitutes, bacterial cellulose wet-coating is become bacteria cellulose fibre; The bacteria cellulose superfine fibre is handled through the filter press press filtration, prepared the bacteria cellulose superfine fibre bar of 100% moisture content.Superfine fibre diameter 100nm, superfine fibre length 40mm.With above bacteria cellulose superfine fibre bar through ribbon through PROCESS FOR TREATMENT such as shredding, combing, one-tenth net, slivering, spinning processing, form bacteria cellulose superfine fibre yarn, through through compile, weft-knitted processing technology is prepared into the bacteria cellulose micro-fiber knitted fabric.Above bacteria cellulose micro-fiber knitted fabric is after liquid nitrogen is handled, put into the vacuum freeze drier freeze-drying, treat in the micro-fiber knitted fabric to prepare the macro morphology when keeping hygrometric state, the ultra-fine dry state fabric knitted cloth of the porous bacteria cellulose of constancy of volume behind the moisture-free; Above micro-fiber knitted fabric is positioned in the horse expense stove, and under the protective atmosphere of straight argon, according to certain heating curve, temperature reaches 700 ℃ and kept 1 hour, prepares the carbon nano-fiber knitted cloth.This carbon nano-fiber knitted cloth forms the graphitization nano carbon fabric knitted cloth through 2200 ℃ of graphitization processing.
Embodiment 2
It is between the gripping roller of 50mm that bacterial cellulose wet-coating after the bleaching processing is placed a pair of diameter, feeds according to certain speed (50 mm/ minutes); Puncture at a high speed, isolate and combing effect through needle-like, polishing wheel surface needle-like combing acupuncture superhard, that the elastic stainless steel silk constitutes, bacterial cellulose wet-coating is become bacteria cellulose fibre; The bacteria cellulose superfine fibre is handled through the filter press press filtration, prepared the bacteria cellulose superfine fibre bar of 100% moisture content.Superfine fibre diameter 100nm, superfine fibre length 60mm.With above bacteria cellulose superfine fibre bar through ribbon through PROCESS FOR TREATMENT such as shredding, combing, one-tenth net, slivering, spinning processing, form bacteria cellulose superfine fibre yarn, through through compile, weft-knitted processing technology is prepared into the bacteria cellulose micro-fiber knitted fabric.Above bacteria cellulose micro-fiber knitted fabric is after liquid nitrogen is handled, put into the vacuum freeze drier freeze-drying, treat in the micro-fiber knitted fabric to prepare the macro morphology when keeping hygrometric state, the ultra-fine dry state fabric knitted cloth of the porous bacteria cellulose of constancy of volume behind the moisture-free; Above micro-fiber knitted fabric is positioned in the horse expense stove, and under the protective atmosphere of straight argon, according to certain heating curve, temperature reaches 700 ℃ and kept 1 hour, prepares the carbon nano-fiber knitted cloth.This carbon nano-fiber knitted cloth forms the graphitization nano carbon fabric knitted cloth through 2500 ℃ of graphitization processing.
Embodiment 3
It is between the gripping roller of 80mm that bacterial cellulose wet-coating after the bleaching processing is placed a pair of diameter, feeds according to certain speed (1000 mm/ minutes); Puncture at a high speed, isolate and combing effect through needle-like, polishing wheel surface needle-like combing acupuncture superhard, that the elastic stainless steel silk constitutes, bacterial cellulose wet-coating is become bacteria cellulose fibre; The bacteria cellulose superfine fibre is handled through the filter press press filtration, prepared the bacteria cellulose superfine fibre bar of 90% moisture content.The superfine fibre diameter is less than 100nm, and superfine fibre length is less than 100mm.With above bacteria cellulose superfine fibre bar through ribbon through PROCESS FOR TREATMENT such as shredding, combing, one-tenth net, slivering, spinning processing, form bacteria cellulose superfine fibre yarn, through through compile, weft-knitted processing technology is prepared into the bacteria cellulose micro-fiber knitted fabric.Above bacteria cellulose micro-fiber knitted fabric is after liquid nitrogen is handled, put into the vacuum freeze drier freeze-drying, treat in the micro-fiber knitted fabric to prepare the macro morphology when keeping hygrometric state, the ultra-fine dry state fabric knitted cloth of the porous bacteria cellulose of constancy of volume behind the moisture-free; Above micro-fiber knitted fabric is positioned in the horse expense stove, and under the protective atmosphere of straight argon, according to certain heating curve, temperature reaches 700 ℃ and kept 1 hour, prepares the carbon nano-fiber knitted cloth.This carbon nano-fiber knitted cloth forms the graphitization nano carbon fabric knitted cloth through 2800 ℃ of graphitization processing.
Claims (5)
1. the preparation method of a bacteria cellulose fibre base nano carbon fibre knitted cloth is characterized in that, comprises the steps:
(1) will bleach bacterial cellulose wet-coating after handling and place between a pair of gripping roller or grip roller and feed between the plate, feed with 10 mm ~ 100 m/ minutes speed;
(2) puncture at a high speed, isolate and combing effect through licker-in surface acupuncture from the cellulose membrane of exporting between the roller, bacterial cellulose wet-coating is become bacteria cellulose fibre;
(3) the bacteria cellulose superfine fibre is handled through the filter press press filtration, prepared the bacteria cellulose superfine fibre bar of 15% ~ 50000% moisture content; Superfine fibre diameter 10 ~ 500nm, superfine fibre length 200nm ~ 100mm;
(4) above bacteria cellulose superfine fibre bar is handled through shredding, combing, one-tenth net, slivering, spinning processing technology through ribbon, form bacteria cellulose superfine fibre yarn, through being prepared into the bacteria cellulose micro-fiber knitted fabric through volume, weft-knitted processing technology;
(5) above bacteria cellulose micro-fiber knitted fabric is handled through liquid nitrogen;
(6) above bacteria cellulose micro-fiber knitted fabric is put into the freeze drier freeze-drying;
(7) treat in the bacterial fibers knitted cloth to prepare the macro morphology when keeping hygrometric state, the porous bacteria cellulose fabric knitted cloth of constancy of volume behind the moisture-free;
(8) the bacteria cellulose knitted cloth after the freeze drying is positioned in the horse expense stove, sets certain heating curve, under 600 ℃ ~ 1500 ℃ condition, carrying out carbonization respectively under the protective atmosphere of straight argon, thereby preparing the carbon nano-fiber knitted cloth;
(9) the carbon fiber knitted cloth after the carbonization is placed in the high temperature graphitization stove, under 2200 ℃ ~ 2800 ℃ temperature, is carrying out graphitization respectively under the protective atmosphere of straight argon.
2. the preparation method of bacteria cellulose fibre base nano carbon fibre knitted cloth according to claim 1, it is characterized in that: described bacteria cellulose film is for bleaching the bacterial cellulose wet-coating after handling, bacterial cellulose wet-coating is the former film of bacteria cellulose that utilizes acetobacter xylinum to obtain for the whole bag of tricks of main bacteria seed, and this former film obtains bacterial cellulose wet-coating after the NaOH solution-treated.
3. the preparation method of bacteria cellulose fibre base nano carbon fibre knitted cloth according to claim 1, it is characterized in that: described gripping roller diameter is 20 ~ 3000mm.
4. the preparation method of bacteria cellulose fibre base nano carbon fibre knitted cloth according to claim 1, it is characterized in that: described licker-in comprises central shaft, be with cylinder on the central shaft, the outer wall of cylinder is provided with needle-like combing acupuncture, and diameter of cylinder is 300 ~ 600mm, acupuncture length 0.1 ~ 5cm, acupuncture bar portion diameter is 0.001 ~ 3mm, acupuncture tip diameter is 1 ~ 100um, and needle puncture tip minister's degree is 1 ~ 10mm, 2 ~ 1000/cm of needling density
2
5. the preparation method of bacteria cellulose fibre base nano carbon fibre knitted cloth according to claim 1 is characterized in that: above bacteria cellulose superfine fibre is handled through the liquid nitrogen submergence.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103806130A (en) * | 2014-02-24 | 2014-05-21 | 钟春燕 | Preparation method for bacterial cellulose-based nano active carbon fibers |
| CN108301109A (en) * | 2018-03-27 | 2018-07-20 | 东华大学 | A kind of carbon nano-tube fibre knitted fabric and preparation method thereof |
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| CN103806130A (en) * | 2014-02-24 | 2014-05-21 | 钟春燕 | Preparation method for bacterial cellulose-based nano active carbon fibers |
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| CN108301109A (en) * | 2018-03-27 | 2018-07-20 | 东华大学 | A kind of carbon nano-tube fibre knitted fabric and preparation method thereof |
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