CN102102231A - Method for preparing conductive cellulose fibers - Google Patents
Method for preparing conductive cellulose fibers Download PDFInfo
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Abstract
The invention discloses a method for preparing conductive cellulose fibers, which comprises the following steps of: mixing nano carbon black and carbon nano tube in a certain ration, performing acid washing and purification, and then grinding and dispersing the mixture of carbon and ionic liquid under the condition of an infrared lamp; obtaining nano carbon/cellulose spinning solution containing 8 to 15 weight percent of carbon by using the carbon-containing ionic liquid as a cellulose solvent; and preparing carbon-containing cellulose composite fibers by using a dry-jet wet-spinning or wet-spinning process and using deionized water as a coagulation bath. The method can simply and feasibly realize uniform dispersion of the carbon nano tube and the carbon black in the cellulose fibers, and greatly improves the electric conductivity of the cellulose fibers; and the obtained carbon-containing cellulose composite fibers can be widely applied in the antistatic field of materials for clothes or industries. The solvent used for the process production is nontoxic and can be repeatedly reclaimed and used, and the whole process realizes green production.
Description
Technical field
The present invention relates to the preparation method of the conductive cellulose composite fibre in the chemical fibres industry.Form in the process that the present invention utilizes imidazole type ion liquid and nano carbon black and CNT to grind and interact, impel the nano-sized carbon material evenly to disperse at ionic liquid, thereby overcome the after-processing technology difficulty that nano carbon black and CNT are reunited and caused, simple for process.In addition, utilize rational proportion between nanometer carbon black and the CNT, in cellulosic matrix, can build a large amount of energising networks, thereby improve the electric conductivity of composite fibre greatly.The conventional dry-jet wet-spinning or the technology of wet spinning are adopted in the production of composite fibre, and obtained cellulose composite fiber good conductivity is expected extensive use and takes with industry and use the field.
Background technology
Nanometer carbon black and CNT have good electric conductivity, are the focuses that people study always.Carbon black itself is a semi-conducting material, and the nanometer carbon black particle diameter is little, and specific area is big and coarse, has lower resistivity, is used for different conductions or antistatic article, as antistatic or conductive rubber, plastic products, CABLE MATERIALS; The caliber of CNT generally in several nanometers to tens nanometers, and the length of CNT is typical monodimension nanometer material generally at several microns to several millimeters, the structure of CNT makes it have good electric conductivity.In addition, nano carbon black and CNT all have anti-strong acid, and highly basic and good heat endurance are the ideal fillers of polymer composites.CNT or nano carbon black have wide application potential as the polymer composites of filler preparation at aspects such as stealth material, high performance structures material, multifunctional materials.But because nano carbon black and CNT all belong to nanoscale, its surface energy is big, and it is serious to reunite each other, greatly reduces the material serviceability.
Along with the exhaustion day by day of petroleum resources, the development and utilization natural macromolecular material more and more is subject to people's attention.Cellulose is the abundantest natural macromolecular material of a nature middle storage capacity, makes full use of cellulosic material and has very important realistic meaning.Imidazole type ion liquid [BMIM] Cl is cellulosic fine solvent, utilize this ion liquid dissolving and preparation cellulosic material to become the focus of research in recent years, its preparation process is according to related process cellulose pulp directly to be dissolved in to form cellulose solution in the ionic liquid, then by dry-wet spinning or wet spinning.Utilize ionic liquid for characteristics such as the cellulose fibre of solvent preparation have that mechanical property is good, even structure, dyeability are good, have higher prospects for commercial application.
In the process that imidazole type ion liquid [BMIM] Cl and nano-sized carbon material grind, can interact between CATION and the carbon in the ionic liquid, reduce Van der Waals force between the nano-sized carbon, thereby the even carbon nanotube of agglomerated is disperseed.Coupled ion liquid can dissolve and prepare the characteristics of cellulose fibre as solvent, the nano-sized carbon material at first can be dispersed in the ionic liquid, utilizes ionic liquid to be solvent then, preparation composite fibre cellulose fiber.It is few to utilize natural polymer to prepare the research of conductive material at present, and patent ZL200410052885.6 receives quantitative nanometer carbon black by adding in cellulose spinning fluid, find that mechanical property, electric conductivity and the thermal property of fiber is improved to some extent.Patent CN200710036886.5 has significantly improved the mechanical property and the conductance of cellulose fibre by add quantitative CNT in the cellulose fibre preparation process.More than two patents all relate to the modification of nano-sized carbon material, its complex disposal process, and the electric conductivity of the fiber of preparation promotes not obvious.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of conductive cellulose fiber production method.
Principle of the present invention is to utilize milled processed between CNT and the ionic liquid, makes to form between nanometer charcoal material and the ionic liquid to interact, and impels the nano-sized carbon material evenly to disperse in ionic liquid.Utilize the mixture of ionic liquid and nano-sized carbon material to prepare cellulose spin dope, and prepare carbon/cellulose composite fiber through doing wet method or wet spinning for solvent.Utilize nano carbon black and CNT (carbon nano-tube) rational proportion, in the middle of cellulosic matrix, build conductive network mutually, thereby prepared electric conductivity fiber with excellent cellulose fiber.
One of purpose of the present invention is to provide a kind of cellulose base composite fibre that contains nano-sized carbon, and this composite fibre is prepared by following method:
1. with nano carbon black and the CNT reflux certain hour in certain density acid solution addressed, after cleaning, filtration, drying, obtain the nano-sized carbon material of purifying;
2. in the infrared lamp drier, the nano carbon black of purifying and the CNT mass ratio according to 1: 10~1: 20 is mixed, ionic liquid and nano-sized carbon substance weight are according to 765~1380: 1 mixes to put into and contains the agate mill and grind, grinding rate remains on 40r/min~70r/min, milling time remained on 1~4 hour, can obtain the ionic liquid solution of carbon containing;
3. be 300~1200 cellulose cotton pulp or wood pulp with the degree of polymerization, be ground into the particle of 2~5 μ m with food masher, 50~70 ℃ of following vacuumizes 5~12 hours;
4. above-mentioned 2 gained are contained dry resultant cellulose pulp particle in nano-sized carbon examples of substances liquid and above-mentioned 3 with 10~16: 1 weight ratio preparation, join in the dissolver, under 90 ℃~110 ℃ through stirring, under vacuum environment, dissolved 2~6 hours, and promptly obtained the spinning solution that is used to prepare carbon/cellulose composite fiber of black.
5. the aforesaid temperature that is used to prepare the spinning solution of carbon/cellulose composite fiber is adjusted to 80~100 ℃, spray through spinnerets, air gap by 10~150mm is behind the air layer between spinning plate surface and the coagulating bath face, enter solidification forming in the deionized water solution, through washing, to obtain the carbon containing quality after the drying be carbon/cellulose composite fiber of 8%~15%.The perhaps just aforesaid temperature that is used to prepare the spinning solution of carbon/cellulose composite fiber is adjusted to 80~100 ℃, spray through spinnerets, directly enter into deionized water solution by wet-spinning frame, through washing, can to obtain the carbon containing quality after the drying be carbon/cellulose composite fiber of 8%~15%.
The order of magnitude of prepared carbon/cellulose composite fiber conductance is 10
7~10
4Ω .cm.
Carbon/the cellulose composite fiber of this method preparation has following advantage:
(1) under infrared lamp, after nano-sized carbon material and ionic liquid mixing, in the agate mill, can impel nano-sized carbon in ionic liquid, evenly to disperse through grinding after a while, this is the key of preparation conductive cellulose composite fibre;
(2) rational proportion between nano carbon black and the CNT forms conductive channel in cellulosic matrix, can significantly improve the electric conductivity of cellulose composite fiber;
(3) ionic liquid is cellulosic fine solvent, and it is good to have a solubility property, characteristics such as rate of recovery height, environmentally safe;
(4) production of adopting conventional dried wet processing or wet spinning technology all can realize fiber comparatively smoothly, deionized water, technology simple possible are selected in coagulating bath;
(5) Zhi Bei carbon/cellulose composite fiber has bigger application prospect taking with the fabrics for industrial use field.
The specific embodiment
Below by example the present invention is specifically described.Following examples only are used for the present invention is further specified, and can not be interpreted as limiting the scope of the invention, and the person skilled in the art in this field can content make some nonessential improvement and adjustment to the present invention according to the present invention.
Embodiment 1:
1. with nano carbon black and CNT mass ratio, put into the nitric acid reflux 48 hours of 3.0M, after filtration, obtain the nano carbon black and the carbon nano tube of purifying after the cleaning, drying according to 1: 10;
2. be under the infrared lamp of 800w at power, with nano-sized carbon material and 354g ionic liquid mixed grinding in the agate mill of 2g purifying, grinding rate 60r/min, milling time 2 hours;
3. be 1000 cellulose cotton pulp with the degree of polymerization, pulp be ground into the particle that diameter is 2 μ m~5 μ m, these cotton pulp particles are placed on vacuum-10 * 10 with cotton bag parcel with food masher
4Dry 6 hours of the following balance of Pa and 50 ℃;
4. getting 23g evenly mixes through the cotton pulp dregs of rice particle of dried and the carbon containing ionic liquid that milled processed is crossed, place dissolver, under 90 ℃,, promptly obtain the spinning solution that is used to prepare carbon/cellulose composite fiber of black through stirring, vacuum dissolving 5 hours;
5. after the aforesaid temperature that is used to prepare the spinning solution of carbon/cellulose composite fiber being adjusted to 90~95 ℃, spinnerets ejection through 100 holes, aperture 0.15mm, by length is the air gap layer of 80mm, enter solidification forming in the deionized water, obtain carbon content and be carbon/cellulose composite fiber of 8% behind washing and drying, its electrical conductivity of fibres order of magnitude is 10
7Ω .cm.
Embodiment 2:
1. with nano carbon black and CNT mass ratio, put into concentration and be 95% sulfuric acid reflux 36 hours, after filtration, obtain the nano carbon black and the carbon nano tube of purifying after the cleaning, drying according to 1: 15;
2. be under the infrared lamp of 1000w at power, with nano-sized carbon material and 255g ionic liquid mixed grinding in the agate mill of 3g purifying, grinding rate 70r/min, milling time 1.5 hours;
3. be 800 cellulose cotton pulp with the degree of polymerization, pulp be ground into the particle that diameter is 2 μ m~5 μ m, these cotton pulp particles are placed on vacuum-10 * 10 with cotton bag parcel with food masher
4Dry 5 hours of the following balance of Pa and 50 ℃;
4. getting 17g evenly mixes through the cotton pulp dregs of rice particle of dried and the carbon containing ionic liquid that milled processed is crossed, place dissolver, under 105 ℃,, promptly obtain the spinning solution that is used to prepare carbon/cellulose composite fiber of black through stirring, vacuum dissolving 6 hours;
5. after the aforesaid temperature that is used to prepare the spinning solution of carbon/cellulose composite fiber being adjusted to 95~100 ℃, spinnerets ejection through 100 holes, aperture 0.2mm, by length is the air gap layer of 100mm, enter solidification forming in the deionized water, obtain carbon content and be carbon/cellulose composite fiber of 15% behind washing and drying, its electrical conductivity of fibres order of magnitude is 10
4Ω .cm.
Embodiment 3:
1. with nano carbon black and CNT mass ratio, put into the chloroazotic acid reflux 24 hours, after filtration, obtain the nano carbon black and the carbon nano tube of purifying after the cleaning, drying according to 1: 18;
2. be under the infrared lamp of 500w at power, with nano-sized carbon material and 517.5g ionic liquid mixed grinding in the agate mill of 5g purifying, grinding rate 70r/min, milling time 4 hours;
3. be 900 cellulose wood pulp with the degree of polymerization, pulp be ground into the particle that diameter is 2 μ m~5 μ m, these cotton pulp particles are placed on vacuum-10 * 10 with cotton bag parcel with food masher
4Dry 5 hours of the following balance of Pa and 60 ℃;
4. getting 45g evenly mixes through the cotton pulp dregs of rice particle of dried and the carbon containing ionic liquid that milled processed is crossed, place dissolver, under 100 ℃,, promptly obtain the spinning solution that is used to prepare carbon/cellulose composite fiber of black through stirring, vacuum dissolving 6 hours;
5. after the aforesaid temperature that is used to prepare the spinning solution of carbon/cellulose composite fiber being adjusted to 90~95 ℃, spinnerets ejection through 100 holes, aperture 0.15mm, enter solidification forming in the deionized water, obtain carbon content and be carbon/cellulose composite fiber of 10% behind washing and drying, its electrical conductivity of fibres order of magnitude is 10
5Ω .cm.
Claims (8)
1. the preparation method of the cellulose fibre of a carbon containing is characterized in that may further comprise the steps:
(1) nano carbon black and CNT are according to the certain quality proportioning and carry out purification process;
(2) nano-sized carbon material behind the purifying and ionic liquid are mixed, under infrared lamp, grind, be dispersed in the ionic liquid with impelling nanometer carbon black and even carbon nanotube;
(3) utilize ground carbon containing ionic liquid to be solvent, prepare certain density cellulose spinning fluid;
(4) cellulose spinning fluid for preparing is adopted dry-jet wet spinning process or wet spinning process, adopting deionized water is that solvent can obtain fiber of the present invention.
2. preparation method according to claim 1, the quality proportioning that it is characterized in that nano carbon black and CNT is 1: 10~1: 20, preferably at 1: 12~1: 18.
3. preparation method according to claim 1 is characterized in that nano carbon black and CNT gross weight are 8~15% of cellulose gross weight.
4. preparation method according to claim 1 is characterized in that the purification process of nano carbon black and CNT comprises the steps:
The nano-sized carbon material of being addressed be impregnated in the acid solution, and acid solution refluxes at a certain temperature, and the impurity of carbon nano tube surface obtains the nano-sized carbon material of purifying then via the oxidation removal of acid solution after washed with de-ionized water, filtration, drying.
5. preparation method according to claim 2 is characterized in that milled processed comprises the steps:
Purified nano-sized carbon material and ionic liquid mixing back are ground under infrared light.The infrared lamp power selection is 500w~1200w, and nano-sized carbon material and ionic liquid grind in the agate mill, and grinding rate is 40r/min~70r/min, and milling time is 1~4 hour, preferably at 2.5~3 hours.
6. preparation method according to claim 1 is characterized in that acid solution comprises chloroazotic acid, nitric acid, sulfuric acid etc.
7. preparation method according to claim 1 is characterized in that:
(1) with the degree of polymerization is 300~1200 cellulose cotton pulp or wood pulp, is ground into the particle of 2-5 μ m with food masher, 50~70 ℃ of following vacuumizes 5~12 hours;
(2) with the described carbon containing ion liquid solvent of claim 4 and aforementioned (1) dry cellulose grain and with 16~10: 1 weight ratio joins in the dissolver, under 90 ℃~110 ℃ through stirring, dissolving is 2-6 hour under the condition that vacuumizes, and promptly obtains to be used to prepare the spinning solution of carbon/cellulose composite fiber.
8. preparation method according to claim 7, it is characterized in that the aforementioned temperature that is used to prepare the spinning solution of carbon/cellulose composite fiber is adjusted to 80~100 ℃, spray through spinnerets, air gap by 10~150mm is behind the air layer between spinning plate surface and the coagulating bath face, enter the deionized water solidification forming, through washing, to obtain nano-sized carbon substance weight content after the drying be carbon/cellulose composite fiber of 8%~15%.Perhaps adopt the mode of wet spinning, spinning solution sprays through spinnerets, enters solidification forming in the deionized water, through washing, to obtain nano-sized carbon substance weight content after the drying be carbon/cellulose composite fiber of 8%~15%.
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CN103225173A (en) * | 2013-05-17 | 2013-07-31 | 天津工业大学 | Cellulose/carbon nano tube composite nanofiber membrane preparation method |
CN104086783A (en) * | 2014-07-08 | 2014-10-08 | 黑龙江大学 | Method for preparing graphene oxide/carbon nano tube/cellulose composite gel from ionic liquid |
CN104594077A (en) * | 2015-01-14 | 2015-05-06 | 中国科学院过程工程研究所 | Method for preparing carbon nanometer conductive solution and conductive fibers by using ionic liquids |
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