CN104593890B - Attapulgite hybrid conductive fibers and preparation method thereof - Google Patents
Attapulgite hybrid conductive fibers and preparation method thereof Download PDFInfo
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Abstract
The invention discloses attapulgite hybrid conductive fibers and a preparation method thereof. The preparation method of the attapulgite hybrid conductive fibers is characterized by comprising the following steps: dropwise adding antimony-doped tin oxide nano-powder (ATO powder) into attapulgite ammonia water solutions; stirring, performing hydrochloric acid titration neutralization and drying to obtain conductive powder; performing high-temperature activation on the dried conductive powder with polyvinylpyrrolidone or polyethylene pyrrole at the temperature of 400-800 DEG C to obtain a white attapulgite hybrid nano-conductive agent; preparing the nano-conductive agent into the nano-conductive powder; dispersing the dispersed attapulgite hybrid nano-conductive powder into a melted polymer at a high speed; extruding and pelleting by screws to obtain conductive slices; and performing melted spinning, winding and stretching on the conductive slices to obtain DTY conductive fibers. The surface specific resistance of the attapulgite hybrid conductive fibers is 10<2>-10<10> omega.cm, and the charge semi-attenuation time is 0.01-15s. The conductive fibers have functions of static electricity resistance, electricity conductivity and electromagnetic shielding, and are suitable for the fields of clothes, furniture, military projects, medical treatments and the like.
Description
Technical field
The present invention relates to a kind of nano hybridization and there is fiber and the manufacture method of conducting function.
Background technology
With constantly widening of conducting powder application, the demand of conducting powder will be increased every year year by year.The U.S. at present
To the demand of high molecular composite conductive material every year with the speed increase of 20%-30%, its main direction of studying is that exploitation height is led
Electrically, the conducting powder of low cost.
The domestic conducting powder currently using many based on carbon black, but due to carbon black powder, graphite powder, carbon fiber electric conductivity
Difference, heat-moisture resistance is poor, and color is deep, should not produce light-colored conductive material；And expensive, the color depth of bronze and argentum powder；Copper powder,
Nikel powder, aluminium powder etc. because having easy oxidation, the shortcomings of electric conductivity is unstable, so domestic at present be devoted to greatly light-colour electrically conductive powder
Research and development, the exploitation of light-colour electrically conductive powder filled up a blank of domestic conductive filler.Before the market of light-colour electrically conductive powder
Scape is very good.
Attapulgite is a kind of natural one-dimensional rod-like nano material, has fibrous or rough club shaped structure, table
Reveal various excellent physicochemical properties, be widely used in chemical industry, agricultural, weaving, building materials, geological prospecting, casting and
The fields such as pharmacy.
Attapulgite unique monodimension nano stick lattice structures shape it be the reason preparing polymer nanocomposites
Think mineral resources, can be combined in micron filling, nanometer enhancing and electric conductivity and polymer.If Zeng Yongbin et al. is with former
The pani of position polymerization sulphuric acid doping on the Surface coating of attapulgite, the nano composite material specific insulation of synthesis up to
To 3 ω .cm.
Although up to the present there being some to prepare the nanometer electricity-conductive powder of attapulgite ground mass, having no and being applied to fiber
In, additionally there are problems with, the hydridization insufficient (electric conductivity is unstable) of attapulgite, particle agglomeration phenomenon are serious
(limitation can be only applied in the fiber of thin film, coating or wet method spinning).
The present invention is optionally scattered in a certain phase using the separated of blend and inorganic conductive material, ensure that
Conductive agent reaches higher conductive effect in relatively low content, in addition keeps preferable spinnability and mechanical property.
Content of the invention
The invention aims to providing a kind of white conductive fiber and the method preparing white conductive fiber；
Another object of the present invention is to provide a kind of nano hybridization technology, so that high polymer is grafted with attapulgite
Reaction, can preferably disperse conductive nano agent；
Another object of the present invention is using having the high polymer of л type structure come hydridization and dispersed electro-conductive powder body, manufacture
The stable, method of the preferable conductive fiber of electric conductivity.
Present invention be characterized in that there is following preparation process and step:
1. a kind of nano-powder of antimony-doped tin oxide (ato powder body) is added dropwise in the ammonia spirit of attapulgite,
Carry out high-speed stirred 20min～12h at a temperature of 10～80 DEG C, then carry out ph titration neutralization with hydrochloric acid, deionized water is cleaned,
Put into be dried in baking oven and obtain conductive powder body；By the conductive powder body being dried and Polyvinylpyrrolidone or polyvinyl pyrrole
Carry out high-temperature activation at a temperature of 400～800 DEG C, obtain the conductive nano agent of the attapulgite hydridization of white；
Described ato is 1/1～99/0.1 with the mass ratio of attapulgite；
Described conductive powder body is 1/1～99/1 with Polyvinylpyrrolidone or polyvinyl pyrrole mass ratio；
2. dose volume is than for 99.5/0.5～0.5/99.5 petroleum ether or ethanol water, successively by silane coupler,
The conductive nano agent of attapulgite hydridization, the high polymer of hydrophilic and petroleum ether or ethanol water carry out ball in ball mill
Mill, Ball-milling Time is 10min～12h, is dried standby at a temperature of 80～150 DEG C, and scattered nanometer conductive powder is obtained
Body；
Described silane coupler is one or more of kh-550, kh-560, kh-570, kh-902, kh-590；
Described hydrophilic polymer refers to a kind of in polypyrrole, polypyrrole alkanone, Polyethylene Glycol, polyether ester, preferably poly- pyrrole
Cough up；
Described silane coupler accounts for the 0.1%～20% of petroleum ether or ethanol water；
The conductive nano agent of described attapulgite hydridization and silane coupler mass ratio are 95/5～99/1；
The high polymer of described hydrophilic and silane coupler mass ratio are 1/2～10/1；
3. the nanometer electricity-conductive powder high speed of scattered attapulgite hydridization is scattered in molten polymer, carries out screw rod
Extruding pelletization, obtains conductive section；
The mass fraction that the nanometer electricity-conductive powder of described attapulgite hydridization accounts for total amount is 0.5%～50%；
Described polymer is not limited to polypropylene, polyester (pet), polybutylene terephthalate (PBT) (pbt) or gathers
Propylene glycol ester terephthalate (ptt)；
4. the nanometer electricity-conductive powder of scattered attapulgite hydridization is put in ethylene glycol solution, carry out ultrasonic, ball milling,
Sand milling or grinding distribution；It is added in p-phthalic acid and is esterified, esterification adds the metatitanic acid of 50ppm～500ppm after terminating
N-butyl, 0.05%～5% dodecyl quaternary ammonium salt carry out being polymerized arrived in-situ polymerization conductive section；
The mass fraction that the nanometer electricity-conductive powder of described attapulgite hydridization accounts for total amount is 0.1%～2%；
The mass fraction that described ethylene glycol accounts for total amount is 40%～50%；
Described p-phthalic acid accounts for the mass fraction 50～60% of total amount；
5. conductive section is carried out melt spinning again, be wound for 600-4000m/min in spinning speed, obtain conduction
Preorientation fiber (poy fiber)；
6. more obtained poy fiber is carried out hot-stretch in 70～150 DEG C and obtain dty conductive fiber.
The surface specific resistance of the attapulgite hydridization conductive fiber that the present invention provides is 102～1010ω .cm, electric charge half is decayed
0.01～15s.This conductive fiber has antistatic, conduction, electromagnetic shielding it is adaptable to the field such as clothing, furniture, military project, medical treatment.
The present invention rationale here is that:
1. contain in attapulgite moisture also contain hydroxyl (- oh) can be with the superpolymer polyethylene pyrrolidine of hydrophilic
Ketone or polyvinyl pyrrole react, after attapulgite high-temperature activation, thus high polymer can be connect with attapulgite
Branch reaction, can be well dispersed in attapulgite, so both can improve the bonding situation between attapulgite and polymer,
By the polymer being grafted in attapulgite, inorganic nano-particle can be separated again, prevent its reunion, reach good dispersion；
2. polypyrrole and polypyrrole alkanone have л type structure it is easy to there is electron transition, can be by present in ato
Electronic defects is filled, thus leading to the conductive powder body of attapulgite hydridization, even if adding little amount also can reach the good of conduction
Good performance, the fault of construction additionally, due to ato is filled, and its electric conductivity is more stable.
3. the hydrophilizing agent of small molecule of the present invention can also use as dispersant and grafting agent, but due to conductive powder body
Need to be added in polymer and carry out melt spinning or high temperature polymerization, small molecule hydrophilizing agent occurs thermal degradation, lead to polymerization, spin
The difficulty of silk.
4. the present invention adopts in-situ polymerization, and conductive powder body can be reacted with polymer completely, forms copolymerization
Thing, dodecyl quaternary ammonium salt can form more stable chemical bonding structure with attapulgite, so that conductive nano agent is difficult from poly-
Run off in compound, even if so millesimal addition also can reach high electrical conductivity.
Compared with prior art, it is an advantage of the current invention that:
The attapulgite hydridization conductive fiber that the present invention provides has white, the fiber of light high conductivity, meets different necks
The requirement of domain fabric；
The present invention passes through to control the reaction conditions such as hydridization, high-temperature activation, dispersion, polymerization, controls the electric conductivity of conductive fiber；
The present invention preparation attapulgite hydridization conductive fiber, Financial cost is low, stable performance, can be with large-scale commercial system
Standby；
The present invention adopts non-antimony-based catalyst, reduces pollution, response speed is fast, reduce energy loss.
Specific embodiment
With reference to embodiment, type of the present invention is described in detail.
Below by embodiment, type of the present invention is specifically described it should be pointed out that following examples are to use
In being further described to type of the present invention it is impossible to be interpreted as the restriction to type protection domain of the present invention, the technology in this field is ripe
Practice personnel according to the invention described above content, the present invention can be made with some nonessential improvement and adjust.
The volume resistivity assay method of fiber:
The method of the volume resistivity of the test fiber according to gb/t12703 tests the fiber volume ratio resistance of fabric
Value, instrument is lfy-405(yg321) (humidity 30%, temperature room temperature, voltage 100v).
The method of testing of fiber half-life:
The method test fiber half-life of the volume resistivity of the test fiber according to gb/t12703, instrument is quiet
Voltage half-life tester (b-033) (humidity 30%, temperature room temperature, voltage 10kv, time 30s).
Embodiment 1
Nanometer ato powder body is added dropwise in the ph=11 ammonia spirit of attapulgite, the mass ratio of ato and attapulgite
For 4/1, at a temperature of 80 DEG C, carry out high-speed stirred 20min, then carry out ph titration neutralization with hydrochloric acid, deionized water is cleaned, put
Enter to be dried in baking oven and obtain conductive powder body；The conductive powder body of the drying that mass ratio is 99/1 and Polyvinylpyrrolidone in
Carry out high-temperature activation at a temperature of 800 DEG C, obtain the conductive nano agent of the attapulgite hydridization of white；
Dose volume ratio is for 5/5(v/v) petroleum ether aqueous solution, prepare the petroleum ether water of 20% silane coupler kh-570
Solution, addition attapulgite hybridized nanometer conductive agent, the polyether ester of hydrophilic carry out ball milling in ball mill, and Ball-milling Time is
12h, is dried standby at a temperature of 150 DEG C, scattered nanometer electricity-conductive powder is obtained；
The conductive nano agent of described attapulgite hydridization and silane coupler mass ratio are 95/5；
Described polyether ester and silane coupler mass ratio are 1/2；
The nanometer electricity-conductive powder high speed of the above-mentioned scattered attapulgite hydridization accounting for gross mass 0.5% is scattered in poly- third
In alkene polymer, carry out Screw Extrusion pelletize, obtain conducting polypropylene section;Conductive section is carried out melt spinning again, is spinning
Silk speed is wound for 4000m/min, obtains conducting polypropylene poy fiber.Embodiment 2
Nanometer ato powder body is added dropwise in the ph=9 ammonia spirit of attapulgite, the mass ratio 1/ of ato and attapulgite
1, carry out high-speed stirred 12h at a temperature of 10 DEG C, then carry out ph titration neutralization with hydrochloric acid, deionized water is cleaned, and puts into baking oven
In be dried and obtain conductive powder body；Mass ratio is that 1/1 conductive powder body being dried carries out height with polypyrrole at a temperature of 400 DEG C
Temperature activation, obtains the conductive nano agent of the attapulgite hydridization of white；
Dose volume ratio for 1/99 ethanol water, prepare 0.1% the ethanol water of silane coupler kh-560, plus
Enter attapulgite hybridized nanometer conductive agent, polypyrrole and carry out ball milling in ball mill, Ball-milling Time is 12h, enters at a temperature of 80 DEG C
Row drying for standby, is obtained scattered nanometer electricity-conductive powder；
In above-mentioned steps, the conductive nano agent of attapulgite hydridization and silane coupler mass ratio are 99/1；
In above-mentioned steps, polypyrrole and silane coupler mass ratio are 10/1；
The nanometer electricity-conductive powder high speed accounting for gross mass 5% attapulgite hydridization is scattered in polyester pet, carries out screw rod and squeeze
Go out pelletize, obtain conductive polyester section；
Conductive section is carried out melt spinning again, is wound for 600m/min in spinning speed, obtain conductive poy fine
Dimension；Again obtained poy fiber is carried out hot-stretch in 150 DEG C and obtain dty conductive fiber.
Embodiment 3
Nanometer ato powder body is added dropwise in the ph=10 ammonia spirit of attapulgite, the mass ratio of ato and attapulgite
9/1, carry out high-speed stirred 6h at a temperature of 50 DEG C, then carry out ph titration neutralization with hydrochloric acid, deionized water is cleaned, and puts into baking oven
In be dried and obtain conductive powder body；Mass ratio is that 1/2 conductive powder body being dried carries out height with polypyrrole at a temperature of 600 DEG C
Temperature activation, obtains the conductive nano agent of the attapulgite hydridization of white；
Dose volume ratio for 10/90 ethanol water, prepares 2% ethanol water of silane coupler kh-590, addition
Attapulgite hybridized nanometer conductive agent, polypyrrole carries out ball milling in ball mill, and Ball-milling Time is 1h, carries out at a temperature of 100 DEG C
Drying for standby, is obtained scattered nanometer electricity-conductive powder；
In above-mentioned steps, the conductive nano agent of attapulgite hydridization and silane coupler mass ratio are 95/5；
In above-mentioned steps, polypyrrole and silane coupler mass ratio are 1/1；
The nanometer electricity-conductive powder of attapulgite hydridization in above-mentioned steps is put in ethylene glycol solution, carries out ultrasonic disperse；
It is added in p-phthalic acid and is esterified, esterification adds 50ppm tetrabutyl titanate, 0.05% dodecyl quaternary ammonium salt after terminating
It is polymerized, obtained the conductive section of in-situ polymerization；
The mass fraction that in above-mentioned steps, the nanometer electricity-conductive powder of attapulgite hydridization accounts for total amount is 2%；
The mass fraction that in above-mentioned steps, ethylene glycol accounts for total amount is 40%；
Described p-phthalic acid accounts for the mass fraction 58% of total amount；
Conductive section is carried out melt spinning again, is wound for 4000m/min in spinning speed, obtain conductive fdy fine
Dimension.
Fibre is recorded by fiber ratio resistance and charge decay instrument by the conductive fiber that the present embodiment methods described is obtained
The ratio resistance of dimension is 8.5 × 107ω .cm, charge decay value is 1.8s.
Embodiment 4
Nanometer ato powder body is added dropwise in the ph=10 ammonia spirit of attapulgite, the mass ratio of ato and attapulgite
8/2, carry out high-speed stirred 1h at a temperature of 50 DEG C, then carry out ph titration neutralization with hydrochloric acid, deionized water is cleaned, and puts into baking oven
In be dried and obtain conductive powder body；Mass ratio is that 1/10 conductive powder body being dried is carried out at a temperature of 600 DEG C with polypyrrole
High-temperature activation, obtains the conductive nano agent of the attapulgite hydridization of white；
Dose volume ratio for 10/90 ethanol water, prepares 1% ethanol water of silane coupler kh-902, addition
Attapulgite hybridized nanometer conductive agent, Polyethylene Glycol carries out ball milling in ball mill, and Ball-milling Time is 1h, enters at a temperature of 100 DEG C
Row drying for standby, is obtained scattered nanometer electricity-conductive powder；
In above-mentioned steps, the conductive nano agent of attapulgite hydridization and silane coupler mass ratio are 98/2；
In above-mentioned steps, polypyrrole and silane coupler mass ratio are 5/1；
The nanometer electricity-conductive powder high speed accounting for gross mass 50% attapulgite hydridization is scattered in pbt, carries out Screw Extrusion and make
Grain, obtains conductive pbt section；
Conductive section is carried out melt spinning again, is wound for 1000m/min in spinning speed, obtain conductive poy fine
Dimension.
Fibre is recorded by fiber ratio resistance and charge decay instrument by the conductive fiber that the present embodiment methods described is obtained
The ratio resistance of dimension is 4.8 × 105ω .cm, charge decay value is 0.3s.
Embodiment 5
Nanometer ato powder body is added dropwise in the ph=10 ammonia spirit of attapulgite, the mass ratio of ato and attapulgite
7/3, carry out high-speed stirred 50min at a temperature of 50 DEG C, then carry out ph titration neutralization with hydrochloric acid, deionized water is cleaned, put into
It is dried in baking oven and obtain conductive powder body；Mass ratio is 1/10 conductive powder body and the polypyrrole being dried at a temperature of 800 DEG C
Carry out high-temperature activation, obtain the conductive nano agent of the attapulgite hydridization of white；
For 99.5/0.5 ethanol water, the ethanol preparing 1.5% silane coupler kh-550 is water-soluble for dose volume ratio
Liquid, addition attapulgite hybridized nanometer conductive agent, polypyrrole alkanone carries out ball milling in ball mill, and Ball-milling Time is 3h, and 100
It is dried standby at a temperature of DEG C, scattered nanometer electricity-conductive powder is obtained；
In above-mentioned steps, the conductive nano agent of attapulgite hydridization and silane coupler mass ratio are 98/2；
In above-mentioned steps, polypyrrole and silane coupler mass ratio are 2/1；
The nanometer electricity-conductive powder high speed accounting for gross mass 10% attapulgite hydridization is scattered in ptt, carries out Screw Extrusion and make
Grain, obtains conductive ptt section；
Conductive ptt section is carried out melt spinning again, is wound for 3000m/min in spinning speed, obtains conductive poy
Fiber.
Fibre is recorded by fiber ratio resistance and charge decay instrument by the conductive fiber that the present embodiment methods described is obtained
The ratio resistance of dimension is 9.7 × 106ω .cm, charge decay value is 0.5s.
Claims (4)
1. a kind of preparation method of the conductive fiber of attapulgite hydridization is it is characterised in that adopt following preparation process and step:
A () nanometer ato powder body is added dropwise in the ammonia spirit of attapulgite, carry out high-speed stirred at a temperature of 10～80 DEG C
20min～12h, then carry out ph titration neutralization with hydrochloric acid, deionized water is cleaned, is put into be dried in baking oven and obtain conducting powder
Body；The conductive powder body being dried is carried out high temperature work with Polyvinylpyrrolidone or polyvinyl pyrrole at a temperature of 400～800 DEG C
Change, obtain the conductive nano agent of the attapulgite hydridization of white；
Described ato is 1/1～99/0.1 with the mass ratio of attapulgite；
Described conductive powder body is 1/1～99/1 with Polyvinylpyrrolidone or polyvinyl pyrrole mass ratio；
(b) dose volume than for 99.5/0.5～0.5/99.5 petroleum ether or ethanol water, successively by silane coupler, concavo-convex
The conductive nano agent of excellent stone hydridization, the high polymer of hydrophilic and petroleum ether or ethanol water carry out ball milling, ball in ball mill
Consume time as 10min～12h, be dried standby at a temperature of 80～150 DEG C, scattered nanometer electricity-conductive powder is obtained；
Described silane coupler is one or more of kh-550, kh-560, kh-570, kh-902, kh-590；
The high polymer of described hydrophilic refers to a kind of in polypyrrole, polypyrrole alkanone, Polyethylene Glycol, polyether ester；
Described silane coupler accounts for the 0.1%～20% of petroleum ether or ethanol water；
The conductive nano agent of described attapulgite hydridization and silane coupler mass ratio are 95/5～99/1；
The high polymer of described hydrophilic and silane coupler mass ratio are 1/2～10/1；
C () the nanometer electricity-conductive powder high speed of scattered attapulgite hydridization is scattered in molten polymer, carry out screw rod and squeeze
Go out pelletize, obtain conductive section；
The mass fraction that the nanometer electricity-conductive powder of described attapulgite hydridization accounts for total amount is 0.5%-50%；
Described polymer be polypropylene, polyethylene terephthalate pet, polybutylene terephthalate (PBT) pbt or
PTT ptt；
D conductive section is carried out melt spinning by () again, be wound for 600-4000m/min in spinning speed, obtain conductive poy
Fiber.
2. preparation method according to claim 1, the conductive section of step (c) can also be obtained by another kind of technical scheme,
Its feature comprises the following steps, and the nanometer electricity-conductive powder of scattered attapulgite hydridization is put in ethylene glycol solution, carries out
Ultrasonic, ball milling, sand milling or grinding distribution；Be added in p-phthalic acid and be esterified, esterification terminate after add 50ppm～
The tetrabutyl titanate of 500ppm, 0.05%～5% dodecyl quaternary ammonium salt carry out being polymerized the conduction of arrived in-situ polymerization is cut
Piece；
The mass fraction that the nanometer electricity-conductive powder of described attapulgite hydridization accounts for total amount is 0.1%～2%；
The mass fraction that described ethylene glycol accounts for total amount is 40%～50%；
Described p-phthalic acid accounts for the mass fraction 50～60% of total amount.
3. preparation method according to claim 1, its feature comprises the following steps, by obtained poy fiber in 70～
150 DEG C carry out hot-stretch and obtain dty conductive fiber.
4. the conductive fiber of the attapulgite hydridization that a kind of arbitrary preparation method of use claims 1 to 3 is obtained is it is characterised in that fiber
Surface specific resistance be 102～1010ω .cm, electric charge partly decays to 0.01～15s.
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| CN105802248A (en) * | 2016-04-12 | 2016-07-27 | 国电环境保护研究院 | Method for preparing conductive composite with attapulgite as substrate |
| CN106498540B (en) * | 2016-10-09 | 2018-12-18 | 绍兴圣兔纺织有限公司 | A kind of preparation method of high intensity antistatic fibre |
| CN107151323A (en) * | 2017-04-25 | 2017-09-12 | 安徽博硕科技有限公司 | A kind of preparation method of polypyrrole/nano antimony tin oxide/attapulgite conductive composite material |
| CN109908008B (en) * | 2019-02-27 | 2022-04-19 | 北京中蓝港湾科技有限公司 | Moisturizing cream containing attapulgite and preparation method thereof |
| CN112195527A (en) * | 2020-09-17 | 2021-01-08 | 滁州兴邦聚合彩纤有限公司 | Production process of high-strength fiber |
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| CN104593890A (en) | 2015-05-06 |
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Effective date of registration: 20170630 Address after: 215228 Sheng Hong fiber, Shengze Town, Wujiang District, Jiangsu, Suzhou Patentee after: Suzhou Sheng Hong Fiber Co., Ltd. Address before: 215228, Shengze Town, Wujiang District, Jiangsu City, Suzhou Province Hong Sheng Technology Patentee before: Jiangsu Shenghong Science and Technology Co., Ltd. |