CN104593890A - 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
Along with constantly widening of conducting powder Application Areas, will increase year by year every year the demand of conducting powder.The current U.S. is to the demand of high molecular composite conductive material every year with the speed increase of 20%-30%, and its main direction of studying is exploitation high conductivity, the conducting powder of low cost.
The conducting powder of domestic present use is master mainly with carbon black, but due to the poorly conductive of carbon black powder, graphite powder, carbon fiber, heat-moisture resistance is poor, and color is dark, should not produce light-colored conductive material; And bronze and silver powder is expensive, color depth; Copper powder, nickel powder, aluminium powder etc. are because having easy oxidation, and the shortcomings such as electric conductivity is unstable, so the domestic research and development being mostly devoted to light-colour electrically conductive powder at present, a blank of domestic conductive filler has been filled up in the exploitation of light-colour electrically conductive powder.The market prospects of light-colour electrically conductive powder are very good.
Attapulgite is a kind of natural one-dimensional rod-like nano material, there is threadiness or rough club shaped structure, show the physicochemical properties of various excellence, be widely used in the fields such as chemical industry, agricultural, weaving, building materials, geological prospecting, casting and pharmacy.
It is the desirable mineral resources preparing polymer nanocomposites that the monodimension nano stick lattice structure of attapulgite uniqueness determines it, can fill, nanometer strengthens and electric conductivity and polymer carry out compound at micron.As the people such as Zeng Yongbin with situ aggregation method on the Surface coating of attapulgite sulfuric acid doping PANI, the nano composite material specific insulation of synthesis can reach 3 Ω .cm.
Although up to the present there are some to prepare the nanometer electricity-conductive powder of concave convex rod ground mass, but have no and be applied in fiber, also there is following problem in addition, the hydridization insufficient (electric conductivity is unstable) of attapulgite, particle agglomeration phenomenon serious (limitation can only be applied in the fiber of film, coating or wet method spinning).
The present invention adopt blend being separated and inorganic conductive material be optionally scattered in a certain mutually in, can ensure that conductive agent reaches higher conductive effect in lower content, keep good spinnability and mechanical property in addition.
Summary of the invention
The object of the invention is to provide a kind of white conductive fiber and preparing the method for white conductive fiber;
Another object of the present invention is to provide a kind of nano hybridization technology, enables high polymer and attapulgite generation graft reaction, can better dispersing nanometer conductive agent;
Another object of the present invention utilizes the high polymer with л type structure to come hydridization and dispersed electro-conductive powder, manufactures method that is stable, the good conductive fiber of electric conductivity.
The present invention is characterized in that having following preparation process and step:
1. a kind of nano-powder (ATO powder) of antimony-doped tin oxide is added dropwise in the ammonia spirit of attapulgite, high-speed stirred 20min ~ 12h is carried out at 10 ~ 80 DEG C of temperature, pH titration neutralization is carried out again with hydrochloric acid, by washed with de-ionized water, put into baking oven and carry out drying and obtain conductive powder body; The conductive powder body of drying and polyvinylpyrrolidone or polyvinyl pyrrole are carried out high-temperature activation at 400 ~ 800 DEG C of temperature, obtains the conductive nano agent of the attapulgite hydridization of white;
Described ATO and the mass ratio of attapulgite are 1/1 ~ 99/0.1;
Described conductive powder body and polyvinylpyrrolidone or polyvinyl pyrrole mass ratio are 1/1 ~ 99/1;
2. dose volume is than being 99.5/0.5 ~ 0.5/99.5 benzinum or ethanol water, successively the conductive nano agent of silane coupler, attapulgite hydridization, the high polymer of hydrophilic and benzinum or ethanol water are carried out ball milling in ball mill, Ball-milling Time is 10min ~ 12h, drying for standby is carried out, obtained scattered nanometer electricity-conductive powder at 80 ~ 150 DEG C of temperature;
Described silane coupler is one or more in KH-550, KH-560, KH-570, KH-902, KH-590;
Described hydrophilic polymer refers in polypyrrole, polypyrrole alkane ketone, polyethylene glycol, polyether ester a kind of, preferred polypyrrole;
Described silane coupler accounts for 0.1% ~ 20% of benzinum 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. by the nanometer electricity-conductive powder high speed dispersion of scattered attapulgite hydridization in molten polymer, carry out Screw Extrusion granulation, obtain conduction 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 polytrimethylene terephthalate (PTT);
4. the nanometer electricity-conductive powder of scattered attapulgite hydridization is put into ethylene glycol solution, carry out ultrasonic, ball milling, sand milling or grinding distribution; Join in terephthalic acid (TPA) and carry out esterification, add after esterification terminates the tetrabutyl titanate of 50ppm ~ 500ppm, 0.05% ~ 5% dodecyl quaternary ammonium salt carry out being polymerized arrive the conduction section of in-situ polymerization;
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 terephthalic acid (TPA) accounts for the mass fraction 50 ~ 60% of total amount;
5. conduction section being carried out melt spinning again, is that 600-4000m/min reels at spinning speed, obtains conduction preorientation fiber (POY fiber);
6. again obtained POY fiber is carried out hot-stretch in 70 ~ 150 DEG C and obtain DTY conductive fiber.
The surface specific resistance of concave convex rod hydridization conductive fiber provided by the invention is 10
2~ 10
10Ω .cm, electric charge half decay 0.01 ~ 15s.This conductive fiber has antistatic, conduction, electromagnetic shielding, is applicable to the fields such as clothes, furniture, military project, medical treatment.
general principle of the present invention is:
1. namely also can react with the superpolymer polyethylene pyrrolidones of hydrophilic or polyvinyl pyrrole containing hydroxyl (-OH) containing moisture in attapulgite, after attapulgite high-temperature activation, thus high polymer can with attapulgite generation graft reaction, can be dispersed in attapulgite well, so both can improve the bonding situation between attapulgite with polymer, by the polymer be grafted in attapulgite, inorganic nano-particle is separated again, prevent it from reuniting, reach good dispersion;
2. polypyrrole and polypyrrole alkane ketone have л type structure, be easy to electron transition occurs, the electronic defects existed in ATO can be filled, thus cause the conductive powder body of concave convex rod hydridization, even if add the superperformance that little amount also can reach conduction, in addition because the fault of construction of ATO is filled, its electric conductivity is more stable.
3. the micromolecular hydrophilizing agent of the present invention also can use as dispersant and grafting agent, but carries out melt spinning or high temperature polymerization because conductive powder body needs to join in polymer, Small molecular hydrophilizing agent generation thermal degradation, causes the difficulty of polymerization, spinning.
4. the present invention adopts in-situ polymerization, can by conductive powder body completely and polymer react, form copolymer, dodecyl quaternary ammonium salt can form more stable chemical bonding structure with attapulgite, millesimal addition conductive nano agent not easily run off from polymer, even if so also can reach high electrical conductivity.
compared with prior art, the invention has the advantages that:
Concave convex rod hydridization conductive fiber provided by the invention has the fiber of white, light high conductivity, meets the requirement of different field fabric;
The present invention, by controlling the reaction conditions such as hydridization, high-temperature activation, dispersion, polymerization, controls the electric conductivity of conductive fiber;
Concave convex rod hydridization conductive fiber prepared by the present invention, financial cost is low, stable performance, can large-scale commercial preparation;
The present invention adopts non-antimony-based catalyst, and decreasing pollution, reaction speed are fast, reduction energy loss.
Detailed description of the invention
Below in conjunction with embodiment, type of the present invention is described in detail.
Below by embodiment, type of the present invention is specifically described; it is to be noted; following examples are just for being further described type of the present invention; can not be interpreted as the restriction to type protection domain of the present invention, the person skilled in the art in this field can make some nonessential improvement and adjustment according to the invention described above content to the present invention.
The volume resistivity assay method of fiber:
According to the fiber volume fraction resistance value of the method test fabric of the volume resistivity of the test fiber of GB/T12703, instrument is LFY-405(YG321) (humidity 30%, temperature normal temperature, voltage 100v).
The method of testing of fiber half-life:
According to the method test fiber half-life of the volume resistivity of the test fiber of GB/T12703, instrument is electrostatic pressure half-life tester (B-033) (humidity 30%, temperature normal temperature, voltage 10kV, time 30s).
Embodiment 1
Nano ATO powder is added dropwise in the pH=11 ammonia spirit of attapulgite, the mass ratio of ATO and attapulgite is 4/1, at 80 DEG C of temperature, carry out high-speed stirred 20min, then carries out pH titration neutralization with hydrochloric acid, by washed with de-ionized water, put into baking oven and carry out drying and obtain conductive powder body; Be that conductive powder body and the polyvinylpyrrolidone of the drying of 99/1 carries out high-temperature activation at 800 DEG C of temperature by mass ratio, obtain the conductive nano agent of the attapulgite hydridization of white;
Dose volume is than being 5/5(v/v) the benzinum aqueous solution, the benzinum aqueous solution of the Silane coupling reagent KH-570 of preparation 20%, add attapulgite hybridized nanometer conductive agent, the polyether ester of hydrophilic carries out ball milling in ball mill, Ball-milling Time is 12h, drying for standby is carried out, obtained scattered nanometer electricity-conductive powder at 150 DEG C of temperature;
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;
By the above-mentioned scattered nanometer electricity-conductive powder high speed dispersion accounting for the attapulgite hydridization of gross mass 0.5% in polyacrylic polymer, carry out Screw Extrusion granulation, obtain conducting polypropylene section; Conduction section is carried out melt spinning again, is that 4000m/min reels at spinning speed, obtains conducting polypropylene POY fiber.Embodiment 2
Nano ATO powder is added dropwise in the pH=9 ammonia spirit of attapulgite, the mass ratio 1/1 of ATO and attapulgite, carries out high-speed stirred 12h at 10 DEG C of temperature, then carries out pH titration neutralization with hydrochloric acid, by washed with de-ionized water, put into baking oven and carry out drying and obtain conductive powder body; Be that conductive powder body and the polypyrrole of 1/1 drying carries out high-temperature activation at 400 DEG C of temperature by mass ratio, obtain the conductive nano agent of the attapulgite hydridization of white;
Dose volume ratio is 1/99 ethanol water, the ethanol water of the silane coupler KH-560 of preparation 0.1%, add attapulgite hybridized nanometer conductive agent, polypyrrole carries out ball milling in ball mill, Ball-milling Time is 12h, drying for standby is carried out, obtained scattered nanometer electricity-conductive powder at 80 DEG C of temperature;
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;
By accounting for the nanometer electricity-conductive powder high speed dispersion of gross mass 5% attapulgite hydridization in polyester PET, carrying out Screw Extrusion granulation, obtaining conductive polyester section;
Conduction section is carried out melt spinning again, is that 600m/min reels at spinning speed, obtains conduction POY fiber; Again obtained POY fiber is carried out hot-stretch in 150 DEG C and obtain DTY conductive fiber.
Embodiment 3
Nano ATO powder is added dropwise in the pH=10 ammonia spirit of attapulgite, the mass ratio 9/1 of ATO and attapulgite, carries out high-speed stirred 6h at 50 DEG C of temperature, then carries out pH titration neutralization with hydrochloric acid, by washed with de-ionized water, put into baking oven and carry out drying and obtain conductive powder body; Be that conductive powder body and the polypyrrole of 1/2 drying carries out high-temperature activation at 600 DEG C of temperature by mass ratio, obtain the conductive nano agent of the attapulgite hydridization of white;
Dose volume ratio is 10/90 ethanol water, prepare the ethanol water of the silane coupler KH-590 of 2%, add attapulgite hybridized nanometer conductive agent, polypyrrole carries out ball milling in ball mill, Ball-milling Time is 1h, drying for standby is carried out, obtained scattered nanometer electricity-conductive powder at 100 DEG C of temperature;
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 into ethylene glycol solution, carries out ultrasonic disperse; Join in terephthalic acid (TPA) and carry out esterification, after esterification terminates, add 50ppm tetrabutyl titanate, 0.05% dodecyl quaternary ammonium salt is polymerized, obtain the conduction section of in-situ polymerization;
In above-mentioned steps, the nanometer electricity-conductive powder of attapulgite hydridization accounts for the mass fraction of total amount is 2%;
In above-mentioned steps, ethylene glycol accounts for the mass fraction of total amount is 40%;
Described terephthalic acid (TPA) accounts for the mass fraction 58% of total amount;
Conduction section is carried out melt spinning again, is that 4000m/min reels at spinning speed, obtains conducting electricity FDY fiber.
The ratio resistance that the conductive fiber obtained by method described in the present embodiment records fiber by fiber ratio resistance and charge decay instrument is 8.5 × 10
7Ω .cm, charge decay value is 1.8s.
Embodiment 4
Nano ATO powder is added dropwise in the pH=10 ammonia spirit of attapulgite, the mass ratio 8/2 of ATO and attapulgite, carries out high-speed stirred 1h at 50 DEG C of temperature, then carries out pH titration neutralization with hydrochloric acid, by washed with de-ionized water, put into baking oven and carry out drying and obtain conductive powder body; Be that conductive powder body and the polypyrrole of 1/10 drying carries out high-temperature activation at 600 DEG C of temperature by mass ratio, obtain the conductive nano agent of the attapulgite hydridization of white;
Dose volume ratio is 10/90 ethanol water, prepare the ethanol water of the silane coupler KH-902 of 1%, add attapulgite hybridized nanometer conductive agent, polyethylene glycol carries out ball milling in ball mill, Ball-milling Time is 1h, drying for standby is carried out, obtained scattered nanometer electricity-conductive powder at 100 DEG C of temperature;
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;
By accounting for the nanometer electricity-conductive powder high speed dispersion of gross mass 50% attapulgite hydridization in PBT, carrying out Screw Extrusion granulation, obtaining conduction PBT section;
Conduction section is carried out melt spinning again, is that 1000m/min reels at spinning speed, obtains conduction POY fiber.
The ratio resistance that the conductive fiber obtained by method described in the present embodiment records fiber by fiber ratio resistance and charge decay instrument is 4.8 × 10
5Ω .cm, charge decay value is 0.3s.
Embodiment 5
Nano ATO powder is added dropwise in the pH=10 ammonia spirit of attapulgite, the mass ratio 7/3 of ATO and attapulgite, carries out high-speed stirred 50min at 50 DEG C of temperature, then carries out pH titration neutralization with hydrochloric acid, by washed with de-ionized water, put into baking oven and carry out drying and obtain conductive powder body; Be that conductive powder body and the polypyrrole of 1/10 drying carries out high-temperature activation at 800 DEG C of temperature by mass ratio, obtain the conductive nano agent of the attapulgite hydridization of white;
Dose volume is than being 99.5/0.5 ethanol water, prepare the ethanol water of the silane resin acceptor kh-550 of 1.5%, add attapulgite hybridized nanometer conductive agent, polypyrrole alkane ketone carries out ball milling in ball mill, Ball-milling Time is 3h, drying for standby is carried out, obtained scattered nanometer electricity-conductive powder at 100 DEG C of temperature;
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;
By accounting for the nanometer electricity-conductive powder high speed dispersion of gross mass 10% attapulgite hydridization in PTT, carrying out Screw Extrusion granulation, obtaining conducting electricity PTT slice;
Conduction PTT slice is carried out melt spinning again, is that 3000m/min reels at spinning speed, obtains conduction POY fiber.
The ratio resistance that the conductive fiber obtained by method described in the present embodiment records fiber by fiber ratio resistance and charge decay instrument is 9.7 × 10
6Ω .cm, charge decay value is 0.5s.
Claims (5)
1. a preparation method for the conductive fiber of attapulgite hydridization, is characterized in that adopting following preparation process and step:
A nano ATO powder is added dropwise in the ammonia spirit of attapulgite by (), high-speed stirred 20min ~ 12h is carried out at 10 ~ 80 DEG C of temperature, carry out pH titration neutralization with hydrochloric acid again, by washed with de-ionized water, put into baking oven and carry out drying and obtain conductive powder body; The conductive powder body of drying and polyvinylpyrrolidone or polyvinyl pyrrole are carried out high-temperature activation at 400 ~ 800 DEG C of temperature, obtains the conductive nano agent of the attapulgite hydridization of white;
Described ATO and the mass ratio of attapulgite are 1/1 ~ 99/0.1;
Described conductive powder body and polyvinylpyrrolidone or polyvinyl pyrrole mass ratio are 1/1 ~ 99/1;
B () dose volume is than being 99.5/0.5 ~ 0.5/99.5 benzinum or ethanol water, successively the conductive nano agent of silane coupler, attapulgite hydridization, the high polymer of hydrophilic and benzinum or ethanol water are carried out ball milling in ball mill, Ball-milling Time is 10min ~ 12h, drying for standby is carried out, obtained scattered nanometer electricity-conductive powder at 80 ~ 150 DEG C of temperature;
Described silane coupler is one or more in KH-550, KH-560, KH-570, KH-902, KH-590;
Described hydrophilic polymer refers in polypyrrole, polypyrrole alkane ketone, polyethylene glycol, polyether ester a kind of, preferred polypyrrole;
Described silane coupler accounts for 0.1% ~ 20% of benzinum 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 dispersion of scattered attapulgite hydridization in molten polymer, is carried out Screw Extrusion granulation by (), obtain conduction 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 polytrimethylene terephthalate (PTT).
2. one of preparation method according to claim 1, its feature comprises the following steps, and the nanometer electricity-conductive powder of scattered attapulgite hydridization is put into ethylene glycol solution, carries out ultrasonic, ball milling, sand milling or grinding distribution; Join in terephthalic acid (TPA) and carry out esterification, add after esterification terminates the tetrabutyl titanate of 50ppm ~ 500ppm, 0.05% ~ 5% dodecyl quaternary ammonium salt carry out being polymerized arrive the conduction section of in-situ polymerization;
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 terephthalic acid (TPA) accounts for the mass fraction 50 ~ 60% of total amount.
3. according to one of preparation method described in claim 1 to 2, its feature comprises the following steps, and conduction section is carried out melt spinning again, is that 600-4000m/min reels at spinning speed, obtains conduction POY fiber.
4. one of preparation method according to claim 3, its feature comprises the following steps, and obtained POY fiber is carried out hot-stretch in 70 ~ 150 DEG C and obtains DTY conductive fiber.
5. a conductive fiber for the concave convex rod hydridization obtained by the preparation method described in Claims 1-4, is characterized in that the surface specific resistance of fiber is 10
2~ 10
10Ω .cm, electric charge partly decays to 0.01 ~ 15s.
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| CN109908008A (en) * | 2019-02-27 | 2019-06-21 | 北京中蓝港湾科技有限公司 | A kind of moisturizing face cream and preparation method containing attapulgite |
| 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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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. |