CN103013057B - Preparation method of anti-static polyester material based on carbon nanotube - Google Patents
Preparation method of anti-static polyester material based on carbon nanotube Download PDFInfo
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- CN103013057B CN103013057B CN201110288909.8A CN201110288909A CN103013057B CN 103013057 B CN103013057 B CN 103013057B CN 201110288909 A CN201110288909 A CN 201110288909A CN 103013057 B CN103013057 B CN 103013057B
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Abstract
The invention relates to a preparation method of an anti-static polyester material. The polyester material is improved by a modified carbon nanotube; and based on good electrical conductivity of a carbon nanotube, the carbon nanotube is modified with the method by adding a metal oxide and a dispersing agent to obtain a modified carbon nanotube with good dispersing effect, low cost and good electric conduction effect. In a melting compounding modification method, the thermal stability in the polyester material processing process is improved by adding a high molecular composite aid, and a polyester composite material with high performance and low volume resistance of less than 107(omega)cm is obtained. The method provided by the invention has simple technology and is easy to operate; the material performance is good, and the cost is relatively low; and the method has great application value and is suitable for industrial production.
Description
Technical field
The present invention relates to a kind of antistatic polyester material, particularly a kind of preparation method of the antistatic polyester material based on carbon nanotube.
Background technology
The macromolecular materials such as plastics, rubber, synthon, all there is superior electrical insulation capability, its basic reason is that the chemical bond in this family macromolecule is covalent linkage, therefore they can not ionize, can not transmit electronics or ion, there is very high surface resistivity and volume resistance, when their phase mutual friction or contact separation, will produce very high static.Resistance is larger, and static discharges just slower, thereby more easily produces electrostatic attraction or repulsion, electroshock or electric shock, even produces discharge spark and causes major accident.
The production of synthon and processing in textile industry, the production of various electrostatic susceptibility elements, transportation, storage in electronic industry, because the accumulation of static charge tends to cause heavy losses.In the U.S., plastic electronic parts scrap rate in storage and transport process reaches 50%, and loss is up to 5,000,000,000 dollars.The loss that the annual electrostatic accident of petrochemical enterprise in China produces is up to more than 1,000,000 yuan, so the control of static has caused people's common concern.
Polyester is widely used because of its good physics, chemical property, but because static behaviour has a strong impact on its processing characteristics, and directly impact is produced and is used.Chinese scholars has been done a large amount of research at solution polyester electrostatic problem, is summed up and mainly contains following several method: 1. in polyester matrix, add the synthetic antistatic resin of static inhibitor; 2. composite spinning method, take conventional polyester as skin, and the resin with static resistance of take is core; 3. first make electro-conductive fiber (as steel fiber, charcoal fiber, white conductive fiber etc.), then twist with the fingers, interweave and obtain with the mixed fibre of conventional polyester, friendship; 4. graft copolymerization, causes by initiator or the means such as radiation exposure, on trevira, carries out grafting with hydrophilic monomers such as vinylformic acid, methacrylic acids; 5. fabric post-treatment, conventionally adopting polyethylene glycol dimethacrylate and acrylic acid aqueous solution etc. is post-finishing agent.In sum, should guarantee that antistatic effect considers actual production feasibility again during antistatic polyester design of material.
Carbon nanotube is a kind of tubular structure nano-carbon material, and last century, the nineties was found by Japanese scientist Iijima.Carbon nanotube has good conductivity and chemical stability, and has filamentary structure.When preparing antistatic macromolecule material, add the carbon nanotube of small amount just can reach the requirement of leading static.Because its addition is few, color is easily covered by polymer matrix, is easy to obtain light tone product, also helps the design of other performance of macromolecular material simultaneously, is therefore subject to extensive concern.The active group of carbon nano tube surface is considerably less, very weak with the interaction of macromolecular material group, and the length-to-diameter ratio of carbon nanotube and specific surface area large, during for the preparation of polymer composite, be difficult to be uniformly dispersed in polymkeric substance, very easily there is agglomeration, cannot embody its excellent properties.Therefore the surface modification of carbon nanotube is seemed to very important.The people such as Gregoriou (Macromolecules2006,39,9150-9156) reported and first utilized strong acid treatment multi-walled carbon nano-tubes (MWCNT) surface, obtain PET-MWCNT matrix material with the method for polyethylene terephthalate (PET) blend afterwards, and studied the impact of carbon nanotube on PET crystallization behavior and chain conformation in great detail, the shortcoming of this method is the structure of strong acid treatment carbon nanotube meeting destroying carbon nanometer tube itself, lingering section impurity, and the introducing of strong acid easily causes environmental pollution.The people such as Luo Guohua (Comput.Sci.Technol.2006,66,1022-1029; Chinese invention patent 200410033773) by adding the mode of coupling agent to improve the dispersiveness of carbon nanotube in polymkeric substance in melt-processed process, but the material result that this method is only prepared when using Single Walled Carbon Nanotube is better, when using multi-walled carbon nano-tubes, will obtain the matrix material that volume specific resistance is lower and need to add relatively large carbon nanotube, material cost is apparently higher than traditional antistatic material.Chinese invention patent 200680001853 and 200610023797 discloses respectively and utilized graphite and carbon black is additive, a series of thermoplastic polymers of carbon nano-tube modification are (as acrylonitrile-butadiene-styrene (ABS), polyphenylmethyl olefin(e) acid methyl esters, polymeric amide, polyethylene etc.), owing to having introduced graphite and carbon black, the color of material is single, is difficult to expand its Application Areas.
It is higher that the above-mentioned method to surface modification of carbon nanotube is applied to antistatic polyester material preparation cost, and still have dispersed bad shortcoming, is difficult to be applied to industrial production.
Summary of the invention
The object of the invention is to solve above-mentioned deficiency, a kind of preparation method of the antistatic polyester material based on carbon nanotube is provided.
Realizing technical scheme of the present invention is: a kind of antistatic polyester material based on carbon nanotube is prepared by following method:
(1) carbon nanotube and metal oxide are put into the aqueous dispersant that contains 1-50% weight percent, disperse 1-10min in dispersator, drying, obtains the carbon nanotube of modifying after grinding;
(2) by the carbon nanotube of above-mentioned modification, vibrin, auxiliary agent is added in homogenizer and is uniformly dispersed;
(3) above-mentioned finely dispersed pellet is compound through twin screw extruder melting, extrudes and pelletizing, is prepared into antistatic polyester pellet.
The preparation method of the above-mentioned antistatic polyester material based on carbon nanotube, described carbon nanotube is multi-walled carbon nano-tubes or Single Walled Carbon Nanotube.
The preparation method of the above-mentioned antistatic polyester material based on carbon nanotube, described metal oxide is one or more in titanium dioxide, zinc oxide, tindioxide, Indium sesquioxide.
Above-mentioned based on carbon nanotube the preparation method of antistatic polyester material, described dispersion agent is one or more in alkyl sodium sulfonate, γ-aminopropyl triethoxysilane, γ-(methacryloxypropyl) propyl trimethoxy silicane, whiteruss.
The preparation method of the above-mentioned antistatic polyester material based on carbon nanotube, the ratio of quality and the number of copies of described metal oxide, dispersion agent and carbon nanotube is: (1-500): (50-200): 100.
The preparation method of the above-mentioned antistatic polyester material based on carbon nanotube, described vibrin is one or more in pet resin, polytrimethylene terephthalate, polybutylene terephthalate resin, polylactic resin.
The preparation method of the above-mentioned antistatic polyester material based on carbon nanotube, described auxiliary agent is one or more in antioxidant 1010, triphenylphosphate, phosphorous acid, stearic acid, nano-calcium carbonate, calcium stearate, Zinic stearas, Magnesium Stearate, terephthalic acid calcium, terephthalic acid zinc, terephthalic acid magnesium.
The preparation method of the above-mentioned antistatic polyester material based on carbon nanotube, the ratio of quality and the number of copies of the carbon nanotube of the modification of described step (2), auxiliary agent, polyester is (1-20): (0.1-2): 100.
The above-mentioned preparation method based on carbon nanotube anti-static polyester material, the melting composite steps of described step (3) is carried out in twin screw extruder, and the screw speed of described twin screw extruder is 20-250 rev/min, and melt temperature is 190-280 ℃.
The present invention utilizes metal oxide and dispersion agent to improve carbon nano tube surface performance, make metal oxide-coated in carbon nano tube surface, by method for melt processing, the even carbon nanotube of surface modification is distributed in polyester, makes carbon nanotube in matrix, form conductive network.Carbon nanotube after surface modification not only has good consistency with polyester matrix, and can effectively improve the interaction of carbon nanotube and polyester matrix, obtains high-performance antistatic polyester material.
The present invention has positive effect: (1) carbon nano tube modified method is simple, is easy to suitability for industrialized production; (2) the carbon nanotube Heat stability is good of modifying, the dispersion effect in polyester material is good; (3) add a small amount of carbon nanotube and can obtain antistatic polyester material, save production cost, can obtain the antistatic polyester material that color and luster is more shallow simultaneously.(4) by adding the method for auxiliary addition agent to improve the thermostability of modified carbon nano-tube and polyester matrix, obtain high performance antistatic polyester material in the course of processing.
Embodiment
(embodiment 1)
The carbon nanotube and the 0.5g zinc oxide that by 5g length, are 10 μ m, diameter 50nm are put into the sodium dodecyl sulfate aqueous solution that 250g contains 2% weight percent, disperse 5min in dispersator, and drying obtains the carbon nanotube of modifying after grinding.The carbon nanotube of 1 part of modification, 0.5 part of antioxidant 1010 and 100 parts of polyethylene terephthalates are added to after being uniformly dispersed in homogenizer and add twin screw extruder melting compound, extrusion machine fused mass temperature is controlled at 265 ℃ of left and right, screw speed is set as 50 revs/min, extrudate is through water-cooled, pelletizing after forced air drying, obtain antistatic polyester material, volume specific resistance is 6 * 10
6Ω cm.
(embodiment 2)
The carbon nanotube and the 0.5g titanium dioxide that by 15g length, are 10 μ m, diameter 50nm are put into the sodium dodecyl sulfate aqueous solution that 750g contains 1% weight percent, disperse 10min in dispersator, and drying obtains the carbon nanotube of modifying after grinding.The carbon nanotube of 5 parts of modifications, 0.1 portion of triphenylphosphate and 100 parts of polyethylene terephthalates are added to after being uniformly dispersed in homogenizer and add twin screw extruder melting compound, extrusion machine fused mass temperature is controlled at 265 ℃ of left and right, screw speed is set as 250 revs/min, extrudate is through water-cooled, pelletizing after forced air drying, obtain antistatic polyester material, volume specific resistance is 4 * 10
5Ω cm.
(embodiment 3)
The carbon nanotube and the 0.5g tindioxide that by 5g length, are 10 μ m, diameter 50nm are put into the γ-aminopropyl triethoxysilane aqueous solution that 25g contains 50% weight percent, in dispersator, disperse 1min, drying, obtains the carbon nanotube of modifying after grinding.The carbon nanotube of 5 parts of modifications, 2 parts of Zinic stearass and 100 parts of Poly(Trimethylene Terephthalate) are added to after being uniformly dispersed in homogenizer and add twin screw extruder melting compound, extrusion machine fused mass temperature is controlled at 245 ℃ of left and right, screw speed is set as 80 revs/min, extrudate is through water-cooled, pelletizing after forced air drying, obtain antistatic polyester material, volume specific resistance is 3 * 10
6Ω cm.
(embodiment 4)
The carbon nanotube and the 0.5g titanium dioxide that by 5g length, are 10 μ m, diameter 50nm are put into the sodium dodecyl sulfate aqueous solution that 250g contains 2% weight percent, disperse 5min in dispersator, and drying obtains the carbon nanotube of modifying after grinding.The carbon nanotube of 5 parts of modifications, 0.5 part of terephthalic acid calcium and 100 parts of polybutylene terephthalates are added to after being uniformly dispersed in homogenizer and add twin screw extruder melting compound, extrusion machine fused mass temperature is controlled at 235 ℃ of left and right, screw speed is set as 200 revs/min, extrudate is through water-cooled, pelletizing after forced air drying, obtain antistatic polyester material, volume specific resistance is 5 * 10
5Ω cm.
(embodiment 5)
The carbon nanotube and the 0.5g zinc oxide that by 5g length, are 10 μ m, diameter 50nm are put into γ-(methacryloxypropyl) propyl trimethoxy silicane aqueous solution that 250g contains 2% weight percent, in dispersator, disperse 5min, drying, obtains the carbon nanotube of modifying after grinding.The carbon nanotube of 5 parts of modifications, 0.5 part of terephthalic acid zinc, 0.5 part of antioxidant 1010 and 100 parts of polyethylene terephthalates are added to after being uniformly dispersed in homogenizer and add twin screw extruder melting compound, extrusion machine fused mass temperature is controlled at 265 ℃ of left and right, screw speed is set as 50 revs/min, extrudate is through water-cooled, pelletizing after forced air drying, obtain antistatic polyester material, volume specific resistance is 2 * 10
4Ω cm.
(embodiment 6)
The carbon nanotube and the 25g zinc oxide that by 5g length, are 10 μ m, diameter 50nm are put into γ-(methacryloxypropyl) propyl trimethoxy silicane aqueous solution that 500g contains 2% weight percent, in dispersator, disperse 5min, drying, obtains the carbon nanotube of modifying after grinding.The carbon nanotube of 10 parts of modifications, 0.5 part of antioxidant 1010 and 100 parts of polyethylene terephthalates are added to after being uniformly dispersed in homogenizer and add twin screw extruder melting compound, extrusion machine fused mass temperature is controlled at 265 ℃ of left and right, screw speed is set as 50 revs/min, extrudate is through water-cooled, pelletizing after forced air drying, obtain antistatic polyester material, volume specific resistance is 4 * 10
5Ω cm.
(embodiment 7)
The carbon nanotube and the 25g titanium dioxide that by 5g length, are 10 μ m, diameter 50nm are put into the γ-aminopropyl triethoxysilane aqueous solution that 500g contains 2% weight percent, in dispersator, disperse 5min, drying, obtains the carbon nanotube of modifying after grinding.The carbon nanotube of 10 parts of modifications, 0.5 part of antioxidant 1010,0.5 part of phosphorous acid and 100 parts of polyethylene terephthalates are added to after being uniformly dispersed in homogenizer and add twin screw extruder melting compound, extrusion machine fused mass temperature is controlled at 265 ℃ of left and right, screw speed is set as 50 revs/min, extrudate is through water-cooled, pelletizing after forced air drying, obtain antistatic polyester material, volume specific resistance is 3 * 10
5Ω cm.
(embodiment 8)
The carbon nanotube and the 0.05g Indium sesquioxide that by 5g length, are 10 μ m, diameter 50nm are put into the whiteruss aqueous solution that 250g contains 2% weight percent, disperse 10min in dispersator, and drying obtains the carbon nanotube of modifying after grinding.The carbon nanotube of 5 parts of modifications, 0.5 part of stearic acid and 100 parts of polyethylene terephthalates are added to after being uniformly dispersed in homogenizer and add twin screw extruder melting compound, extrusion machine fused mass temperature is controlled at 265 ℃ of left and right, screw speed is set as 50 revs/min, extrudate is through water-cooled, pelletizing after forced air drying, obtain antistatic polyester material, volume specific resistance is 8 * 10
5Ω cm.
(embodiment 9)
The carbon nanotube and the 0.5g zinc oxide that by 5g length, are 10 μ m, diameter 50nm are put into the sodium dodecyl sulfate aqueous solution that 250g contains 2% weight percent, disperse 5min in dispersator, and drying obtains the carbon nanotube of modifying after grinding.The carbon nanotube of 5 parts of modifications, 0.5 part of antioxidant 1010,0.5 part of Magnesium Stearate and 100 parts of poly-poly(lactic acid) are added to after being uniformly dispersed in homogenizer and add twin screw extruder melting compound, extrusion machine fused mass temperature is controlled at 205 ℃ of left and right, screw speed is set as 20 revs/min, extrudate is through water-cooled, pelletizing after forced air drying, obtain antistatic polyester material, volume specific resistance is 5 * 10
6Ω cm.
(embodiment 10)
The carbon nanotube and the 0.5g zinc oxide that by 25g length, are 10 μ m, diameter 50nm are put into the γ-aminopropyl triethoxysilane aqueous solution that 250g contains 4% weight percent, in dispersator, disperse 5min, drying, obtains the carbon nanotube of modifying after grinding.The carbon nanotube of 20 parts of modifications, 2 parts of terephthalic acid calcium and 100 parts of polybutylene terephthalates are added to after being uniformly dispersed in homogenizer and add twin screw extruder melting compound, extrusion machine fused mass temperature is controlled at 235 ℃ of left and right, screw speed is set as 50 revs/min, extrudate is through water-cooled, pelletizing after forced air drying, obtain antistatic polyester material, volume specific resistance is 3 * 10
4Ω cm.
(embodiment 11)
The carbon nanotube and the 25g titanium dioxide that by 5g length, are 10 μ m, diameter 50nm are put into γ-(methacryloxypropyl) propyl trimethoxy silicane aqueous solution that 150g contains 10% weight percent, in dispersator, disperse 5min, drying, obtains the carbon nanotube of modifying after grinding.The carbon nanotube of 15 parts of modifications, 0.5 part of antioxidant 1010,30 parts of polyethylene terephthalates and 70 parts of polybutylene terephthalates are added to after being uniformly dispersed in homogenizer and add twin screw extruder melting compound, extrusion machine fused mass temperature is controlled at 255 ℃ of left and right, screw speed is set as 200 revs/min, extrudate is through water-cooled, pelletizing after forced air drying, obtain antistatic polyester material, volume specific resistance is 6 * 10
4Ω cm.
(embodiment 12)
The carbon nanotube and the 0.5g zinc oxide that by 5g length, are 20 μ m, diameter 80nm are put into the sodium dodecyl sulfate aqueous solution that 250g contains 2% weight percent, disperse 10min in dispersator, and drying obtains the carbon nanotube of modifying after grinding.The carbon nanotube of 5 parts of modifications, 0.5 part of antioxidant 1010,1 part of Magnesium Stearate and 100 parts of polyethylene terephthalates are added to after being uniformly dispersed in homogenizer and add twin screw extruder melting compound, extrusion machine fused mass temperature is controlled at 280 ℃ of left and right, screw speed is set as 250 revs/min, extrudate is through water-cooled, pelletizing after forced air drying, obtain antistatic polyester material, volume specific resistance is 7 * 10
5Ω cm.
Above-described specific embodiment; object of the present invention, technical scheme and beneficial effect are further described; institute is understood that; the foregoing is only specific embodiments of the invention; be not limited to the present invention; within the spirit and principles in the present invention all, any modification of making, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (9)
1. a preparation method for the antistatic polyester material based on carbon nanotube, is characterized in that comprising the steps:
(1) carbon nanotube and metal oxide are put into the aqueous dispersant that contains 1～50% weight percent, in dispersator, disperse 1～10min, after drying, grinding, obtain the carbon nanotube of modifying;
(2) carbon nanotube of above-mentioned modification, vibrin, auxiliary agent are added in homogenizer and are uniformly dispersed;
(3) above-mentioned finely dispersed pellet is compound through twin screw extruder melting, extrudes and pelletizing, is prepared into antistatic polyester pellet.
2. the preparation method of the antistatic polyester material based on carbon nanotube according to claim 1, is characterized in that: described carbon nanotube is multi-walled carbon nano-tubes or Single Walled Carbon Nanotube.
3. the preparation method of the antistatic polyester material based on carbon nanotube according to claim 1, is characterized in that: described metal oxide is one or more in titanium dioxide, zinc oxide, tindioxide, Indium sesquioxide.
4. the preparation method of the antistatic polyester material based on carbon nanotube according to claim 1, is characterized in that: described dispersion agent is one or more in alkyl sodium sulfonate, γ-aminopropyl triethoxysilane, γ-(methacryloxypropyl) propyl trimethoxy silicane, whiteruss.
5. the preparation method of the antistatic polyester material based on carbon nanotube according to claim 1, is characterized in that: the ratio of quality and the number of copies of described metal oxide, dispersion agent and carbon nanotube is: (1～500): (50～200): 100.
6. the preparation method of the antistatic polyester material based on carbon nanotube according to claim 1, is characterized in that: described vibrin is one or more in pet resin, polytrimethylene terephthalate, polybutylene terephthalate resin, polylactic resin.
7. the preparation method of the antistatic polyester material based on carbon nanotube according to claim 1, is characterized in that: described auxiliary agent is one or more in antioxidant 1010, triphenylphosphate, phosphorous acid, stearic acid, nano-calcium carbonate, calcium stearate, Zinic stearas, Magnesium Stearate, terephthalic acid calcium, terephthalic acid zinc, terephthalic acid magnesium.
8. the preparation method of the antistatic polyester material based on carbon nanotube according to claim 1, is characterized in that: the ratio of quality and the number of copies of the carbon nanotube of the modification of described step (2), auxiliary agent, polyester is (1～20): (0.1～2): 100.
9. the preparation method of antistatic polyester material according to claim 1, it is characterized in that: the melting composite steps of described step (3) is carried out in twin screw extruder, the screw speed of described twin screw extruder is 20～250 revs/min, and melt temperature is 190～280 ℃.
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| CN106046708A (en) * | 2016-06-30 | 2016-10-26 | 嘉兴市高正高分子材料有限公司 | Preparation method of activated carbon nanotube modified PET antistatic thin film |
| CN106243637A (en) * | 2016-06-30 | 2016-12-21 | 嘉兴市高正高分子材料有限公司 | The PET antistatic film that a kind of Activated Carbon Nanotubes is modified |
| CN106046709A (en) * | 2016-06-30 | 2016-10-26 | 嘉兴市高正高分子材料有限公司 | Carbon nanotube modified PET antistatic thin film |
| CN106906643A (en) * | 2017-03-31 | 2017-06-30 | 江苏盛纺纳米材料科技股份有限公司 | A kind of antistatic afterfinish method for non-weaving cloth |
| CN108975715A (en) * | 2018-08-13 | 2018-12-11 | 苏州华龙化工有限公司 | A kind of preparation method of the antistatic glass fibre for air filtration |
| CN109912941B (en) * | 2019-03-15 | 2021-04-02 | 广东格瑞纳思薄膜科技有限公司 | Antistatic high-hardness nano-composite optical grade PET (polyethylene terephthalate) slice and preparation method thereof |
| CN110183764B (en) * | 2019-06-29 | 2022-02-18 | 山东东宏管业股份有限公司 | Processing method of antistatic and self-cleaning carbon nanotube pipe |
| CN112175363B (en) * | 2020-10-30 | 2022-08-12 | 华碳创新(广东)材料技术有限公司 | Polyethylene terephthalate material containing carbon nano tube and preparation method thereof |
| TWI788009B (en) | 2021-09-13 | 2022-12-21 | 南亞塑膠工業股份有限公司 | Conductive polyester composition |
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