CN105331058A - Method for preparing conductive polyester master batch with in-situ polymerization method - Google Patents
Method for preparing conductive polyester master batch with in-situ polymerization method Download PDFInfo
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- CN105331058A CN105331058A CN201510788212.5A CN201510788212A CN105331058A CN 105331058 A CN105331058 A CN 105331058A CN 201510788212 A CN201510788212 A CN 201510788212A CN 105331058 A CN105331058 A CN 105331058A
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Abstract
The invention provides a method for preparing conductive polyester master batch with an in-situ polymerization method. The conductive polyester master batch is mainly prepared from 5wt%-20wt% of graphene, 15wt%-30wt% of glycol, 60wt%-80wt% of terephthalic acid, 0.1wt%-0.5wt% of a catalyst, a dispersing agent and a stabilizer through chemical synthesis under a high-temperature and high-pressure condition. Graphene, glycol and the dispersing agent are subjected to ultrasonic dispersion, a graphene dispersing liquid is prepared; the dispersing liquid, terephthalic acid, the catalyst and the stabilizer are put into a reaction kettle, and the conductive master batch is prepared under a high-temperature and high-pressure condition. The method is different from traditional solid-phase blending melting granulating, sufficiently solves the problem that graphene cannot be dispersed uniformly in a plastic substrate and has a good application prospect.
Description
Technical field
The present invention relates to a kind of preparation method for conductive agglomerate, especially a kind of conductive polyester material obtained by in-situ polymerization.
Background technology
Graphene is called as " changing the material of 21 century ", and according to test, it is the two-dimensional material that occurring in nature is the strongest now, is ten times of common iron and steel.Graphene has excellent room temperature thermal conductivity and light transmission, and simultaneously as the material that resistivity known is in the world minimum, it also has superpower conductivity.Feature many above causes Graphene to have great application prospect in fields such as new forms of energy, space flight, electronics, military projects, becomes international study hotspot.
Have benefited from the development of electronics integrated technology and components and parts miniaturization, the concept of " wearable device " budded out into popularity gradually in recent years.Its key concept be little electronics is directly loaded with fabric among, to realize the portable function of such as Electrocardiography and so on.This just must overcome a key issue, and the interaction problems of namely weave subject and electronics subject, the research therefore for electro-conductive fiber is arisen at the historic moment.The research of electro-conductive fiber is long-standing, and its initial object is the safety for protecting human body under antistatic or high voltage environment, mainly comprises steel fiber, carbon black series fiber, conductive metal compound fiber and conducting polymer fiber type.Now along with the functionalization of clothing develops, more and more new requirement be it is also proposed to electro-conductive fiber.
Summary of the invention
For overcoming the deficiencies in the prior art, the invention provides a kind of method that situ aggregation method prepares conductive polyester master batch, the method is different from the method for traditional melt blending, by the mode of in-situ polymerization, Graphene is made conductive polyester master batch, be intended to solve the unmanageable problem of Graphene under powder state, have a good application prospect.
Situ aggregation method prepares a method for conductive polyester master batch, it is characterized in that, described conductive polyester master batch obtains primarily of the chemosynthesis under high-temperature and high-pressure conditions of Graphene, ethylene glycol, terephthalic acid, catalyzer, dispersion agent, stablizer; Graphene being placed in ethylene glycol adopts high-speed shearing machine just to disperse, and drips dispersion agent simultaneously and obtains homodisperse Graphene slurry; This slurry, terephthalic acid, catalyzer, stablizer are placed in high-temperature high-pressure reaction kettle, and discharging after for some time, pelletizing can obtain conductive polyester master batch.
The usage quantity of described Graphene is 5 ~ 20wt% of master batch quality.
The dispersion agent selected is one or more the combination in silane coupling agent, titanate coupling agent, aluminate coupling agent, and usage quantity is 0.05 ~ 0.3wt% of master batch quality.
The usage quantity of ethylene glycol is 15 ~ 30wt% of master batch quality.
The usage quantity of terephthalic acid is 60 ~ 80wt% of master batch quality.
Catalyzer is the combination of one or more in weisspiessglanz, antimony glycol, Cobaltous diacetate, ionic polymerization catalyst, and usage quantity is 0.1 ~ 0.5wt% of master batch quality.
Stablizer is the combination of one or more in organotin, lead salt, TriMethylolPropane(TMP), rare-earth stabilizer, and usage quantity is 0.01 ~ 0.1wt% of master batch quality.
Graphene, dispersion agent, ethylene glycol are obtained Graphene slurry by high-speed shearing machine, when again Graphene slurry, terephthalic acid, catalyzer, stablizer being placed in high-temperature high-pressure reaction kettle, polymerization temperature is 230 ~ 290 DEG C, pressure change in whole reaction process is-0.2 ~ 0.5MPa, and discharging, shearing, granulation can obtain conductive polyester master batch.
The graphene conductive polyester master particle adopting the inventive method to prepare has following advantage:
The present invention adopts situ aggregation method to obtain graphene conductive polyester master particle, makes Graphene can be uniformly dispersed in polyester matrix;
After this master batch is made fiber, there is good electroconductibility and intensity, can be used in the intelligent clothing fields such as wearable device.
Embodiment
Below by embodiment, the present invention is specifically described.Following examples, only for the invention will be further described, can not be interpreted as limiting the scope of the invention, the adjustment that professional and technical personnel's content according to the present invention in this field is made, and still belong to protection scope of the present invention.
Embodiment 1:
Take out 5g Graphene and be placed in 15g ethylene glycol, use high-speed shearing machine to disperse, drip 0.05g silane coupling agent simultaneously, obtained Graphene slurry.This slurry, 60g terephthalic acid, weisspiessglanz 0.1g, organotin 0.01g are dropped in high-temperature high-pressure reaction kettle, keep temperature 230 DEG C, original pressure 0.5MPa, along with reaction is carried out, is evacuated to-0.2MPa, after pressurize for some time, and blowing pelletizing.
Embodiment 2:
Take out 10g Graphene and be placed in 20g ethylene glycol, use high-speed shearing machine to disperse, drip 0.1g titanate coupling agent simultaneously, obtained Graphene slurry.This slurry, 70g terephthalic acid, antimony glycol 0.3g, lead salt 0.05g are dropped in high-temperature high-pressure reaction kettle, keep temperature 260 DEG C, original pressure 0.5MPa, along with reaction is carried out, is evacuated to-0.2MPa, after pressurize for some time, and blowing pelletizing.
Embodiment 3:
Take out 20g Graphene and be placed in 30g ethylene glycol, use high-speed shearing machine to disperse, drip 0.3g aluminate coupling agent simultaneously, obtained Graphene slurry.This slurry, 80g terephthalic acid, Cobaltous diacetate 0.5g, TriMethylolPropane(TMP) 0.1g are dropped in high-temperature high-pressure reaction kettle, keeps temperature 290 DEG C, original pressure 0.5MPa, along with reaction is carried out, be evacuated to-0.2MPa, after pressurize for some time, blowing pelletizing.
Claims (8)
1. prepare a method for conductive polyester master batch with situ aggregation method, it is characterized in that, described conductive polyester master batch obtains primarily of the chemosynthesis under high-temperature and high-pressure conditions of Graphene, ethylene glycol, terephthalic acid, catalyzer, dispersion agent, stablizer; Graphene being placed in ethylene glycol adopts high-speed shearing machine just to disperse, and drips dispersion agent simultaneously and obtains homodisperse Graphene slurry; This slurry, terephthalic acid, catalyzer, stablizer are placed in high-temperature high-pressure reaction kettle, and discharging after for some time, pelletizing can obtain conductive polyester master batch.
2. a kind of situ aggregation method according to claim 1 prepares the method for conductive polyester master batch, it is characterized in that, the usage quantity of described Graphene is 5 ~ 20wt% of master batch quality.
3. a kind of situ aggregation method according to claim 1 prepares the method for conductive polyester master batch, it is characterized in that, the dispersion agent selected is one or more the combination in silane coupling agent, titanate coupling agent, aluminate coupling agent, and usage quantity is 0.05 ~ 0.3wt% of master batch quality.
4. a kind of situ aggregation method according to claim 1 prepares the method for conductive polyester master batch, it is characterized in that, the usage quantity of ethylene glycol is 15 ~ 30wt% of master batch quality.
5. a kind of situ aggregation method according to claim 1 prepares the method for conductive polyester master batch, it is characterized in that, the usage quantity of terephthalic acid is 60 ~ 80wt% of master batch quality.
6. a kind of situ aggregation method according to claim 1 prepares the method for conductive polyester master batch, it is characterized in that, catalyzer is the combination of one or more in weisspiessglanz, antimony glycol, Cobaltous diacetate, ionic polymerization catalyst, and usage quantity is 0.1 ~ 0.5wt% of master batch quality.
7. a kind of situ aggregation method according to claim 1 prepares the method for conductive polyester master batch, it is characterized in that, stablizer is the combination of one or more in organotin, lead salt, TriMethylolPropane(TMP), rare-earth stabilizer, and usage quantity is 0.01 ~ 0.1wt% of master batch quality.
8. a kind of situ aggregation method according to claim 1 prepares the method for conductive polyester master batch, it is characterized in that, Graphene, dispersion agent, ethylene glycol are obtained Graphene slurry by high-speed shearing machine, when again Graphene slurry, terephthalic acid, catalyzer, stablizer being placed in high-temperature high-pressure reaction kettle, polymerization temperature is 230 ~ 290 DEG C, pressure change in whole reaction process is-0.2 ~ 0.5MPa, and discharging, shearing, granulation can obtain conductive polyester master batch.
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105778067A (en) * | 2016-03-26 | 2016-07-20 | 佛山佛塑科技集团股份有限公司 | Internal addition synthetic composite material of infrared barrier polyester chip and preparation method thereof |
| CN105951206A (en) * | 2016-06-27 | 2016-09-21 | 仪征盛大纺织新材料有限公司 | Anti-electrostatic modified PBT fiber |
| CN105970340A (en) * | 2016-06-27 | 2016-09-28 | 仪征盛大纺织新材料有限公司 | Preparation method of antistatic modified PBT fiber |
| CN107083578A (en) * | 2017-04-27 | 2017-08-22 | 南通强生石墨烯科技有限公司 | The preparation method of graphene elastic polyester in-situ polymerization composite functional fiber |
| CN109369898A (en) * | 2018-10-14 | 2019-02-22 | 东华大学 | A kind of high fluidity conductive polyester master batch and preparation method thereof |
| CN109679075A (en) * | 2018-12-21 | 2019-04-26 | 南通强生石墨烯科技有限公司 | In-situ polymerization modified graphene terylene compound slice and its preparation method and application |
| CN109762146A (en) * | 2018-12-28 | 2019-05-17 | 上海普利特化工新材料有限公司 | A kind of graphene in-situ polymerization thermotropic liquid crystal polymer composite material and preparation method |
| CN109971133A (en) * | 2017-12-27 | 2019-07-05 | 宁波长阳科技股份有限公司 | A kind of reflectance coating with conductive and heat-conductive surface layer and a kind of preparation method of graphene master batch |
| CN110128634A (en) * | 2019-04-30 | 2019-08-16 | 福建省银河服饰有限公司 | A kind of preparation method of graphene Modified polyester chips |
| CN110628052A (en) * | 2019-09-25 | 2019-12-31 | 宁波石墨烯创新中心有限公司 | Graphene dispersion liquid, graphene/polymer composite material and preparation method thereof |
| CN111393823A (en) * | 2020-04-22 | 2020-07-10 | 福州大学 | Gn-PET/PC alloy with excellent mechanical property and preparation method thereof |
| CN111676541A (en) * | 2020-06-10 | 2020-09-18 | 浙江恒澜科技有限公司 | Preparation method of antistatic low-temperature far infrared polyester fiber |
| CN114318645A (en) * | 2022-01-04 | 2022-04-12 | 新材料与产业技术北京研究院金华分院 | Functional fabric and preparation method and application thereof |
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Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105778067A (en) * | 2016-03-26 | 2016-07-20 | 佛山佛塑科技集团股份有限公司 | Internal addition synthetic composite material of infrared barrier polyester chip and preparation method thereof |
| CN105951206A (en) * | 2016-06-27 | 2016-09-21 | 仪征盛大纺织新材料有限公司 | Anti-electrostatic modified PBT fiber |
| CN105970340A (en) * | 2016-06-27 | 2016-09-28 | 仪征盛大纺织新材料有限公司 | Preparation method of antistatic modified PBT fiber |
| CN105951206B (en) * | 2016-06-27 | 2018-05-01 | 仪征盛大纺织新材料有限公司 | A kind of antistatic modified PBT fibers |
| CN107083578A (en) * | 2017-04-27 | 2017-08-22 | 南通强生石墨烯科技有限公司 | The preparation method of graphene elastic polyester in-situ polymerization composite functional fiber |
| CN109971133A (en) * | 2017-12-27 | 2019-07-05 | 宁波长阳科技股份有限公司 | A kind of reflectance coating with conductive and heat-conductive surface layer and a kind of preparation method of graphene master batch |
| CN109369898A (en) * | 2018-10-14 | 2019-02-22 | 东华大学 | A kind of high fluidity conductive polyester master batch and preparation method thereof |
| CN109369898B (en) * | 2018-10-14 | 2020-09-15 | 东华大学 | High-fluidity conductive polyester master batch and preparation method thereof |
| CN109679075A (en) * | 2018-12-21 | 2019-04-26 | 南通强生石墨烯科技有限公司 | In-situ polymerization modified graphene terylene compound slice and its preparation method and application |
| CN109762146A (en) * | 2018-12-28 | 2019-05-17 | 上海普利特化工新材料有限公司 | A kind of graphene in-situ polymerization thermotropic liquid crystal polymer composite material and preparation method |
| CN110128634A (en) * | 2019-04-30 | 2019-08-16 | 福建省银河服饰有限公司 | A kind of preparation method of graphene Modified polyester chips |
| CN110628052A (en) * | 2019-09-25 | 2019-12-31 | 宁波石墨烯创新中心有限公司 | Graphene dispersion liquid, graphene/polymer composite material and preparation method thereof |
| CN111393823A (en) * | 2020-04-22 | 2020-07-10 | 福州大学 | Gn-PET/PC alloy with excellent mechanical property and preparation method thereof |
| CN111676541A (en) * | 2020-06-10 | 2020-09-18 | 浙江恒澜科技有限公司 | Preparation method of antistatic low-temperature far infrared polyester fiber |
| CN111676541B (en) * | 2020-06-10 | 2022-10-11 | 浙江恒逸石化研究院有限公司 | Preparation method of antistatic low-temperature far-infrared polyester fiber |
| CN114318645A (en) * | 2022-01-04 | 2022-04-12 | 新材料与产业技术北京研究院金华分院 | Functional fabric and preparation method and application thereof |
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