CN105350107A - Preparation method of light-colored PET polyester conductive fiber based on conductive zinc oxide - Google Patents
Preparation method of light-colored PET polyester conductive fiber based on conductive zinc oxide Download PDFInfo
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- CN105350107A CN105350107A CN201510686002.5A CN201510686002A CN105350107A CN 105350107 A CN105350107 A CN 105350107A CN 201510686002 A CN201510686002 A CN 201510686002A CN 105350107 A CN105350107 A CN 105350107A
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Abstract
The invention discloses a preparation method of light-colored PET polyester conductive fiber based on conductive zinc oxide. The preparation method includes preparing a dispersion liquid of conductive zinc oxide and ethanediol in high concentration, adding a modifier when the particle size D90 of the dispersion liquid is less than 100 nm to perform hydroxylation surface modification of zinc oxide, and adding terephthalic acid, dispersion liquid of conductive zinc oxide and ethanediol, catalyst and stabilizing agent into a polyreactor with a esterification-polycondensation technology to prepare the PET polyester conductive fiber with high conductivity. The conductive particle zinc oxide in the conductive fiber prepared by the invention is dispersed uniformly, and the electrical conductivity of the fiber is greatly improved.
Description
Technical field
The present invention relates to a kind of preparation method of the light PET polyester electric conduction fiber based on conductive zinc oxide.
Background technology
Polyethylene terephthalate (PET) fiber weaving and industrial circle in application widely, but the hydrophobicity of polyester fiber and insulating properties very poor, cause it easily to accumulate electrostatic in dry environments.And static discharge is not only harmful, and the kindling material of imflammable gas or dust can be become and set off an explosion and fire.For preventing electrostatic from causing various disaster, industrial quarters generally adopts compound or co-blended spinning method and post treatment method to adhere to or deposit high connductivity component to prepare PET polyester electric conduction fiber in common PET polyester fibre surface.
In the compound or co-blended spinning preparation method of PET polyester electric conduction fiber, be dispersed in PET polyester fondant by conductive fill powder (carbon black, metal or metal oxide etc.) by melt blending, prepared conductive fiber has and conducts electricity durability preferably.But the conductive powder body that the content added is higher, its particle agglomeration is relatively more serious, and particle diameter is comparatively large, and this not only can make polyester material spinnability be deteriorated, but also polyester fiber intensity can be caused obviously to decline.
The present invention is based on zinc oxide conductive component, by introducing esterification-polycondensating process, the high concentration conductive zinc oxide ethylene glycol dispersion liquid prepared and terephthalic acid (TPA) being prepared light PET polyester electric conduction fiber.Conducting particles in conductive fiber prepared by the method is uniformly dispersed, and realize individual particle dispersion, the dispersion particle diameter in PET is between 30-100nm, and the conductance of fiber and fibre strength obtain to be improved significantly.
Summary of the invention
The object of the invention is to break through and adopt conductive component in melt spinning method preparation process more serious at fibrous inside particle agglomeration at present, particle diameter is larger, this not only can make polyester material spinnability be deteriorated, but also the shortcoming that polyester fiber intensity obviously declines can be caused, be dispersed in PET polyester fondant by melt blending, prepared conductive fiber has and conducts electricity durability preferably.
For reaching above-mentioned expection object, the present invention adopts following technical scheme:
A kind of preparation method of the light PET polyester electric conduction fiber based on conductive zinc oxide, it is characterized in that, by introducing esterification-polycondensating process, the high concentration conductive zinc oxide ethylene glycol dispersion liquid prepared and terephthalic acid (TPA) are prepared light PET polyester electric conduction fiber, this technique comprises the steps:
A. by ethylene glycol, conductive zinc oxide and dispersant premix composition mixed liquor in proportion, nano-level grinder is used to carry out dispersion treatment, until add the hydroxylated surface modification that dressing agent carries out zinc oxide when the granularity D90 of solid particle reaches 100nm in mixed dispersion liquid;
B. conductive zinc oxide ethylene glycol dispersion liquid obtained for step a, terephthalic acid (TPA), catalyst, stabilizing agent are added in polymerization reaction kettle and carry out esterification, the airtight rear nitrogen replacement of reactor 2 times, wherein, the mass ratio of conductive zinc oxide ethylene glycol dispersion liquid, terephthalic acid (TPA), catalyst, stabilizing agent is 1 ~ 2:2:0.001 ~ 0.1:0.0005 ~ 0.05, reactor pressure is 0.2 ~ 1MPa, temperature is 200 ~ 250 DEG C, and reaction time of esterification is 1 ~ 3 hour;
C. after step b has reacted, open vacuum system, then heat up and carry out polycondensation reaction, wherein temperature is 270 ~ 350 DEG C, and reaction system pressure remains on below 100Pa, and the reaction time is 2 ~ 5h;
D., after step c reacts completely, product, by bottom valve discharging, tank cooling, obtains the PET material of conductive zinc oxide compound;
The PET material of the conductive zinc oxide compound e. steps d obtained carries out melt spinning, thus prepares anlistatig light PET polyester electric conduction fibrous material.
In step a, described dispersant is one in BYK190, BYK106, BYK182, BYK184, moral modest 904S, MOK5032 or its combination, and wherein the mass ratio of ethylene glycol, conductive zinc oxide and dispersant is 1:(0.3 ~ 0.6): (0.05 ~ 0.3).
In step a, described conductive zinc oxide is the zinc oxide Al of aluminium doping
xznO, titanium doped zinc oxide Ti
xthe zinc oxide Ga of ZnO, gallium doping
xznO, wherein 0.01≤x≤0.1.
In step a, described dressing agent is one in silane coupler, titanate coupling agent, polyethylene glycol or polyethers or its combination.
In step b, described catalyst material is, the one in cobalt acetate, antimonous oxide, 2-diimide pyridine iron, 2-diimide pyridine cobalt, imvite/niobium chloride or methylaluminoxane or its combination.
In step b, described stabilizing agent is one in trimethyl phosphate, polyvinyl alcohol, phosphoric acid, triphenyl phosphate or triethyl phosphate or its combination.
The high concentration conductive zinc oxide ethylene glycol dispersion liquid prepared and terephthalic acid (TPA) are carried out esterification-polycondensation reaction to prepare light PET polyester electric conduction fiber by the present invention.The product that obtain with the present invention's preparation---PET polyester electric conduction fiber to overcome in conventional spinning method the shortcomings such as conduction easy reunion, fibre strength reduction, and having can continuous production and the advantage such as cost is lower, can be applied in field of textile industry.
Detailed description of the invention
Below by instantiation, the details that the present invention realizes is described, but protection scope of the present invention is not limited to these embodiments.
Embodiment 1: by 100g ethylene glycol, 30g conductive zinc oxide Al
0.01znO and 5g dispersant B YK190 is premix composition mixed liquor in proportion, uses nano-level grinder to carry out dispersion treatment, until add the hydroxylated surface modification that dressing agent silane coupler carries out zinc oxide when the granularity D90 of solid particle reaches 100nm in mixed dispersion liquid; Obtained 135g conductive zinc oxide ethylene glycol dispersion liquid, 270g terephthalic acid (TPA), 0.135g cobalt acetate catalyst, 0.0675g tripotassium phosphate ester stabilizer are added in polymerization reaction kettle and carries out esterification, the airtight rear nitrogen replacement of reactor 2 times, wherein reactor pressure is 0.2MPa, temperature is 200 DEG C, and reaction time of esterification is 1 hour; After having reacted, open vacuum system, be then warming up to 270 DEG C and carry out polycondensation reaction, reaction system pressure remains on below 100Pa, and the reaction time is 2h; After question response is complete, product, by bottom valve discharging, tank cooling, obtains the PET material of conductive zinc oxide compound; The PET material of obtained conductive zinc oxide compound is carried out melt spinning, thus prepares anlistatig light PET polyester electric conduction fibrous material.
Embodiment 2: by 100g ethylene glycol, 40g conductive zinc oxide Al
0.1znO and 10g dispersant B YK106 is premix composition mixed liquor in proportion, nano-level grinder is used to carry out dispersion treatment, until add the hydroxylated surface modification that dressing agent titanate coupling agent carries out zinc oxide when the granularity D90 of solid particle reaches 100nm in mixed dispersion liquid; Obtained 150g conductive zinc oxide ethylene glycol dispersion liquid, 200g terephthalic acid (TPA), 0.5g antimonous oxide catalyst, 1g polyvinyl alcohol stabilizing agent are added in polymerization reaction kettle and carries out esterification, the airtight rear nitrogen replacement of reactor 2 times, wherein reactor pressure is 0.5MPa, temperature is 225 DEG C, and reaction time of esterification is 2 hours; After having reacted, open vacuum system, be then warming up to 300 DEG C and carry out polycondensation reaction, reaction system pressure remains on below 100Pa, and the reaction time is 3.5h; After question response is complete, product, by bottom valve discharging, tank cooling, obtains the PET material of conductive zinc oxide compound; The PET material of obtained conductive zinc oxide compound is carried out melt spinning, thus prepares anlistatig light PET polyester electric conduction fibrous material.
Embodiment 3: by 100g ethylene glycol, 60g conductive zinc oxide Ti
0.01znO and 30g dispersant B YK182 is premix composition mixed liquor in proportion, uses nano-level grinder to carry out dispersion treatment, until add the hydroxylated surface modification that dressing agent polyethylene glycol carries out zinc oxide when the granularity D90 of solid particle reaches 100nm in mixed dispersion liquid; Obtained 190g conductive zinc oxide ethylene glycol dispersion liquid, 190g terephthalic acid (TPA), 7.5g2-diimide pyridine iron catalyst, the agent of 3.75g phosphoric acid stabilize are added in polymerization reaction kettle and carries out esterification, the airtight rear nitrogen replacement of reactor 2 times, wherein reactor pressure is 1MPa, temperature is 250 DEG C, and reaction time of esterification is 3 hours; After having reacted, open vacuum system, be then warming up to 350 DEG C and carry out polycondensation reaction, reaction system pressure remains on below 100Pa, and the reaction time is 5h; After question response is complete, product, by bottom valve discharging, tank cooling, obtains the PET material of conductive zinc oxide compound; The PET material of obtained conductive zinc oxide compound is carried out melt spinning, thus prepares anlistatig light PET polyester electric conduction fibrous material.
Embodiment 4: by 100g ethylene glycol, 60g conductive zinc oxide Ti
0.1znO and 30g dispersant B YK184 is premix composition mixed liquor in proportion, uses nano-level grinder to carry out dispersion treatment, until add the hydroxylated surface modification that dressing agent polyethers carries out zinc oxide when the granularity D90 of solid particle reaches 100nm in mixed dispersion liquid; Obtained 190g conductive zinc oxide ethylene glycol dispersion liquid, 190g terephthalic acid (TPA), 7.5g2-diimide pyridine Co catalysts, 3.75g triphenyl phosphate stabilizing agent are added in polymerization reaction kettle and carries out esterification, the airtight rear nitrogen replacement of reactor 2 times, wherein reactor pressure is 1MPa, temperature is 250 DEG C, and reaction time of esterification is 3 hours; After having reacted, open vacuum system, be then warming up to 350 DEG C and carry out polycondensation reaction, reaction system pressure remains on below 100Pa, and the reaction time is 5h; After question response is complete, product, by bottom valve discharging, tank cooling, obtains the PET material of conductive zinc oxide compound; The PET material of obtained conductive zinc oxide compound is carried out melt spinning, thus prepares anlistatig light PET polyester electric conduction fibrous material.
Embodiment 5: by 100g ethylene glycol, 60g conductive zinc oxide Ga
0.01the modest 904S of ZnO and 30g dispersant moral is premix composition mixed liquor in proportion, nano-level grinder is used to carry out dispersion treatment, until add the hydroxylated surface modification that dressing agent polyethylene glycol carries out zinc oxide when the granularity D90 of solid particle reaches 100nm in mixed dispersion liquid; Obtained 190g conductive zinc oxide ethylene glycol dispersion liquid, 190g terephthalic acid (TPA), 7.5g imvite/niobium chloride catalyst, 3.75g triethyl phosphate stabilizing agent are added in polymerization reaction kettle and carries out esterification, the airtight rear nitrogen replacement of reactor 2 times, wherein reactor pressure is 1MPa, temperature is 250 DEG C, and reaction time of esterification is 3 hours; After having reacted, open vacuum system, be then warming up to 350 DEG C and carry out polycondensation reaction, reaction system pressure remains on below 100Pa, and the reaction time is 5h; After question response is complete, product, by bottom valve discharging, tank cooling, obtains the PET material of conductive zinc oxide compound; The PET material of obtained conductive zinc oxide compound is carried out melt spinning, thus prepares anlistatig light PET polyester electric conduction fibrous material.
Embodiment 6: by 100g ethylene glycol, 60g conductive zinc oxide Ga
0.1znO and 30g dispersant MOK5032 is premix composition mixed liquor in proportion, uses nano-level grinder to carry out dispersion treatment, until add the hydroxylated surface modification that dressing agent polyethylene glycol carries out zinc oxide when the granularity D90 of solid particle reaches 100nm in mixed dispersion liquid; Obtained 190g conductive zinc oxide ethylene glycol dispersion liquid, 190g terephthalic acid (TPA), 7.5g methylaluminoxane catalyst, the agent of 3.75g phosphoric acid stabilize are added in polymerization reaction kettle and carries out esterification, the airtight rear nitrogen replacement of reactor 2 times, wherein reactor pressure is 1MPa, temperature is 250 DEG C, and reaction time of esterification is 3 hours; After having reacted, open vacuum system, be then warming up to 350 DEG C and carry out polycondensation reaction, reaction system pressure remains on below 100Pa, and the reaction time is 5h; After question response is complete, product, by bottom valve discharging, tank cooling, obtains the PET material of conductive zinc oxide compound; The PET material of obtained conductive zinc oxide compound is carried out melt spinning, thus prepares anlistatig light PET polyester electric conduction fibrous material.
Claims (6)
1. the preparation method based on the light PET polyester electric conduction fiber of conductive zinc oxide, it is characterized in that, by introducing esterification-polycondensating process, the high concentration conductive zinc oxide ethylene glycol dispersion liquid prepared and terephthalic acid (TPA) are prepared light PET polyester electric conduction fiber, this technique comprises the steps:
A. by ethylene glycol, conductive zinc oxide and dispersant premix composition mixed liquor in proportion, nano-level grinder is used to carry out dispersion treatment, until add the hydroxylated surface modification that dressing agent carries out zinc oxide when the granularity D90 of solid particle reaches 100nm in mixed dispersion liquid;
B. conductive zinc oxide ethylene glycol dispersion liquid obtained for step a, terephthalic acid (TPA), catalyst, stabilizing agent are added in polymerization reaction kettle and carry out esterification, the airtight rear nitrogen replacement of reactor 2 times, wherein, the mass ratio of conductive zinc oxide ethylene glycol dispersion liquid, terephthalic acid (TPA), catalyst, stabilizing agent is 1 ~ 2:2:0.001 ~ 0.1:0.0005 ~ 0.05, reactor pressure is 0.2 ~ 1MPa, temperature is 200 ~ 250 DEG C, and reaction time of esterification is 1 ~ 3 hour;
C. after step b has reacted, open vacuum system, then heat up and carry out polycondensation reaction, wherein temperature is 270 ~ 350 DEG C, and reaction system pressure remains on below 100Pa, and the reaction time is 2 ~ 5 hours;
D., after step c reacts completely, product, by bottom valve discharging, tank cooling, obtains the PET material of conductive zinc oxide compound;
The PET material of the conductive zinc oxide compound e. steps d obtained carries out melt spinning, thus prepares anlistatig light PET polyester electric conduction fibrous material.
2. the preparation method of a kind of PET polyester electric conduction fiber based on conductive zinc oxide according to claim 1, it is characterized in that, in step a, described dispersant is one in BYK190, BYK106, BYK182, BYK184, moral modest 904S, MOK5032 or its combination, and wherein the mass ratio of ethylene glycol, conductive zinc oxide and dispersant is 1:(0.3 ~ 0.6): (0.05 ~ 0.3).
3. the preparation method of a kind of PET polyester electric conduction fiber based on conductive zinc oxide according to claim 1, is characterized in that, in step a, described conductive zinc oxide is the zinc oxide Al of aluminium doping
xznO, titanium doped zinc oxide Ti
xthe zinc oxide Ga of ZnO, gallium doping
xznO, wherein 0.01≤x≤0.1.
4. the preparation method of a kind of PET polyester electric conduction fiber based on conductive zinc oxide according to claim 1, is characterized in that, in step a, described dressing agent is one in silane coupler, titanate coupling agent, polyethylene glycol or polyethers or its combination.
5. the preparation method of a kind of PET polyester electric conduction fiber based on tin-antiomony oxide according to claim 1, it is characterized in that, in step b, described catalyst material is, the one in cobalt acetate, antimonous oxide, 2 diimide pyridine irons, 2 diimide pyridine cobalts, imvite/niobium chloride or methylaluminoxane or its combination.
6. the preparation method of a kind of PET polyester electric conduction fiber based on tin-antiomony oxide according to claim 1, it is characterized in that, in step b, described stabilizing agent is one in trimethyl phosphate, polyvinyl alcohol, phosphoric acid, triphenyl phosphate or triethyl phosphate or its combination.
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| CN109097857A (en) * | 2018-08-21 | 2018-12-28 | 随月丽 | A kind of preparation method of rare earth cladded type conducting PET fiber |
| CN113430674A (en) * | 2021-07-20 | 2021-09-24 | 上海水星家用纺织品股份有限公司 | Low-sensitization polyester fiber and preparation method thereof |
| CN113430674B (en) * | 2021-07-20 | 2022-06-21 | 上海水星家用纺织品股份有限公司 | Low-sensitization polyester fiber and preparation method thereof |
| CN115353614A (en) * | 2022-08-30 | 2022-11-18 | 科泽新材料股份有限公司 | Composite catalyst, preparation method thereof and application thereof in antimony-free polyester synthesis |
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