CN105350107B - A kind of preparation method of the light PET polyester electric conductions fiber based on conductive zinc oxide - Google Patents
A kind of preparation method of the light PET polyester electric conductions fiber based on conductive zinc oxide Download PDFInfo
- Publication number
- CN105350107B CN105350107B CN201510686002.5A CN201510686002A CN105350107B CN 105350107 B CN105350107 B CN 105350107B CN 201510686002 A CN201510686002 A CN 201510686002A CN 105350107 B CN105350107 B CN 105350107B
- Authority
- CN
- China
- Prior art keywords
- zinc oxide
- conductive zinc
- conductive
- ethylene glycol
- dispersion liquid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Polyesters Or Polycarbonates (AREA)
- Artificial Filaments (AREA)
Abstract
The present invention discloses a kind of preparation method of the light PET polyester electric conductions fiber based on conductive zinc oxide, by preparing high concentration conductive zinc oxide ethylene glycol dispersion liquid, the hydroxylated surface modification that dressing agent carries out zinc oxide is added when its granularity D90 is in below 100nm, then terephthalic acid (TPA), conductive zinc oxide ethylene glycol dispersion liquid, catalyst, stabilizer are added in polymerization reaction kettle using esterifying polycondensation technique, so as to prepare the high PET Polyester Fibers of electric conductivity.Conducting particles zinc oxide in conductive fiber prepared by this method is uniformly dispersed, and the conductance of fiber is significantly improved.
Description
Technical field
The present invention relates to a kind of preparation method of the light PET polyester electric conductions fiber based on conductive zinc oxide.
Background technology
PET（PET）Application of the fiber in weaving and industrial circle widely, but polyester
The hydrophobicity and insulating properties of fiber are very poor, cause it easily to accumulate electrostatic in dry environments.And static discharge is not only to human body
It is harmful, and the kindling material of imflammable gas or dust can be turned into and set off an explosion and fire.To prevent electrostatic from causing various disasters,
Industrial quarters typically adheres to or deposited height in common PET polyester fibre surface using compound or co-blended spinning method and post treatment method and leads
Electric component prepares PET polyester electric conduction fibers.
In the compound or co-blended spinning preparation method of PET polyester electric conduction fibers, by conductive fill powder（Carbon black, metal
Or metal oxide etc.）It is dispersed in by melt blending in PET polyester fondants, prepared conductive fiber has preferable conductive
Durability.But, the higher conductive powder body of the content of addition, its particle agglomeration is than more serious, and particle diameter is larger, and this can not only make to gather
Ester material spinnability is deteriorated, and also results in polyester fiber intensity and be decreased obviously.
The present invention is based on zinc oxide conductive component, by introducing esterification-polycondensating process by the conductive oxygen of the high concentration prepared
Change zinc ethylene glycol dispersion liquid with terephthalic acid (TPA) to prepare light PET polyester electric conductions fiber.In conductive fiber prepared by this method
Conducting particles be uniformly dispersed, realize individual particle disperse, the dispersion particle diameter in PET between 30-100nm, fiber
Conductance and fibre strength are significantly improved.
The content of the invention
It is an object of the invention to break through at present using conductive component in melt spinning method preparation process in fibrous inside
Grain is reunited than more serious, and particle diameter is larger, and this can not only make polyester material spinnability be deteriorated, and also result in polyester fiber intensity
The shortcoming being decreased obviously, is dispersed in PET polyester fondants by melt blending, and prepared conductive fiber has preferable conductive
Durability.
To reach above-mentioned expected purpose, the present invention is adopted the following technical scheme that:
A kind of preparation method of the light PET polyester electric conductions fiber based on conductive zinc oxide, it is characterised in that by introducing
The high concentration conductive zinc oxide ethylene glycol dispersion liquid prepared and terephthalic acid (TPA) are prepared light PET by esterification-polycondensating process
Polyester electric conduction fiber, the technique comprises the following steps：
A. ethylene glycol, conductive zinc oxide and dispersant are premixed into composition mixed liquor in proportion, carried out using nano-level grinder
Decentralized processing, until adding the hydroxyl that dressing agent carries out zinc oxide when the granularity D90 of solid particle reaches 100nm in mixed dispersion liquid
Base surface is modified；
B. conductive zinc oxide ethylene glycol dispersion liquid, terephthalic acid (TPA), catalyst, stabilizer made from step a are added poly-
Close and esterification is carried out in reactor, nitrogen displacement is used 2 times after reactor is closed, wherein, conductive zinc oxide ethylene glycol dispersion liquid,
Terephthalic acid (TPA), catalyst, the mass ratio of stabilizer are 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. step b reaction after the completion of, open vacuum system, then heating carry out polycondensation reaction, wherein temperature be 270~
350 DEG C, reaction system pressure is maintained at 100 below Pa, and the reaction time is 2~5 h；
D. after after step c reactions completely, product is discharged by bottom valve, tank cooling, produce what conductive zinc oxide was combined
PET material；
E. PET material conductive zinc oxide made from step d being combined carries out melt spinning, so as to prepare anlistatig
Light PET polyester electric conductions fibrous material.
In step a, described dispersant is in BYK190, BYK106, BYK182, BYK184, moral modest 904S, MOK5032
One kind or its combination, wherein the mass ratio of ethylene glycol, conductive zinc oxide and dispersant be 1:(0.3~0.6):(0.05~
0.3)。
In step a, described conductive zinc oxide is the zinc oxide Al that aluminium adulteratesxZnO, titanium doped zinc oxide TixZnO, gallium
The zinc oxide Ga of dopingxZnO, wherein 0.01≤x≤0.1.
In step a, described dressing agent is one kind in silane coupler, titanate coupling agent, polyethylene glycol or polyethers
Or its combination.
In step b, described catalyst material is that cobalt acetate, antimony oxide, 2- diimides pyridine iron, 2- are double sub-
Amido pyridine cobalt, montmorillonite/niobium chloride or one kind in MAO or its combination.
In step b, described stabilizer is trimethyl phosphate, polyvinyl alcohol, phosphoric acid, triphenyl phosphate or triethyl group phosphoric acid
One kind or its combination in ester.
The high concentration conductive zinc oxide ethylene glycol dispersion liquid prepared and terephthalic acid (TPA) are carried out being esterified-polycondensation by the present invention
React to prepare light PET polyester electric conductions fiber.With the present invention be prepared product --- PET polyester electric conduction fibers overcome
The shortcomings of conductive easy reunion, fibre strength are reduced in conventional spinning method, has the advantages that continuously prepare, energy relatively low with cost
It is enough to be applied in field of textile industry.
Embodiment
The details realized below by instantiation to the present invention is described, but protection scope of the present invention is not limited to
These embodiments.
Embodiment 1：By 100g ethylene glycol, 30g conductive zinc oxides Al0.01ZnO and 5g dispersant Bs YK190 is premixed in proportion
Mixed liquor is constituted, decentralized processing is carried out using nano-level grinder, until the granularity D90 of solid particle reaches in mixed dispersion liquid
The hydroxylated surface modification that dressing agent silane coupler carries out zinc oxide is added during 100nm；By obtained 135g conductive zinc oxides
Ethylene glycol dispersion liquid, 270g terephthalic acid (TPA)s, 0.135g acetic acid Co catalysts, 0.0675g tripotassium phosphates ester stabilizer add poly-
Close and esterification is carried out in reactor, nitrogen displacement is used 2 times after reactor is closed, wherein reactor pressure is 0.2MPa, temperature
For 200 DEG C, reaction time of esterification is 1 hour；After the completion of reaction, vacuum system is opened, 270 DEG C of progress polycondensations are then heated to anti-
Should, reaction system pressure is maintained at 100 below Pa, and the reaction time is 2h；After question response is complete, product discharged by bottom valve,
Tank is cooled down, and produces the compound PET material of conductive zinc oxide；The PET material that obtained conductive zinc oxide is combined is melted
Spinning, so as to prepare anlistatig light PET polyester electric conductions fibrous material.
Embodiment 2：By 100g ethylene glycol, 40g conductive zinc oxides Al0.1ZnO and 10g dispersant Bs YK106 is premixed in proportion
Mixed liquor is constituted, decentralized processing is carried out using nano-level grinder, until the granularity D90 of solid particle reaches in mixed dispersion liquid
The hydroxylated surface modification that dressing agent titanate coupling agent carries out zinc oxide is added during 100nm；By obtained 150g electric conductive oxidations
It is anti-that zinc ethylene glycol dispersion liquid, 200g terephthalic acid (TPA)s, 0.5g antimony oxides catalyst, 1g polyvinyl alcohol stabilizer add polymerization
Answer and esterification is carried out in kettle, use nitrogen displacement 2 times after reactor is closed, wherein reactor pressure is 0.5MPa, and temperature is 225
DEG C, reaction time of esterification is 2 hours；After the completion of reaction, vacuum system is opened, 300 DEG C of progress polycondensation reactions are then heated to, instead
System pressure is answered to be maintained at 100 below Pa, the reaction time is 3.5h；After question response is complete, product discharged by bottom valve,
Tank is cooled down, and produces the compound PET material of conductive zinc oxide；The PET material that obtained conductive zinc oxide is combined is melted
Spinning, so as to prepare anlistatig light PET polyester electric conductions fibrous material.
Embodiment 3：By 100g ethylene glycol, 60g conductive zinc oxides Ti0.01ZnO and 30g dispersant Bs YK182 is premixed in proportion
Mixed liquor is constituted, decentralized processing is carried out using nano-level grinder, until the granularity D90 of solid particle reaches in mixed dispersion liquid
The hydroxylated surface modification that dressing agent polyethylene glycol carries out zinc oxide is added during 100nm；By obtained 190g conductive zinc oxides second
Glycol dispersion liquid, 190g terephthalic acid (TPA)s, 7.5g 2- diimide pyridines iron catalyst, 3.75g phosphoric acid stabilizer add polymerization
Esterification is carried out in reactor, nitrogen displacement is used 2 times after reactor is closed, wherein reactor pressure is 1MPa, and temperature is 250
DEG C, reaction time of esterification is 3 hours；After the completion of reaction, vacuum system is opened, 350 DEG C of progress polycondensation reactions are then heated to, instead
System pressure is answered to be maintained at 100 below Pa, the reaction time is 5h；After question response is complete, product is discharged by bottom valve, tank
Cooling, produces the compound PET material of conductive zinc oxide；The PET material that obtained conductive zinc oxide is combined carries out melt spinning,
So as to prepare anlistatig light PET polyester electric conductions fibrous material.
Embodiment 4：By 100g ethylene glycol, 60g conductive zinc oxides Ti0.1ZnO and 30g dispersant Bs YK184 is premixed in proportion
Mixed liquor is constituted, decentralized processing is carried out using nano-level grinder, until the granularity D90 of solid particle reaches in mixed dispersion liquid
The hydroxylated surface modification that dressing agent polyethers carries out zinc oxide is added during 100nm；By obtained 190g conductive zinc oxides ethylene glycol
Dispersion liquid, 190g terephthalic acid (TPA)s, 7.5g 2- diimide pyridines Co catalysts, 3.75g triphenyl phosphates stabilizer add poly-
Close and esterification is carried out in reactor, use nitrogen displacement 2 times after reactor is closed, wherein reactor pressure is 1MPa, temperature is
250 DEG C, reaction time of esterification is 3 hours；After the completion of reaction, vacuum system is opened, 350 DEG C of progress polycondensations are then heated to anti-
Should, reaction system pressure is maintained at 100 below Pa, and the reaction time is 5h；After question response is complete, product discharged by bottom valve,
Tank is cooled down, and produces the compound PET material of conductive zinc oxide；The PET material that obtained conductive zinc oxide is combined is melted
Spinning, so as to prepare anlistatig light PET polyester electric conductions fibrous material.
Embodiment 5：By 100g ethylene glycol, 60g conductive zinc oxides Ga0.01The modest 904S of ZnO and 30g dispersant morals is pre- in proportion
Mixed composition mixed liquor, decentralized processing is carried out using nano-level grinder, until the granularity D90 of solid particle reaches in mixed dispersion liquid
The hydroxylated surface modification that dressing agent polyethylene glycol carries out zinc oxide is added during 100nm；By obtained 190g conductive zinc oxides second
Glycol dispersion liquid, 190g terephthalic acid (TPA)s, 7.5g montmorillonites/chlorination niobium catalytic, 3.75g triethyl phosphate stabilizers add
Enter and esterification is carried out in polymerization reaction kettle, nitrogen displacement is used 2 times after reactor is closed, wherein reactor pressure is 1MPa, temperature
Spend for 250 DEG C, reaction time of esterification is 3 hours；After the completion of reaction, vacuum system is opened, 350 DEG C of progress polycondensations are then heated to
Reaction, reaction system pressure is maintained at 100 below Pa, and the reaction time is 5h；After question response is complete, product is gone out by bottom valve
Material, tank cooling, produce the compound PET material of conductive zinc oxide；The PET material that obtained conductive zinc oxide is combined is carried out
Melt spinning, so as to prepare anlistatig light PET polyester electric conductions fibrous material.
Embodiment 6：By 100g ethylene glycol, 60g conductive zinc oxides Ga0.1ZnO and 30g dispersants MOK5032 is premixed in proportion
Mixed liquor is constituted, decentralized processing is carried out using nano-level grinder, until the granularity D90 of solid particle reaches in mixed dispersion liquid
The hydroxylated surface modification that dressing agent polyethylene glycol carries out zinc oxide is added during 100nm；By obtained 190g conductive zinc oxides second
Glycol dispersion liquid, 190g terephthalic acid (TPA)s, 7.5g MAOs catalyst, 3.75g phosphoric acid stabilizer add polymerization reaction kettle
Middle carry out esterification, nitrogen displacement is used 2 times after reactor is closed, and wherein reactor pressure is 1MPa, and temperature is 250 DEG C, ester
It is 3 hours to change the reaction time；After the completion of reaction, vacuum system is opened, 350 DEG C of progress polycondensation reactions, reactant are then heated to
It is that pressure is maintained at 100 below Pa, the reaction time is 5h；After question response is complete, product is discharged by bottom valve, tank is cold
But, the compound PET material of conductive zinc oxide is produced；The PET material that obtained conductive zinc oxide is combined carries out melt spinning, from
And prepare anlistatig light PET polyester electric conductions fibrous material.
Claims (1)
1. a kind of preparation method of the light PET polyester electric conductions fiber based on conductive zinc oxide, it is characterised in that by introducing ester
Change-polycondensating process gathers the high concentration conductive zinc oxide ethylene glycol dispersion liquid prepared with terephthalic acid (TPA) to prepare light PET
Ester conductive fiber, the technique comprises the following steps：
A. ethylene glycol, conductive zinc oxide and dispersant are premixed into composition mixed liquor in proportion, disperseed using nano-level grinder
Processing, until adding the hydroxylating that dressing agent carries out zinc oxide when the granularity D90 of solid particle reaches 100nm in mixed dispersion liquid
Surface is modified；
B. conductive zinc oxide ethylene glycol dispersion liquid, terephthalic acid (TPA), catalyst, stabilizer made from step a are added into polymerization anti-
Answer and esterification is carried out in kettle, with nitrogen displacement 2 times after reactor is closed, wherein, conductive zinc oxide ethylene glycol dispersion liquid, to benzene
Dioctyl phthalate, catalyst, the mass ratio of stabilizer are 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 the completion of step b reactions, vacuum system is opened, then heating carries out polycondensation reaction, and wherein temperature is 270~350 DEG C,
Reaction system pressure is maintained at 100 below Pa, and the reaction time is 2~5 hours；
D. after after step c reactions completely, product is discharged by bottom valve, tank cooling, the compound PET materials of conductive zinc oxide are produced
Material；
E. PET material conductive zinc oxide made from step d being combined carries out melt spinning, so as to prepare anlistatig light color
PET polyester electric conduction fibrous materials；
In step a, described dispersant is one in BYK190, BYK106, BYK182, BYK184, moral modest 904S, MOK5032
Plant or its combination, the wherein 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 that aluminium adulteratesxZnO, titanium doped zinc oxide TixZnO, gallium doping
Zinc oxide GaxZnO, wherein 0.01≤x≤0.1；
In step a, described dressing agent be one kind in silane coupler, titanate coupling agent, polyethylene glycol or polyethers or its
Combination；
In step b, described catalyst material is, cobalt acetate, antimony oxide, 2 diimide pyridine irons, 2 diimide pyrroles
Pyridine cobalt, montmorillonite/niobium chloride or one kind in MAO or its combination；
In step b, described stabilizer is in trimethyl phosphate, polyvinyl alcohol, phosphoric acid, triphenyl phosphate or triethyl phosphate
One kind or its combination.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510686002.5A CN105350107B (en) | 2015-10-22 | 2015-10-22 | A kind of preparation method of the light PET polyester electric conductions fiber based on conductive zinc oxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510686002.5A CN105350107B (en) | 2015-10-22 | 2015-10-22 | A kind of preparation method of the light PET polyester electric conductions fiber based on conductive zinc oxide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105350107A CN105350107A (en) | 2016-02-24 |
| CN105350107B true CN105350107B (en) | 2017-08-25 |
Family
ID=55326163
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510686002.5A Active CN105350107B (en) | 2015-10-22 | 2015-10-22 | A kind of preparation method of the light PET polyester electric conductions fiber based on conductive zinc oxide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105350107B (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106065498A (en) * | 2016-06-04 | 2016-11-02 | 江苏启弘新材料科技有限公司 | The preparation method of antistatic fibre based on point discharge effect |
| CN108624980A (en) * | 2017-03-24 | 2018-10-09 | 中国石化仪征化纤有限责任公司 | A kind of conducting PET fiber and preparation method thereof |
| CN108018617B (en) * | 2017-12-06 | 2020-06-23 | 杭州皮克新材料科技有限公司 | Preparation method of moisture-absorbing antistatic polyester |
| CN109097857A (en) * | 2018-08-21 | 2018-12-28 | 随月丽 | A kind of preparation method of rare earth cladded type conducting PET fiber |
| 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 |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102816312B (en) * | 2011-06-10 | 2014-08-06 | 中国石油天然气股份有限公司 | Preparation method of antistatic polyethylene glycol terephthalate |
| CN102330189A (en) * | 2011-06-21 | 2012-01-25 | 江苏鹰翔化纤股份有限公司 | Preparation method of nano-tin dioxide modified polyester fiber |
| CN102345178A (en) * | 2011-06-21 | 2012-02-08 | 江苏鹰翔化纤股份有限公司 | Preparation method of nano silver oxide modified polyester fiber |
| CN103361765B (en) * | 2012-03-30 | 2015-04-29 | 浙江恒逸高新材料有限公司 | Anti-static modified polyester staple fiber and preparation method thereof |
-
2015
- 2015-10-22 CN CN201510686002.5A patent/CN105350107B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN105350107A (en) | 2016-02-24 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105350107B (en) | A kind of preparation method of the light PET polyester electric conductions fiber based on conductive zinc oxide | |
| CN107768663B (en) | Method for preparing transition metal oxide having oxygen defect | |
| CN103774265B (en) | A kind of anti-bacterial fibre and preparation method thereof | |
| CN104909365B (en) | Bitumen ball aoxidizes nonfused promotion method | |
| CN101302580B (en) | Preparation of all-sefstromite concentrate pellet ore | |
| CN108299653A (en) | Phosphorus-nitrogen flame retardant functionalization graphene and preparation method thereof | |
| CN108786780A (en) | A kind of nano combined Zn2TiO4The preparation method of functional material and its dispersion liquid | |
| CN107266711A (en) | Graphene oxide hybrid fire retardant and preparation method thereof | |
| CN101613265A (en) | A kind of processing method of producing Zinic stearas | |
| CN108503804A (en) | A kind of method of grapheme material modified poly ester master batch and grapheme material modified poly ester master batch therefrom and application | |
| CN104183852B (en) | Phenolic resin-graphite-graphene composite battery bipolar grid plate and preparation method thereof | |
| CN107201572A (en) | A kind of preparation method of automatically cleaning polyester and its fiber | |
| CN109772342A (en) | A kind of preparation method of hydrogenation of carbon dioxide methanol catalyst | |
| CN108455902B (en) | Preparation method of flame-retardant artificial stone containing nano perovskite oxide | |
| CN110498411B (en) | Modified graphene oxide and processing technology | |
| CN107383620A (en) | A kind of polypropylene fire retardant mastre batch and preparation method thereof | |
| CN101851007A (en) | Tungsten-molybdenum-based superfine composite oxide solid solution and preparation method thereof | |
| CN105778440A (en) | Environment-friendly pbt material and preparing method thereof | |
| CN104258866A (en) | Preparation method and application of microwave catalyst | |
| CN106882826A (en) | A kind of preparation method of flame retardant of magnesium hydroxide | |
| CN109880369A (en) | A kind of nano-TiO2Composite material and preparation method | |
| CN108408709A (en) | A kind of preparation process of pollution-free inexpensive iron manganese phosphate for lithium crystalline material | |
| CN105762342A (en) | Graphene microchip/lithium iron phosphate compound positive pole material and preparation method thereof | |
| CN106554031A (en) | A kind of preparation method and flame retardant of magnesium hydroxide of flame retardant of magnesium hydroxide | |
| CN105950001A (en) | Polysilane modified thin film coating and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |