CN1670087A - Method for dispersing nano stibium doped tin oxide in glycol - Google Patents

Method for dispersing nano stibium doped tin oxide in glycol Download PDF

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Publication number
CN1670087A
CN1670087A CN 200510024671 CN200510024671A CN1670087A CN 1670087 A CN1670087 A CN 1670087A CN 200510024671 CN200510024671 CN 200510024671 CN 200510024671 A CN200510024671 A CN 200510024671A CN 1670087 A CN1670087 A CN 1670087A
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Prior art keywords
ato
ball
ethylene glycol
dispersion agent
powder
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CN 200510024671
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CN1290939C (en
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邵玮
陈晓蕾
李春忠
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East China University of Science and Technology
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East China University of Science and Technology
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Publication of CN1290939C publication Critical patent/CN1290939C/en
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Abstract

The invention relates to the method for dispersing ATO in glycol which mainly comprises, aqueous phase ball grinding the nano ATO powder with dispersing agent under the condition of pH=5-9, then carrying out ball grinding in ethylene alcohol under the condition of pH=7-9. The obtained nano ATO/ethylene alcohol organic slurry has not only fine dispersity but also good stability.

Description

Nano stibium doped tin oxide is dispersing method in ethylene glycol
Technical field
The present invention relates to a kind of nano stibium doped tin oxide (ATO) dispersing method in organic solvent, specifically, relate to a kind of nano ATO dispersing method in ethylene glycol.
Background technology
Terylene has excellent properties such as high strength, high-modulus, high resilience, antifriction scrape along be acidproof, has obtained widespread use.But the terylene water-absorbent is poor, very easily produces static and is difficult to loss, and under general state, the ratio resistance of terylene is 10 14More than the Ω cm, friction voltage is greater than 1000 volts, and electrostatic half-life was several hours, even several days.The electrostatic problem of terylene has directly had influence on the security of production, processing and the application of terylene textiles, has restricted the development of terylene to the high-grade application field.
The electroconductibility of nano stibium doped tin oxide (ATO) is not subjected to the restriction of environment humidity, has avoided organic antistatic agents to rely on the shortcoming of environment, has therefore represented wide application prospect in fields such as electronics, plastics, coating.The original position of nano ATO and PET dacron polyester is compound, makes the ATO particle can really reach nanoscale and disperses, and its transmitance to visible light is increased, and transparency increases, thereby outward appearance, the color and luster of polyester do not exerted an influence; ATO particle nanoscale disperses, and its specific surface area is increased, and forms the conduction network chain, and the nanoscale dispersed particles will improve significantly to the mechanical property of polyester material; In addition, the compound one side of original position has solved terylene anti-static function persistent problem, has avoided the later stage antistatic finish process of terylene on the other hand, has reduced making link, has reduced cost.
Summary of the invention
The original position that realizes nano ATO and PET is compound, and nano ATO homodisperse in ethylene glycol is crucial.How nano ATO is evenly dispersed in and just becomes the technical issues that need to address of the present invention in the ethylene glycol.
The said nano ATO of the present invention dispersing method in ethylene glycol comprises the steps:
(1) nano ATO powder, dispersion agent and deionized water are placed ball grinder, the consumption of dispersion agent is a nano ATO weight 0.1~2.5%, is ball milling 24~72 hours under 5~9 conditions at pH, and gained ball milling slurry is in 90~120 ℃ of dryings and grind to form powder;
(2) will be by step (1) gained place a container that has whipping appts through the ATO of water ball-milling processing powder, ethylene glycol and dispersion agent, through the ATO of water ball-milling processing powder consumption is that the consumption of ethylene glycol weight 5~30%, dispersion agent is for through the ATO of water ball-milling processing powder weight 0.1~2.5%, at pH is to stir under 7~9 conditions 2~6 hours, and moving in the ball grinder more then, ball milling can obtain ATO/ ethylene glycol organic ink in 24~72 hours;
Wherein: described nano ATO powder adopts existing liquid-phase precipitation method to be prepared from, and does not repeat them here.
Said dispersion agent is an organosilicon compound, as (but being not limited to) aminopropyl triethoxysilane (HK550), glycidyl ether oxygen propyl trimethoxy silicane (HK560), methacryloxypropyl trimethoxy silicon (HK570) or/and 2-aminoethyl-aminopropyl trimethoxysilane (HK792).
The present invention successfully is scattered in the nano ATO powder in the ethylene glycol, and the nano ATO of gained/ethylene glycol organic ink not only has excellent dispersiveness but also has satisfactory stability, lays a good foundation for the original position of nano ATO powder and PET is compound.
Description of drawings
Fig. 1 is the Electronic Speculum figure of nano ATO/ethylene glycol organic ink of making by embodiment 2 described methods.
Fig. 2 is the Electronic Speculum figure of nano ATO/ethylene glycol organic ink of making by embodiment 5 described methods.
Embodiment
The present invention is further elaborated below by embodiment, and its purpose only is can better understand content of the present invention and unrestricted protection scope of the present invention:
Embodiment 1
The 100ml deionized water is poured in the 300ml ball grinder, added 20g nano ATO powder, 0.1g dispersion agent KH560, dispersed with stirring is regulated pH value to 9.21 with 1: 1 ammoniacal liquor dilute solution.280g zirconium pearl is added ball grinder, and the ball milling time is 72 hours.Take off ball grinder, pour out slurry, elimination zirconium pearl 110 ℃ of oven dry, is ground water slurry, obtains the 18gATO powder.
Add the 90ml ethylene glycol solution in the 150ml beaker, stir with the high speed electromagnetic stirrer, add the ATO powder that 15g handles through water, 0.075g KH560 regulates pH value to 9.38 with 1: 1 ammoniacal liquor dilute solution, and high speed electromagnetic stirred 3 hours, rotating speed 1820r/min.Mixed solution is poured in the ball grinder, added zirconium pearl 250g, be put on the ball mill ball milling 48 hours.Elimination zirconium pearl obtains nano ATO/ethylene glycol organic ink.
Embodiment 2
The 100ml deionized water is poured in the 300ml ball grinder, added 20g nano ATO powder, 0.1g dispersion agent KH570, dispersed with stirring is regulated pH value to 9.42 with 1: 1 ammoniacal liquor dilute solution.280g zirconium pearl is added ball grinder, and the ball milling time is 72 hours.Take off ball grinder, pour out slurry, elimination zirconium pearl 110 ℃ of oven dry, is ground water slurry, obtains the 17.5gATO powder.
In the 150ml glass beaker, add the 90ml ethylene glycol solution, stir, add the ATO powder that 15g handles through water with the high speed electromagnetic stirrer, 0.075g KH570, regulate pH value to 9.54 with 1: 1 ammoniacal liquor dilute solution, high speed electromagnetic stirred 3 hours, rotating speed 1820r/min.Mixed solution is poured in the ball grinder, added zirconium pearl 250g, be put on the ball mill ball milling 48 hours.Elimination zirconium pearl obtains nano ATO/ethylene glycol organic ink, and its Electronic Speculum figure as shown in Figure 1.
Embodiment 3
The 100ml deionized water is poured in the 300ml ball grinder, added 20g nano ATO powder, 0.1g dispersion agent KH550, dispersed with stirring is regulated pH value to 9.58 with 1: 1 ammoniacal liquor dilute solution.280g zirconium pearl is added ball grinder, and the ball milling time is 72 hours.Take off ball grinder, pour out slurry, elimination zirconium pearl 110 ℃ of oven dry, is ground water slurry, obtains the 18.2gATO powder.
In the 150ml glass beaker, add the 90ml ethylene glycol solution, stir, add the ATO powder that 15g handles through water with the high speed electromagnetic stirrer, 0.15g KH550, regulate pH value to 9.45 with 1: 1 ammoniacal liquor dilute solution, high speed electromagnetic stirred 3 hours, rotating speed 1820r/min.Mixed solution is poured in the ball grinder, added zirconium pearl 250g, be put on the ball mill ball milling 48 hours.Elimination zirconium pearl obtains nano ATO/ethylene glycol organic ink.
Embodiment 4
The 100ml deionized water is poured in the 300ml ball grinder, added 20g nano ATO powder, 0.1g dispersion agent KH792, dispersed with stirring is regulated pH value to 9.34 with 1: 1 ammoniacal liquor dilute solution.280g zirconium pearl is added ball grinder, and the ball milling time is 60 hours.Take off ball grinder, pour out slurry, elimination zirconium pearl 110 ℃ of oven dry, is ground water slurry, obtains the 18.4gATO powder.
In the 150ml glass beaker, add the 90ml ethylene glycol solution, stir, add the ATO powder that 15g handles through water with the high speed electromagnetic stirrer, 0.15g KH792, regulate pH value to 9.46 with 1: 1 ammoniacal liquor dilute solution, high speed electromagnetic stirred 3 hours, rotating speed 2920 commentaries on classics/min.Mixed solution is poured in the ball grinder, added zirconium pearl 250g, be put on the ball mill ball milling 48 hours.Elimination zirconium pearl obtains nano ATO/ethylene glycol organic ink.
Embodiment 5
The 100ml deionized water is poured in the 300ml ball grinder, added 20g nano ATO powder, 0.1g dispersion agent KH570, dispersed with stirring is regulated pH value to 9.43 with 1: 1 ammoniacal liquor dilute solution.280g zirconium pearl is added ball grinder, and the ball milling time is 60 hours.Take off ball grinder, pour out slurry, elimination zirconium pearl 110 ℃ of oven dry, is ground water slurry, obtains the 18.9gATO powder.
In the 150ml glass beaker, add the 90ml ethylene glycol solution, stir, add the ATO powder that 15g handles through water with the high speed electromagnetic stirrer, 0.2g KH570, regulate pH value to 9.28 with 1: 1 ammoniacal liquor dilute solution, high speed electromagnetic stirred 3 hours, rotating speed 2920 commentaries on classics/min.Mixed solution is poured in the ball grinder, added zirconium pearl 250g, be put on the ball mill ball milling 48 hours.Elimination zirconium pearl obtains nano ATO/ethylene glycol organic ink, and its Electronic Speculum figure as shown in Figure 2.
Embodiment 6
The 100ml deionized water is poured in the 300ml ball grinder, added 20g nano ATO powder, 0.1g dispersion agent KH570, dispersed with stirring is regulated pH value to 9.56 with 1: 1 ammoniacal liquor dilute solution.280g zirconium pearl is added ball grinder, and the ball milling time is 60 hours.Take off ball grinder, pour out slurry, elimination zirconium pearl 110 ℃ of oven dry, is ground water slurry, obtains the 19.0gATO powder.
Add the 90ml ethylene glycol solution in the 150ml glass beaker, stir with the high speed electromagnetic stirrer, add the ATO powder that 15g handles through water, 0.15g KH570 regulates the pH value extremely with 1: 1 ammoniacal liquor dilute solution, and high speed electromagnetic stirred 3 hours, rotating speed 1820r/min.Mixed solution is poured in the ball grinder, added zirconium pearl 250g, be put on the ball mill ball milling 60 hours.Elimination zirconium pearl obtains nano ATO/ethylene glycol organic ink.

Claims (2)

1, a kind of nano stibium doped tin oxide dispersing method in ethylene glycol, it comprises the steps:
(1) nano ATO powder, dispersion agent and deionized water are placed ball grinder, the consumption of dispersion agent is a nano ATO weight 0.1~2.5%, is ball milling 24~72 hours under 5~9 conditions at pH, and gained ball milling slurry is in 90~120 ℃ of dryings and grind to form powder;
(2) will be by step (1) gained place a container that has whipping appts through the ATO of water ball-milling processing powder, ethylene glycol and dispersion agent, through the ATO of water ball-milling processing powder consumption is that the consumption of ethylene glycol weight 5~30%, dispersion agent is for through the ATO of water ball-milling processing powder weight 0.1~2.5%, at pH is to stir under 7~9 conditions 2~6 hours, and moving in the ball grinder more then, ball milling can obtain ATO/ ethylene glycol organic ink in 24~72 hours;
Wherein: said dispersion agent is an organosilicon compound.
2, dispersing method as claimed in claim 1, it is characterized in that wherein said dispersion agent is that aminopropyl triethoxysilane, glycidyl ether oxygen propyl trimethoxy silicane, methacryloxypropyl trimethoxy silicon are or/and 2-aminoethyl-aminopropyl trimethoxysilane.
CN 200510024671 2005-03-25 2005-03-25 Method for dispersing nano stibium doped tin oxide in glycol Expired - Fee Related CN1290939C (en)

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CN1290939C CN1290939C (en) 2006-12-20

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1876289B (en) * 2006-07-12 2010-12-22 华东理工大学 Method for preparing antimony doped stannic oxide nanometer electricity-conductive powder
CN101245217B (en) * 2007-11-30 2011-04-06 东南大学 Stibium doping nano-tin dioxide unsaturated polyester resin heat insulating coating film and manufacture method thereof
CN101219859B (en) * 2007-11-30 2011-09-28 华南理工大学 Nano-oiliness ATO heat-insulating slurry, production method and uses thereof
CN101235132B (en) * 2008-01-10 2012-03-21 华东理工大学 Modified method for preparing polyester resin containing stibium doping tin dioxide nano particles
CN102492317A (en) * 2011-10-17 2012-06-13 大连交通大学 Antimony-doped tin oxide slurry and preparation method thereof
CN103275521A (en) * 2013-06-18 2013-09-04 浙江大学 Preparation method of nano tin antimony oxide water-based slurry
CN110003685A (en) * 2019-04-15 2019-07-12 广西大学 A kind of preparation method of antimony-doped stannic oxide nano pulp

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1876289B (en) * 2006-07-12 2010-12-22 华东理工大学 Method for preparing antimony doped stannic oxide nanometer electricity-conductive powder
CN101245217B (en) * 2007-11-30 2011-04-06 东南大学 Stibium doping nano-tin dioxide unsaturated polyester resin heat insulating coating film and manufacture method thereof
CN101219859B (en) * 2007-11-30 2011-09-28 华南理工大学 Nano-oiliness ATO heat-insulating slurry, production method and uses thereof
CN101235132B (en) * 2008-01-10 2012-03-21 华东理工大学 Modified method for preparing polyester resin containing stibium doping tin dioxide nano particles
CN102492317A (en) * 2011-10-17 2012-06-13 大连交通大学 Antimony-doped tin oxide slurry and preparation method thereof
CN103275521A (en) * 2013-06-18 2013-09-04 浙江大学 Preparation method of nano tin antimony oxide water-based slurry
CN103275521B (en) * 2013-06-18 2014-11-26 浙江大学 Preparation method of nano tin antimony oxide water-based slurry
CN110003685A (en) * 2019-04-15 2019-07-12 广西大学 A kind of preparation method of antimony-doped stannic oxide nano pulp
CN110003685B (en) * 2019-04-15 2021-01-05 广西大学 Preparation method of antimony-doped tin dioxide nano slurry

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