CN105970323B - A kind of antistatic powder and preparation method thereof - Google Patents
A kind of antistatic powder and preparation method thereof Download PDFInfo
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- CN105970323B CN105970323B CN201610292820.1A CN201610292820A CN105970323B CN 105970323 B CN105970323 B CN 105970323B CN 201610292820 A CN201610292820 A CN 201610292820A CN 105970323 B CN105970323 B CN 105970323B
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/09—Addition of substances to the spinning solution or to the melt for making electroconductive or anti-static filaments
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/92—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters
Abstract
The invention discloses a kind of antistatic powder and preparation method thereof, and in particular to a kind of aluminium-doped zinc oxide powder and preparation method thereof, wherein the molar ratio of aluminium and zinc is in aluminium-doped zinc oxide powder（0.5~2）∶100.Preparation process of the present invention is simple, and production cost is low, available for large-scale production.Aluminium-doped zinc oxide powder prepared by the present invention is of light color, environment-protecting and non-poisonous, particle size is small and dispersion performance is good, and powder volume resistivity is 104Ω cm, available for the antistatic effect that polyester fiber is improved in polyester fiber, expand the application range of polyester product.
Description
Technical field
The invention belongs to zinc oxide conductive powder material technical field, and in particular to a kind of zinc oxide of aluminium doping is antistatic
Powder and preparation method thereof.
Background technology
With the fast development of electronics industry, electronic equipment easily accumulates a large amount of electrostatic under some working environments
Lotus, hinders the normal work of electronic device even to destroy some components, threatens the health of operating personnel.Doping zinc-oxide is led
Electric powder as plastics, coating, fiber and other material a kind of functional filler, the property such as its is antistatic, electromagnetic shielding can be assigned
Can, cause the extensive concern of people.
Zinc oxide is a kind of typical semi-conducting material, its energy gap at room temperature is 3.4eV, and activation can be
60meV, is wide band gap semiconducter.In order to improve the electric conductivity of zinc oxide, common group iii elements and column IV element carry out it
Prepared by doping, such as silicon, germanium, boron, aluminium, gallium, indium, tin, and the most notable with the doping effect of aluminium, indium, gallium.Although aluminium, indium and
The high-valency metals such as gallium can be successfully incorporated into zinc oxide lattice by certain method, but relative to the rare gold of both indium and gallium
Belong to, storage capacity of the aluminium in the earth's crust more horn of plenty, price is more cheap, and the whiteness of powder is high.Existing preparation method ratio
Such as：
Synthesize zinc nitrate-urea leucosol microemulsion, filtered after standing, aluminum nitrate is added in filtrate and forms zinc nitrate
Aluminium mixed liquor, configures sodium carbonate liquor, with the double instillation polyvinyl alcohol water solutions of zinc nitrate aluminum solutions, synthesizing white precipitate forerunner
Body, stands filtering, filter cake elutes through deionized water, dries, being ground up, sieved, calcine after obtain aluminum-doped zinc oxide nanometer powder；
Or zinc acetate and aluminum nitrate are put into beaker, the mixed solution of ethylene glycol monomethyl ether and monoethanolamine is added, is stirred by magnetic force
Mix and be made into uniform colloidal sol, xerogel is obtained after dry, grinding obtains dry gel powder, i.e. hydro-thermal reaction predecessor, and hydro-thermal is anti-
Answer predecessor to be put into water heating kettle, and add absolute ethyl alcohol as solvent, and NaOH, as mineralizer, sealing reaction kettle will
Reaction kettle is placed in 120 DEG C~180 DEG C baking ovens, and product is taken out after reaction, filtered to obtain sediment；Sediment is washed, does
Aluminium-doped zinc oxide powder is obtained after dry.The existing complex process for preparing aluminium-doped zinc oxide powder, it is of high cost, and particle diameter, point
Scattered property is difficult to control.Therefore, it is necessary to research and develop new aluminium-doped zinc oxide powder and preparation method, the oxide powder and zinc of aluminium doping is obtained
Body due to it is of light color, production cost is low, environmentally friendly, can with taking fiber to improve fiber antistatic effect.
The content of the invention
It is an object of the invention to provide a kind of antistatic powder, that is, aluminium-doped zinc oxide powder and preparation method thereof, prepares
Aluminium-doped zinc oxide powder body material good conductivity, with short production cycle, technique is simple, cost is low, be suitable for industrially scalable life
Production.
To realize the object of the invention, the present invention uses following technical scheme：
A kind of antistatic powder, is aluminium-doped zinc oxide powder；In the aluminium-doped zinc oxide powder, mole of aluminium and zinc
Than for（0.5~2）: 100, the average grain diameter of antistatic powder is 260 nm.In aluminium-doped zinc oxide, the Al ions of trivalent take
For divalence Zn ions when, electronegative defect can be made to be produced in the lattice structure of ZnO, cause occur one in the crystal of ZnO
A positively charged center and non-bonding electrons, the electrons break away from constraint of the positive charge to it, become free electron.Aluminium adulterates
Concentration is bigger, and the defects of ZnO crystal structure will be more, and the concentration of free electron can also increase so that aluminium-doped zinc oxide
The electric conductivity of material greatly improves.But if when the doping concentration of aluminium reaches a certain amount of, saturation state, trivalent can be tended to
Aluminium ion just no longer substitutes divalent zinc, but is directly combined with ZnO, generates the ZnAl of insulation2O4So that aluminium-doped zinc oxide material
The electric conductivity of material declines.In the antistatic powder of the present invention, doping concentration of the aluminium in zinc oxide lattice is 0.5~2
At.%, the aluminium-doped zinc oxide powder of synthesis is environment-protecting and non-poisonous, particle size is small and dispersion performance is good, its volume resistivity is 104
Ω cm, have excellent antistatic property.
The invention also discloses the preparation method of above-mentioned antistatic powder, include the following steps：
（1）Zinc salt is added to the water, is made into the zinc solution that concentration is 0.5 ~ 2 mol/L；Then under water bath condition, stir
Mix down, add aluminium salt, obtain mixed liquor；In the mixed liquor, the molar ratio of aluminium and zinc is（0.5~2）∶100；
（2）Under stirring, surfactant is added into step（1）Mixed liquor in；Then ammonium hydroxide is added dropwise and adjusts mixed liquor
PH value is 7~8, is aged 0~5 h again after continuing 1~2 h of stirring, obtains reaction solution；Mole of the surfactant and zinc salt
Than for 1: 4~20；
（3）By step（2）Reaction solution obtain precursor powder after being filtered by vacuum, wash filter cake；By precursor
End vacuum drying obtains antistatic powder after 550~750 DEG C of calcinings.
In above-mentioned technical proposal, step（1）In, the temperature of water bath condition is 50~70 DEG C, is stirred as magnetic agitation；Step
（2）In, stir as magnetic agitation；Step（3）In, it is dried in vacuo to be dried in vacuo 24~48 h in 60~80 DEG C of baking oven,
When calcination time is 1~2 small.
In above-mentioned technical proposal, zinc salt is soluble zinc salt, and aluminium salt is aluminum soluble salt；Zinc salt includes zinc acetate, nitric acid
Zinc, zinc sulfate or zinc chloride；The aluminium salt includes aluminum sulfate, aluminum nitrate or aluminium chloride；The surfactant is poly- second
Glycol and/or triethanolamine.Surfactant polyethylene and triethanolamine can effectively control crystallite dimension and to nanometer
Grain surface is modified, and prevents excessive grain from growing up.
In above-mentioned technical proposal, step（3）In, washing filter cake is first washed with deionized to neutrality for filter cake, then with nothing
Water-ethanol washs, to remove foreign ion and surfactant.
In above-mentioned technical proposal, step（3）In, calcination atmosphere is air.Presoma calcining can be completed in Muffle furnace,
Without reducing atmosphere, calcination process is safely controllable, and calcining heat is low, and calcination time is short, and not high to equipment requirement, energy consumption is low.
The bath temperature of the present invention is controlled at 50~70 DEG C, and the progress of reaction can be accelerated by carrying out reaction at this temperature,
Meanwhile bath temperature is not high, the generation of uneven precipitated phase can be effectively prevented.
Due to the utilization of above-mentioned technical proposal, this programme has the following advantages compared with prior art：
The present invention is under the conditions of controlledly synthesis, before being prepared for aluminium doping as raw material using soluble zinc salt, aluminum soluble salt
Body zinc hydroxide powder is driven, low temperature calcination is that can obtain the Zinc oxide powder of aluminium doping in air atmosphere by presoma；Pass through
The method synthesis aluminium-doped zinc oxide powder it is environment-protecting and non-poisonous, particle size is small and dispersion performance is good, its volume resistivity be 104
Ω cm, available for the antistatic effect that polyester fiber is improved in polyester fiber, expand the application range of polyester product.The present invention
Method prepares aluminium-doped zinc oxide powder without reducing atmosphere, and calcination process is safely controllable, and calcining heat is low, and calcination time is short,
And preparation method is not high to equipment requirement, and energy consumption is low, resource can be greatlyd save, reduces cost, for large-scale production.
Brief description of the drawings
The XRD spectrum of prepared aluminium-doped zinc oxide powder in Fig. 1 embodiments and comparative example；
The grain size distribution of prepared aluminium-doped zinc oxide powder in Fig. 2 example IVs.
Embodiment
Embodiment one
21.950 grams of acetic acid dihydrate zinc are weighed, are added in the beaker equipped with 100 mL deionized waters, constant temperature water bath 50
DEG C magnetic agitation causes its all to dissolve, and then adds 0.188 gram of ANN aluminium nitrate nonahydrate（The molar ratio 0.5 of aluminium and zinc:100）, stir
After mixing about 10 min, add 2 grams of polyethylene glycol 400s, ammonium hydroxide be then slowly added dropwise until PH=7, continue stirring 1 it is small when
It is aged 2 h again afterwards；Reaction solution obtained above is filtered by vacuum, and is washed through repeatedly washing and alcohol, the precipitated powder that will be collected into
End is placed in glass culture dish, is put into 60 DEG C of baking oven and is dried in vacuo 48 h；Dried powder sample is put into Muffle furnace
Middle calcining, calcining heat is 550 DEG C, 2 h of constant temperature, after natural cooling in stove, obtains the zinc oxide antistatic powder of aluminium doping
End, powder volume resistivity test result are as shown in table 1.
Embodiment two
21.950 grams of acetic acid dihydrate zinc are weighed, are added in the beaker equipped with 200 mL deionized waters, constant temperature water bath 60
DEG C magnetic agitation causes its all to dissolve, and then adds 0.375 gram of ANN aluminium nitrate nonahydrate（The molar ratio 1 of aluminium and zinc:100）, stirring
After about 10 min, add 4 grams of triethanolamines, ammonium hydroxide be then slowly added dropwise until PH=8, continue stirring 2 it is small when after it is old again
Change 3 h；Reaction solution obtained above is filtered by vacuum, and is washed through repeatedly washing and alcohol, the precipitation powder being collected into is placed in
In glass culture dish, it is put into 70 DEG C of baking oven and is dried in vacuo 36 h；Dried powder sample is put into Muffle furnace and is forged
Burn, calcining heat is 600 DEG C, 2 h of constant temperature, after natural cooling in stove, obtains the antistatic powder of zinc oxide of aluminium doping.Powder
Body volume resistivity test result is as shown in table 1.
Embodiment three
27.260 grams of zinc chloride are weighed, are added in the beaker equipped with 100 mL deionized waters, 70 DEG C of magnetic force of constant temperature water bath
Stirring causes it all to dissolve, and then adds 0.400 gram of aluminium chloride（The molar ratio 1.5 of aluminium and zinc:100）, after 10 min of stir about,
Add 10 grams of polyethylene glycol 400s, ammonium hydroxide be then slowly added dropwise until PH=8, continue stirring 2 it is small when after be aged 5 h again；
Reaction solution obtained above is filtered by vacuum, and is washed through repeatedly washing and alcohol, the precipitation powder being collected into is placed in glass training
Support in ware, be put into 70 DEG C of baking oven and be dried in vacuo 48 h；Dried powder sample is put into Muffle furnace and is calcined, is calcined
Temperature is 750 DEG C, 1 h of constant temperature, after natural cooling in stove, obtains the zinc oxide conductive powder body of aluminium doping.Powder volume resistance
Rate test result is as shown in table 1.
Example IV
29.750 grams of zinc nitrate hexahydrates are weighed, are added in the beaker equipped with 100 mL deionized waters, constant temperature water bath 70
DEG C magnetic agitation causes its all to dissolve, and then adds 0.750 gram of ANN aluminium nitrate nonahydrate（The molar ratio 2 of aluminium and zinc:100）, stirring
After about 10 min, add 5 grams of polyethylene glycol 400s, ammonium hydroxide be then slowly added dropwise until PH=7.5, continue stirring 1 it is small when
It is aged 1 h again afterwards；Reaction solution obtained above is filtered by vacuum, and is washed through repeatedly washing and alcohol, the precipitated powder that will be collected into
End is placed in glass culture dish, is put into 80 DEG C of baking oven and is dried in vacuo 24 h；Dried powder sample is put into Muffle furnace
Middle calcining, calcining heat is 650 DEG C, 2 h of constant temperature, after natural cooling in stove, obtains the zinc oxide antistatic powder of aluminium doping
End.Powder volume resistivity test result is as shown in table 1.Powder granularity dissipates instrument by laser light and measures, test result such as Fig. 2 institutes
Show.It can be seen that powder granularity is in normal distribution, its average grain diameter is about 260 nm.
Comparative example one
21.950 grams of acetic acid dihydrate zinc are weighed, are added in the beaker equipped with 100 mL deionized waters, constant temperature water bath 50
DEG C magnetic agitation causes its all to dissolve, and adds 2 grams of polyethylene glycol 400s, and ammonium hydroxide is then slowly added dropwise until PH=7, continue
Stir 1 it is small when after be aged 2 h again；Reaction solution obtained above is filtered by vacuum, and is washed through repeatedly washing and alcohol, will be collected into
Precipitation powder be placed in glass culture dish, be put into 60 DEG C of baking oven and be dried in vacuo 48 h；Dried powder sample is put
Enter in Muffle furnace and calcine, calcining heat is 600 DEG C, and 2 h of constant temperature, after natural cooling in stove, obtains zinc oxide antistatic powder
End.Powder volume resistivity test result is as shown in table 1.
The XRD test results of above-mentioned powder are as shown in Figure 1.As can be seen that pharmaceutical composition is mutually ZnO from Fig. 1
Phase, does not have impurities phase ZnAl2O4, illustrate that Al ions realize that alternative dopings enter ZnO lattices, and generate without dephasign.
As can be seen from Table 1, with the defects of the increase of aluminium doping concentration in zinc oxide lattice, ZnO crystal structure
It will increase, the concentration of free electron can also improve so that the electric conductivity of aluminium-doped zinc oxide material greatly improves, the body of powder
Product resistivity accordingly reduces.Compared with the electric conductivity of the Zinc oxide powder to undope, its volume resistivity is from 108The order of magnitude reduces
To 104The order of magnitude.
The volume resistivity of 1 aluminium-doped zinc oxide powder of table
| Embodiment one | Embodiment two | Embodiment three | Example IV | Comparative example one | |
| Volume resistivity（Ω·cm） | 8.3×104 | 6.4×104 | 4.6×104 | 2.6×104 | 2.8×108 |
Claims (5)
1. a kind of preparation method of antistatic powder, it is characterised in that include the following steps：
（1）Zinc salt is added to the water, is made into the zinc solution that concentration is 0.5 ~ 2 mol/L；Then under water bath condition, stirring
Under, aluminium salt is added, obtains mixed liquor；In the mixed liquor, the molar ratio of aluminium and zinc is（0.5~2）∶100；
（2）Under stirring, surfactant is added into step（1）Mixed liquor in；Then the pH value that ammonium hydroxide adjusts mixed liquor is added dropwise
For 7~8,0~5 h is aged again after continuing 1~2 h of stirring, obtains reaction solution；The molar ratio of the surfactant and zinc salt is
1: 4~20；
（3）By step（2）Reaction solution obtain precursor powder after being filtered by vacuum, wash filter cake；Precursor powder is true
Sky is dry after 550~750 DEG C of calcinings, obtains antistatic powder；
Step（3）In, it is dried in vacuo to be dried in vacuo 24~48 h in 60~80 DEG C of baking oven；Calcination time is small for 1~2
When；Calcination atmosphere is air.
2. the preparation method of antistatic powder according to claim 1, it is characterised in that：Step（1）In, the temperature of water bath condition
Spend for 50~70 DEG C；Stir as magnetic agitation.
3. the preparation method of antistatic powder according to claim 1, it is characterised in that：Step（2）In, stir and stirred for magnetic force
Mix.
4. the preparation method of antistatic powder according to claim 1, it is characterised in that：The zinc salt includes zinc acetate, nitre
Sour zinc, zinc sulfate or zinc chloride；The aluminium salt includes aluminum sulfate, aluminum nitrate or aluminium chloride；The surfactant is poly-
Ethylene glycol and/or triethanolamine.
5. the preparation method of antistatic powder according to claim 1, it is characterised in that：Step（3）In, washing filter cake is filter
Cake is first washed with deionized to neutrality, then is washed with absolute ethyl alcohol.
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| CN103818946A (en) * | 2013-11-27 | 2014-05-28 | 上海纳米技术及应用国家工程研究中心有限公司 | Co-doped conductive oxidation powder material and preparation method thereof |
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| CN1590302A (en) * | 2003-08-29 | 2005-03-09 | 中国科学院过程工程研究所 | Coprecipitation method for preparing ultra fine zinc oxide powder possessing high electric conductivity |
| CN101857428A (en) * | 2010-05-21 | 2010-10-13 | 华东理工大学 | Preparation method of conductive zinc oxide powder |
| CN103570056A (en) * | 2013-11-22 | 2014-02-12 | 江苏省东泰精细化工有限责任公司 | Method for preparing conductive powder by recoating aluminum-doped nano zinc oxide with aluminum |
| CN103818946A (en) * | 2013-11-27 | 2014-05-28 | 上海纳米技术及应用国家工程研究中心有限公司 | Co-doped conductive oxidation powder material and preparation method thereof |
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