CN105970323A - Antistatic powder and preparation method thereof - Google Patents
Antistatic powder and preparation method thereof Download PDFInfo
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- CN105970323A CN105970323A CN201610292820.1A CN201610292820A CN105970323A CN 105970323 A CN105970323 A CN 105970323A CN 201610292820 A CN201610292820 A CN 201610292820A CN 105970323 A CN105970323 A CN 105970323A
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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
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Abstract
The invention discloses antistatic powder and a preparation method thereof and concretely relates to aluminum-doped zinc oxide powder and a preparation method thereof. A mole ratio of aluminum to zinc in the aluminum-doped zinc oxide powder is (0.5-2): 100. The preparation method has simple processes and a low production cost and can be used for large scale production. The aluminum-doped zinc oxide powder has a light color, small particle sizes and good dispersity, is environmentally friendly and nontoxic, has volume resistivity of 104 omega.cm, can be used for improving antistatic ability of polyester fibers and widens a polyester product application scope.
Description
Technical field
The invention belongs to zinc oxide conductive powder material technical field, be specifically related to zinc oxide antistatic powder of a kind of aluminum doping and preparation method thereof.
Background technology
Along with the fast development of electronics industry, under some working environment, electronic equipment easily accumulates a large amount of electrostatic charge, hinders the normal work of electronic device even to destroy some parts, and threat operator's is healthy.Doping zinc-oxide conductive powder body is as plastics, coating, a kind of functional filler of fiber and other material, it is possible to gives its performance such as antistatic, electromagnetic shielding, has caused the extensive concern of people.
Zinc oxide is a kind of typical semi-conducting material, and its energy gap at room temperature is 3.4eV, and activation energy is 60meV, for wide band gap semiconducter.In order to improve the electric conductivity of zinc oxide, conventional group iii elements and column IV element are doped preparation to it, such as silicon, germanium, boron, aluminum, gallium, indium, stannum etc., and with aluminum, indium, gallium doping effect the most notable.Although the high-valency metals such as aluminum, indium and gallium can be successfully incorporated in zinc oxide lattice by certain method, but relative to indium and gallium rare metal, the aluminum more horn of plenty of the storage capacity in the earth's crust, price is the most cheap, and the whiteness of powder body is high.Existing preparation method is such as:
Synthesize zinc nitrate-carbamide leucosol microemulsion, filter after standing, filtrate adds aluminum nitrate and forms nitric acid zinc-aluminium mixed liquor, configuration sodium carbonate liquor, instill in polyvinyl alcohol water solution with zinc nitrate aluminum solutions pair, synthesis white precipitate presoma, stand filter, filter cake through deionized water drip washing, be dried, grind sieve, calcine after obtain aluminum-doped zinc oxide nanometer powder；Or zinc acetate and aluminum nitrate are put in beaker, adds the mixed solution of ethylene glycol monomethyl ether and ethanolamine, be made into uniform colloidal sol by magnetic agitation, obtain xerogel after drying, grinding obtains dry gel powder, i.e. hydro-thermal reaction predecessor, puts in water heating kettle by hydro-thermal reaction predecessor, and add dehydrated alcohol as solvent, and NaOH is as mineralizer, sealed reactor, reactor is placed in 120 DEG C～180 DEG C of baking ovens, take out product after reaction, be precipitated thing through filtering；Precipitate is scrubbed, obtains aluminium-doped zinc oxide powder body after drying.The existing complex process preparing aluminium-doped zinc oxide powder body, cost is high, and particle diameter, dispersibility are wayward.Accordingly, it would be desirable to research and develop new aluminium-doped zinc oxide powder and preparation method, obtain aluminum doping Zinc oxide powder due to of light color, production cost is low, environmentally friendly, can be used in take on fiber to improve fiber antistatic effect.
Summary of the invention
It is an object of the invention to provide a kind of antistatic powder i.e. aluminium-doped zinc oxide powder body and preparation method thereof, the aluminium-doped zinc oxide powder body material good conductivity of preparation, with short production cycle, technique simple, low cost, is suitable for industrial-scale production.
For realizing the object of the invention, the present invention by the following technical solutions:
A kind of antistatic powder, for aluminium-doped zinc oxide powder；In described aluminium-doped zinc oxide powder, aluminum is (0.5～2) with the mol ratio of zinc: 100, and the mean diameter of antistatic powder is 260
nm.In aluminium-doped zinc oxide, during the Zn ion of the Al ionic replacement bivalence of trivalent, electronegative defect can be made to produce in the lattice structure of ZnO, cause the crystal of ZnO occurs a positively charged center and non-bonding electrons, this electrons breaks away from the positive charge constraint to it, becomes free electron.Aluminum doping content is the biggest, and the defect in ZnO crystal structure will be the most, and the concentration of free electron also can increase so that the electric conductivity of aluminium-doped zinc oxide material is greatly improved.But, if the doping content of aluminum reaches a certain amount of, then can tend to saturation, trivalent aluminium ion the most no longer replaces divalent zinc, but is directly combined with ZnO, generates the ZnAl of insulation2O4So that the electric conductivity of aluminium-doped zinc oxide material declines.In the antistatic powder of the present invention, aluminum doping content in zinc oxide lattice is 0.5～2
At.%, the aluminium-doped zinc oxide powder environment-protecting asepsis of synthesis, particle size is little and dispersive property good, and its specific insulation is 104Ω cm, has the antistatic property of excellence.
The invention also discloses the preparation method of above-mentioned antistatic powder, comprise the steps:
(1) being added to the water by zinc salt, being made into concentration is 0.5 ~ 2
The zinc solution of mol/L；Then, under water bath condition, under stirring, add aluminium salt, obtain mixed liquor；In described mixed liquor, aluminum is (0.5～2) with the mol ratio of zinc: 100；
(2), under stirring, surfactant is added in the mixed liquor of step (1)；Then the pH value of dropping ammonia regulation mixed liquor is 7～8, is aged 0～5 h again, obtains reactant liquor after continuing stirring 1～2 h；Described surfactant is 1: 4～20 with the mol ratio of zinc salt；
(3) reaction solution of step (2) is obtained precursor powder after vacuum filtration, washing filter cake；In 550～750 DEG C of calcinings after being vacuum dried by precursor powder, obtain antistatic powder.
In technique scheme, in step (1), the temperature of water bath condition is 50～70 DEG C, stirs as magnetic agitation；In step (2), stir as magnetic agitation；In step (3), being vacuum dried as being vacuum dried 24～48 h in the baking oven of 60～80 DEG C, calcination time is 1～2 hour.
In technique scheme, zinc salt is soluble zinc salt, and aluminium salt is aluminum soluble salt；Zinc salt includes zinc acetate, zinc nitrate, zinc sulfate or zinc chloride；Described aluminium salt includes aluminum sulfate, aluminum nitrate or aluminum chloride；Described surfactant is Polyethylene Glycol and/or triethanolamine.Surfactant polyethylene and triethanolamine can effectively control crystallite dimension and modify nano grain surface, prevents excessive grain from growing up.
In technique scheme, in step (3), washing filter cake is that filter cake is first washed with deionized to neutrality, then with absolute ethanol washing, to remove foreign ion and surfactant.
In technique scheme, in step (3), calcination atmosphere is air.Presoma calcining can complete in Muffle furnace, it is not necessary to reducing atmosphere, calcination process is safely controllable, and calcining heat is low, and calcination time is short, the highest to equipment requirements, and energy consumption is low.
The bath temperature of the present invention controls at 50～70 DEG C, carries out reaction at this temperature and can accelerate the carrying out of reaction, and meanwhile, bath temperature is the highest, can effectively prevent the generation of uneven precipitated phase.
Due to the utilization of technique scheme, this programme compared with prior art has the advantage that
The present invention, under the conditions of controlledly synthesis, is prepared for the presoma zinc hydroxide powder body of aluminum doping, presoma low temperature calcination in air atmosphere i.e. can get the Zinc oxide powder of aluminum doping with soluble zinc salt, aluminum soluble salt for raw material；The aluminium-doped zinc oxide powder environment-protecting asepsis that synthesized by the method, particle size is little and dispersive property good, and its specific insulation is 104Ω cm, can be used for improving in polyester fiber the antistatic effect of polyester fiber, expands the range of application of polyester product.The inventive method prepares aluminium-doped zinc oxide powder body without reducing atmosphere, and calcination process is safely controllable, and calcining heat is low, and calcination time is short, and preparation method is the highest to equipment requirements, and energy consumption is low, can be greatly saved resource, reduces cost, for large-scale production.
Accompanying drawing explanation
The XRD figure spectrum of aluminium-doped zinc oxide powder body prepared in Fig. 1 embodiment and comparative example；
The grain size distribution of aluminium-doped zinc oxide powder body prepared in Fig. 2 embodiment four.
Detailed description of the invention
Embodiment one
Weigh 21.950 gram of two acetate hydrate zinc, join equipped with 100
In the beaker of mL deionized water, 50 DEG C of magnetic agitation of constant temperature water bath cause it and all dissolve, and are subsequently adding 0.188 gram of ANN aluminium nitrate nonahydrate (aluminum and mol ratio 0.5:100 of zinc), stir about 10
After min, add 2 grams of PEG400s, be added dropwise over ammonia the most lentamente until PH=7, after continuing stirring 1 hour, be aged 2 h again；By reaction solution vacuum filtration obtained above, and wash through repeatedly washing and alcohol, the precipitation powder collected is placed in glass culture dish, puts into and the baking oven of 60 DEG C is vacuum dried 48 h；Being put into by dried powder sample in Muffle furnace and calcine, calcining heat is 550 DEG C, constant temperature 2 h, after natural cooling in stove, obtains the zinc oxide antistatic powder of aluminum doping, and powder body specific insulation test result is as shown in table 1.
Embodiment two
Weigh 21.950 gram of two acetate hydrate zinc, join equipped with 200
In the beaker of mL deionized water, 60 DEG C of magnetic agitation of constant temperature water bath cause it and all dissolve, and are subsequently adding 0.375 gram of ANN aluminium nitrate nonahydrate (aluminum and mol ratio 1:100 of zinc), stir about 10
After min, add 4 grams of triethanolamine, be added dropwise over ammonia the most lentamente until PH=8, after continuing stirring 2 hours, be aged 3 h again；By reaction solution vacuum filtration obtained above, and wash through repeatedly washing and alcohol, the precipitation powder collected is placed in glass culture dish, puts into and the baking oven of 70 DEG C is vacuum dried 36 h；Being put into by dried powder sample in Muffle furnace and calcine, calcining heat is 600 DEG C, constant temperature 2 h, after natural cooling in stove, obtains the zinc oxide antistatic powder of aluminum doping.Powder body specific insulation test result is as shown in table 1.
Embodiment three
Weigh 27.260 grams of zinc chloride, join equipped with 100
In the beaker of mL deionized water, 70 DEG C of magnetic agitation of constant temperature water bath cause it and all dissolve, and are subsequently adding 0.400 gram of aluminum chloride (aluminum and mol ratio 1.5:100 of zinc), stir about 10
After min, add 10 grams of PEG400s, be added dropwise over ammonia the most lentamente until PH=8, after continuing stirring 2 hours, be aged 5 h again；By reaction solution vacuum filtration obtained above, and wash through repeatedly washing and alcohol, the precipitation powder collected is placed in glass culture dish, puts into and the baking oven of 70 DEG C is vacuum dried 48 h；Being put into by dried powder sample in Muffle furnace and calcine, calcining heat is 750 DEG C, constant temperature 1 h, after natural cooling in stove, obtains the zinc oxide conductive powder body of aluminum doping.Powder body specific insulation test result is as shown in table 1.
Embodiment four
Weigh 29.750 grams of zinc nitrate hexahydrates, join equipped with 100
In the beaker of mL deionized water, 70 DEG C of magnetic agitation of constant temperature water bath cause it and all dissolve, and are subsequently adding 0.750 gram of ANN aluminium nitrate nonahydrate (aluminum and mol ratio 2:100 of zinc), stir about 10
After min, add 5 grams of PEG400s, be added dropwise over ammonia the most lentamente until PH=7.5, after continuing stirring 1 hour, be aged 1 h again；By reaction solution vacuum filtration obtained above, and wash through repeatedly washing and alcohol, the precipitation powder collected is placed in glass culture dish, puts into and the baking oven of 80 DEG C is vacuum dried 24 h；Being put into by dried powder sample in Muffle furnace and calcine, calcining heat is 650 DEG C, constant temperature 2 h, after natural cooling in stove, obtains the zinc oxide antistatic powder of aluminum doping.Powder body specific insulation test result is as shown in table 1.Powder granularity dissipates instrument by laser light and measures, and test result is as shown in Figure 2.It can be seen that powder granularity is normal distribution, its mean diameter is about 260
nm。
Comparative example one
Weigh 21.950 gram of two acetate hydrate zinc, join equipped with 100
In the beaker of mL deionized water, 50 DEG C of magnetic agitation of constant temperature water bath cause it and all dissolve, and add 2 grams of PEG400s, are added dropwise over ammonia the most lentamente until PH=7, are aged 2 h again after continuing stirring 1 hour；By reaction solution vacuum filtration obtained above, and wash through repeatedly washing and alcohol, the precipitation powder collected is placed in glass culture dish, puts into and the baking oven of 60 DEG C is vacuum dried 48 h；Being put into by dried powder sample in Muffle furnace and calcine, calcining heat is 600 DEG C, constant temperature 2 h, after natural cooling in stove, obtains zinc oxide antistatic powder.Powder body specific insulation test result is as shown in table 1.
The XRD test result of above-mentioned powder body is as shown in Figure 1.It can be seen that pharmaceutical composition is ZnO phase mutually from Fig. 1, there is no impurity phase ZnAl2O4, illustrate that Al ion realizes alternative dopings and enters ZnO lattice, and do not have dephasign to generate.
As can be seen from Table 1, along with aluminum increase of doping content in zinc oxide lattice, the defect in ZnO crystal structure will increase, and the concentration of free electron also can improve, the electric conductivity making aluminium-doped zinc oxide material is greatly improved, and the specific insulation of powder body reduces accordingly.Compared with the electric conductivity of plain Zinc oxide powder, its specific insulation is from 108The order of magnitude is reduced to 104The order of magnitude.
The specific insulation of table 1 aluminium-doped zinc oxide powder body
| Embodiment one | Embodiment two | Embodiment three | Embodiment four | Comparative example one | |
| Specific insulation (Ω cm) | 8.3×104 | 6.4×104 | 4.6×104 | 2.6×104 | 2.8×108 |
Claims (10)
1. an antistatic powder, it is characterised in that: described antistatic powder is aluminium-doped zinc oxide powder；In described aluminium-doped zinc oxide powder, aluminum is (0.5～2) with the mol ratio of zinc: 100.
Antistatic powder the most according to claim 1, it is characterised in that: the mean diameter of described antistatic powder is 260 nm.
3. the preparation method of antistatic powder described in claim 1, it is characterised in that comprise the 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, under stirring, add aluminium salt, obtain mixed liquor；In described mixed liquor, aluminum is (0.5～2) with the mol ratio of zinc: 100；
(2), under stirring, surfactant is added in the mixed liquor of step (1)；Then the pH value of dropping ammonia regulation mixed liquor is 7～8, is aged 0～5 h again, obtains reactant liquor after continuing stirring 1～2 h；Described surfactant is 1: 4～20 with the mol ratio of zinc salt；
(3) reaction solution of step (2) is obtained precursor powder after vacuum filtration, washing filter cake；In 550～750 DEG C of calcinings after being vacuum dried by precursor powder, obtain antistatic powder.
The preparation method of antistatic powder the most according to claim 3, it is characterised in that: in step (1), the temperature of water bath condition is 50～70 DEG C；Stirring is magnetic agitation.
The preparation method of antistatic powder the most according to claim 3, it is characterised in that: in step (2), stir as magnetic agitation.
The preparation method of antistatic powder the most according to claim 3, it is characterised in that: in step (3), it is vacuum dried as being vacuum dried 24～48 h in the baking oven of 60～80 DEG C；Calcination time is 1～2 hour.
The preparation method of antistatic powder the most according to claim 3, it is characterised in that: described zinc salt includes zinc acetate, zinc nitrate, zinc sulfate or zinc chloride；Described aluminium salt includes aluminum sulfate, aluminum nitrate or aluminum chloride；Described surfactant is Polyethylene Glycol and/or triethanolamine.
The preparation method of antistatic powder the most according to claim 3, it is characterised in that: in step (3), washing filter cake is that filter cake is first washed with deionized to neutrality, then uses absolute ethanol washing.
The preparation method of antistatic powder the most according to claim 3, it is characterised in that: in step (3), calcination atmosphere is air.
10. antistatic powder application in preparing anti-static polyester fiber described in claim 1.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108586979A (en) * | 2018-04-17 | 2018-09-28 | 安徽伙伴电气有限公司 | Jewelling alloy flame-proof environmental protection cable during a kind of skyscraper vertical lifting is used |
| CN110183827A (en) * | 2019-05-21 | 2019-08-30 | 苏州博利迈新材料科技有限公司 | A kind of preparation method of flame-retardant and anti-static polyester material |
| CN116426144A (en) * | 2022-12-29 | 2023-07-14 | 北京星驰恒动科技发展有限公司 | Radiation-resistant thermal control filler, antistatic thermal control coating and preparation method thereof |
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|---|---|---|---|---|
| CN108586979A (en) * | 2018-04-17 | 2018-09-28 | 安徽伙伴电气有限公司 | Jewelling alloy flame-proof environmental protection cable during a kind of skyscraper vertical lifting is used |
| CN110183827A (en) * | 2019-05-21 | 2019-08-30 | 苏州博利迈新材料科技有限公司 | A kind of preparation method of flame-retardant and anti-static polyester material |
| CN116426144A (en) * | 2022-12-29 | 2023-07-14 | 北京星驰恒动科技发展有限公司 | Radiation-resistant thermal control filler, antistatic thermal control coating and preparation method thereof |
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