CN102249293A - Method for preparing pyrophillite-based antimony-doped tin oxide compound conductive powder - Google Patents
Method for preparing pyrophillite-based antimony-doped tin oxide compound conductive powder Download PDFInfo
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- CN102249293A CN102249293A CN2011100982444A CN201110098244A CN102249293A CN 102249293 A CN102249293 A CN 102249293A CN 2011100982444 A CN2011100982444 A CN 2011100982444A CN 201110098244 A CN201110098244 A CN 201110098244A CN 102249293 A CN102249293 A CN 102249293A
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- agalmatolite
- conductive powder
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Abstract
The invention discloses a method for preparing pyrophillite-based antimony-doped tin oxide compound conductive powder. The method is characterized in that a chemical precipitation process for respectively dropwise adding a tin salt and an antimony salt is adopted. The method is a preparation method for the compound conductive powder, the surface of which is covered with a layer of antimony-doped tin oxide. The method provided by the invention can be used for reducing the preparation cost of conductive powder. The acquired powder has light color and excellent conductivity.
Description
(1) technical field
The present invention relates to a kind of is the preparation method of matrix antimony-doped tin oxide composite conductive powder with the agalmatolite, belongs to the electro-conductive material technical field.
(2) background technology
Along with fast development of social economy, the range of application of various metallic substance, plastics, fiber, rubber, coating enlarges day by day.These materials are owing to be subjected to friction, bump etc. easily to produce static, and static focus be to a certain degree will causing discharge, even may cause puncture or presence of fire, and the while also can produce certain interference to wirelessreceiver, make the radar can't works better.For preventing or eliminate static, will in coating, plastics, fiber, rubber, add conducting powder, make it have functions such as conduction, anti-electrostatic, thereby eliminate the harm that static brings.
Conductive powder is a kind of functional materials, and at present mainly the form with conductive filler material is applied on the macromolecular material (comprising electrically conducting coating), makes macromolecular material have functions such as electroconductibility, antistatic, shielding electromagnetic wave.Traditional conductive powder body commonly used has carbon system (carbon black, carbon fiber, graphite), metal series (metal-powder, tinsel, steel fiber), organic series and metal oxide series.The main drawback of carbon series conductive powder is the carbon black bad dispersibility, the goods color is dark and color is single; Metal powder costs an arm and a leg, and easily is oxidized to the metal oxide with electroconductibility, conductivity instability, poor corrosion resistance; Non-refractory, not corrosion-resistant during the organic conductive powder as filler, and water tolerance, oil-proofness are poor, static resistance is also unstable, only can be applicable to that relative humidity is greater than 60% environment; And metal-oxide powder exists electroconductibility not good mostly, saturate defective, and be easy to take place precipitated and separated in the use, influence the work-ing life of base-material.
The light color inorganic compound conductive powder body is that material (as mica, quartz, kaolin, barite etc.) with a kind of inexpensive, light weight is as substrate or core, by electroless plating calcining method again, coat one deck or which floor chemical stability is good, erosion resistance is strong, specific conductivity is high metal (as Ag, Ni, Cu etc.) or oxide compound (inorganic oxides such as weisspiessglanz, stannic oxide, titanium dioxide) on its surface and the matrix material that obtains.The electroconductibility of this kind material, Corrosion Protection are all more superior, and color tunable, can make various light-colored conductive powders according to application requiring.
Patent ZL200710035919.4 (a kind of preparation method of inorganic compound conductive powder body) has reported that a kind of is the preparation method of matrix antimony-doped tin oxide composite conductive powder with the kaolinite.This invention adds dispersion agent in kaolinite mineral, make homodisperse suspension ore pulp; Adopt the form precipitation from homogeneous solution of chemical coprecipitation, the throw out that obtains is made composite conductive powder through filtering and washing, solid-liquid separation, drying, roasting, pulverizing with oxyhydroxide or hydrous oxide.Different with above-mentioned patent is, it is the method that matrix prepares light composite conductive powder with the agalmatolite powder that the present invention has developed a kind of, changed conventional tin antimony mixture chemical coprecipitation simultaneously, the chemical precipitation method technological line that has adopted pink salt and antimonic salt to drip has respectively obtained powder of light color, good conductivity.
(3) summary of the invention
It is matrix that the technical problem to be solved in the present invention provides a kind of agalmatolite powder with cheapness, the chemical precipitation method technological line that has adopted pink salt and antimonic salt to drip respectively, the surface coats the preparation method of the composite conductive powder of one deck antimony-doped tin oxide, this method can reduce the preparation cost of conductive powder body, and gained powder color is more shallow, electroconductibility is better.
For solving the problems of the technologies described above, the present invention adopts following technical scheme:
A kind of preparation method of agalmatolite base antimony-doped tin oxide composite conductive powder may further comprise the steps:
(1) pyrophyllite powder and deionized water being made into solid content is 10%～20% agalmatolite suspension ore pulp;
(2) with concentration be the hydrochloric acid preparation SnCl of 1～2mol/L respectively
4And SbCl
3Hydrochloric acid soln, SnCl wherein
4Concentration be 0.1～0.5mol/L, the mol ratio of Sn and Sb is 2～15: 1;
(3) with SnCl
4Hydrochloric acid soln add in the agalmatolite suspension ore pulp, mix, obtain the mixed slurry of agalmatolite and pink salt; SnCl wherein
4With the mass ratio of agalmatolite be 60～150: 100;
(4) with SbCl
3Hydrochloric acid soln under agitation splash in above-mentioned and mixed slurry agalmatolite and pink salt, simultaneously hierarchy of control pH value be 1.0～3.0 and temperature be 30～60 ℃, make pink salt and antimonic salt hydrolysis and produce co-precipitation, appendix is on the agalmatolite surface equably;
(5) the reaction product constant temperature with step (4) leaves standstill, then suction filtration, wash and do not have Cl in the filtrate
-Till (available 1mol/L AgNO
3Check does not have precipitation and produces), drying, calcining, pulverizing can obtain agalmatolite base antimony-doped tin oxide composite conductive powder again.
The pyrophyllite powder that the present invention uses is an eka-silicon aluminium silicate mineral powder, and the particle diameter of described pyrophyllite powder is preferably the 325-800 order.
Further, in the step (1), when preparation agalmatolite suspension ore pulp, agalmatolite and deionized water are fully stirred in 30～60 ℃, make the agalmatolite particles dispersed even.
Further, in the step (4), with SbCl
3Hydrochloric acid soln when splashing into the mixed slurry of agalmatolite and pink salt, preferably controlling stirring velocity is 600～1000r/min, preferred rate of addition is 1～2ml/min.Preferably pass through the form hierarchy of control pH of the NaOH solution of dropping 1～2mol/L.
Further, in the step (5), drying temperature is preferably 60～80 ℃, and be 2～5h time of drying.Calcining temperature is preferably 400～700 ℃, and calcination time is preferably 0.5～2h.
With existing carbon is to compare with metal series conductive powder body, and the present invention has the following advantages:
1, the present invention selects the matrix of cheap agalmatolite mineral as composite conductive powder for use, not only greatly reduces the preparation cost of conductive powder body, and has greatly improved the use value of agalmatolite resource.
2, the conductivity of products obtained therefrom of the present invention and powder color can be regulated by the add-on of pink salt and antimonic salt.
3, the present invention has advantages such as cost is low, product stability is good, and prepared composite granule color is more shallow, electroconductibility is better, is easy to be modulated into versicolor permanent conductive additives such as near-white, is easy to realize industrial production, and wide application prospect is arranged.
(4) embodiment
The agalmatolite micro mist that produces with blue or green field, Zhejiang district is the composite conductive powder of base-material preparation light color.
Embodiment 1:
(1) 10g pyrophyllite powder (particle diameter is 325 orders) and 90g deionized water being mixed with solid content is 10% solution, and placing temperature is that 50 ℃ electric-heated thermostatic water bath fully stirs, and mineral grain is uniformly dispersed, and makes agalmatolite suspension ore pulp.
(2) be that the hydrochloric acid of 2mol/L is prepared SnCl respectively with concentration
45H
2O and SbCl
3Hydrochloric acid soln, SnCl wherein
4Concentration be 0.5mol/L, SbCl
3The concentration of solution is Sn in molar ratio: Sb=5: 1 configuration places dissolving fully on the magnetic stirring apparatus.
(3) with SnCl
4Hydrochloric acid soln add in the agalmatolite suspension ore pulp, mix, obtain the mixed slurry of agalmatolite and pink salt; SnCl wherein
4Mass ratio (m with agalmatolite
SnC14/ m
Agalmatolite) be 80: 100.
(4) with SbCl
3Hydrochloric acid soln and the sodium hydroxide of 1.5mol/L splash into the mixed slurry that fills agalmatolite and pink salt simultaneously and keep stirring in the reactor with 50 ℃ of constant temperature, stirring velocity is 800r/min, rate of addition is 1ml/min, system pH is controlled at pH=2.0.
(5) reacted product constant temperature is left standstill 30min, suction filtration, washing do not have Cl in filtrate
-, 80 ℃ of dry 3h, 600 ℃ of calcining 1h, promptly obtaining with the agalmatolite after the pulverizing is the composite conductive powder of matrix.
After tested, the whiteness of resulting composite conductive powder is 58; Volume specific resistance is 2.80K Ω cm.
Embodiment 2:
(1) 10g pyrophyllite powder (particle diameter is 800 orders) and 40g deionized water being mixed with solid content is 20% solution, and placing temperature is that 60 ℃ electric-heated thermostatic water bath fully stirs, and mineral grain is uniformly dispersed, and makes agalmatolite suspension ore pulp.
(2) be that the hydrochloric acid of 1mol/L is prepared SnCl respectively with concentration
45H
2O and SbCl
3Hydrochloric acid soln, SnCl wherein
4Concentration be 0.1mol/L, SbCl
3The concentration of solution is Sn in molar ratio: Sb=15: 1 configuration places dissolving fully on the magnetic stirring apparatus.
(3) with SnCl
4Hydrochloric acid soln add in the agalmatolite suspension ore pulp, mix, obtain the mixed slurry of agalmatolite and pink salt; SnCl wherein
4Mass ratio (m with agalmatolite
SnC14/ m
Agalmatolite) be 60: 100.
(4) with SbCl
3Hydrochloric acid soln and the sodium hydroxide of 1mol/L splash into the mixed slurry that fills agalmatolite and pink salt simultaneously and keep stirring in the reactor with 60 ℃ of constant temperature, stirring velocity is 1000r/min, rate of addition is 1ml/min, system pH is controlled at pH=2.0.
(5) reacted product constant temperature is left standstill 30min, suction filtration, washing do not have Cl in filtrate
-, 60 ℃ of dry 5h, 400 ℃ of calcining 2h, promptly obtaining with the agalmatolite after the pulverizing is the composite conductive powder of matrix.
After tested, the whiteness of resulting composite conductive powder is 64; Volume specific resistance is 4.76K Ω cm.
Embodiment 3:
(1) 15g pyrophyllite powder (particle diameter is 600 orders) and 85g deionized water being mixed with solid content is 15% solution, and placing temperature is that 30 ℃ electric-heated thermostatic water bath fully stirs, and mineral grain is uniformly dispersed, and makes agalmatolite suspension ore pulp.
(2) be that the hydrochloric acid of 1.5mol/L is prepared SnCl respectively with concentration
45H
2O and SbCl
3Hydrochloric acid soln, SnCl wherein
4Concentration be 0.25mol/L, SbCl
3The concentration of solution is Sn in molar ratio: Sb=2: 1 configuration places dissolving fully on the magnetic stirring apparatus.
(3) with SnCl
4Hydrochloric acid soln add in the agalmatolite suspension ore pulp, mix, obtain the mixed slurry of agalmatolite and pink salt; SnCl wherein
4Mass ratio (m with agalmatolite
SnC14/ m
Agalmatolite) be 150: 100.
(4) with SbCl
3Hydrochloric acid soln and the sodium hydroxide of 2mol/L splash into the mixed slurry that fills agalmatolite and pink salt simultaneously and keep stirring in the reactor with 30 ℃ of constant temperature, stirring velocity is 600r/min, rate of addition is 2ml/min, system pH is controlled at pH=1.0.
(5) reacted product constant temperature is left standstill 30min, suction filtration, washing do not have Cl in filtrate
-, 70 ℃ of dry 4h, 700 ℃ of calcining 0.5h, promptly obtaining with the agalmatolite after the pulverizing is the composite conductive powder of matrix.
After tested, the whiteness of resulting composite conductive powder is 60; Volume specific resistance is 1.98K Ω cm.
Embodiment 4:
(1) 12g pyrophyllite powder (particle diameter is 400 orders) and 88g deionized water being mixed with solid content is 12% solution, and placing temperature is that 50 ℃ electric-heated thermostatic water bath fully stirs, and mineral grain is uniformly dispersed, and makes agalmatolite suspension ore pulp.
(2) be that the hydrochloric acid of 1mol/L is prepared SnCl respectively with concentration
45H
2O and SbCl
3Hydrochloric acid soln, SnCl wherein
4Concentration be 0.5mol/L, SbCl
3The concentration of solution is Sn in molar ratio: Sb=10: 1 configuration places dissolving fully on the magnetic stirring apparatus.
(3) with SnCl
4Hydrochloric acid soln add in the agalmatolite suspension ore pulp, mix, obtain the mixed slurry of agalmatolite and pink salt; SnCl wherein
4Mass ratio (m with agalmatolite
SnC14/ m
Agalmatolite) be 100: 100.
(4) with SbCl
3Hydrochloric acid soln and the sodium hydroxide of 1mol/L splash into the mixed slurry that fills agalmatolite and pink salt simultaneously and keep stirring in the reactor with 50 ℃ of constant temperature, stirring velocity is 800r/min, rate of addition is 1ml/min, system pH is controlled at pH=3.0.
(5) reacted product constant temperature is left standstill 30min, suction filtration, washing do not have Cl in filtrate
-, 80 ℃ of dry 2h, 500 ℃ of calcining 1h, promptly obtaining with the agalmatolite after the pulverizing is the composite conductive powder of matrix.
After tested, the whiteness of resulting composite conductive powder is 63; Volume specific resistance is 5.78K Ω cm.
Embodiment 5:
(1) 10g pyrophyllite powder (particle diameter is 800 orders) and 90g deionized water being mixed with solid content is 10% solution, and placing temperature is that 60 ℃ electric-heated thermostatic water bath fully stirs, and mineral grain is uniformly dispersed, and makes agalmatolite suspension ore pulp.
(2) be that the hydrochloric acid of 1mol/L is prepared SnCl respectively with concentration
45H
2O and SbCl
3Hydrochloric acid soln, SnCl wherein
4Concentration be 0.1mol/L, SbCl
3The concentration of solution is Sn in molar ratio: Sb=5: 1 configuration places dissolving fully on the magnetic stirring apparatus.
(3) with SnCl
4Hydrochloric acid soln add in the agalmatolite suspension ore pulp, mix, obtain the mixed slurry of agalmatolite and pink salt; SnCl wherein
4Mass ratio (m with agalmatolite
SnC14/ m
Agalmatolite) be 90: 100.
(4) with SbCl
3Hydrochloric acid soln and the sodium hydroxide of 2mol/L splash into the mixed slurry that fills agalmatolite and pink salt simultaneously and keep stirring in the reactor with 60 ℃ of constant temperature, stirring velocity is 700r/min, rate of addition is 1ml/min, system pH is controlled at pH=2.0.
(5) reacted product constant temperature is left standstill 30min, suction filtration, washing do not have Cl in filtrate
-, 80 ℃ of dry 3h, 500 ℃ of calcining 1h, promptly obtaining with the agalmatolite after the pulverizing is the composite conductive powder of matrix.
After tested, the whiteness of resulting composite conductive powder is 62; Volume specific resistance is 3.46K Ω cm.
Claims (6)
1. the preparation method of an agalmatolite base antimony-doped tin oxide composite conductive powder may further comprise the steps:
(1) pyrophyllite powder and deionized water being made into solid content is 10%～20% agalmatolite suspension ore pulp;
(2) with concentration be the hydrochloric acid preparation SnCl of 1～2mol/L respectively
4And SbCl
3Hydrochloric acid soln, SnCl wherein
4Concentration be 0.1～0.5mol/L, the mol ratio of Sn and Sb is 2～15: 1;
(3) with SnCl
4Hydrochloric acid soln add in the agalmatolite suspension ore pulp, mix, obtain the mixed slurry of agalmatolite and pink salt; SnCl wherein
4With the mass ratio of agalmatolite be 60～150: 100;
(4) with SbCl
3Hydrochloric acid soln under agitation splash in above-mentioned and mixed slurry agalmatolite and pink salt, simultaneously hierarchy of control pH value be 1.0～3.0 and temperature be 30～60 ℃, make pink salt and antimonic salt hydrolysis and produce co-precipitation, appendix is on the agalmatolite surface equably;
(5) the reaction product constant temperature with step (4) leaves standstill, then suction filtration, wash and do not have Cl in the filtrate
-Till, drying, calcining, pulverizing can obtain agalmatolite base antimony-doped tin oxide composite conductive powder again.
2. the preparation method of agalmatolite base antimony-doped tin oxide composite conductive powder as claimed in claim 1 is characterized in that: when preparation agalmatolite suspension ore pulp, agalmatolite and deionized water are fully stirred in 30～60 ℃, make the agalmatolite particles dispersed even.
3. the preparation method of agalmatolite base antimony-doped tin oxide composite conductive powder as claimed in claim 1 is characterized in that: with SnCl
4Hydrochloric acid soln add in the agalmatolite suspension ore pulp, mix, obtain the mixed slurry of agalmatolite and pink salt;
4. the preparation method of agalmatolite base antimony-doped tin oxide composite conductive powder as claimed in claim 1 is characterized in that: with SbCl
3Hydrochloric acid soln when splashing into the mixed slurry of agalmatolite and pink salt, the control stirring velocity is 600～1000r/min, rate of addition is 1～2ml/min.
5. the preparation method of agalmatolite base antimony-doped tin oxide composite conductive powder as claimed in claim 1 is characterized in that: drying temperature is 60～80 ℃ in the step (4), and be 2～5h time of drying.
6. the preparation method of agalmatolite base antimony-doped tin oxide composite conductive powder as claimed in claim 1 is characterized in that: calcining temperature is 400～700 ℃ in the step (4), and calcination time is 0.5～2h.
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Cited By (5)
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| CN104004387A (en) * | 2014-06-17 | 2014-08-27 | 安徽工业大学 | Silicate powder wrapped in ATO nanometer particles and application of silicate powder |
| CN105513716A (en) * | 2016-01-04 | 2016-04-20 | 常州纳欧新材料科技有限公司 | Inorganic light color conductive powder preparation method |
| CN105702382A (en) * | 2016-01-18 | 2016-06-22 | 常州大学 | Method for preparing light-colored conductive potassium titanate powder |
| CN107967967A (en) * | 2017-12-05 | 2018-04-27 | 山东电盾科技股份有限公司 | The preparation method of stibium-doped zinc oxide, tin oxide cladding silica conducting powder |
| CN113307304A (en) * | 2021-04-26 | 2021-08-27 | 温州大学 | CsPbX3Preparation method and application of @ pyrophyllite composite material |
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2011
- 2011-04-19 CN CN2011100982444A patent/CN102249293A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104004387A (en) * | 2014-06-17 | 2014-08-27 | 安徽工业大学 | Silicate powder wrapped in ATO nanometer particles and application of silicate powder |
| CN104004387B (en) * | 2014-06-17 | 2016-04-13 | 安徽工业大学 | A kind of silicate powder of ATO nanoparticle parcel and application thereof |
| CN105513716A (en) * | 2016-01-04 | 2016-04-20 | 常州纳欧新材料科技有限公司 | Inorganic light color conductive powder preparation method |
| CN105513716B (en) * | 2016-01-04 | 2017-02-01 | 常州纳欧新材料科技有限公司 | Inorganic light color conductive powder preparation method |
| CN105702382A (en) * | 2016-01-18 | 2016-06-22 | 常州大学 | Method for preparing light-colored conductive potassium titanate powder |
| CN105702382B (en) * | 2016-01-18 | 2017-03-22 | 常州大学 | Method for preparing light-colored conductive potassium titanate powder |
| CN107967967A (en) * | 2017-12-05 | 2018-04-27 | 山东电盾科技股份有限公司 | The preparation method of stibium-doped zinc oxide, tin oxide cladding silica conducting powder |
| CN107967967B (en) * | 2017-12-05 | 2019-05-21 | 山东电盾科技股份有限公司 | The preparation method of stibium-doped zinc oxide, tin oxide cladding silica conducting powder |
| CN113307304A (en) * | 2021-04-26 | 2021-08-27 | 温州大学 | CsPbX3Preparation method and application of @ pyrophyllite composite material |
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Application publication date: 20111123 |