CN101818365B - Method for preparing nano stibium powder - Google Patents
Method for preparing nano stibium powder Download PDFInfo
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- CN101818365B CN101818365B CN2009101174724A CN200910117472A CN101818365B CN 101818365 B CN101818365 B CN 101818365B CN 2009101174724 A CN2009101174724 A CN 2009101174724A CN 200910117472 A CN200910117472 A CN 200910117472A CN 101818365 B CN101818365 B CN 101818365B
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Abstract
The invention discloses a method for preparing powder nano stibium composite, which comprises the following steps of: firstly preparing electrolyte from distilled water and concentrated hydrochloric acid, adding octyl phenol polyoxyethylene ether into the electrolyte, the mol ratio of the octyl phenol polyoxyethylene ether and the hydrochloric acid being 1:100-300, then uniformly stirring the electrolytic emulsion; secondly injecting the electrolytic emulsion into an electrolytic bath, and taking pure stibium as an anodeand stainless steel as a cathode, wherein the area ratio of the anode to the cathode is 1:2-5 and the distance between the anode and the cathode is 20 to 50mm; setting current density for electrolysis as 0.01-0.2A/cm<2> and the electrolytic time as 20-120 minutes; adding the cathode to which stibium powder is attached into absolute ethyl alcohol, and putting the cathode in an ultrasonic cleaner for desorption by ultra-sonic oscillation for 5 to 20 minutes to obtain black stibium solution; and filtering the solution, and drying the filtrate for 1 to 3 hours at the temperature of between 60 and 100 DEG C in a vacuum environment to obtain the powder nano stibium composite.
Description
Technical field
The present invention relates to the electrochemical preparation method of nano stibium powder.
Background technology
Nano metal powder purity with the electrolytic process preparation is high at present, and shape is dendroid mostly, and good suppression performance and sintering character are arranged, and has obtained at aspects such as powder metallurgy, nuclear power, chemical industry and novel alloy materials using widely.But electrochemical process prepares nano stibium powder does not then appear in the newspapers, and traditional electrolytic process to prepare the Nano metal powder granularity of comparing with liquid phase reduction thicker, size composition disperses; When the metal powder of certain particle size fraction of needs; Need to adopt the method for classification (screening) to meet the demands, this has just prolonged the production cycle, has increased the cost of product; Make powder activity in turnover and treating processes reduce again, give the sintering character deleterious impact.The Nano metal powder of usual method preparation is the unstable state material, and their are prone to sex change with the ambiance reaction, is prone between particle interact and reunites, and its dispersion liquid is difficult to stable for extended periods of time usually, greatly limitations its range of application.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of nano stibium powder.
The present invention is a kind of preparation method of powder nanometer antimony mixture, the steps include:
(1) at first is mixed with electrolytic solution, 3～6 moles every liter of the content of hydrochloric acid in the electrolytic solution with zero(ppm) water and concentrated hydrochloric acid.Electrolyte quota well after, add the octyl phenol Soxylat A 25-7, the mol ratio of octyl phenol Soxylat A 25-7 and hydrochloric acid is 1: 100～300, then uses magnetic stirring apparatus that electrolytic emulsion is stirred.
(2) emulsion that stirs being injected electrolyzer, is anode with the star antimony, and stainless steel is a negative electrode, and anode is 1: 2～5 with the area ratio of negative electrode, and the pole piece spacing is 20～50mm.
(3) electrolytic current density is 0.01A/cm
2～0.2A/cm
2Electrolysis time is 20～120 minutes; Under galvanic effect, anodic antimony constantly dissolves and gets in the electrolytic solution, and near the antimony ion the negative electrode in the solution is constantly separated out again and is deposited on the negative electrode; The octyl phenol Soxylat A 25-7 that is dissolved in the electrolytic solution carries out the original position coating to the antimony atoms of separating out, and the antimony powder loosely that makes generation is attached to cathode surface.Simultaneously near the antimony ion the anode relies on the directional migration of diffusion and electric charge to move near the negative electrode continuously, thereby guarantees electrolyticly to carry out smoothly;
The negative electrode that (4) will adhere to antimony powder is put into absolute ethyl alcohol, puts into ultrasonic cleaner and adopts ultra-sonic oscillation to carry out desorption, and the ultra-sonic oscillation time is 5～20 minutes, obtains the antimony solution of black;
(5) solution is filtered,, can obtain powder nanometer antimony mixture filtrate in 60 ℃～100 ℃ vacuum environment dry 1～3 hour.
Beneficial effect of the present invention is: the present invention is the electrochemical preparation method that adopts protected by organic monomolecular layer, and at the fine and close organic supramolecular modifier of surface chemistry absorption one deck of inorganic nano nuclear, the stability of effectively improve it is with dispersed.The nanometer spherical grain diameter of preparing is about 8nm～50nm.
Usefulness of the present invention also is: tiny, the evengranular nano stibium powder of particle diameter can be prepared in (1).(2) dispersed better, solved the problem that dentrite that electrochemical process prepares and wet chemical nanometer powder are generally reunited.(3) solved the ubiquitous problem of oxidation of nano-metal particle.
Prepare Nano metal powder with existing protected by organic monomolecular layer and compare, this method have raw material be simple and easy to, characteristics such as technology is simple, cost is low.Prepared nano stibium powder is stable in the air, and particle diameter is even.
Description of drawings
The transmission electron microscope picture of the nanometer spherical antimony powder of Fig. 1 the inventive method preparation, wherein scale is 50nm.
Embodiment
The present invention is a kind of preparation method of powder nanometer antimony mixture, and its preparation process is:
1, at first is mixed with electrolytic solution, 3～6 moles every liter of the content of hydrochloric acid in the electrolytic solution with zero(ppm) water and concentrated hydrochloric acid.Electrolyte quota well after, add the octyl phenol Soxylat A 25-7, the mol ratio of octyl phenol Soxylat A 25-7 and hydrochloric acid is 1: 100～300, then uses magnetic stirring apparatus that electrolytic emulsion is stirred.
2. the emulsion that stirs being injected electrolyzer, is anode with the star antimony, and stainless steel is a negative electrode, and anode is 1: 2～5 with the area ratio of negative electrode, and the pole piece spacing is 20～50mm.
3, electrolytic current density is 0.01A/cm
2～0.2A/cm
2, electrolysis time is 20～120 minutes.Under galvanic effect; Anodic antimony constantly dissolves and gets in the electrolytic solution; Near the negative electrode in the solution antimony ion is constantly separated out again and is deposited on the negative electrode; The octyl phenol Soxylat A 25-7 that is dissolved in the electrolytic solution carries out the original position coating to the antimony atoms of separating out, and the antimony powder loosely that makes generation is attached to cathode surface.Simultaneously near the antimony ion the anode relies on the directional migration of diffusion and electric charge to move near the negative electrode continuously, thereby guarantees electrolyticly to carry out smoothly.
The negative electrode that 4, will adhere to antimony powder is put into absolute ethyl alcohol, puts into ultrasonic cleaner and carries out ultrasonic, desorption, and ultrasonic time is 5～20 minutes, obtains the antimony powder end suspension-s of black.
5, solution is filtered,, can obtain the nano stibium powder end of black filtrate in 60 ℃～100 ℃ vacuum environment dry 1～3 hour.
Be more concrete embodiment below:
Embodiment 1:
Get concentrated hydrochloric acid 250ml, be made into electrolytic solution with 500mL zero(ppm) water.
In above-mentioned electrolytic solution, add 5mL octyl phenol Soxylat A 25-7, under the effect of magnetic stirring apparatus, mix.
With prepared emulsion is electrolytic solution, and star antimony is an anode, and stainless (steel) wire is a negative electrode, prepares nano stibium powder through electrochemical process.Anode is 1: 3 with the area ratio of negative electrode, and the pole piece spacing is 30mm, and cathode current density is 0.015A/cm
2, electrolysis time is 30min.Electrolysis is put into the negative electrode pole piece in the absolute ethyl alcohol after accomplishing, and puts into ultrasonic cleaner and adopts ultra-sonic oscillation to carry out desorption, and the ultra-sonic oscillation time is 5 minutes, obtains black antimony solution.The solution that obtains is filtered, collect the pressed powder of black, use the absolute ethyl alcohol cleaning many times then, 60 ℃ were descended dry 3 hours in vacuum drying oven, promptly obtained black powder nanometer antimony mixture.
Embodiment 2:
Get concentrated hydrochloric acid 180ml, be made into electrolytic solution with 500mL zero(ppm) water.
In above-mentioned electrolytic solution, add 5mL octyl phenol Soxylat A 25-7, under the effect of magnetic stirring apparatus, mix.
With prepared emulsion is electrolytic solution, and star antimony is an anode, and stainless (steel) wire is a negative electrode, prepares nano stibium powder through electrochemical process.Anode is 1: 4 with the area ratio of negative electrode, and the pole piece spacing is 20mm, and cathode current density is 0.05A/cm
2, electrolysis time is 40 minutes.Electrolysis is put into the negative electrode pole piece in the absolute ethyl alcohol after accomplishing, and puts into ultrasonic cleaner and adopts ultra-sonic oscillation to carry out desorption, and the ultra-sonic oscillation time is 5 minutes, obtains black antimony solution.The solution that obtains is filtered, collect the pressed powder of black, use the absolute ethyl alcohol cleaning many times then, 80 ℃ were descended dry 2 hours in vacuum drying oven, promptly obtained black powder nanometer antimony mixture.
Embodiment 3:
Get concentrated hydrochloric acid 400ml, be made into electrolytic solution with 500mL zero(ppm) water.
In above-mentioned electrolytic solution, add 5mL octyl phenol Soxylat A 25-7, under the effect of magnetic stirring apparatus, mix.
With prepared emulsion is electrolytic solution, and star antimony is an anode, and stainless (steel) wire is a negative electrode, prepares nano stibium powder through electrochemical process.Anode is 1: 5 with the area ratio of negative electrode, and the pole piece spacing is 50mm, and cathode current density is 0.15A/cm
2, electrolysis time is 50 minutes.Electrolysis is put into the negative electrode pole piece in the absolute ethyl alcohol after accomplishing, and puts into ultrasonic cleaner and adopts ultra-sonic oscillation to carry out desorption, and the ultra-sonic oscillation time is 5 minutes, obtains black antimony solution.The solution that obtains is filtered, collect the pressed powder of black, use the absolute ethyl alcohol cleaning many times then, 100 ℃ were descended dry 1 hour in vacuum drying oven, promptly obtained black powder nanometer antimony mixture.
Claims (1)
1. the preparation method of a powder nanometer antimony mixture the steps include:
(1) at first is mixed with electrolytic solution with zero(ppm) water and concentrated hydrochloric acid; The content of hydrochloric acid is 3～6 moles every liter in the electrolytic solution, electrolyte quota well after, add the octyl phenol Soxylat A 25-7; The mol ratio of octyl phenol Soxylat A 25-7 and hydrochloric acid is 1: 100～300, then electrolytic emulsion is stirred;
(2) emulsion being injected electrolyzer, is anode with the star antimony, and stainless steel is a negative electrode, and anode is 1: 2～5 with the area ratio of negative electrode, and the pole piece spacing is 20～50mm;
(3) electrolytic current density is 0.01A/cm
2～0.2A/cm
2, electrolysis time is 20～120 minutes; Under galvanic effect; Anodic antimony constantly dissolves and gets in the electrolytic solution; Near the negative electrode in the solution antimony ion is constantly separated out again and is deposited on the negative electrode; The octyl phenol Soxylat A 25-7 that is dissolved in the electrolytic solution carries out the original position coating to the antimony atoms of separating out, and the antimony powder loosely that makes generation is attached to cathode surface; Near the anode antimony ion relies on the directional migration of diffusion and electric charge to move near the negative electrode continuously simultaneously;
The negative electrode that (4) will adhere to antimony powder is put into absolute ethyl alcohol, puts into ultrasonic cleaner and adopts ultra-sonic oscillation to carry out desorption, and the ultra-sonic oscillation time is 5～20 minutes, obtains the antimony solution of black;
(5) solution is filtered,, can obtain black powder nanometer antimony mixture filtrate in 60 ℃～100 ℃ vacuum environment dry 1～3 hour.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102166655B (en) * | 2011-03-17 | 2012-10-31 | 兰州理工大学 | Preparation method for nanometer antimony powder |
| CN105297133B (en) * | 2015-10-28 | 2017-12-12 | 南京理工大学 | A kind of preparation method of the few layer antimony alkene of monocrystalline |
| CN108179441A (en) * | 2017-12-26 | 2018-06-19 | 广西生富锑业科技股份有限公司 | A kind of production method of high purity antimony |
| CN113122889B (en) * | 2021-03-11 | 2022-12-16 | 上海应用技术大学 | Preparation method of silver-polyaniline composite material for solar cell |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1472367A (en) * | 2003-06-16 | 2004-02-04 | 昆明理工恒达科技有限公司 | Preparing method for conductive composite bronze powder and composite bronze conductive sizing agent |
| CN1686645A (en) * | 2005-04-26 | 2005-10-26 | 黄德欢 | Method of preparing nano-bronze powder using electric deposition |
| CN1844473A (en) * | 2005-04-06 | 2006-10-11 | 四川大学 | Electrolytic emulsifying method for grain size controllable copper, silver and etc. ultrafine metal powder |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1472367A (en) * | 2003-06-16 | 2004-02-04 | 昆明理工恒达科技有限公司 | Preparing method for conductive composite bronze powder and composite bronze conductive sizing agent |
| CN1844473A (en) * | 2005-04-06 | 2006-10-11 | 四川大学 | Electrolytic emulsifying method for grain size controllable copper, silver and etc. ultrafine metal powder |
| CN1686645A (en) * | 2005-04-26 | 2005-10-26 | 黄德欢 | Method of preparing nano-bronze powder using electric deposition |
Non-Patent Citations (1)
| Title |
|---|
| 徐建林等."电化学法制备纳米铜粉".《兰州理工大学学报》.2008,第34卷(第3期),第9-11页. |
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