CN102248158A - Preparation method of super-hydrophobic magnetic powder - Google Patents
Preparation method of super-hydrophobic magnetic powder Download PDFInfo
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- CN102248158A CN102248158A CN2011101894116A CN201110189411A CN102248158A CN 102248158 A CN102248158 A CN 102248158A CN 2011101894116 A CN2011101894116 A CN 2011101894116A CN 201110189411 A CN201110189411 A CN 201110189411A CN 102248158 A CN102248158 A CN 102248158A
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Abstract
The invention provides a preparation method of super-hydrophobic magnetic powder, relating to a preparation method of a hydrophobic material. The invention solves the problems that the traditional method is complex in process and a super-hydrophobic material prepared by the traditional method is difficult to separate. One method provided by the invention comprises the following steps of: 1, placing magnetic powder into a solution containing a metal ion capable of taking place a replacement reaction with the magnetic powder, stirring and reacting at room temperature, washing, and drying; and 2, then soaking the dried mixture in a lauric acid solution, and stoving after filtering to obtain a super-hydrophobic magnetic powder material. The other method provided by the invention comprises the following steps of: firstly, sintering ferric acetate, cobalt acetate or nickel acetate; and secondly, soaking the sintered ferric acetate, cobalt acetate or nickel acetate in an organic siloxane solution, filtering and stoving to obtain the super-hydrophobic magnetic powder. In the methods provided by the invention, the low-cost raw materials are adopted, the manufacturing process is simple and convenient, the products are easy to separate and are convenient and fast to use, thus the super-hydrophobic magnetic powder is applicable to mass production.
Description
Patent application of the present invention is to be 201010271708.2 by application number, and the applying date is on 09 03rd, 2010, and denomination of invention is divided an application for the patent of invention of " preparation method of super hydrophobic magnetic powder ".
Technical field
The present invention relates to the preparation method of hydrophobic material.
Background technology
Super hydrophobic material has broad application prospects at aspects such as industry agricultural and national defence, and recently, its performance super-hydrophobic and super oleophylic receives publicity in environmental protection especially.The main preparation principle of super hydrophobic material comprises to be modified with the low-surface-energy material rough surface, perhaps makes up rough surface on the low-surface-energy material.On the preparation method of super hydrophobic material, mainly contain template, etching method, vapour deposition process and photochemical method or the like, but these methods all exist complicated operation, conditional request harshness, shortcomings such as instrument and equipment complexity.At present, super hydrophobic material is mainly used in material surface automatically cleaning, field such as anti-pollution.And do not consider also that in the application aspect environmental protection and the water-oil separating super hydrophobic material is in operability aspect the practical application and agility.
ANGEWANGTE CHEMIE-INTERNATIONAL EDITION magazine (2004,43, one piece of a kind of skin covering of the surface that adopts the super-hydrophobic and super oleophylic of spraying process preparation 2012-2014) once reporting.The material installation complexity that this kind method is used, the complicated difficulty of preparation process and method is controlled, and Zhi Bei super hydrophobic surface film lacks operability in actual applications simultaneously.
Nature nanotechnology magazine (2008,3,332-336) once reported one piece of performance of using the thread film of MnO2 nanometer to have super-hydrophobic and super hydrophilic controlled effect, and this film can adsorb the organic matter than 20 times of weights of material itself.This nano thin-film with controllability can the different organic matter of selective absorption, but is not suitable for extensive large-area processing in actual use, and actual operability is relatively poor, and the film that reclaims adsorb organic compound also is a difficult point.
In sum, the super hydrophobic material of the existing method preparation problem that has complex process, be difficult to separate.
Summary of the invention
Purpose of the present invention is for the super hydrophobic material complex process that solves existing method preparation, the problem that is difficult to separate; And provide the preparation method of super hydrophobic magnetic powder.
The preparation method of super hydrophobic magnetic powder is undertaken by following step among the present invention: one, magnetic powder is placed contain can with the solution of the metal cation salt of magnetic powder generation displacement reaction, the concentration that GOLD FROM PLATING SOLUTION belongs to ion is 0.01～1.0mol/L, stirring reaction 1～60min under the room temperature, spend deionised water to pH value then and be neutrality, oven dry; Two, will place concentration through the magnetic powder that step 1 is handled is that 0.01～1.0mol/L laurate solution soaks 0.5h～2h, and the solvent in the laurate solution is ethanol, methyl alcohol, acetone or toluene, filters the back oven dry and obtains super-hydrophobic magnetic powder material.This method has the feature of super-hydrophobic and super oleophylic.The super-hydrophobic magnetic material that utilizes the method to make can divide dried up and hydrophobic organic compound fast under the effect of magnetic field.The prices of raw and semifnished materials that the present invention adopts are cheap, and preparation method is easy, the super-hydrophobic magnetic material of adsorb organic compound can be separated fast with magnet etc., and are easy to use, are fit to large-scale production.
The preparation method of super hydrophobic magnetic powder of the present invention also can be undertaken by following step: step 1, ferric acetate, cobalt acetate or nickel acetate are placed quartz ampoule, sintering in air or argon atmospher, sintering temperature is 300～800 ℃, sintering time is 1～24 hour, cooling obtains black powder then; It is that 0.01mol/L～1.0mol/L organosiloxane solution soaks 0.5h～2h that step 2, the black powder that step 1 is obtained place concentration, solvent in the organosiloxane solution is ethanol, methyl alcohol, acetone or toluene, filter then, obtain super hydrophobic magnetic powder after the oven dry.This method has the feature of super-hydrophobic and super oleophylic.The super-hydrophobic magnetic material that utilizes the method to make can divide dried up and hydrophobic organic compound fast under the effect of magnetic field.The prices of raw and semifnished materials that the present invention adopts are cheap, and preparation method is easy, the super-hydrophobic magnetic material of adsorb organic compound can be separated fast with magnet etc., and are easy to use, are fit to large-scale production.
Description of drawings
Fig. 1 is the contact angle schematic diagram of water droplet (6ml) at super-hydrophobic micron iron powder material surface; Fig. 2 is the contact angle schematic diagram of water droplet (6ml) at super-hydrophobic nano iron powder material surface; Fig. 3 is that water droplet (6ml) is at super-hydrophobic nano Fe
2O
3The contact angle schematic diagram of-C material surface; Fig. 4 is the contact angle schematic diagram of water droplet (6ml) at super-hydrophobic nano NiO-C material surface; Fig. 5 is the contact angle schematic diagram of water droplet (6ml) at super-hydrophobic nano CoO-C material surface; Fig. 6 is that oil droplet (4ml) is at super-hydrophobic nano Fe
2O
3The contact infiltration schematic flow sheet of-C material surface; Fig. 7 is with the state diagram of lubricating oil in water after the oil red stain dyeing; Fig. 8 is the figure behind the super-hydrophobic magnetic CoO-C powder of adding; Fig. 9 removes super-hydrophobic magnetic CoO-C coatings; Figure 10 is the state diagram behind the super-hydrophobic magnetic CoO-C powder of removal.
The specific embodiment
The specific embodiment one: the preparation method of super hydrophobic magnetic powder is undertaken by following step in the present embodiment: one, magnetic powder is placed contain can with the solution of the metal cation salt of magnetic powder generation displacement reaction, the concentration that GOLD FROM PLATING SOLUTION belongs to ion is 0.01～1.0mol/L, stirring reaction 1～60min under the room temperature, spend deionised water to pH value then and be neutrality, oven dry; Two, will place concentration through the magnetic powder that step 1 is handled is that 0.01～1.0mol/L laurate solution soaks 0.5h～2h, and the solvent in the laurate solution is ethanol, methyl alcohol, acetone or toluene, filters the back oven dry and obtains super-hydrophobic magnetic powder material.
Super-hydrophobic magnetic powder material by the preparation of present embodiment method evenly is sprinkling upon water and hydrophobic organic compound surface, carrying out the visible magnetic powder of agitation as appropriate can not sink at the bottom of the liquid and swim in liquid level, and organic matter carried out selective absorption, use magnet etc. the super-hydrophobic magnetic material of adsorb organic compound can be separated fast then, realized oil/water separating method easy and simple to handle.
The specific embodiment two: what present embodiment and the specific embodiment one were different is: the temperature of drying in the step 1 is 80～90 ℃, and drying the used time is 1～3h.Other step is identical with the specific embodiment one with parameter.
The specific embodiment three: what present embodiment was different with the specific embodiment one or two is: the temperature of drying in the step 2 is 80～90 ℃, and drying the used time is 3～8h.Other step is identical with the specific embodiment one or two with parameter.
The specific embodiment four: what present embodiment was different with one of specific embodiment one to three is: the described magnetic powder of step 1 is micron order iron powder or nano grade iron powder, and containing to be CuSO with the solution of the metal cation salt of magnetic powder generation displacement reaction
4Solution.Other step is identical with one of specific embodiment one to three with parameter.
The specific embodiment five: what present embodiment was different with one of specific embodiment one to three is: the described magnetic powder of step 1 is micron order cobalt powder or nanoscale cobalt powder, and containing to be AgNO with the solution of the metal cation salt of magnetic powder generation displacement reaction
3Solution.Other step is identical with one of specific embodiment one to three with parameter.
The specific embodiment six: what present embodiment was different with one of specific embodiment one to three is: the described magnetic powder of step 1 is micron order nickel powder or nanoscale nickel powder, and containing to be AgNO with the solution of the metal cation salt of magnetic powder generation displacement reaction
3Solution.Other step is identical with one of specific embodiment one to three with parameter.
The specific embodiment seven: the preparation method of super hydrophobic magnetic powder is undertaken by following step in the present embodiment: step 1, ferric acetate, cobalt acetate or nickel acetate are placed quartz ampoule, sintering in air or argon atmospher, sintering temperature is 300～800 ℃, sintering time is 1～24 hour, cooling obtains black powder then; It is that 0.01mol/L～1.0mol/L organosiloxane solution soaks 0.5h～2h that step 2, the black powder that step 1 is obtained place concentration, solvent in the organosiloxane solution is ethanol, methyl alcohol, acetone or toluene, filter then, obtain super hydrophobic magnetic powder after the oven dry.
Super-hydrophobic magnetic powder material by the preparation of present embodiment method evenly is sprinkling upon water and hydrophobic organic compound surface, carrying out the visible magnetic powder of agitation as appropriate can not sink at the bottom of the liquid and swim in liquid level, and organic matter carried out selective absorption, use magnet etc. the super-hydrophobic magnetic material of adsorb organic compound can be separated fast then, realized oil/water separating method easy and simple to handle.
The specific embodiment eight: what present embodiment and the specific embodiment seven were different is: the temperature of drying in the step 2 is 80～90 ℃, and drying the used time is 3～5h.Other step is identical with the specific embodiment seven with parameter.
The specific embodiment nine: the preparation method of super hydrophobic magnetic powder is undertaken by following step in the present embodiment: one, the iron powder of 5.0g 3.4 μ m being placed 200mL concentration is 0.02mol/L CuSO
4In the solution, stirring reaction 30min under the room temperature, it is neutral spending deionised water to pH value then, dries under 80 ℃ of conditions; Two, will place concentration through the magnetic powder that step 1 is handled is that 0.005mol/L laurate ethanolic solution soaks 2h, filters the back oven dry and obtains super-hydrophobic magnetic powder material.
Super-hydrophobic CA=159 ° of the magnetic powder material contact angle (Fig. 1) that present embodiment makes.
Use little basin to contain a little water, on the water surface, drip several edible oils, after treating that organic matter is dizzy and opening, get a little super-hydrophobic iron powder for preparing and be spread on the liquid level, iron powder does not sink, on bubbling through the water column, and affine preferably effect is arranged with organic matter, use magnet that the super-hydrophobic iron powder of adsorb organic compound is separated, liquid level is become totally, reached the effect that water separates with organic matter.
The specific embodiment ten: the preparation method of super hydrophobic magnetic powder is undertaken by following step in the present embodiment: one, the iron powder of 3.0g 100nm being placed 200mL concentration is 0.03mol/L CuSO
4In the solution, stirring reaction 40min under the room temperature, it is neutral spending deionised water to pH value then, dries under 80 ℃ of conditions; Two, will place concentration through the magnetic powder that step 1 is handled is that 0.005mol/L laurate ethanolic solution soaks 50min, filters the back oven dry and obtains super-hydrophobic magnetic powder material.
Super-hydrophobic CA=158 ° of the magnetic powder material contact angle (Fig. 2) that present embodiment makes.
Use little basin to contain a little water, on the water surface, drip several benzinums, after treating that organic matter is dizzy and opening, get a little super-hydrophobic nano iron powder for preparing and be spread on the liquid level, iron powder does not sink, on bubbling through the water column, form affine preferably effect with the organic matter on the water surface, use magnet that the super-hydrophobic nano iron powder of adsorb organic compound is separated, liquid level is become totally very soon, reached the effect that water separates with organic matter.
The specific embodiment 11: the preparation method of super hydrophobic magnetic powder is undertaken by following step in the present embodiment: one, the cobalt powder of 3.0g 200nm being placed 200mL concentration is 0.01mol/L AgNO
3In the solution, stirring reaction 20min under the room temperature, it is neutral spending ion-cleaning to pH value then, dries under 80 ℃ of conditions; Two, will place concentration through the magnetic powder that step 1 is handled is that 0.005mol/L laurate ethanolic solution soaks 50min, filters the back oven dry and obtains super-hydrophobic magnetic powder material.
Use little basin to contain a little water, on the water surface, drip several benzinums, after treating that organic matter is dizzy and opening, get a little super-hydrophobic magnetic cobalt powder for preparing and be spread on the liquid level, powder does not sink, on bubbling through the water column, form affine preferably effect with the organic matter on the water surface, use magnet that the super-hydrophobic nano cobalt powder of adsorb organic compound is separated, liquid level is become totally very soon, reached the effect that water separates with organic matter.
The specific embodiment 12: the preparation method of super hydrophobic magnetic powder is undertaken by following step in the present embodiment: one, the nickel powder of 3.0g 100nm being placed 200mL concentration is 0.02mol/L AgNO
3In the solution, stirring reaction 30min under the room temperature, it is neutral spending ion-cleaning to pH value then, dries under 80 ℃ of conditions; Two, will place concentration through the magnetic powder that step 1 is handled is that 0.01mol/L laurate ethanolic solution soaks 60min, filters the back oven dry and obtains super-hydrophobic magnetic powder material.
Use little basin to contain a little water, on the water surface, drip several benzinums, after treating that organic matter is dizzy and opening, get a little super-hydrophobic magnetic nickel powder for preparing and be spread on the liquid level, powder does not sink, on bubbling through the water column, form affine preferably effect with the organic matter on the water surface, use magnet that the super-hydrophobic nano nickel powder of adsorb organic compound is separated, liquid level is become totally very soon, reached the effect that water separates with organic matter.
The specific embodiment 13: the preparation method of super hydrophobic magnetic powder is undertaken by following step in the present embodiment: step 1, the 5.0g ferric acetate is placed quartz ampoule, sintering in argon atmospher, sintering temperature are 600 ℃, and sintering time is 1 hour, cooling obtains black powder then; It is that 0.01mol/L organosiloxane ethanolic solution soaks 1h that step 2, the black powder that step 1 is obtained place concentration, and the solvent in the organosiloxane solution is an acetone, filters then, obtains super-hydrophobic magnetic Fe after the oven dry
2O
3(particle diameter is 30～200nm) for-C powder.
Super-hydrophobic CA=162 ° of the magnetic powder material contact angle (Fig. 3) that present embodiment makes.
4 μ l oil droplets drop in the process of osmosis on super hydrophobic material surface and see Fig. 6.Oil droplet only needs 4s in the whole process of osmosis of material surface, illustrates that super hydrophobic material has good lipophile, is fit to be used for carry out water oil and separates.
Use little basin to contain a little water, on the water surface, drip several benzinums, after treating that organic matter is dizzy and opening, get the super-hydrophobic magnetic Fe that a little prepares
2O
3-C powder is spread on the liquid level, and powder does not sink, and on bubbling through the water column, with the affine preferably effect of organic matter film formation on the water surface, uses the super-hydrophobic nano Fe of magnet with adsorb organic compound
2O
3-C powder separation becomes totally liquid level very soon, has reached the effect that water separates with organic matter.
The specific embodiment 14: the preparation method of super hydrophobic magnetic powder is undertaken by following step in the present embodiment: step 1, the 5.0g nickel acetate is placed quartz ampoule, sintering in argon atmospher, sintering temperature are 400 ℃, and sintering time is 1 hour, cooling obtains black powder then; It is that 0.01mol/L organosiloxane ethanolic solution soaks 1h that step 2, the black powder that step 1 is obtained place concentration, solvent in the organosiloxane solution is a toluene, filter then, obtain super-hydrophobic magnetic NiO-C powder (particle diameter is at 50-250nm) after the oven dry.
Super-hydrophobic CA=152 ° of the magnetic powder material contact angle (Fig. 4) that present embodiment makes
Use little basin to contain a little water, on the water surface, drip several benzinums, after treating that organic matter is dizzy and opening, get a little super-hydrophobic magnetic NiO-C powder for preparing and be spread on the liquid level, powder does not sink, on bubbling through the water column, form affine preferably effect with the organic matter film on the water surface, use the super-hydrophobic nano NiO-C powder separation of magnet, liquid level is become totally very soon, reached the effect that water separates with organic matter adsorb organic compound.
The specific embodiment 15: the preparation method of super hydrophobic magnetic powder is undertaken by following step in the present embodiment: step 1, the 5.0g cobalt acetate is placed quartz ampoule, sintering in argon atmospher, sintering temperature are 400 ℃, and sintering time is 1 hour, cooling obtains black powder then; It is that 0.01mol/L organosiloxane ethanolic solution soaks 1h that step 2, the black powder that step 1 is obtained place concentration, solvent in the organosiloxane solution is an ethanol, filter then, obtain super-hydrophobic magnetic CoO-C powder (particle diameter is at 30-250nm) after the oven dry.
Super-hydrophobic CA=162 ° of the magnetic powder material contact angle (Fig. 5) that present embodiment makes
Use little basin to contain a little water, at the lubricating oil that splashes on the water surface after oil red stain dyeing, treat the dizzy (see figure 7) afterwards of opening of organic matter, getting a little super-hydrophobic magnetic CoO-C powder for preparing is spread on the liquid level, powder does not sink, on bubbling through the water column, form affine preferably effect (see figure 8) with the organic matter film on the water surface, use the super-hydrophobic nano CoO-C powder separation (see figure 9) of magnet with adsorb organic compound, make the liquid level clean (see figure 10) that becomes very soon, reached the effect that water separates with organic matter.
Claims (2)
1. the preparation method of super hydrophobic magnetic powder, the preparation method who it is characterized in that super hydrophobic magnetic powder is undertaken by following step: step 1, with a kind of quartz ampoule that places in ferric acetate, cobalt acetate and the nickel acetate, sintering in air or argon atmospher, sintering temperature is 300～800 ℃, sintering time is 1～24 hour, cooling obtains black powder then; It is that 0.01mol/L～1.0mol/L organosiloxane solution soaks 0.5h～2h that step 2, the black powder that step 1 is obtained place concentration, solvent in the organosiloxane solution is ethanol, methyl alcohol, acetone or toluene, filter then, obtain super hydrophobic magnetic powder after the oven dry.
2. the preparation method of super hydrophobic magnetic powder according to claim 1 is characterized in that the temperature of drying in the step 2 is 80～90 ℃, time 3～8h.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0261579A1 (en) * | 1986-09-16 | 1988-03-30 | Tokin Corporation | A method for producing a rare earth metal-iron-boron permanent magnet by use of a rapidly-quenched alloy powder |
| EP0686704A1 (en) * | 1994-06-10 | 1995-12-13 | Sandvik Aktiebolag | Method of preparing powders for hard materials |
| CN1928158A (en) * | 2006-09-15 | 2007-03-14 | 哈尔滨工业大学 | Method for constructing super-drainage structure on metal copper surface |
| CN101143734A (en) * | 2007-09-13 | 2008-03-19 | 河南科技大学 | Method for preparing lithium ionic cell nano-crystal nickel oxide anode material |
| CN101417823A (en) * | 2008-11-14 | 2009-04-29 | 中国科学院上海硅酸盐研究所 | Wet chemical preparation method of nickel oxide hollow microsphere without template |
-
2010
- 2010-09-03 CN CN2011101894116A patent/CN102248158A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0261579A1 (en) * | 1986-09-16 | 1988-03-30 | Tokin Corporation | A method for producing a rare earth metal-iron-boron permanent magnet by use of a rapidly-quenched alloy powder |
| EP0686704A1 (en) * | 1994-06-10 | 1995-12-13 | Sandvik Aktiebolag | Method of preparing powders for hard materials |
| CN1928158A (en) * | 2006-09-15 | 2007-03-14 | 哈尔滨工业大学 | Method for constructing super-drainage structure on metal copper surface |
| CN101143734A (en) * | 2007-09-13 | 2008-03-19 | 河南科技大学 | Method for preparing lithium ionic cell nano-crystal nickel oxide anode material |
| CN101417823A (en) * | 2008-11-14 | 2009-04-29 | 中国科学院上海硅酸盐研究所 | Wet chemical preparation method of nickel oxide hollow microsphere without template |
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Application publication date: 20111123 |