CN102126730B - Method for preparing copper borate/SiO2 composite particles - Google Patents
Method for preparing copper borate/SiO2 composite particles Download PDFInfo
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- CN102126730B CN102126730B CN 201010583365 CN201010583365A CN102126730B CN 102126730 B CN102126730 B CN 102126730B CN 201010583365 CN201010583365 CN 201010583365 CN 201010583365 A CN201010583365 A CN 201010583365A CN 102126730 B CN102126730 B CN 102126730B
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- composite particles
- nitrate solution
- copper borate
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Abstract
The invention discloses a method for preparing copper borate/SiO2 composite particles with shells in different thickness through ultrasonic dispersion. The method comprises: based on utilizing water as a dispersion medium, uniformly mixing borax solution and copper nitrate solution which are prepared through ultrasonic dispersion to prepare copper borate particles, filtering, washing and dispersing the reaction mixture to absolute ethyl alcohol or n-butyl alcohol in an ultrasonic manner and adding tetraethoxysilane to the mixture and mixing the mixture uniformly, adding ammonia water to control the pH value and obtaining the SiO2 covered copper borate particles through ultrasonic treatment. The method has the advantages of reaction without heating, simple and convenient synthetic process, environment-friendly reaction media and the like.
Description
Technical field
The present invention relates to a kind of copper borate/SiO
2The preparation method of composite particles, specifically, the present invention relates to a kind of is that dispersion medium at room temperature prepares copper borate/SiO with water, absolute ethyl alcohol or propyl carbinol
2The method of composite particles.
Background technology
Borate can be used for many-sided researchs such as optics, tribology and fire retardant material.The research that borate is used for oil dope starts from eighties of last century.In recent years, the borate of bibliographical information nanostructure industriallization [Huang Wenxuan, lubricant additive application guide, Sinopec press, 2004].
Along with the continuous development of synthetic technology, people utilize the borate of the synthetic nano-micro structure of multiple means, prepare borate such as methods such as hydrothermal method, microemulsion method, collosol and gel and solid reaction processes.People such as Tian Yumei [Tian Yumei, the synthetic and performance study of inorganic nano oil dope, Jilin University's doctorate paper, 2006] have successfully prepared the zinc borate Nano microsphere through microemulsion method, find that this microballoon has good friction reducing effect in base oil.
Hud typed composite particles is to serve as nuclear and with other a kind of material particulate that is shell, shell can be that inorganics also can be organic and macromolecular material with a kind of material.Hud typed composite particles receives people's attention because of the performance that can have two kinds of materials simultaneously.
Summary of the invention
To the deficiency of prior art, the object of the present invention is to provide a kind of is nuclear with the copper borate, with SiO
2Preparing method for the composite particles of shell.
The present invention realizes through following measure:
A kind of copper borate/SiO
2The preparation method of composite particles, step is following:
(1) ultra-sonic dispersion prepares borax soln and copper nitrate solution, and borax soln and copper nitrate solution are fully mixed to system appearance deposition, and sedimentation and filtration, washing are obtained filter cake;
(2) with the filter cake ultra-sonic dispersion in absolute ethyl alcohol or propyl carbinol, add tetraethoxy and mix, add alkaline matter then and regulate the pH value, supersound process obtains copper borate/SiO
2Composite particles.The prepared composite particulate is between 20nm-70nm.
Aforesaid preparation method, preferably scheme is, and the concentration of the said copper nitrate solution of step (1) is 0.8-1.1mol/L, and the concentration of said borax soln is 0.09-0.11mol/L.More preferably, the concentration of said copper nitrate solution is 1.0mol/L, and the concentration of said borax soln is 0.10mol/L.
Aforesaid preparation method, preferred scheme is that the mol ratio of cupric nitrate and borax is 1 in the said system of step (1): 1-1.2.
Aforesaid preparation method, preferred scheme is that step obtains filter cake with absolute ethanol washing in (1).
Aforesaid preparation method, preferred scheme is that the mol ratio of said tetraethoxy of step (2) and borax is 0.04-0.13: 1.
Aforesaid preparation method, preferred scheme are that the said alkaline matter of step (2) is an ammoniacal liquor, regulates the pH value between 8-10.More preferably, regulate pH=9.
Aforesaid preparation method, preferred scheme is that the said supersound process time of step (2) is not less than 10min.More preferably, said supersound process time is 10-20min.
Aforesaid preparation method, in the preferred scheme, ultrasonic frequency is controlled to be 30-50KHz, more preferably 40KHz.
The present invention obtains borax soln and copper nitrate solution through ultra-sonic dispersion, borax soln and copper nitrate solution thorough mixing is obtained the copper borate of nano-micro structure.Reaction mixture filtration washing ultra-sonic dispersion in absolute ethyl alcohol or propyl carbinol, is added tetraethoxy and mixes.Add ammoniacal liquor control pH value, ultrasonic obtaining through SiO
2The copper borate particulate that coats.The present invention prepares borate/SiO with ultrasonic dispersion
2Have special advantages, such as solute can fully disperse, easy reliable, the good reproducibility of preparation method etc.All reactions of the present invention are at room temperature carried out, and reaction is a dispersion medium with water, ethanol or propyl carbinol.Obtain the SiO of different thickness through the add-on of control tetraethoxy
2Shell, prepared composite particles is between 20nm-70nm.This method has reaction and at room temperature carries out (not needing heating), and synthesis technique is easy, advantages such as environmental protection.
In addition, technical superiority of the present invention also is embodied in:
1, shell SiO
2Thickness can be controlled easy handling through the add-on of tetraethoxy.
2, used dispersion medium environmental protection.
3, the coating of shell can be controlled through the pH value, is convenient to implement.
Description of drawings
Fig. 1 is embodiment 3 gained copper borate/SiO
2Composite particles TEM photo.
Embodiment
Specify technical scheme of the present invention below in conjunction with accompanying drawing and embodiment, but protection domain is not limited thereto.
The raw materials used commercial goods that is all among the embodiment, raw material is easy to get.If amplifying, industrializing implementation, equal proportion get final product.
General operation of the present invention: a kind of copper borate/SiO
2The preparation method of composite particles, step is following: (1) ultra-sonic dispersion prepares borax soln and copper nitrate solution, and borax soln and copper nitrate solution are fully mixed to system appearance deposition, and sedimentation and filtration, washing are obtained filter cake; (2) with the filter cake ultra-sonic dispersion in absolute ethyl alcohol or propyl carbinol, add tetraethoxy and mix, add alkaline matter then and regulate the pH value, supersound process obtains copper borate/SiO
2Composite particles.
The hydrolysis of tetraethoxy elder generation generates single silicic acid, and condensation obtains SiO between the silicic acid
2Silicon-dioxide is electronegative under alkaline condition, and the mountain forms covalent linkage in the coating that electrostatic attraction obtains the copper borate surface.More its coating thicknesses of tetraethoxy that add are big more.
Embodiment 1: ultra-sonic dispersion prepares copper nitrate solution 3ml and the 0.09mol/L borax soln 30ml of 0.8mol/L.Deposition is appearred in two kinds of solution mixed systems, with sedimentation and filtration, obtain filter cake with absolute ethanol washing.The filter cake ultra-sonic dispersion in absolute ethyl alcohol, is added the 3ml tetraethoxy.In system, add ammoniacal liquor and make the pH value of system equal 8, at room temperature ultrasonic then 15min.Obtain spherical copper borate/SiO
2Particulate, the about 5nm of the about 50nm shell thickness of diameter of particle.
Embodiment 2: ultra-sonic dispersion prepares copper nitrate solution 3ml and the 0.11mol/L borax soln 30ml of 1.1mol/L.Deposition is appearred in two kinds of solution mixed systems, with sedimentation and filtration, obtain filter cake with absolute ethanol washing.The filter cake ultra-sonic dispersion in propyl carbinol, is added the 5ml tetraethoxy.In system, add ammoniacal liquor and make the pH value of system equal 10, at room temperature ultrasonic then 10min.Obtain spherical copper borate/SiO
2Particulate, the about 10nm of the about 50nm shell thickness of diameter of particle.
Embodiment 3: ultra-sonic dispersion prepares copper nitrate solution 3ml and the 0.10mol/L borax soln 30ml of 1.0mol/L.Deposition is appearred in two kinds of solution system that mixes, with sedimentation and filtration, obtain filter cake with absolute ethanol washing.The filter cake ultra-sonic dispersion in propyl carbinol, is added the 4ml tetraethoxy.In system, add ammoniacal liquor and make the pH value of system equal 9, at room temperature ultrasonic then 20min.Obtain spherical copper borate/SiO
2Particulate, the about 10nm of the about 50nm shell thickness of diameter of particle.
Fig. 1 is embodiment 3 gained copper borate/SiO
2Composite particles TEM photo, this explains SiO
2Successfully be coated on the about 10nm of surface crust thickness of copper borate.
Claims (9)
1. copper borate/SiO
2The preparation method of composite particles is characterized in that, step is following:
(1) ultra-sonic dispersion prepares borax soln and copper nitrate solution, and borax soln and copper nitrate solution are fully mixed to system appearance deposition, and sedimentation and filtration, washing are obtained filter cake;
(2) with the filter cake ultra-sonic dispersion in absolute ethyl alcohol or propyl carbinol, add tetraethoxy and mix, add alkaline matter then and regulate the pH value, supersound process obtains copper borate/SiO
2Composite particles.
2. the described preparation method of claim 1 is characterized in that, the concentration of the said copper nitrate solution of step (1) is 0.8-1.1mol/L, and the concentration of said borax soln is 0.09-0.11mol/L.
3. the described preparation method of claim 2 is characterized in that, the concentration of said copper nitrate solution is 1.0mol/L, and the concentration of said borax soln is 0.10mol/L.
4. the described preparation method of claim 1 is characterized in that, the mol ratio of cupric nitrate and borax is 1 in the said system of step (1): 1-1.2.
5. the described preparation method of claim 1 is characterized in that, step obtains filter cake with absolute ethanol washing in (1).
6. the described preparation method of claim 1 is characterized in that, the said alkaline matter of step (2) is an ammoniacal liquor, regulates the pH value between 8-10.
7. the described preparation method of claim 6 is characterized in that, regulates pH=9.
8. the described preparation method of claim 1 is characterized in that, the said supersound process time of step (2) is not less than 10min.
9. the described preparation method of claim 8 is characterized in that, the said supersound process time is 10-20min.
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| CN 201010583365 CN102126730B (en) | 2010-12-13 | 2010-12-13 | Method for preparing copper borate/SiO2 composite particles |
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| CN 201010583365 CN102126730B (en) | 2010-12-13 | 2010-12-13 | Method for preparing copper borate/SiO2 composite particles |
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| CN102126730B true CN102126730B (en) | 2012-12-12 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4292382A (en) * | 1979-06-27 | 1981-09-29 | Saft Leclanche | Positive active material for an electric cell, a method of preparing the positive active material and a cell which uses it |
| US4913886A (en) * | 1989-06-05 | 1990-04-03 | Amoco Corporation | Production of improved copper aluminum borate |
| CN101254927A (en) * | 2008-03-28 | 2008-09-03 | 江南大学 | Method for preparing active zinc borate by one-step proccess |
| CN101343774A (en) * | 2008-08-26 | 2009-01-14 | 吉林大学 | Preparation of hydrophobic nature nano boric acid copper crystal whisker with in situ one-step method |
-
2010
- 2010-12-13 CN CN 201010583365 patent/CN102126730B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4292382A (en) * | 1979-06-27 | 1981-09-29 | Saft Leclanche | Positive active material for an electric cell, a method of preparing the positive active material and a cell which uses it |
| US4913886A (en) * | 1989-06-05 | 1990-04-03 | Amoco Corporation | Production of improved copper aluminum borate |
| CN101254927A (en) * | 2008-03-28 | 2008-09-03 | 江南大学 | Method for preparing active zinc borate by one-step proccess |
| CN101343774A (en) * | 2008-08-26 | 2009-01-14 | 吉林大学 | Preparation of hydrophobic nature nano boric acid copper crystal whisker with in situ one-step method |
Non-Patent Citations (1)
| Title |
|---|
| 胡泽善等.纳米硼酸铜颗粒的制备及其用作润滑油添加剂的摩擦学性能.《摩擦学学报》.2000,第20卷(第4期),第292-295页. * |
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