CN103273075A - HPAA nano-iron particle dispersing method - Google Patents
HPAA nano-iron particle dispersing method Download PDFInfo
- Publication number
- CN103273075A CN103273075A CN2013101706883A CN201310170688A CN103273075A CN 103273075 A CN103273075 A CN 103273075A CN 2013101706883 A CN2013101706883 A CN 2013101706883A CN 201310170688 A CN201310170688 A CN 201310170688A CN 103273075 A CN103273075 A CN 103273075A
- Authority
- CN
- China
- Prior art keywords
- iron
- hpaa
- nano
- iron particle
- solution
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Abstract
The invention discloses an HPAA nano-iron particle dispersing method and relates to an iron particle dispersing method. The nano-iron particle material prepared with the method belongs to nomo-metal materials prepared with the chemical method. According to the HPAA nano-iron particle dispersing method, soluble ferrous iron or trivalent iron is dissolved in distilled water (or mixed liquor of distilled water and ethyl alcohol) in a salting-in mode by adding of a certain dispersing agent and with the liquid phase chemical reduction method to form ferric salt solution, iron ions are then directly reduced to zero-valent iron by means of a reducing agent with a strong reducing property such as hydroboron, the product obtained in this way is treated with vacuum drying after being filtered and washed, and then a nano-iron powder material with good dispersing performance and a nanometer microstructure is obtained. The nano-iron particle prepared with the method is spherical, small in diameter, small in particle size range and oxidation resistant. The method is simple and easy to realize, the whole technological process is easy to control, the method can be carried out at normal temperatures and pressures, the problem of agglomeration of nano-iron is solved, and actual production requirements are met.
Description
Technical field
The present invention relates to a kind of nano iron particles preparation method, particularly relate to a kind of method of HPAA dispersing nanometer iron particle.
Background technology
Usually particle size is called nano material at powder or the material of 1~100 nanometer (nm) scope.Nano material all has a wide range of applications in every field because of its unique character.Nanometer iron is because of its transitional region between the elementide of the conventional fine powder of macroscopic view and microcosmic, so present some unique character, one of them important characteristic is exactly skin effect.Because particle diameter is little, specific area is big, and surface-active is strong, and nanometer iron has in the pollutant reparation than common iron powder special advantages more.The external a lot of nanometer iron that studies show that can reduce many pollutants in the removal water, as dissolving, property organic chloride, PCBs and nitrobenzene compounds etc.
Because nanometer abrasive grit footpath is little, active strong, therefore easily coalescent, easy oxidation often is that existing usefulness is now made, all must starvation in preparation and when using, use inconvenient, the cost height, therefore, be restricted in actual applications, preparation method commonly used at present has physics method and chemical method.Certain methods is possible in theory, but the practical operation conditional request is very high, is not easy to accomplish.
Summary of the invention
The object of the present invention is to provide a kind of method of HPAA dispersing nanometer iron particle, utilize solvent directly in the liquid reduction process, to add dispersant, effectively stop the reunion of nano iron particles, directly add dispersant in the liquid reduction process, this nanometer iron powder end particle diameter can solve the agglomeration traits that produces in nanometer iron production process below 100nm, make the nanometer abrasive grit footpath of producing little, be uniformly dispersed, particle size range is narrow, has the favorable actual application effect.
The objective of the invention is to be achieved through the following technical solutions:
A kind of method of HPAA dispersing nanometer iron particle, described method comprises following process:
(1) be raw material with solubility ferrous iron or trivalent iron salt, with distilled water or distilled water and alcohol mixed solution, its volume ratio is 7:3, configuration solution, and making wherein, iron concentration reaches 0.2-2mol/L;
(2) in (1), add surfactant, make its concentration reach 0.2-0.4g/L, add complexing agent and make its concentration reach 0.002-0.005g/L;
(3) in (2), add dispersant, make its mass concentration reach 0.05-1%;
(4) the configuration boron hydride aqueous solution, making its concentration is 0.02-0.1mol/L;
(5) gained solution is under the stirring in (3), and to wherein splashing into solution (4), dripping speed is 1-10ml/s, and the course of reaction temperature is room temperature, drips solution (4) to reacting completely;
(6) after (5) process finished, the gained product was carried out suction filtration, and repeatedly washs with distilled water and absolute ethyl alcohol;
(7) products therefrom namely obtains black and disperses nano iron particles through 60 ℃ of vacuum drying 10-24h.
The method of described a kind of HPAA dispersing nanometer iron particle, described divalent iron salt is frerrous chloride, described trivalent iron salt is ferric sulfate or iron chloride.
The method of described a kind of HPAA dispersing nanometer iron particle, described surfactant is soluble starch.
The method of described a kind of HPAA dispersing nanometer iron particle, described complexing agent is citric acid.
The method of described a kind of HPAA dispersing nanometer iron particle, described dispersant are HPAA(2-hydroxyl phosphoryl acetic acid).
The method of described a kind of HPAA dispersing nanometer iron particle, described reducing agent is sodium borohydride or potassium borohydride.
Advantage of the present invention and effect are:
1, He Cheng nano iron particles dispersion of materials is functional, effectively solves the nano iron particles agglomeration traits; And the product purity height, particle diameter is little, and epigranular has certain non-oxidizability;
2, synthetic route is simple, and technical process control easily;
3, carry out the production preparation process under the normal temperature and pressure, meet the production actual needs.
The specific embodiment
The present invention is described in detail below in conjunction with embodiment.
Embodiment 1:
Preparation dispersing nanometer iron particle, preparation process is:
(1) takes by weighing iron chloride, it is dissolved in the distilled water, be made into the solution that iron concentration is 0.8 mol;
(2) in (1), add the surfactant soluble starch in the gained solution, make its concentration reach 0.4 grams per liter, add the complexing agent citric acid, make its concentration reach 0.004 grams per liter;
(3) with HPAA(2-hydroxyl phosphoryl acetic acid) add in (2) gained solution after 100 times of the stoste dilutions, make its mass concentration reach 0.05%.
(4) take by weighing sodium borohydride and be dissolved in the distilled water, be made into the solution that sodium borohydride content is 0.02 mol;
(5) be under the stirring at (3) gained solution, solution (4) splashed into carry out reduction reaction, rate of addition is 5 milliliters/second, and temperature control is at 20 degrees centigrade, until reacting completely in the course of reaction;
(6) after (5) reaction finishes, the solid product suction filtration that reaction is obtained, and with distilled water drip washing product three times, absolute ethyl alcohol drip washing product three times;
(7) with (6) products therefrom in 60 degrees centigrade of vacuum drying 10h, can obtain the finely dispersed nano iron particles of black.
Embodiment 2:
Preparation dispersing nanometer iron particle, preparation process is:
(1) takes by weighing ferric sulfate, it is dissolved in distilled water and absolute ethyl alcohol mixed solution (in the volume ratio=7:3), is made into the solution that iron concentration is 0.2 mol;
(2) in (1), add the surfactant soluble starch in the gained solution, make its concentration reach 0.2 grams per liter, add the complexing agent citric acid, make its concentration reach 0.002 grams per liter;
(3) with HPAA(2-hydroxyl phosphoryl acetic acid) add in (2) gained solution after 100 times of the stoste dilutions, make its content reach the 1:1000(volume ratio);
(4) take by weighing sodium borohydride and be dissolved in the distilled water, be made into the solution that sodium borohydride content is 0.02 mol;
(5) be under the stirring at (3) gained solution, solution (4) splashed into carry out reduction reaction, rate of addition is 5 milliliters/second, and temperature control is at 20 degrees centigrade, until reacting completely in the course of reaction;
(6) after (5) reaction finishes, the solid product suction filtration that reaction is obtained, and with distilled water drip washing product three times, absolute ethyl alcohol drip washing product three times;
(7) with (6) products therefrom in 60 degrees centigrade of vacuum drying 24h, can obtain the finely dispersed nano iron particles of black.
Embodiment 3:
Preparation dispersing nanometer iron particle, preparation process is:
(1) takes by weighing frerrous chloride, it is dissolved in the distilled water, be made into the solution that iron concentration is 1.6 mol;
(2) in (1), add the surfactant soluble starch in the gained solution, make its concentration reach 0.4 grams per liter, add the complexing agent citric acid, make its concentration reach 0.004 grams per liter;
(3) with HPAA(2-hydroxyl phosphoryl acetic acid) add in (2) gained solution after 100 times of the stoste dilutions, make its mass concentration reach 0.05%;
(4) take by weighing potassium borohydride and be dissolved in the distilled water, be made into the solution that potassium borohydride content is 0.02 mol;
(5) be under the stirring at (3) gained solution, solution (4) splashed into carry out reduction reaction, rate of addition is 10 milliliters/second, and temperature control is at 20 degrees centigrade, until reacting completely in the course of reaction;
(6) after (5) reaction finishes, the solid product suction filtration that reaction is obtained, and with distilled water drip washing product three times, absolute ethyl alcohol drip washing product three times;
(7) with (6) products therefrom in 60 degrees centigrade of vacuum drying 24h, can obtain the finely dispersed nano iron particles of black.
Claims (6)
1. the method for a HPAA dispersing nanometer iron particle is characterized in that described method comprises following process:
(1) be raw material with solubility ferrous iron or trivalent iron salt, with distilled water or distilled water and alcohol mixed solution, its volume ratio is 7:3, configuration solution, and making wherein, iron concentration reaches 0.2-2mol/L;
(2) in (1), add surfactant, make its concentration reach 0.2-0.4g/L, add complexing agent and make its concentration reach 0.002-0.005g/L;
(3) in (2), add dispersant, make its mass concentration reach 0.05-1%;
(4) the configuration boron hydride aqueous solution, making its concentration is 0.02-0.1mol/L;
(5) gained solution is under the stirring in (3), and to wherein splashing into solution (4), dripping speed is 1-10ml/s, and the course of reaction temperature is room temperature, drips solution (4) to reacting completely;
(6) after (5) process finished, the gained product was carried out suction filtration, and repeatedly washs with distilled water and absolute ethyl alcohol;
(7) products therefrom namely obtains black and disperses nano iron particles through 60 ℃ of vacuum drying 10-24h.
2. the method for a kind of HPAA dispersing nanometer iron particle according to claim 1 is characterized in that, described divalent iron salt is frerrous chloride, and described trivalent iron salt is ferric sulfate or iron chloride.
3. the method for a kind of HPAA dispersing nanometer iron particle according to claim 1 is characterized in that, described surfactant is soluble starch.
4. the method for a kind of HPAA dispersing nanometer iron particle according to claim 1 is characterized in that, described complexing agent is citric acid.
5. the method for a kind of HPAA dispersing nanometer iron particle according to claim 1 is characterized in that, described dispersant is HPAA(2-hydroxyl phosphoryl acetic acid).
6. the method for a kind of HPAA dispersing nanometer iron particle according to claim 1 is characterized in that, described reducing agent is sodium borohydride or potassium borohydride.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN2013101706883A CN103273075A (en) | 2013-05-10 | 2013-05-10 | HPAA nano-iron particle dispersing method |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN2013101706883A CN103273075A (en) | 2013-05-10 | 2013-05-10 | HPAA nano-iron particle dispersing method |
Publications (1)
Publication Number | Publication Date |
---|---|
CN103273075A true CN103273075A (en) | 2013-09-04 |
Family
ID=49055753
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN2013101706883A Pending CN103273075A (en) | 2013-05-10 | 2013-05-10 | HPAA nano-iron particle dispersing method |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN103273075A (en) |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103551590A (en) * | 2013-11-06 | 2014-02-05 | 沈阳化工大学 | Method for preparing dispersed iron nanoparticles from caprolactam type ionic liquid |
CN103611944A (en) * | 2013-11-26 | 2014-03-05 | 沈阳化工大学 | Preparation method of ClO3- ionic liquid dispersed iron nanoparticles |
CN103769599A (en) * | 2014-01-06 | 2014-05-07 | 沈阳化工大学 | Disperse nano-iron particle preparing method |
CN103785849A (en) * | 2014-01-06 | 2014-05-14 | 沈阳化工大学 | Preparation method of TH-908 dispersed iron nano-particles |
CN104999087A (en) * | 2015-06-26 | 2015-10-28 | 沈阳化工大学 | Method for preparing dispersed nano-iron particles by means of SBA-15 |
CN105081340A (en) * | 2014-05-07 | 2015-11-25 | 沈阳农业大学 | Dispersed nano iron particle and preparation method thereof |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
KR20090055380A (en) * | 2007-11-28 | 2009-06-02 | 광주과학기술원 | Methods of controllable synthesis of nanoscale zerovalent iron |
CN102133646A (en) * | 2011-03-23 | 2011-07-27 | 沈阳化工大学 | Preparation method of dispersed iron nanoparticles |
CN102208563A (en) * | 2011-04-18 | 2011-10-05 | 电子科技大学 | Substrate for flexible luminescent device and preparation method thereof |
CN101844230B (en) * | 2010-05-19 | 2012-11-14 | 华南师范大学 | Nano zero-valent iron prepared by using iron and steel acid-cleaning wastewater and preparation method and application thereof |
-
2013
- 2013-05-10 CN CN2013101706883A patent/CN103273075A/en active Pending
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
KR20090055380A (en) * | 2007-11-28 | 2009-06-02 | 광주과학기술원 | Methods of controllable synthesis of nanoscale zerovalent iron |
CN101844230B (en) * | 2010-05-19 | 2012-11-14 | 华南师范大学 | Nano zero-valent iron prepared by using iron and steel acid-cleaning wastewater and preparation method and application thereof |
CN102133646A (en) * | 2011-03-23 | 2011-07-27 | 沈阳化工大学 | Preparation method of dispersed iron nanoparticles |
CN102208563A (en) * | 2011-04-18 | 2011-10-05 | 电子科技大学 | Substrate for flexible luminescent device and preparation method thereof |
Non-Patent Citations (2)
Title |
---|
张光华: "《水处理化学品制备与应用指南》", 31 October 2003, 中国石化出版社 * |
王超等: "不同分散剂对纳米铁粉分散性能的影响", 《铸造技术》 * |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103551590A (en) * | 2013-11-06 | 2014-02-05 | 沈阳化工大学 | Method for preparing dispersed iron nanoparticles from caprolactam type ionic liquid |
CN103611944A (en) * | 2013-11-26 | 2014-03-05 | 沈阳化工大学 | Preparation method of ClO3- ionic liquid dispersed iron nanoparticles |
CN103769599A (en) * | 2014-01-06 | 2014-05-07 | 沈阳化工大学 | Disperse nano-iron particle preparing method |
CN103785849A (en) * | 2014-01-06 | 2014-05-14 | 沈阳化工大学 | Preparation method of TH-908 dispersed iron nano-particles |
CN105081340A (en) * | 2014-05-07 | 2015-11-25 | 沈阳农业大学 | Dispersed nano iron particle and preparation method thereof |
CN104999087A (en) * | 2015-06-26 | 2015-10-28 | 沈阳化工大学 | Method for preparing dispersed nano-iron particles by means of SBA-15 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN102133646B (en) | Preparation method of dispersed iron nanoparticles | |
CN103273077A (en) | Preparing method of [Bmim] BF4 dispersed nano-iron particle | |
CN103273076A (en) | HDTMPA K6 nano-iron particle dispersing method | |
CN103273075A (en) | HPAA nano-iron particle dispersing method | |
CN103769599A (en) | Disperse nano-iron particle preparing method | |
CN105798320B (en) | A kind of method of low temperature preparation copper nanoparticle | |
CN101554664B (en) | Method for preparing nano-scale silver powder | |
CN103599737B (en) | One has carbon shell magnetic Nano material and preparation method | |
CN101716685B (en) | Method for preparing spherical superfine silver powder by using chemical reduction method | |
CN104014811B (en) | A kind of octreotide acetate that utilizes is for the method for Template preparation coralloid nano cobalt | |
CN103466702B (en) | Method for preparing porous bismuth oxide nano-material without template | |
CN103058278B (en) | Preparation method of tin antimony oxide nano-powder | |
CN104722276B (en) | A kind of melon ring/graphene oxide magnetic composite and preparation method thereof | |
CN104190423B (en) | A kind of spherical shape α-Fe2O3Preparation method | |
CN104028269A (en) | Graphene loaded metal nano composite material, and preparation method and application thereof | |
CN101497135A (en) | Method for preparing spherical silver nano granule | |
CN103611944A (en) | Preparation method of ClO3- ionic liquid dispersed iron nanoparticles | |
CN104310468B (en) | One prepares the method for monodisperse titanium dioxide (B) nanoparticle | |
CN102627330A (en) | Preparation method of nanometer trimanganese tetroxide | |
CN105271430A (en) | Preparation method of modified super-dispersed ferriferrous oxide | |
CN105417570A (en) | Method for preparing spinel-type complex oxide through co-precipitation, homogenization and spray drying | |
CN104860357B (en) | Mono-dispersed nano sheet and/or nano-rings and preparation thereof and application | |
CN110407238A (en) | A kind of method that crystal seed method prepares flaky alpha-alumina crystals | |
CN105462365A (en) | Electric conduction nanometer copper ink preparation method | |
CN104999087A (en) | Method for preparing dispersed nano-iron particles by means of SBA-15 |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
C06 | Publication | ||
PB01 | Publication | ||
C10 | Entry into substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
C05 | Deemed withdrawal (patent law before 1993) | ||
WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20130904 |