CN108404825B - Nano iron powder microencapsulation method - Google Patents
Nano iron powder microencapsulation method Download PDFInfo
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- CN108404825B CN108404825B CN201810175554.3A CN201810175554A CN108404825B CN 108404825 B CN108404825 B CN 108404825B CN 201810175554 A CN201810175554 A CN 201810175554A CN 108404825 B CN108404825 B CN 108404825B
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- iron powder
- ethyl cellulose
- nano iron
- microencapsulation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/06—Making microcapsules or microballoons by phase separation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
- B22F1/102—Metallic powder coated with organic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
Abstract
The invention discloses a nano iron powder microencapsulation method, which takes ethyl cellulose as a shell material, uses polydimethylsiloxane to initiate the condensation of the ethyl cellulose from the solution thereof, and deposits the ethyl cellulose on the surface of nano iron powder particles to realize the microencapsulation of the nano iron powder; the method has the characteristics of safe and nontoxic shell material raw materials, low price, simple and efficient preparation process, fine and uniform product particles and large loading capacity of the nano iron powder.
Description
Technical Field
The invention belongs to a microencapsulation method of nano iron powder, which can be used for solving the agglomeration problem of reaction medium nano iron powder in underground water in-situ remediation and Permeable Reactive Barrier (PRB) technology.
Background
With the rapid development of our country in recent years, people have attracted attention in the aspects of society, economy and people's living standard, however, as in all countries of the world, environmental problems have become a problem of great concern along with the rapid development, especially in the process of industrialization and agricultural modernization. Underground water is an important drinking water source for human beings, and the cleanness and the water quality safety of the underground water are related to the body health of many people, especially people in arid regions.
In recent years, researches show that the nano iron powder has high reaction activity due to extremely small granularity and large specific surface area, and has the advantages of high reaction rate, low requirement on environment removal and high pollutant removal rate in the process of removing pollutants in some water. However, the extremely small particles and the large specific surface area also cause the nano iron powder to have extremely high specific surface energy, which not only causes the problem of agglomeration of the nano iron powder in the storage and application processes, but also finally causes the great reduction of the utilization rate of the nano iron powder; meanwhile, the burning and explosion risks of the nanometer iron powder are greatly increased. Through microencapsulation to nanometer iron powder, in the middle of binding nanometer iron powder granule in the shell material that has certain permeability, restricted the space that nanometer iron powder granule freely removed, under the prerequisite that does not influence nanometer iron powder activity, avoided the reunion problem between the granule, simultaneously, nanometer iron powder passes through microencapsulation, and the granule grow, specific surface energy reduces, greatly reduced nanometer iron powder's explosion risk.
Microencapsulation of nano-iron powder by calcium alginate and polystyrene has been studied to solve the above problems. However, no research has been reported on the realization of microencapsulation of nano-iron powder by using ethyl cellulose as a shell material and initiating phase separation by polydimethylsiloxane.
Disclosure of Invention
In order to overcome the problems in the prior art, the invention aims to provide a method for microencapsulating nano iron powder, which uses ethyl cellulose as a shell material, and through adding polydimethylsiloxane, the ethyl cellulose is initiated to be subjected to phase separation from a solution thereof and is deposited on the surface of the nano iron powder, so that the microencapsulation of the nano iron powder is realized.
In order to achieve the purpose, the invention adopts the following technical scheme:
a nano iron powder microencapsulation method comprises the following steps:
(1) adding 0.01-1 part of ethyl cellulose into 20 parts of cyclohexane under the atmosphere environment except oxygen and stirring conditions, and raising the temperature to dissolve the ethyl cellulose to obtain an ethyl cellulose cyclohexane solution;
(2) adding 0-100 parts of nano iron powder into an ethyl cellulose cyclohexane solution, and fully stirring to obtain a mixed solution of the nano iron powder and the ethyl cellulose cyclohexane solution, namely a shell material solution;
(3) adding 1-40 parts of polydimethylsiloxane into the mixed solution obtained in the step (2), initiating ethyl cellulose phase separation, and after the addition is finished, adding 1-50 parts of an organic non-solvent of ethyl cellulose to realize microencapsulation of the iron nanoparticle core material, wherein the shell material is ethyl cellulose;
(4) stopping stirring, carrying out suction filtration and washing of the organic non-solvent of the ethyl cellulose in the step (3) for a plurality of times, and drying the obtained powder to obtain the target product.
The microencapsulation of the nano iron powder is realized by initiating the phase separation of ethyl cellulose from a solution by polydimethylsiloxane.
Preferably, in the step (3), the organic non-solvent of the added ethyl cellulose is n-hexane, petroleum ether, n-heptane, n-octane, n-pentane, isopentane, diethyl ether, liquid paraffin or diisopropyl ether.
The method has the characteristics of safe and nontoxic shell material raw materials, low price, simple and efficient preparation process, fine and uniform product particles and large loading capacity of the nano iron powder.
Detailed Description
The present invention will be described in further detail with reference to specific examples.
Example 1
The microencapsulation method of the nanometer iron powder comprises the following steps:
(1) under the atmosphere environment of gas except oxygen and stirring conditions, adding 1.0g of ethyl cellulose into 50ml of cyclohexane, and heating to 60 ℃ at the stirring speed of 350rpm to dissolve the ethyl cellulose;
(2) adding 10g of nano iron powder into the ethyl cellulose cyclohexane solution in the step (1), and uniformly dispersing under the condition of full stirring to obtain a mixed solution of the core material and the ethyl cellulose cyclohexane solution, namely a shell material solution;
(3) and (3) dripping 25ml of polydimethylsiloxane into the mixed solution obtained in the step (2), initiating the ethyl cellulose to separate phases, adding 50ml of n-hexane after finishing dripping, stopping stirring, standing, performing suction filtration and washing with n-hexane for a plurality of times, and obtaining powdery precipitate, namely the microencapsulated nano iron powder.
By adopting the method of the embodiment, the microencapsulated iron powder has the particle size of 40-50 nm, the particles are uniform and fine, and the effective loading capacity of the iron powder reaches 91.6%.
Example 2
The microencapsulation method of the nanometer iron powder comprises the following steps:
(1) under the atmosphere environment of gas except oxygen and stirring conditions, adding 1.0g of ethyl cellulose into 50ml of cyclohexane, and heating to 60 ℃ at the stirring speed of 350rpm to dissolve the ethyl cellulose;
(2) adding 1.0g of nano iron powder into the ethyl cellulose cyclohexane solution in the step (1), and uniformly dispersing under the condition of full stirring to obtain a mixed solution of the core material and the ethyl cellulose cyclohexane solution, namely a shell material solution;
(3) and (3) dripping 25ml of polydimethylsiloxane into the mixed solution obtained in the step (2), initiating and separating cellulose phase, adding 50ml of n-hexane after finishing dripping, stopping stirring, standing, performing suction filtration and washing with n-hexane for a plurality of times, and obtaining powdery precipitate, namely the microencapsulated nano iron powder.
By adopting the method of the embodiment, the microencapsulated nano iron powder has the particle size of 110-150 nm, the particles are uniform and fine, and the effective loading capacity of the nano iron powder reaches 50.8%.
Claims (1)
1. A nano iron powder microencapsulation method is characterized in that: the method comprises the following steps:
(1) under the atmosphere environment of gas except oxygen and stirring conditions, adding 1.0g of ethyl cellulose into 50mL of cyclohexane, and heating to 60 ℃ at the stirring speed of 350rpm to dissolve the ethyl cellulose;
(2) adding 1.0g of nano iron powder or 10g of nano iron powder into the ethyl cellulose cyclohexane solution obtained in the step (1), and uniformly dispersing under the condition of full stirring to obtain a mixed solution of the core material and the ethyl cellulose cyclohexane solution, namely a shell material solution;
(3) dripping 25mL of polydimethylsiloxane into the mixed solution obtained in the step (2), initiating the separation of ethyl cellulose phase, adding 50mL of n-hexane after finishing dripping, stopping stirring, standing, performing suction filtration and washing with n-hexane for several times, and obtaining powdery precipitate which is the microencapsulated nano iron powder;
the microencapsulation of the nano iron powder is realized by initiating the phase separation of ethyl cellulose from a solution by polydimethylsiloxane.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810175554.3A CN108404825B (en) | 2018-03-02 | 2018-03-02 | Nano iron powder microencapsulation method |
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| CN201810175554.3A CN108404825B (en) | 2018-03-02 | 2018-03-02 | Nano iron powder microencapsulation method |
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| CN108404825A CN108404825A (en) | 2018-08-17 |
| CN108404825B true CN108404825B (en) | 2021-01-29 |
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| CN110216280B (en) * | 2019-07-10 | 2020-07-28 | 清华大学 | Preparation method of activity-continuity-controllable nano iron powder material |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5245589A (en) * | 1975-12-24 | 1977-04-11 | Toyo Jozo Co Ltd | Method of producing microcapsules by emulsification, dispersion, and s olvent removal |
| US4486471A (en) * | 1981-05-29 | 1984-12-04 | Tanabe Seiyaku Co., Ltd. | Process for preparing ethylcellulose microcapsules |
| CN101362067A (en) * | 2007-08-06 | 2009-02-11 | 天津科技大学 | Microcapsule preparation method |
| CN102226072A (en) * | 2011-05-06 | 2011-10-26 | 同济大学 | Preparation method of organic silicon microcapsule powder waterproof agent |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5849433A (en) * | 1981-09-18 | 1983-03-23 | Tanabe Seiyaku Co Ltd | Production of microcapsule |
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2018
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5245589A (en) * | 1975-12-24 | 1977-04-11 | Toyo Jozo Co Ltd | Method of producing microcapsules by emulsification, dispersion, and s olvent removal |
| US4486471A (en) * | 1981-05-29 | 1984-12-04 | Tanabe Seiyaku Co., Ltd. | Process for preparing ethylcellulose microcapsules |
| CN101362067A (en) * | 2007-08-06 | 2009-02-11 | 天津科技大学 | Microcapsule preparation method |
| CN102226072A (en) * | 2011-05-06 | 2011-10-26 | 同济大学 | Preparation method of organic silicon microcapsule powder waterproof agent |
Non-Patent Citations (3)
| Title |
|---|
| Formation of multilayered biopolymer microcapsules and microparticles in a multiphase microfluidic flow;Elisabeth Rondeau et al.;《BIOMICROFLUIDICS》;20120524;第6卷(第2期);全文 * |
| 乙基纤维素微胶囊化Vc工艺参数及其活性保护的研究;李书国等;《食品工业科技》;20050531;第26卷(第5期);全文 * |
| 乙基纤维素-无机变色材料微胶囊制备原理及制备技术研究;裴婷;《印染助剂》;20090531;第26卷(第5期);全文 * |
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