CN101391783A - Microemulsion solvent thermal synthesizing method of magnesium carbonate hollow and nano stick - Google Patents
Microemulsion solvent thermal synthesizing method of magnesium carbonate hollow and nano stick Download PDFInfo
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- CN101391783A CN101391783A CNA2008101531290A CN200810153129A CN101391783A CN 101391783 A CN101391783 A CN 101391783A CN A2008101531290 A CNA2008101531290 A CN A2008101531290A CN 200810153129 A CN200810153129 A CN 200810153129A CN 101391783 A CN101391783 A CN 101391783A
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Abstract
The invention relates to a method for thermal preparing magnesium carbonate hollow and porous nano rod with microemulsion-assisted solvent, belonging to the technical field of an inorganic nanometer material preparation process. The invention takes cyclohexane as solvent, makes use of the precipitation reaction of carbonate and magnesium ions, and uses surfactant as soft template, so as to prepare the magnesium carbonate hollow and porous nano rod, wherein, the soft template is some surfactant; the carbonate and the magnesium ions come from soluble carbonate and magnesium salt. The magnesium carbonate nano rod which is synthesized by the method has the diameter of 10 to 30nm or so and the length of up to several hundred nanometers. As the nano rod is characterized by hollow property or porous surface, the nano rod can be used as adsorbent, and can also be used as additive of coatings and plastic.
Description
Technical field
The invention belongs to the inorganic nano material preparation process technology field, relate to the preparation method of inorganic nano material, specifically the micro emulsion solvent process for thermosynthesizing of magnesiumcarbonate hollow and porous nano rod.Can be applicable to coating, plastics, sorbent material and magnesium oxide and prepare aspects such as intermediate.
Background technology
Magnesiumcarbonate is the additive of important matrix material, as is added in plastics and the rubber, can reduce the mechanical property of base material to some extent.Also can be used for other magnesium salts such as magnesium oxide, magnesium hydroxide, sal epsom and magnesium chloride and prepare raw material.In addition, also can be used as sorbent material and discoloring agent, remove the heavy metal ion in the sewage and wastewater from chemical industry decoloured.The performance that studies show that material to a great extent with reduce crystal particle scale to nanometer scale direct relation arranged, yet the bibliographical information of magnesiumcarbonate low-dimensional nano structure also seldom at present.
The present invention with increase magnesiumcarbonate specific surface area, and then improves magnesiumcarbonate Adsorption of Heavy Metal Ions and decoloring ability by the magnesiumcarbonate of preparation low-dimensional nano structure.The preparation method of a kind of operational safety, simple magnesiumcarbonate hollow and porous nano rod also is provided simultaneously.
Summary of the invention
The invention provides the synthetic method of a kind of magnesiumcarbonate hollow and porous nano rod, this method has synthetic magnesiumcarbonate nanometer rod, controlled amount, degree of crystallinity height, operational safety, easy, good process repeatability, the advantage of constant product quality.
Characteristics of the present invention are by the mol ratio that changes water and tensio-active agent and other reaction conditions, can realize the controlled preparation to magnesiumcarbonate nanometer rod size and pattern; Use high boiling cyclohexane give to be solvent simultaneously, make operation safer.
Magnesiumcarbonate hollow and porous nano rod synthesis step are as follows:
In beaker, add a certain amount of hexanaphthene and propyl carbinol, under agitation add certain amount of surfactant again, be stirred to solution and be transparent.A certain amount of carbonate and magnesium salt solution are added above-mentioned solution, and control carbonate and magnesium ion concentration are 0.01-1.5mol/L, and the mol ratio of water and tensio-active agent is 5-60, obtains microemulsion solution.Be closed in the reactor that is lined with tetrafluoroethylene above-mentioned microemulsion is close again, then 100-160 ℃ of heating crystallizations 3-12 hours, after crystallization finishes temperature of reaction kettle is reduced to room temperature, product water is washed till neutrality, obtains the magnesiumcarbonate nanometer rod in 3 hours 80 ℃ of vacuum-dryings.
Description of drawings
Accompanying drawing the 1, the 2nd, the transmission electron microscope photo of synthetic magnesiumcarbonate hollow nanometer rod (by preparation in the embodiment 1).
Accompanying drawing the 3, the 4th, the transmission electron microscope photo of synthetic magnesiumcarbonate porous nano rod (by preparation in the embodiment 2).
Accompanying drawing the 5, the 6th, the transmission electron microscope photo of synthetic magnesiumcarbonate nanometer rod (by preparation in the embodiment 3).
Accompanying drawing 7 is transmission electron microscope photos (by preparation in the embodiment 4) of synthetic magnesiumcarbonate nano rod bundle.
Accompanying drawing 8 is transmission electron microscope photos (by preparation in the embodiment 5) of synthetic magnesiumcarbonate nanometer rod.
Specific embodiments
Embodiment 1
In the 80mL beaker, add 20mL hexanaphthene and 1mL Pentyl alcohol, under agitation add the 1g cetyl trimethylammonium bromide again, be stirred to solution and be transparent (mol ratio of water and cetyl trimethylammonium bromide is 20).Two parts of above-mentioned microemulsion preparations, add 1mL1mol/L yellow soda ash and 1mol/L magnesium chloride brine respectively, after stirring 30min two microemulsions are mixed, continue to stir 30min, be transferred in the 80mL reactor, in 140 ℃ of ageing 12h, naturally cool to room temperature, the gained white precipitate at 80 ℃ of following freeze-day with constant temperature 12h, gets final product with Virahol and deionized water wash in vacuum drying oven.
For becoming 10, other condition is constant with the mol ratio of water and cetyl trimethylammonium bromide in the embodiment 1.
Embodiment 3
For becoming 15, other condition is constant with the mol ratio of water and cetyl trimethylammonium bromide in the embodiment 1.
Embodiment 4
For becoming 25, other condition is constant with the mol ratio of water and cetyl trimethylammonium bromide in the embodiment 1.
Embodiment 5
For becoming 15, carbonate and magnesium ion concentration become 1.5mol/L with the mol ratio of water and cetyl trimethylammonium bromide in the embodiment 1, and other condition is constant.
Embodiment 6
For becoming 10, crystallization temperature becomes 120 ℃ with the mol ratio of water and cetyl trimethylammonium bromide in the embodiment 1, and other condition is constant.
Embodiment 7
For becoming 15, crystallization temperature becomes 120 ℃ with the mol ratio of water and cetyl trimethylammonium bromide in the embodiment 1, and other condition is constant.
Embodiment 8
For becoming 20, crystallization temperature becomes 120 ℃ with the mol ratio of water and cetyl trimethylammonium bromide in the embodiment 1, and other condition is constant.
Embodiment 9
Tensio-active agent in the embodiment 1 is become polyoxyethylene glycol, and other condition is constant.
Embodiment 10
Crystallization time in the embodiment 1 was become 6 hours by 12 hours, and other condition is constant.
Embodiment 11
Crystallization temperature in the embodiment 1 is become 160 ℃ by 140 ℃, and other condition is constant.
Embodiment 12
For becoming 15, carbonate and magnesium ion concentration become 0.5mol/L with the mol ratio of water and cetyl trimethylammonium bromide in the embodiment 1, and other condition is constant.
The present invention can describe in detail by embodiment, but the invention is not restricted to above embodiment.
Claims (5)
1. the micro emulsion solvent process for thermosynthesizing of magnesiumcarbonate hollow and porous nano rod is characterized in that comprising the steps:
A. microemulsion solution preparation: in beaker, add a certain amount of hexanaphthene and propyl carbinol, under agitation add certain amount of surfactant again, be stirred to solution and be transparent; A certain amount of carbonate and magnesium salt solution are added above-mentioned solution, and control carbonate and magnesium ion concentration are 0.01-1.5mol/L, and the mol ratio of water and tensio-active agent is 5-60, obtains microemulsion solution;
B. solvent thermal carbonate synthesis magnesium hollow and porous nano rod: above-mentioned precursor is loaded on heating crystallization in the airtight reactor that is lined with tetrafluoroethylene, treat that the crystallization afterreaction still temperature that finishes reduces to room temperature, product water is washed till neutrality, obtained magnesiumcarbonate hollow and porous nano rod in 3 hours 80 ℃ of vacuum-dryings then; Wherein, crystallization temperature is 100-160 ℃, and crystallization time is 3-12 hours.
2. according to the magnesiumcarbonate hollow of right 1 requirement and the micro emulsion solvent process for thermosynthesizing of porous nano rod, it is characterized in that described carbonate and magnesium salts are the carbonate and the magnesium salts of solubility.
3. according to the magnesiumcarbonate hollow of right 1 requirement and the micro emulsion solvent process for thermosynthesizing of porous nano rod, it is characterized in that described solvent is a hexanaphthene.
4. according to the magnesiumcarbonate hollow of right 1 requirement and the micro emulsion solvent process for thermosynthesizing of porous nano rod, it is characterized in that described tensio-active agent is long-chain phosphoric acid salt, long-chain vitriol, cetyl trimethylammonium bromide and polyoxyethylene glycol.
5. according to the magnesiumcarbonate hollow of right 1 requirement and the micro emulsion solvent process for thermosynthesizing of porous nano rod, it is characterized in that described crystallization temperature preferentially is selected from 140 ℃, time priority is selected from 12 hours.
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| CNA2008101531290A CN101391783A (en) | 2008-11-18 | 2008-11-18 | Microemulsion solvent thermal synthesizing method of magnesium carbonate hollow and nano stick |
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| CNA2008101531290A CN101391783A (en) | 2008-11-18 | 2008-11-18 | Microemulsion solvent thermal synthesizing method of magnesium carbonate hollow and nano stick |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101948634A (en) * | 2010-09-06 | 2011-01-19 | 天津工业大学 | Preparation method of cadmium carbonate-Trypan blue composite nanorod bundle by reflux |
| CN101613120B (en) * | 2009-07-29 | 2011-05-25 | 中国科学院青海盐湖研究所 | Spherical and radial magnesium carbonate and preparation method thereof |
| CN102280634A (en) * | 2011-07-05 | 2011-12-14 | 南开大学 | Lithium manganese oxide electrode material with porous structure as well as manufacturing method and application thereof |
| CN105442302A (en) * | 2015-12-07 | 2016-03-30 | 江南石墨烯研究院 | Water treatment composite weaving net based on oxidized graphene and preparation method and application thereof |
| CN107698009A (en) * | 2017-10-20 | 2018-02-16 | 东南大学 | A kind of carbon containing magnesium salts material for removing removing heavy metals and its preparation method and application |
-
2008
- 2008-11-18 CN CNA2008101531290A patent/CN101391783A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101613120B (en) * | 2009-07-29 | 2011-05-25 | 中国科学院青海盐湖研究所 | Spherical and radial magnesium carbonate and preparation method thereof |
| CN101948634A (en) * | 2010-09-06 | 2011-01-19 | 天津工业大学 | Preparation method of cadmium carbonate-Trypan blue composite nanorod bundle by reflux |
| CN102280634A (en) * | 2011-07-05 | 2011-12-14 | 南开大学 | Lithium manganese oxide electrode material with porous structure as well as manufacturing method and application thereof |
| CN102280634B (en) * | 2011-07-05 | 2013-04-10 | 南开大学 | Lithium manganese oxide electrode material with porous structure as well as manufacturing method and application thereof |
| CN105442302A (en) * | 2015-12-07 | 2016-03-30 | 江南石墨烯研究院 | Water treatment composite weaving net based on oxidized graphene and preparation method and application thereof |
| CN107698009A (en) * | 2017-10-20 | 2018-02-16 | 东南大学 | A kind of carbon containing magnesium salts material for removing removing heavy metals and its preparation method and application |
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Open date: 20090325 |