CN101314479B - Method for preparing eka-one-dimensional nano-strontium carbonate - Google Patents
Method for preparing eka-one-dimensional nano-strontium carbonate Download PDFInfo
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- CN101314479B CN101314479B CN2008101502230A CN200810150223A CN101314479B CN 101314479 B CN101314479 B CN 101314479B CN 2008101502230 A CN2008101502230 A CN 2008101502230A CN 200810150223 A CN200810150223 A CN 200810150223A CN 101314479 B CN101314479 B CN 101314479B
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Abstract
The present invention provides a method for preparing a standard one dimension nanometer strontium carbonate. The method comprises the following steps that: a slurry with a solid to liquid ratio of between 1:3 and 1:10 is prepared from recrystallized and purified strontium hydroxide octo-hydrate and de-ionized water, heated to a temperature of between 60 and 100 DEG C, passed through by carbon dioxide until the pH value reaches between 6 and 8, and washed and filtered to give high purity strontium carbonate; and then the obtained high purity strontium carbonate is prepared into a slurry according to a solid to liquid ratio of between 1:5 and 1:20, afterwards, a pattern control additive with a weight of 0.1 to 10 percent of that of the strontium carbonate, a surface active agent with a weight of 0.1 to 5 percent of that of the strontium carbonate and a dispersant of a weight of 0.1 to 5 percent of that of the strontium carbonate are added into the slurry to form a mixed slurry, the mixed slurry is poured into an autoclave, stirred for reaction for 1 to 10 hours at a temperature of between 200 and 300 DEG C, and finally subject to aging, washing, solid-liquid separation and drying, and thus the one dimension nanometer strontium carbonate with an average diameter no more than 50 nm, and a length between 300nm to 3 mu m is obtained. The method is simple in technology, convenient in operation, short in process, less in equipment investment, low in manufacturing cost and stable in product quality.
Description
Technical field
The invention belongs to inorganic salt material technology field, relate to the method for accurate a kind of nano strontium carbonate preparation, relate in particular to a kind of adopt hydrothermal treatment consists and add auxiliary agent combine and prepare the method that eka-one-dimensional nano-strontium carbonate prepares.
Background technology
Strontium carbonate powder is topmost strontium product salt, is mainly used in to produce color monitor glass bulb, magneticsubstance, pyrotechnics etc., and Application Areas relates to electronics, material, chemical industry, sugaring, metallurgy, military project etc.Different Application Areass has different requirements to the purity of strontium carbonate product, and the particle diameter of Strontium carbonate powder is also had different requirements.As to be used to produce CRT glass bulb requirement Strontium carbonate powder be granular, need just can reach requirement by granulation; The Strontium carbonate powder that is used to produce magneticsubstance requires to be powdery, and particle diameter requires at 1 μ m.In addition, the different application field requires also very strict to the pattern of high-purity strontium carbonate, as be used for the spherical or subsphaeroidal high-purity strontium carbonate of electronic ceramics production requirement etc., the wire Strontium carbonate powder has good reinforcing effect, platy strontium carbonate particles higher activity etc. arranged, so the morphology control of strontium carbonate product and the Strontium carbonate powder technology of preparation different-shape are had very vast market prospect.
The nano material is meant that the three-dimensional space yardstick has at least one dimension to be in the material of nanometer scale (1-100nm), the material of new generation that it is made up of the nanoparticle of size between atom, molecule and meta system.Because the yardstick of its component units is little, the interface takies sizable composition.Therefore, nano material has multiple characteristics, and this just causes having been occurred being different from by the system that nanoparticle constitutes many special propertys of common bulk macroscopic material system.When the material yardstick entered nano level, various special effects caused the performance of nano material to be compared with macroscopic material huge variation has taken place.
Quasi-one dimensional nanostructure ((Quasi) One-dimensional nanostructures/1D nanostructres) be meant in three-dimensional space, have two-dimension sizes be in nanometer scale nanostructure, be one of field, forward position comparatively active in the nanoscale science and technology.Quasi-one-dimensional nanometer material comprises nanofiber (nanofiber): elongated shape, length-to-diameter ratio 〉=10; Nano-cable (nanocable): nano wire is coated with the nanostructure of one or more layers different structure material; Nanometer rod (nanorod): thin club shaped structure, general length-to-diameter ratio≤10; Nanotube (nanotube): elongated shape also has hollow structure, i.e. the thin tube-like structure; Nano belt (nanobelt, nanoribbon): the banded nanostructure of elongate strip, long-width ratio 〉=10, general flakiness ratio 〉=3.Two dimensional features have been had concurrently, promptly in the existing certain yardstick of width (Xie Ting etc., Materials Science and Engineering journal, the 24th volume, the 2nd phase, the 311st～315 page, 2006 years).
Eka-one-dimensional nano-strontium carbonate of the present invention is meant that a kind of diameter is not more than 50 nanometers, and length belongs to the category of nano wire and nanometer rod in the strontium carbonate product of 300 nanometers to 3 micrometer ranges.The Strontium carbonate powder nanometer rod is mainly used in the compound organic polymeric optical material of preparation free of birefringence, as free of birefringence polycarbonate optic polymer.The Strontium carbonate powder nano wire can be applicable to have in the supporting material that absorbs the X ray function.
Wen Chuangeng etc. have reported a kind of special liquid-phase precipitation method of using at " chemical industry progress " second volume the 5th phase (2005), the nano strontium carbonates of the i.e. two kinds of quick high-strength mechanical mixed precipitation of solution methods preparation, obtain about narrow diameter distribution, favorable dispersity, average particle diameter 29.3nm, particle morphology is the spheric nano strontium carbonate substantially.But this method complicated process of preparation, the cost height, quality product and pattern are wayward.
Summary of the invention
It is simple to the purpose of this invention is to provide a kind of technology, easy to operate, the preparation method of the eka-one-dimensional nano-strontium carbonate of constant product quality.
Strontium hydroxide after the present invention purifies with recrystallization is as raw material, with carbonic acid gas as precipitation agent, neutralization reaction takes place prepare high-purity strontium carbonate, resulting high-purity strontium carbonate product can be bar-shaped, spherical or other shape (pattern of high-purity strontium carbonate product and granularity are subjected to the conditional decision of reaction process, promptly with the feeding speed and the feeding mode of the concentration of strontium hydroxide, temperature of reaction, carbonic acid gas, the speed that stirs is relevant with mode), the particle diameter of high-purity strontium carbonate is in the scope of 1～30 μ m.Then by adding morphology control agent, tensio-active agent and dispersion agent, and under high temperature that hydrothermal method provides, highly compressed environment, the transition process of dissolution-recrystallization takes place in strontium carbonate product again, make the speed of growth generation disproportionation of Strontium carbonate powder on different crystallization directions, promptly bigger with speed of growth gap on different crystallization directions, growth is promoted on some direction, and the growth of other direction is suppressed, thereby can grow eka-one-dimensional nano-strontium carbonate.
The concrete grammar that the present invention prepares eka-one-dimensional nano-strontium carbonate is: will be mixed with solid-to-liquid ratio through eight water strontium hydroxides behind the recrystallization purifying and deionized water is 1: 3～1: 10 slip, be heated to 60～100 ℃, logical carbonic acid gas, pH value to slip is 6～8, and filtration, washing obtain high-purity strontium carbonate; Again the gained high-purity strontium carbonate is made into slip with 1: 5～1: 20 solid-to-liquid ratio, the morphology control additive that in slip, adds Strontium carbonate powder quality 0.1～10% then, the dispersion agent of the tensio-active agent of Strontium carbonate powder quality 0.1～5% and Strontium carbonate powder quality 0.1～5%, form mixed slurry, in autoclave, 200～300 ℃ of following stirring reactions 1～10 hour, obtain mean diameter and be not more than 50nm through ageing, washing, solid-liquid separation, drying at last, length is about the eka-one-dimensional nano-strontium carbonate of 300nm～3 μ m.
The morphology control additive adopts soluble strontium salt, as strontium hydroxide, strontium sulfide, strontium acetate, strontium chloride,
Strontium nitrate, or wherein two kinds and two or more mixtures.
Tensio-active agent adopts the N-acyl glutamate; hydroxyl ethylenediamine triacetic acid trisodium; bromination dodecyl trimethyl ammonium (CTAB); chlorination dodecyl trimethyl ammonium (CTAC); chlorination octadecyl dimethyl benzene ethyl ammonium, N-3; 4,5-tribromosalicylanilide (TBS), N-3; 4; 4 ,-Trichlorocarbanilide (TCC), dodecyl dimethyl benzyl ammonium chloride; cetyltrimethylammonium chloride; the two octadecyl Dimethyl Ammonium of chlorination, in the octadecyl trimethyl ammonium chloride, or wherein two kinds and two or more mixtures.
Described dispersion agent is a polyoxyethylene glycol, Zhong Xin polyoxyethylenated alcohol, Benzyldiphenyl phenol polyethenoxy ether, at least a in the polyoxyethylene nonylphenol ether.
For the particle diameter control that the makes high-purity strontium carbonate scope at 1～30 μ m, the ventilation speed control of carbonic acid gas is within 0.5～10L/min scope.
The nano strontium carbonate of the present invention's preparation is bar-shaped or fibrous, and mean diameter is less than 50nm, and length is about the eka-one-dimensional nano-strontium carbonate of 300nm～3 μ m.
It is simple that the inventive method has technology, easy to operate, and flow process is short, and production cost is low, and facility investment is little, characteristics such as constant product quality.
Embodiment
Embodiment 1, the Sr behind the 100g recrystallization purifying (OH)
28H
2O and 400ml water (mass ratio is 1: 4) add 1000ml and have in the there-necked flask of mechanical stirrer and thermometer, under agitation are heated to 80 ℃, and the strontium hydroxide perfect solution is a colourless transparent solution.Gas flow rate with 2L/min feeds CO in this solution then
2, after about 2 minutes, it is mixed that solution begins to become, and promptly has the Strontium carbonate powder precipitation to generate.Feed CO continuously
2Carry out carbonization after 3 hours, slip becomes the heavy-gravity pasty state, and this moment, the pH value of slip was 6.5.This solution is filtered, with small amount of deionized water washing three times, obtain high-purity strontium carbonate, measuring its granularity with laser particle analyzer is D
50Be 3.7 μ m.With resulting high-purity strontium carbonate and 500ml water making beating (mass ratio is 1: 10), mixed surfactant, the 10g polyoxyethylene glycol formed with strontium hydroxide solution, 0.3g bromination dodecyl trimethyl ammonium and the 0.2g hydroxyl ethylenediamine triacetic acid trisodium of 20ml 0.2mol/L add in the autoclave, under agitation changed shape 4 hours with 230 ℃, naturally cooling ageing 24 hours then, centrifugation is also used 30ml absolute ethanol washing 4 times, and is dry in microwave oven.Resulting product is the about 30～50nm of diameter with its pattern of sem observation, the eka-one-dimensional nano-strontium carbonate of the about 300nm of length～3 μ m.
Embodiment 2, the Sr behind the 100g recrystallization purifying (OH)
28H
2O and 500ml water (mass ratio is 1: 5) add 1000ml and have in the there-necked flask of mechanical stirrer and thermometer, under agitation are heated to 70 ℃, and the strontium hydroxide perfect solution is a colourless transparent solution.Gas flow rate with 4L/min feeds CO in this solution then
2, after about 2 minutes, it is mixed that solution begins to become, and promptly has the Strontium carbonate powder precipitation to generate.Feed CO continuously
2Carry out carbonization after 2 hours, slip becomes the heavy-gravity pasty state, and this moment, the pH value of slip was 6.0.This solution is filtered,, obtain high-purity strontium carbonate, measure its granularity D with laser particle analyzer with small amount of deionized water washing three times
50Be 3.6 μ m.With resulting high-purity strontium carbonate and 600ml water making beating (mass ratio is 1: 12); strontium chloride solution, 0.3gN-acyl glutamic acid sodium and 0.2g N-3 with 20ml 0.2mol/L; 4; the mixed surfactant that the 5-tribromosalicylanilide is formed, secondary octanol polyoxyethylene (10-15) ether of 10g add in the autoclave together; under agitation changed shape 4 hours with 250 ℃; naturally cooling ageing 24 hours then, centrifugation and with 30ml absolute ethanol washing 4 times, dry in microwave oven.Resulting product is the about 20～40nm of diameter with its pattern of sem observation, the eka-one-dimensional nano-strontium carbonate of the about 300nm of length～3 μ m.
Embodiment 3, the Sr behind the 100g recrystallization purifying (OH)
28H
2O and 400ml water (mass ratio is 1: 4) add 1000ml and have in the there-necked flask of mechanical stirrer and thermometer, under agitation are heated to 90 ℃, and the strontium hydroxide perfect solution is a colourless transparent solution.Gas flow rate with 3L/min feeds CO in this solution then
2, after about 2 minutes, it is mixed that solution begins to become, and promptly has the Strontium carbonate powder precipitation to generate.Feed CO continuously
2Carry out carbonization after 3 hours, slip becomes the heavy-gravity pasty state, and this moment, the pH value of slip was 6.5.This solution is filtered,, obtain high-purity strontium carbonate, measure its granularity D with laser particle analyzer with small amount of deionized water washing three times
50Be about 3.7 μ m.With resulting high-purity strontium carbonate and 500ml water making beating (mass ratio is 1: 10), the mixed dispersant of forming with secondary octanol polyoxyethylene (10-15) ether of strontium acetate solution, 0.5g cetyltrimethylammonium chloride tensio-active agent, 5g polyoxyethylene glycol (PEG) and the 5g of 20ml 0.2mol/L adds in the autoclave, under agitation changed shape 4 hours with 270 ℃, naturally cooling ageing 24 hours then, centrifugation is also used 30ml absolute ethanol washing 4 times, and is dry in microwave oven.Resulting product is the about 20～50nm of diameter with its pattern of sem observation, the eka-one-dimensional nano-strontium carbonate of the about 300nm of length～3 μ m.
Claims (6)
1. method for preparing eka-one-dimensional nano-strontium carbonate, be that will to be mixed with solid-to-liquid ratio through eight water strontium hydroxides behind the recrystallization purifying and deionized water be 1: 3～1: 10 slip, be heated to 60～100 ℃, logical carbonic acid gas is 6～8 to the pH value of slip, and filtration, washing obtain high-purity strontium carbonate; Again the gained high-purity strontium carbonate is made into slip with 1: 5～1: 20 solid-to-liquid ratio, the morphology control additive that in slip, adds Strontium carbonate powder quality 0.1～10% then, the dispersion agent of the tensio-active agent of Strontium carbonate powder quality 0.1～5% and Strontium carbonate powder quality 0.1～5%, form mixed slurry, in autoclave, 200～300 ℃ of following stirring reactions 1～10 hour, obtain mean diameter and be not more than 50nm through ageing, washing, solid-liquid separation, drying at last, length is the eka-one-dimensional nano-strontium carbonate of 300nm～3 μ m.
2. prepare the method for eka-one-dimensional nano-strontium carbonate according to claim 1, it is characterized in that: described morphology control additive is at least a in strontium hydroxide, strontium sulfide, strontium acetate, strontium chloride, the strontium nitrate.
3. the method for preparing eka-one-dimensional nano-strontium carbonate according to claim 1; it is characterized in that: described tensio-active agent is the N-acyl glutamate; hydroxyl ethylenediamine triacetic acid trisodium; the bromination dodecyl trimethyl ammonium; the chlorination dodecyl trimethyl ammonium, chlorination octadecyl dimethyl benzene ethyl ammonium, N-3; 4; the 5-tribromosalicylanilide, N-3,4; 4;-Trichlorocarbanilide, dodecyl dimethyl benzyl ammonium chloride, cetyltrimethylammonium chloride; the two octadecyl Dimethyl Ammonium of chlorination, at least a in the octadecyl trimethyl ammonium chloride.
4. prepare the method for eka-one-dimensional nano-strontium carbonate according to claim 1, it is characterized in that: described dispersion agent is a polyoxyethylene glycol, Zhong Xin polyoxyethylenated alcohol, Benzyldiphenyl phenol polyethenoxy ether, at least a in the polyoxyethylene nonylphenol ether.
5. prepare the method for eka-one-dimensional nano-strontium carbonate according to claim 1, it is characterized in that: the ventilation speed of described carbonic acid gas is 0.5～10L/min.
6. prepare the method for eka-one-dimensional nano-strontium carbonate according to claim 1, it is characterized in that: described morphology control additive is mixed with the aqueous solution that concentration is 0.05～0.5mol/L, joins in the high-purity strontium carbonate slip.
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| CN101559964B (en) * | 2009-05-19 | 2011-05-25 | 中国科学院青海盐湖研究所 | Preparation method of platy strontium carbonate particles |
| US8388749B2 (en) * | 2009-10-28 | 2013-03-05 | Ube Material Industries, Ltd. | Strontium carbonate micropowder and process for production |
| CN102765740B (en) * | 2012-06-19 | 2014-03-05 | 南京金焰锶业有限公司 | Preparation method of strontium carbonate with high purity |
| CN103754915B (en) * | 2013-12-13 | 2015-04-29 | 绵阳市远达新材料有限公司 | Preparation method of strontium carbonate |
| CN104016395A (en) * | 2014-06-26 | 2014-09-03 | 中国科学院青海盐湖研究所 | Strontium carbonate powder and preparation method thereof |
| CN104860344B (en) * | 2015-06-01 | 2017-04-19 | 中国科学院青海盐湖研究所 | Preparation method of spherical strontium carbonate |
| CN109179472A (en) * | 2018-09-30 | 2019-01-11 | 南昌航空大学 | A kind of method that marble wastes prepare high whiteness calcium carbide of different crystal formation powder |
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| CN1504411A (en) * | 2002-11-30 | 2004-06-16 | 衡阳市金原纳米科技有限公司 | Process for producing superfine barium carbonate and strontium carbonate |
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| CN1394808A (en) * | 2002-08-02 | 2003-02-05 | 武汉大学 | Nano strontium carbonate and its preparation method |
| CN1504411A (en) * | 2002-11-30 | 2004-06-16 | 衡阳市金原纳米科技有限公司 | Process for producing superfine barium carbonate and strontium carbonate |
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