CN104016394B - A kind of preparation method of ball shaped nano Strontium carbonate powder - Google Patents
A kind of preparation method of ball shaped nano Strontium carbonate powder Download PDFInfo
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- CN104016394B CN104016394B CN201410298981.2A CN201410298981A CN104016394B CN 104016394 B CN104016394 B CN 104016394B CN 201410298981 A CN201410298981 A CN 201410298981A CN 104016394 B CN104016394 B CN 104016394B
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Abstract
The invention discloses a kind of preparation method of ball shaped nano Strontium carbonate powder, comprise step: S101, in soluble strontium salts solution, add pattern agent stirring and dissolving, obtain the first solution; Wherein, in the pattern agent added and strontium salt solution, the mol ratio of strontium ion is 2:1 ~ 1.5; S102, described first solution is proceeded in ultrasonic reactor, in ultrasonic procedure, pass into CO
2gas, until make the pH value of solution for neutral, obtains the second solution; Wherein, CO is passed into
2the flow of gas is 2 ~ 10L/min; S103, described second solution is carried out solid-liquid separation, obtain solid product; S104, by described solid product through washing and drying after obtain described ball shaped nano Strontium carbonate powder.Present invention also offers the ball shaped nano Strontium carbonate powder that a kind of preparation method as above obtains.
Description
Technical field
The invention belongs to chemical technology field, particularly relate to a kind of preparation method of ball shaped nano Strontium carbonate powder.
Background technology
Strontium carbonate powder is a kind of important industrial chemicals, because it has very strong absorption X-ray and the physical and chemical performance of gamma-radiation function and other uniqueness, be widely used in the manufacture of the industrial goods such as color picture tube glass bulb, cathode tube, electronic ceramics, magneticsubstance, fuel, paint, relate to all conglomeraties such as electronics, chemical industry, military project, building materials, non-ferrous metal, aerospace, light industry, medicine, food.Although China has become strontium product major country of production, annual production has accounted for 50% ~ 60% of world wide production, because strontium industry is lack of standardization, cause structure serious unbalance, and low side excess supply capacity, high-end supply scarce capacity.Along with the fast development of electron trade, high-quality electronic-grade, Fluorescence Grade, nano level strontium carbonate product demand are every year with 15% speed increment, and the breach of high-quality strontium carbonate seems more serious.
Along with the fast development of the industries such as domestic and international electronic devices and components, magneticsubstance and stupalith, also there is higher requirement to the quality of strontium carbonate product, the research of Strontium carbonate powder was focused mostly on how to make production high efficiency, purity High Purity etc. in the past.But along with development in science and technology, also have its physical index except the requirement to the chemical index of product and purity or content, impurity aspect, the i.e. requirement of the aspect such as particle morphology, size-grade distribution, thermal property and practicality test, the strontium carbonate product which results in different-shape has different using values.
Chaidamu Basin, Qinghai Province strong wind mountain one is with Strontium Sulphate reserves in explored celestite ore to reach more than 2,000 ten thousand tons, is strontium mineral deposit maximum in the world.In prior art, carbon reduction method explained hereafter technical grade Strontium carbonate powder, cannot produce high-quality strontium carbonate, and environmental pollution is serious.The preparation of high-quality ball shaped nano Strontium carbonate powder mainly controls carbonization process, carbonization is divided into two processes, the i.e. formation of nucleus and nuclei growth, when starting crystallization, if the degree of supersaturation of solution is excessive, in carbonization process, generate the excessive velocities of Strontium carbonate powder, a large amount of nucleus is generated in the very short time, namely the formation speed of nucleus is greater than nucleus growth speed, then Strontium carbonate powder particle is little and many, easily reunites; Otherwise if the growth rate of nucleus is greater than the formation speed of nucleus, then crystalline particle lacks greatly, Strontium carbonate powder grain diameter becomes large, not easily reunites.It is the key preparing ball shaped nano Strontium carbonate powder that growth rate and the formation speed of nucleus are effectively separated, based on more than, exploring a kind of strontium carbonate product of producing high-quality has huge using value.
Summary of the invention
In order to solve prior art Problems existing, the preparation method that the invention provides a kind of ball shaped nano Strontium carbonate powder and the ball shaped nano Strontium carbonate powder obtained according to the method, by the method can prepare spherical effective, uniform particles, particle size range are narrow, the ball shaped nano Strontium carbonate powder of good dispersity.
For achieving the above object, present invention employs following technical scheme:
A preparation method for ball shaped nano Strontium carbonate powder, is characterized in that, comprises step:
S101, in soluble strontium salts solution, add pattern agent stirring and dissolving, obtain the first solution; Wherein, in the pattern agent added and strontium salt solution, the mol ratio of strontium ion is 2:1 ~ 1.5;
S102, described first solution is proceeded in ultrasonic reactor, in ultrasonic process, pass into CO
2gas, until the pH value making solution is 5 ~ 9, obtains the second solution; Wherein, CO is passed into
2the flow of gas is 2 ~ 10L/min;
S103, described second solution is carried out solid-liquid separation, obtain solid product;
S104, by described solid product through washing and drying after obtain described ball shaped nano Strontium carbonate powder.
Preferably, the method also comprises the step of preparation soluble strontium salts solution, specifically comprise: first celestite ore is obtained strontium salt after high temperature reduction, then strontium salt is dissolved in the water of 50 ~ 90 DEG C, removing calcium hydroxide and acid non-soluble substance impurity, obtain the soluble strontium salts solution containing strontium sulfide, sulphur hydrogenation strontium and strontium hydroxide.
Preferably, in step S101, when adding pattern agent in soluble strontium salts solution, mixing solutions is heated to 50 ~ 80 DEG C, to accelerate the dissolution time of mixing solutions and to prevent strontium hydroxide crystallization.
Preferably, in step S102, ultrasonic frequency is 80 ~ 100KHz.
Preferably, in step S103, adopt the method for centrifugation to carry out solid-liquid separation to the second solution, the solid phase obtained to proceed in ultrasonic cleaner and adds EtOH Sonicate dispersion, obtains described solid product.
Preferably, in step S104, distilled water and ethanol is adopted to wash described solid product as washing composition.
Preferably, CO is passed into
2the flow of gas is 4 ~ 8L/min.
Preferably, described pattern agent is disodium ethylene diamine tetraacetate.
Present invention also offers the ball shaped nano Strontium carbonate powder that a kind of preparation method as above obtains.
Wherein, described ball shaped nano Strontium carbonate powder comprises multiple shape approximation in spherical monomer, and the particle diameter of each monomer is 80 ~ 200nm.
Compared with prior art, the advantage of method provided by the invention is mainly reflected in:
(1) feature that, the method has that preparation process technique is simple, operational safety, environmental pollution are little;
(2), the method with yellow water and carbonic acid gas for raw material, by adding pattern agent, ball shaped nano Strontium carbonate powder material is prepared under the condition of ultrasonic disperse, reduce production cost, do not introduce the impurity affecting ball shaped nano Strontium carbonate powder quality in raw material, yellow water prepares the ball shaped nano strontium carbonate powder material of high-quality through carbonation step;
(3) the ball shaped nano Strontium carbonate powder that, the method prepares has the advantage of spherical effective, uniform particles, good dispersity.
Accompanying drawing explanation
Fig. 1 is the process flow sheet of the preparation method of the ball shaped nano Strontium carbonate powder that embodiment of the present invention provides.
Fig. 2 is the scanning electron microscope (SEM) photograph of the ball shaped nano Strontium carbonate powder that the embodiment of the present invention 1 prepares.
Fig. 3 is the XRD figure of the ball shaped nano Strontium carbonate powder that the embodiment of the present invention 1 prepares.
Fig. 4 is the scanning electron microscope (SEM) photograph of the ball shaped nano Strontium carbonate powder that the embodiment of the present invention 2 prepares.
Fig. 5 is the XRD figure of the ball shaped nano Strontium carbonate powder that the embodiment of the present invention 2 prepares.
Fig. 6 is the scanning electron microscope (SEM) photograph of the ball shaped nano Strontium carbonate powder that the embodiment of the present invention 3 prepares.
Fig. 7 is the XRD figure of the ball shaped nano Strontium carbonate powder that the embodiment of the present invention 3 prepares.
Embodiment
Below in conjunction with accompanying drawing, by embodiment, the present invention will be further described.
Consult Fig. 1, the preparation method of the ball shaped nano Strontium carbonate powder provided in this embodiment comprises step:
S101, in soluble strontium salts solution, add pattern agent stirring and dissolving, obtain the first solution; Wherein, in the pattern agent added and strontium salt solution, the mol ratio of strontium ion is 2:1 ~ 1.5.Wherein, when adding pattern agent in soluble strontium salts solution, mixing solutions is heated to 50 ~ 80 DEG C, to accelerate the dissolution time of mixing solutions and to prevent strontium hydroxide crystallization.Wherein, described pattern agent is disodium ethylene diamine tetraacetate (EDTA).
S102, described first solution is proceeded in ultrasonic reactor, in ultrasonic process, pass into CO
2gas, until the pH value making solution is 5 ~ 9, obtains the second solution; Wherein, CO is passed into
2the flow of gas is 2 ~ 10L/min.Wherein, CO is passed into
2the more preferred scope of flow of gas is 4 ~ 8L/min.Wherein, ultrasonic frequency is 80 ~ 100KHz.
S103, described second solution is carried out solid-liquid separation, obtain solid product.Particularly, adopt the method for centrifugation to carry out solid-liquid separation to the second solution, the solid phase obtained to proceed in ultrasonic cleaner and adds EtOH Sonicate dispersion, obtains described solid product.
S104, by described solid product through washing and drying after obtain described ball shaped nano Strontium carbonate powder.Particularly, distilled water and ethanol is adopted to wash described solid product as washing composition.
Wherein, following method is adopted to prepare soluble strontium salts solution, specifically comprise: first celestite ore is obtained after high temperature reduction strontium salt (being commonly called as grey black), then strontium salt is dissolved in the water of 50 ~ 90 DEG C, impurity such as removing calcium hydroxide and acid non-soluble substance etc., obtain the soluble strontium salts solution (being commonly called as yellow water) containing strontium sulfide, sulphur hydrogenation strontium and strontium hydroxide, in solution, strontium ion (in strontium sulfide) volumetric molar concentration is 3 ~ 5mol/L.
Can prepare according to as above method and comprise multiple shape approximation in the nano strontium carbonate powder of spherical monomer, the particle size range of each monomer is 80 ~ 200nm.
Embodiment 1
One, add in the beaker of 900ml by 600ml yellow water, be heated to 60 DEG C, magnetic agitation is dissolved, and dissolves completely, adds 200gEDTA, continue stirring and dissolving, dissolves completely and obtains stock liquid.Wherein: in yellow water, total content of strontium (strontium sulfide, sulphur hydrogenation strontium and strontium hydroxide) and EDTA mol ratio are 2:1.
Two, pour in ultrasonic reactor by the stock liquid obtained, ultrasonic frequency is 100KHz, and ultrasonic temperature is 60 DEG C; Pass into carbonic acid gas and carry out carbonization, the flow of carbonic acid gas is 2L/min, and during carbonization 20min, the pH value of solution is 6, stops carbonization, obtains suspension.Wherein, carbon dioxide gas stream also plays the effect of stirring when carbonization, better can control the pattern of the ball shaped nano Strontium carbonate powder generated.
Three, suspension is separated through whizzer, is separated the solid phase obtained and adopts distilled water and ethanol respectively to wash once, then add ethanol ultrasonic disperse 1h in ultrasonic cleaner, obtain solid product.
Four, adopted by solid product distilled water and ethanol through washing and obtain ball shaped nano strontium carbonate product after drying.
Ball shaped nano strontium carbonate product is analyzed under scanning electron microscope, the scanning electron microscope (SEM) photograph of the ball shaped nano Strontium carbonate powder that the present embodiment as shown in Figure 2 prepares, confirm to obtain as particle diameter is the ball shaped nano strontium carbonate powder material of 80 ~ 200nm.Ball shaped nano strontium carbonate product is carried out XRD diffraction analysis, Fig. 3 is the XRD figure of the ball shaped nano Strontium carbonate powder that shown the present embodiment prepares, the diffraction peak obtained is consistent with Strontium carbonate powder standard diagram (JCPDScardno.05-0418), occurs, belong to rhombic system without assorted peak.
Embodiment 2
One, add in the beaker of 900ml by 500ml yellow water, be heated to 80 DEG C, magnetic agitation is dissolved, and dissolves completely, adds 180gEDTA, continue stirring and dissolving, dissolves completely and obtains stock liquid.Wherein: in yellow water, total content of strontium (strontium sulfide, sulphur hydrogenation strontium and strontium hydroxide) and EDTA mol ratio are 2:1.5.
Two, pour in ultrasonic reactor by the stock liquid obtained, ultrasonic frequency is 80KHz, and ultrasonic temperature is 40 DEG C; Pass into carbonic acid gas and carry out carbonization, the flow of carbonic acid gas is 4L/min, and during carbonization 13min, the pH value of solution is 7, stops carbonization, obtains suspension.Wherein, carbon dioxide gas stream also plays the effect of stirring when carbonization, better can control the pattern of the ball shaped nano Strontium carbonate powder generated.
Three, suspension is separated through whizzer, is separated the solid phase obtained and adopts distilled water and ethanol respectively to wash once, then add ethanol ultrasonic disperse 1h in ultrasonic cleaner, obtain solid product.
Four, adopted by solid product distilled water and ethanol through washing and obtain ball shaped nano strontium carbonate product after drying.
Ball shaped nano strontium carbonate product is analyzed under scanning electron microscope, the scanning electron microscope (SEM) photograph of the ball shaped nano Strontium carbonate powder that the present embodiment as shown in Figure 4 prepares, confirm to obtain as particle diameter is the ball shaped nano strontium carbonate powder material of 80 ~ 200nm.Ball shaped nano strontium carbonate product is carried out XRD diffraction analysis, Fig. 5 is the XRD figure of the ball shaped nano Strontium carbonate powder that shown the present embodiment prepares, the diffraction peak obtained is consistent with Strontium carbonate powder standard diagram (JCPDScardno.05-0418), occurs, belong to rhombic system without assorted peak.
Embodiment 3
One, add in the beaker of 900ml by 550ml yellow water, be heated to 80 DEG C, magnetic agitation is dissolved, and dissolves completely, adds 180gEDTA, continue stirring and dissolving, dissolves completely and obtains stock liquid.Wherein: in yellow water, total content of strontium (strontium sulfide, sulphur hydrogenation strontium and strontium hydroxide) and EDTA mol ratio are 2:1.2.
Two, pour in ultrasonic reactor by the stock liquid obtained, ultrasonic frequency is 90KHz, and ultrasonic temperature is 50 DEG C; Pass into carbonic acid gas and carry out carbonization, the flow of carbonic acid gas is 10L/min, and during carbonization 5min, the pH value of solution is 8, stops carbonization, obtains suspension.Wherein, carbon dioxide gas stream also plays the effect of stirring when carbonization, better can control the pattern of the ball shaped nano Strontium carbonate powder generated.
Three, suspension is separated through whizzer, is separated the solid phase obtained and adopts distilled water and ethanol respectively to wash once, then add ethanol ultrasonic disperse 1h in ultrasonic cleaner, obtain solid product.
Four, adopted by solid product distilled water and ethanol through washing and obtain ball shaped nano strontium carbonate product after drying.
Ball shaped nano strontium carbonate product is analyzed under scanning electron microscope, the scanning electron microscope (SEM) photograph of the ball shaped nano Strontium carbonate powder that the present embodiment as shown in Figure 6 prepares, confirm to obtain as particle diameter is the ball shaped nano strontium carbonate powder material of 80 ~ 200nm.Ball shaped nano strontium carbonate product is carried out XRD diffraction analysis, Fig. 7 is the XRD figure of the ball shaped nano Strontium carbonate powder that shown the present embodiment prepares, the diffraction peak obtained is consistent with Strontium carbonate powder standard diagram (JCPDScardno.05-0418), occurs, belong to rhombic system without assorted peak.
In sum, compared with prior art, the advantage that method provided by the invention has that preparation process technique is simple, operational safety, environmental pollution are little; The method with yellow water and carbonic acid gas for raw material, by adding pattern agent, ball shaped nano Strontium carbonate powder material is prepared under the condition of ultrasonic disperse, ethanol and pattern agent can recycle, reduce production cost, do not introduce the impurity affecting ball shaped nano Strontium carbonate powder quality in raw material, yellow water prepares the ball shaped nano strontium carbonate powder material of high-quality through carbonation step; And the strontium carbonate powder that method of the present invention prepares has the advantage of spherical effective, uniform particles, good dispersity.
The above is only the embodiment of the application; it should be pointed out that for those skilled in the art, under the prerequisite not departing from the application's principle; can also make some improvements and modifications, these improvements and modifications also should be considered as the protection domain of the application.
Claims (4)
1. a preparation method for ball shaped nano Strontium carbonate powder, is characterized in that, comprises step:
S101, in soluble strontium salts solution, add pattern agent stirring and dissolving, obtain the first solution; Wherein, in the pattern agent added and strontium salt solution, the mol ratio of strontium ion is 2:1 ~ 1.5, when adding pattern agent in soluble strontium salts solution, mixing solutions is heated to 50 ~ 80 DEG C, to accelerate the dissolution time of mixing solutions and to prevent strontium hydroxide crystallization;
S102, proceed in ultrasonic reactor by described first solution, ultrasonic frequency is 80 ~ 100KHz, in ultrasonic process, pass into CO
2gas, until the pH value making solution is 5 ~ 9, obtains the second solution; Wherein, CO is passed into
2the flow of gas is 4 ~ 8L/min;
S103, described second solution is carried out solid-liquid separation, obtain solid product;
S104, by described solid product through washing and drying after obtain described ball shaped nano Strontium carbonate powder; Described ball shaped nano Strontium carbonate powder comprises multiple shape approximation in spherical monomer, and the particle diameter of each monomer is 80 ~ 200nm;
Wherein, the step of preparation soluble strontium salts solution specifically comprises: first celestite ore is obtained strontium salt after high temperature reduction, then strontium salt is dissolved in the water of 50 ~ 90 DEG C, removing calcium hydroxide and acid non-soluble substance impurity, obtain the soluble strontium salts solution containing strontium sulfide, sulphur hydrogenation strontium and strontium hydroxide.
2. preparation method according to claim 1, is characterized in that, in step S103, adopts the method for centrifugation to carry out solid-liquid separation to the second solution, and the solid phase obtained to proceed in ultrasonic cleaner and adds EtOH Sonicate dispersion, obtains described solid product.
3. preparation method according to claim 1, is characterized in that, in step S104, adopts distilled water and ethanol to wash described solid product as washing composition.
4. preparation method according to claim 1, is characterized in that, described pattern agent is disodium ethylene diamine tetraacetate.
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| CN107082441A (en) * | 2017-04-14 | 2017-08-22 | 华南理工大学 | A kind of preparation method of hollow rice-shaped strontium carbonate |
| CN110451544A (en) * | 2019-08-14 | 2019-11-15 | 青海民族大学 | A kind of preparation method of ball shaped nano strontium carbonate |
| CN113856236B (en) * | 2021-10-14 | 2023-06-23 | 昆明理工大学 | Method for preparing nano material by regulating and controlling calcium-based solid waste dissolution crystallization by multiple physical fields |
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| CN101269831A (en) * | 2008-04-08 | 2008-09-24 | 中国科学院青海盐湖研究所 | Method for producing high purity strontium carbonate with double decomposition reaction-dissolution-abstraction |
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| CN101559965A (en) * | 2009-05-19 | 2009-10-21 | 中国科学院青海盐湖研究所 | Method for using medium and low-grade celestite ore to produce strontium carbonate under plateau conditions |
| CN102776363A (en) * | 2012-08-21 | 2012-11-14 | 中国科学院青海盐湖研究所 | Process for balling by mixing 200 meshes of celestite mineral powders and reduction coals |
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Patent Citations (4)
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| CN101269831A (en) * | 2008-04-08 | 2008-09-24 | 中国科学院青海盐湖研究所 | Method for producing high purity strontium carbonate with double decomposition reaction-dissolution-abstraction |
| CN101525151A (en) * | 2009-03-20 | 2009-09-09 | 仙桃市中星电子材料有限公司 | Manufacturing technique for high-purity electronic grade strontium titanate |
| CN101559965A (en) * | 2009-05-19 | 2009-10-21 | 中国科学院青海盐湖研究所 | Method for using medium and low-grade celestite ore to produce strontium carbonate under plateau conditions |
| CN102776363A (en) * | 2012-08-21 | 2012-11-14 | 中国科学院青海盐湖研究所 | Process for balling by mixing 200 meshes of celestite mineral powders and reduction coals |
Non-Patent Citations (1)
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| "Spherical nanometer strontium carbonate by ultrasonic method in the water phase";Zhanshou Yang et al.;《Advanced Materials Research》;20140116;第881-883卷;第1003页1.1节、第1004页1.2节、第1006页1-7行、图1-2 * |
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