CN110451544A - A kind of preparation method of ball shaped nano strontium carbonate - Google Patents
A kind of preparation method of ball shaped nano strontium carbonate Download PDFInfo
- Publication number
- CN110451544A CN110451544A CN201910752691.3A CN201910752691A CN110451544A CN 110451544 A CN110451544 A CN 110451544A CN 201910752691 A CN201910752691 A CN 201910752691A CN 110451544 A CN110451544 A CN 110451544A
- Authority
- CN
- China
- Prior art keywords
- solution
- ball shaped
- shaped nano
- strontium carbonate
- preparation
- 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
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/18—Carbonates
- C01F11/186—Strontium or barium carbonate
- C01F11/187—Strontium carbonate
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Nanotechnology (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Geology (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a kind of preparation methods of ball shaped nano strontium carbonate, celestine comprising steps of S10, be dissolved in 50 DEG C~100 DEG C of water and 2~4h of constant temperature by it after high temperature reduction, it is filtered to remove insoluble impurities and obtains soluble strontium salting liquid, crystal control agent is added to strontium salt solution and continues to stir, obtains clear first solution；Surfactant is added in S20, the sodium carbonate liquor for being 10%~25% to mass fraction, preparation forms the second solution；S30, the first solution and the second solution are injected separately into progress hypergravity reaction in supergravity reactor, obtain slurry solution；S40, slurry solution is separated by solid-liquid separation to obtain solid product, solid product is obtained into ball shaped nano strontium carbonate after washing and drying.Method of the invention can prepare the ball shaped nano strontium carbonate that spherical effect is good, particle is uniform, particle size range is narrow.
Description
Technical field
The invention belongs to chemical technology field more particularly to a kind of preparation methods of ball shaped nano strontium carbonate.
Background technique
Strontium carbonate is a kind of important industrial chemicals, due to it have very strong absorption X-ray and gamma-radiation function and
Other unique physical and chemical performances are widely used in color picture tube glass bulb, cathode-ray tube, electronic ceramics, magnetic material
The manufacture of the industrial goods such as material, fuel, paint, be related to electronics, chemical industry, military project, building materials, non-ferrous metal, aerospace, light industry,
All conglomeraties such as medicine, food.Although China has become strontium product major producing country, annual output account for about world wide production 50%~
60%, but since strontium industry is lack of standardization, causes structure serious unbalance, low side excess supply capacity, high-end supply scarce capacity.With
The fast development of electronics industry, high-quality electron level, Fluorescence Grade, nanoscale strontium carbonate product demand every year with 15% speed
Degree increases, and the notch of high-quality strontium carbonate seems more serious.
With the fast development of the industries such as domestic and international electronic component, magnetic material and ceramic material, to strontium carbonate product
Quality also have higher requirement, how focused mostly in the past to the research of strontium carbonate makes to produce high efficiency, purity High Purity etc..
However as development in science and technology, there are also to its object other than chemical index, that is, purity or content to product, the requirement in terms of impurity
Index, the i.e. requirement of particle morphology, size distribution, thermal characteristics and practicability test etc. are managed, which results in different-shapes
Strontium carbonate product has different application values.
Ball shaped nano strontium carbonate is with a wide range of applications and huge application value, how to prepare the good ball of pattern
Shape nano strontium carbonate is to solve the problems, such as in exploration in the industry.
Summary of the invention
For the deficiencies in the prior art, the present invention provides a kind of preparation methods of ball shaped nano strontium carbonate, pass through the party
Method can prepare the ball shaped nano strontium carbonate that spherical effect is good, particle is uniform, particle size range is narrow.
For achieving the above object, present invention employs following technical solutions:
A kind of preparation method of ball shaped nano strontium carbonate comprising step:
S10, celestine is dissolved in after high temperature reduction in 50~100 DEG C of water simultaneously 2~4h of constant temperature, be filtered to remove insoluble
Property impurity obtain soluble strontium salting liquid, be added to strontium salt solution and crystal control agent and continue to stir, it is molten to obtain clear first
Liquid；
Surfactant is added in S20, the sodium carbonate liquor for being 10%~25% to mass fraction, it is molten that preparation forms second
Liquid；
S30, first solution and second solution are injected separately into supergravity reactor and are reacted, obtained
Strontium carbonate slurry solution；Wherein, the injection flow of first solution is 70~160L/h, the injection flow of second solution
For 93~160L/h, the revolving speed of the supergravity reactor is 900~2000r/min；
S40, it is separated by solid-liquid separation the slurry solution to obtain solid product, by the solid product by washing and doing
Ball shaped nano strontium carbonate is obtained after dry.
Wherein, the crystal control agent is disodium ethylene diamine tetraacetate.
Wherein, the molar ratio of strontium ion is 0.4~1 in the additional amount of the crystal control agent and strontium salt solution.
Wherein, the surfactant is cetyl trimethylammonium bromide.
Wherein, the additional amount of the surfactant is the 0.2%~1% of sodium carbonate quality.
Wherein, in the step S40, the slurry solution is separated by solid-liquid separation using the method for centrifuge separation and is consolidated
Body product obtains ball shaped nano strontium carbonate after then drying successively using solid product described in distilled water and ethanol washing.
The preparation method of ball shaped nano strontium carbonate provided in an embodiment of the present invention, using supergravity reactor, in revolving bed
It is middle to there is the sodium carbonate liquor of surfactant to be carbonized the strontium salt solution added with crystal control agent using addition, pass through control
The revolving speed of the feed liquor flow and revolving bed of sodium carbonate liquor and strontium salt solution, can control generation, the speed of growth of nucleus, makes
The microcosmic uniformly mixedization time is less than nucleation induction time, carries out nucleation in uniform micro, thus obtains spherical shape
The ball shaped nano strontium carbonate that effect is good, particle is uniform, particle size range is narrow.
Detailed description of the invention
Fig. 1 is the process flow chart of the preparation method of ball shaped nano strontium carbonate provided in an embodiment of the present invention；
Fig. 2 is the scanning electron microscope (SEM) photograph for the ball shaped nano strontium carbonate that the embodiment of the present invention 1 is prepared；
Fig. 3 is the XRD diagram for the ball shaped nano strontium carbonate that the embodiment of the present invention 1 is prepared；
Fig. 4 is the scanning electron microscope (SEM) photograph for the ball shaped nano strontium carbonate that the embodiment of the present invention 2 is prepared；
Fig. 5 is the XRD diagram for the ball shaped nano strontium carbonate that the embodiment of the present invention 2 is prepared.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, with reference to the accompanying drawing to specific reality of the invention
The mode of applying is described in detail.The example of these preferred embodiments is illustrated in the accompanying drawings.Shown in attached drawing and according to
The embodiments of the present invention of attached drawing description are only exemplary, and the present invention is not limited to these embodiments.
Here, it should also be noted that, in order to avoid having obscured the present invention because of unnecessary details, in the accompanying drawings only
Show with closely related structure and/or processing step according to the solution of the present invention, and be omitted little with relationship of the present invention
Other details.
The present invention provides a kind of preparation methods of ball shaped nano strontium carbonate, and refering to fig. 1, the preparation method includes step
It is rapid:
S10, celestine is dissolved in after high temperature reduction in 50 DEG C~100 DEG C of water simultaneously 2~4h of constant temperature, be filtered to remove not
Solubility impurity obtains soluble strontium salting liquid, and crystal control agent is added in Xiang Suoshu strontium salt solution and continues to stir, is clarified
The first solution.
Specifically, the crystal control agent is selected as disodium ethylene diamine tetraacetate (EDTA).The crystal control agent adds
The molar ratio for entering strontium ion in amount and strontium salt solution is 0.4~1.
S20, surfactant is added to the sodium carbonate liquor that mass fraction is 10%~25%, it is molten that preparation forms second
Liquid.
Specifically, the surfactant is selected as cetyl trimethylammonium bromide (CTMAB).The surfactant
Additional amount be sodium carbonate quality 0.2%~1%.
S30, by first solution and second solution be injected separately into supergravity reactor carry out hypergravity it is anti-
It answers, obtains slurry solution.
Specifically, in the range of the injection flow control of first solution is 70~160L/h, second solution
Flow control is injected in the range of 93~160L/h, the revolving speed of the supergravity reactor is set as 900~2000r/min's
In range.
S40, it is separated by solid-liquid separation the slurry solution to obtain solid product, by the solid product by washing and doing
Ball shaped nano strontium carbonate is obtained after dry.
Specifically, the slurry solution is separated by solid-liquid separation using the method for centrifuge separation to obtain solid product, successively
Using solid product described in distilled water and ethanol washing, ball shaped nano strontium carbonate is obtained after then drying.
Embodiment 1
(1), celestine is dissolved in in 85 DEG C of water after high temperature reduction and is kept the temperature 2h, insoluble impurities is removed, 85
Crystal control agent (disodium ethylene diamine tetraacetate) is added into the strontium salt solution under conditions of DEG C, the additional amount of crystal control agent
Molar ratio with strontium ion in strontium salt solution is 0.6, and continues to stir, and mixes, obtains clear first solution.
(2), cetyl trimethylammonium bromide is added in the sodium carbonate liquor for being 15% to mass fraction, the 16 of addition
Alkyl trimethyl ammonium bromide amount is the 0.7% of sodium carbonate quality, and preparation forms the second solution.
(3), by first solution and second solution be injected separately into supergravity reactor carry out hypergravity it is anti-
It answers, obtains slurry solution.Wherein, the injection flow control of first solution is 85L/h, the injection flow of second solution
Control is 90L/h, and the revolving speed of the supergravity reactor is set as 1200r/min.
(4), the slurry solution is separated by solid-liquid separation using the method for centrifuge separation to obtain solid product, is successively used
Solid product described in distilled water and ethanol washing obtains ball shaped nano strontium carbonate after then drying.
Ball shaped nano strontium carbonate product is analyzed under scanning electron microscope, the ball that the present embodiment as shown in Figure 2 is prepared
The scanning electron microscope (SEM) photograph of shape nano strontium carbonate, the partial size that confirmation obtains each monomer is that the spherical or spherical of 20nm~100nm receives
Rice strontium carbonate powder material, by ball shaped nano strontium carbonate powder material carry out XRD diffraction analysis, Fig. 3 be shown in the present embodiment
The XRD diagram for the ball shaped nano strontium carbonate being prepared, obtained diffraction maximum and strontium carbonate standard diagram (JCPDS card
No.05-0418) unanimously, no miscellaneous peak occurs, and belongs to rhombic system.
Embodiment 2
(1), celestine is dissolved in in 95 DEG C of water after high temperature reduction and is kept the temperature 3.5h, removes insoluble impurities, In
Crystal control agent (disodium ethylene diamine tetraacetate) is added to the strontium salt solution under conditions of 95 DEG C, the additional amount of crystal control agent
Molar ratio with strontium ion in strontium salt solution is 1, and continues to stir, and mixes, obtains clear first solution.
(2), cetyl trimethylammonium bromide is added in the sodium carbonate liquor for being 25% to mass fraction, the 16 of addition
Alkyl trimethyl ammonium bromide amount is the 1% of sodium carbonate quality, and preparation forms the second solution.
(3), by first solution and second solution be injected separately into supergravity reactor carry out hypergravity it is anti-
It answers, obtains aaerosol solution.Wherein, the injection flow control of first solution is 110L/h, the injection stream of second solution
Amount control is 150L/h, and the revolving speed of the supergravity reactor is set as 1900r/min.
(4), the aaerosol solution is separated by solid-liquid separation using the method for centrifuge separation to obtain solid product, is successively used
Solid product described in distilled water and ethanol washing obtains ball shaped nano strontium carbonate after then drying.
Ball shaped nano strontium carbonate product is analyzed under scanning electron microscope, the ball that the present embodiment as shown in Figure 4 is prepared
The scanning electron microscope (SEM) photograph of shape nano strontium carbonate, the partial size that confirmation obtains each monomer is that the spherical or spherical of 20nm~100nm receives
Rice strontium carbonate powder material, by ball shaped nano strontium carbonate powder material carry out XRD diffraction analysis, Fig. 5 be shown in the present embodiment
The XRD diagram for the ball shaped nano strontium carbonate being prepared, obtained diffraction maximum and strontium carbonate standard diagram (JCPDS card
No.05-0418) unanimously, no miscellaneous peak occurs, and belongs to rhombic system.
In conclusion the preparation method of ball shaped nano strontium carbonate provided by the invention can be prepared, spherical effect is good, particle
Uniformly, the narrow ball shaped nano strontium carbonate of particle size range.And this method simple process, safe operation are conducive to large-scale work
Industry metaplasia produces.
The above is only the specific embodiment of the application, it is noted that for the ordinary skill people of the art
For member, under the premise of not departing from the application principle, several improvements and modifications can also be made, these improvements and modifications are also answered
It is considered as the protection scope of the application.
Claims (6)
1. a kind of preparation method of ball shaped nano strontium carbonate, which is characterized in that comprising steps of
S10, celestine is dissolved in after high temperature reduction in 50 DEG C~100 DEG C of water simultaneously 2~4h of constant temperature, be filtered to remove insoluble
Impurity obtains soluble strontium salting liquid, and Xiang Suoshu strontium salt solution is added crystal control agent and continues to stir, and obtains clear first
Solution；
Surfactant is added in S20, the sodium carbonate liquor for being 10%~25% to mass fraction, preparation forms the second solution；
S30, first solution and second solution are injected separately into supergravity reactor and are reacted, obtain carbonic acid
Strontium slurry solution；Wherein, the injection flow of first solution is 70~160L/h, and the injection flow of second solution is 93
~160L/h, the revolving speed of the supergravity reactor are 900~2000r/min；
S40, the slurry solution containing strontium carbonate is separated by solid-liquid separation to obtain solid product, by the solid product by washing
And ball shaped nano strontium carbonate is obtained after drying.
2. the preparation method of ball shaped nano strontium carbonate according to claim 1, which is characterized in that the crystal control agent is
Disodium ethylene diamine tetraacetate.
3. the preparation method of ball shaped nano strontium carbonate according to claim 1 or 2, which is characterized in that the crystal controlling
The molar ratio of strontium ion is 0.4~1 in the additional amount and strontium salt solution of agent.
4. the preparation method of ball shaped nano strontium carbonate according to claim 1, which is characterized in that the surfactant is
Cetyl trimethylammonium bromide.
5. the preparation method of ball shaped nano strontium carbonate according to claim 1 or 4, which is characterized in that the surface-active
The additional amount of agent is the 0.2%~1% of sodium carbonate quality.
6. the preparation method of ball shaped nano strontium carbonate according to claim 1, which is characterized in that in the step S40, adopt
The aaerosol solution is separated by solid-liquid separation with the method for centrifuge separation to obtain solid product, is successively washed using distilled water and ethyl alcohol
The solid product is washed, obtains ball shaped nano strontium carbonate after then drying.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910752691.3A CN110451544A (en) | 2019-08-14 | 2019-08-14 | A kind of preparation method of ball shaped nano strontium carbonate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910752691.3A CN110451544A (en) | 2019-08-14 | 2019-08-14 | A kind of preparation method of ball shaped nano strontium carbonate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110451544A true CN110451544A (en) | 2019-11-15 |
Family
ID=68486719
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910752691.3A Pending CN110451544A (en) | 2019-08-14 | 2019-08-14 | A kind of preparation method of ball shaped nano strontium carbonate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110451544A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113735592A (en) * | 2021-07-21 | 2021-12-03 | 刘建恒 | Production process of composite nano ceramic powder |
| CN114477275A (en) * | 2022-03-08 | 2022-05-13 | 天津泽希新材料有限公司 | Preparation method of novel spherical barium titanate |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104016394A (en) * | 2014-06-26 | 2014-09-03 | 中国科学院青海盐湖研究所 | Spherical nano strontium carbonate and preparation method thereof |
| CN109824077A (en) * | 2019-03-11 | 2019-05-31 | 广西大学 | Spherical calcium carbonate and preparation method thereof |
| CN109911924A (en) * | 2017-12-13 | 2019-06-21 | 财团法人工业技术研究院 | The preparation method of calcium carbonate granule |
-
2019
- 2019-08-14 CN CN201910752691.3A patent/CN110451544A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104016394A (en) * | 2014-06-26 | 2014-09-03 | 中国科学院青海盐湖研究所 | Spherical nano strontium carbonate and preparation method thereof |
| CN109911924A (en) * | 2017-12-13 | 2019-06-21 | 财团法人工业技术研究院 | The preparation method of calcium carbonate granule |
| CN109824077A (en) * | 2019-03-11 | 2019-05-31 | 广西大学 | Spherical calcium carbonate and preparation method thereof |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113735592A (en) * | 2021-07-21 | 2021-12-03 | 刘建恒 | Production process of composite nano ceramic powder |
| CN113735592B (en) * | 2021-07-21 | 2023-01-24 | 刘建恒 | Production process of composite nano ceramic powder |
| CN114477275A (en) * | 2022-03-08 | 2022-05-13 | 天津泽希新材料有限公司 | Preparation method of novel spherical barium titanate |
| CN114477275B (en) * | 2022-03-08 | 2024-05-14 | 天津泽希新材料有限公司 | Preparation method of spherical barium titanate |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107640792A (en) | A kind of high compact small particle nickel cobalt manganese hydroxide and preparation method thereof | |
| CN110054196B (en) | Method for preparing high-purity spherical instant boric acid by organic molecule induction | |
| CN103962570A (en) | Preparation method of nickel nanopowder | |
| CN110451544A (en) | A kind of preparation method of ball shaped nano strontium carbonate | |
| CN103183372B (en) | A kind of template solid phase prepares the method for nano zine oxide | |
| CN103769601B (en) | The preparation method of triangle sheet nano-Ag particles | |
| CN112479241A (en) | Method for preparing flake aluminum oxide by utilizing flake aluminum hydroxide | |
| CN104478699A (en) | Preparation method of high-purity superfine cobalt oxalate powder | |
| CN105271322B (en) | Preparation method of fascicular magnesium carbonate trihydrate crystals | |
| CN101279208B (en) | Method for preparing Y type molecular sieve film | |
| CN104016394B (en) | A kind of preparation method of ball shaped nano Strontium carbonate powder | |
| CN102863005B (en) | Preparation method of multi-shell core-shell micro/nano structure Cu2O | |
| CN110255619A (en) | A method of based on upper conversion nano particle preparation three-dimensional hollow structure molybdenum sulfide | |
| CN108070907A (en) | A kind of method that bittern of dried-up lake prepares basic magnesium chloride whisker | |
| CN108586263A (en) | A kind of simple and convenient process for preparing of tetraethyl ammonium tetrafluoroborate | |
| CN106006713B (en) | A kind of preparation technology of active nano-ZnO | |
| CN108069851A (en) | A kind of method that no ammonia oxalic acid precipitation prepares cobalt oxalate | |
| CN104860344B (en) | Preparation method of spherical strontium carbonate | |
| CN114210965A (en) | Metallic silver and preparation method and application thereof | |
| CN108910947B (en) | Thin-sheet micro-nano (K, Na) NbO3Crystal and method for producing same | |
| CN102581289B (en) | Method for preparing monodisperse high-crystallinity silver powder | |
| CN106745033B (en) | The method for synthesizing RTH zeolite molecular sieves using pyridyl group organic formwork agent | |
| CN105817646B (en) | A kind of preparation method of the ball shape silver powder of high-tap density | |
| CN108149321A (en) | A kind of method of bittern production basic magnesium carbonate whisker for recycling dried-up lake | |
| CN115872451B (en) | Preparation method of sulfur-free spherical manganese carbonate powder |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20191115 |