CN112125765A - Sphere-like superfine barium nitrate and preparation method and application thereof - Google Patents
Sphere-like superfine barium nitrate and preparation method and application thereof Download PDFInfo
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- CN112125765A CN112125765A CN202011021405.5A CN202011021405A CN112125765A CN 112125765 A CN112125765 A CN 112125765A CN 202011021405 A CN202011021405 A CN 202011021405A CN 112125765 A CN112125765 A CN 112125765A
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- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B31/00—Compositions containing an inorganic nitrogen-oxygen salt
- C06B31/02—Compositions containing an inorganic nitrogen-oxygen salt the salt being an alkali metal or an alkaline earth metal nitrate
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- 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
- C01F11/36—Nitrates
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- 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
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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Abstract
The invention belongs to the technical field of recrystallization, and particularly relates to spheroidal superfine barium nitrate and a preparation method and application thereof. The invention provides a preparation method of spheroidal superfine barium nitrate, which comprises the following steps: under the condition of stirring, dropwise adding a saturated aqueous solution of barium nitrate into an anti-solvent, and recrystallizing to obtain the spheroidal superfine barium nitrate; the temperature of the saturated aqueous solution of barium nitrate is higher than that of the anti-solvent. The quasi-spherical superfine barium nitrate prepared by the preparation method provided by the invention has the characteristics that the major axis and the minor axis of the crystal form are close to 1, and the median particle size is small, thereby solving the technical bottleneck of the superfine barium nitrate powder at present. The test result of the embodiment shows that the length-to-axis ratio of the crystal form of the quasi-spherical superfine barium nitrate obtained by the method is 1.01-1.04, and the sphericity is high; the median particle size is 15.437-17.523 mu m, and the product has fine particle size; the purity is 99.2-99.3%, and the purity is high.
Description
Technical Field
The invention belongs to the technical field of recrystallization, and particularly relates to spheroidal superfine barium nitrate and a preparation method and application thereof.
Background
The material is ultra-fine, and the optical, electric, magnetic, mechanical, thermodynamic, surface and interface characteristics of the material are changed surprisingly, so that the material has a wider application prospect. The superfine barium nitrate powder is obtained by screening the barium nitrate powder, and the test research on the superfine barium nitrate shows that the combustion performance and smoke forming performance of the superfine barium nitrate in smoke, fire, smoke, combustion and other chemicals are greatly improved.
Because the crystallization speed of barium nitrate is high, the particle size of a powder product is easy to be large, the particle size distribution of the prior barium nitrate powder is wide and different, and the average particle size reaches 250 mu m. Therefore, no superfine barium nitrate product with a mature system exists in the market.
Disclosure of Invention
In view of the above, the present invention aims to provide a spheroidal superfine barium nitrate and a preparation method thereof, wherein the spheroidal superfine barium nitrate obtained by the preparation method provided by the present invention has characteristics of crystal form long-short axis ratio close to 1 and small median particle size.
In order to achieve the purpose of the invention, the invention provides the following technical scheme:
the invention provides a preparation method of spheroidal superfine barium nitrate, which comprises the following steps:
under the condition of stirring, dropwise adding a saturated aqueous solution of barium nitrate into an anti-solvent, and recrystallizing to obtain the spheroidal superfine barium nitrate; the temperature of the saturated aqueous solution of barium nitrate is higher than that of the anti-solvent.
Preferably, the stirring speed is 400-500 rpm.
Preferably, the anti-solvent is ethanol or acetone.
Preferably, the mass ratio of the barium nitrate saturated aqueous solution to the anti-solvent is (0.5-1): 1.
preferably, the dropping speed is 5.5-6.5 g/min.
Preferably, the temperature of the saturated aqueous solution of barium nitrate is 30-60 ℃.
Preferably, the temperature of the anti-solvent is 0-10 ℃.
The invention also provides the spheroidal ultrafine barium nitrate prepared by the preparation method in the technical scheme, wherein the length-to-axis ratio of the spheroidal ultrafine barium nitrate is less than or equal to 1.05, and the median particle size is less than or equal to 20 mu m.
Preferably, the purity of the quasi-spherical superfine barium nitrate is more than or equal to 98.0 percent, and the total content of moisture and volatile components is less than or equal to 0.10 wt.%.
The invention also provides the application of the sphere-like superfine barium nitrate in the technical scheme or the sphere-like superfine barium nitrate prepared by the preparation method in the technical scheme as a combustion agent or a smoke forming agent in fireworks, firemen, smoke screens or combustion.
The invention also provides a preparation method of the sphere-like superfine barium nitrate, which comprises the following steps: under the conditions of stirring and cooling, dropwise adding a saturated aqueous solution of barium nitrate into an anti-solvent, and recrystallizing to obtain the spheroidal superfine barium nitrate; the temperature of the saturated aqueous solution of barium nitrate is higher than that of the anti-solvent. The invention adopts a solution-antisolvent reverse phase adding method, barium nitrate saturated aqueous solution is added into an antisolvent, barium nitrate is recrystallized under the condition of stirring, and explosive nucleation promotes tiny barium nitrate crystals to be separated out instantly. The preparation method provided by the invention is beneficial to achieving the purpose of refining barium nitrate in the barium nitrate recrystallization, and has the advantages of simplicity, easiness in operation and extremely high industrial application value.
The invention provides spheroidal superfine barium nitrate, wherein the length-to-axis ratio of the spheroidal superfine barium nitrate is less than or equal to 1.05, and the median particle size is less than or equal to 20 mu m. The sphere-like superfine barium nitrate provided by the invention has the characteristics that the major axis and the minor axis of the crystal form are close to 1, and the median particle size is small, thereby solving the technical bottleneck of the superfine barium nitrate powder at present.
The test result of the embodiment shows that the length-to-axis ratio of the crystal form of the spheroidal superfine barium nitrate provided by the invention is 1.01-1.04, and the sphericity is high; the median particle size is 15.437-17.523 mu m, and the product has fine particle size; the purity is 99.2-99.3%, and the purity is high.
Drawings
FIG. 1 is a graph showing a distribution of particle sizes of spheroidal ultrafine barium nitrate obtained in example 1;
FIG. 2 is a graph showing a distribution of particle sizes of the spheroidal ultra-fine barium nitrate obtained in example 2;
FIG. 3 is a graph showing a distribution of particle sizes of the spheroidal ultrafine barium nitrate obtained in example 3.
Detailed Description
The invention provides a preparation method of spheroidal superfine barium nitrate, which comprises the following steps:
under the condition of stirring, dropwise adding a saturated aqueous solution of barium nitrate into an anti-solvent, and recrystallizing to obtain the spheroidal superfine barium nitrate; the temperature of the saturated aqueous solution of barium nitrate is higher than that of the anti-solvent.
In the present invention, unless otherwise specified, each component in the preparation method is a commercially available product well known to those skilled in the art.
Under the condition of stirring, dropwise adding a saturated aqueous solution of barium nitrate into an anti-solvent, and recrystallizing to obtain the spheroidal superfine barium nitrate.
In the invention, the preparation method of the barium nitrate saturated aqueous solution comprises the following steps: and mixing barium nitrate with water, heating and stirring to obtain a saturated aqueous solution of barium nitrate.
In the present invention, the purity of the barium nitrate is preferably not less than 99.5%.
In the invention, the addition amount of barium nitrate in the barium nitrate saturated aqueous solution is calculated according to the following formula:
the addition of barium nitrate equals the mass of water x the solubility of barium nitrate/100; in the formula, the solubility of barium nitrate refers to the solubility of barium nitrate under the temperature condition after stirring and temperature rise, for example, the relationship between the temperature and the solubility of barium nitrate (the saturated aqueous solution temperature of barium nitrate/the solubility of barium nitrate) is: 30 ℃/11.6g, 40 ℃/14.2g, 50 ℃/17.1g or 60 ℃/20.3 g.
In the preparation method of the barium nitrate saturated aqueous solution, the stirring speed is preferably 200-300 rpm, and more preferably 220-280 rpm; the rate of temperature rise is preferably 1 to 2 ℃/min, more preferably 1.2 to 1.8 ℃/min. In the present invention, the apparatus for preparing the saturated aqueous solution of barium nitrate is preferably a dissolver.
In the present invention, the temperature of the saturated aqueous solution of barium nitrate is preferably 30 to 60 ℃, specifically, 30 ℃, 40 ℃, 50 ℃ or 60 ℃.
In the present invention, the antisolvent is preferably ethanol or acetone. In the invention, the mass ratio of the barium nitrate saturated aqueous solution to the anti-solvent is preferably (0.5-1): 1, more preferably (0.6 to 0.9): 1. in the invention, the temperature of the anti-solvent is preferably 0-10 ℃, and more preferably 0-8 ℃. In the present invention, the temperature of the antisolvent is preferably obtained by decreasing the temperature; the cooling rate is preferably 3-5 ℃/min, and more preferably 3.5-4.5 ℃/min.
In the present invention, it is preferable that the antisolvent is placed in a crystallization machine, the barium nitrate saturated aqueous solution is placed in a high-order dropping tank, and the barium nitrate saturated aqueous solution is dropped into the antisolvent.
The invention controls the dropping speed of the barium nitrate saturated aqueous solution through the dead weight of the liquid in the high-order dropping groove and the opening of the valve of the high-order dropping groove, and is beneficial to ensuring the stability of the dropping speed.
Before recrystallization, the invention needs to ensure the dissolving temperature of the barium nitrate saturated aqueous solution to prevent the barium nitrate saturated aqueous solution from reducing temperature, so that the barium nitrate is supersaturated and the barium nitrate is crystallized and separated out in advance, and further the recrystallized barium nitrate product crystal is coarse; the method can prevent the problems that the barium nitrate saturated aqueous solution cannot be subjected to explosive nucleation when the barium nitrate aqueous solution is unsaturated and is recrystallized, the barium nitrate crystal cannot be uniformly crystallized and precipitated, and the barium nitrate crystal product grows to generate the adverse effects of wide particle size distribution and large particle size of the barium nitrate crystal.
In the present invention, the recrystallization is carried out under the condition that the anti-solvent is stirred. In the present invention, the stirring rate is preferably 400 to 500rpm, and more preferably 420 to 480 rpm.
In the invention, the dripping speed is preferably 5.5-6.5 g/min, and more preferably 5.7-6.0 g/min.
After the recrystallization, the invention preferably further comprises the steps of sequentially carrying out solid-liquid separation, drying and screening on the recrystallized product.
The solid-liquid separation is not particularly limited in the present invention, and may be performed by a solid-liquid separation known to those skilled in the art, specifically, by filtration. After solid-liquid separation, drying the obtained solid material; the resulting liquid is preferably subjected to rectification to recover the anti-solvent therefrom. In the invention, the drying temperature is preferably 40-60 ℃, and more preferably 50-60 ℃; the drying time is not particularly limited in the invention, and the moisture in the solid material can be removed. The distillation is not particularly limited in the present invention, and may be a distillation known to those skilled in the art. The sieving is not particularly limited in the present invention, and may be performed by a sieving known to those skilled in the art, specifically, a sieving. In the invention, the number of the sieves in the sieving is preferably 150-200 meshes. In the invention, the undersize product is the quasi-spherical superfine barium nitrate after screening; the invention preferably repeats recrystallization of the oversize obtained after sieving. The invention promotes the easy-agglomeration ultrafine barium nitrate recrystallization product powder to be uniformly dispersed through sieving.
The yield of the spheroidal superfine barium nitrate prepared by the preparation method provided by the invention is preferably more than or equal to 80%.
The invention also provides the spheroidal ultrafine barium nitrate prepared by the preparation method in the technical scheme, wherein the length-to-axis ratio of the spheroidal ultrafine barium nitrate is less than or equal to 1.05, and the median particle size is less than or equal to 20 mu m.
In the invention, the length-to-axis ratio of the spheroidal superfine barium nitrate is less than or equal to 1.05, preferably 1.001-1.05, and more preferably 1.01-1.04. In the invention, the median particle size of the spheroidal superfine barium nitrate is less than or equal to 20 microns, preferably 10-20 microns, and more preferably 15-18 microns.
In the invention, the purity of the quasi-spherical superfine barium nitrate is preferably not less than 98.0%, more preferably 98.5-99.5%, and further preferably 99.0-99.3%. In the invention, the total content of moisture and volatile components in the spheroidal superfine barium nitrate is preferably less than or equal to 0.10 wt.%, and more preferably 0.01-0.05 wt.%.
The invention also provides the application of the sphere-like superfine barium nitrate in the technical scheme or the sphere-like superfine barium nitrate prepared by the preparation method in the technical scheme as a combustion agent or a smoke forming agent in fireworks, firemen, smoke screens or combustion.
In the invention, the application is preferably that the superfine barium nitrate is used for preparing combustion medicaments or smoke-forming medicaments instead of the traditional barium nitrate powder; the formulation of the present invention is not particularly limited, and may be a formulation known to those skilled in the art.
In order to further illustrate the present invention, the sphere-like ultrafine barium nitrate provided by the present invention, the preparation method and the application thereof are described in detail below with reference to the examples, but they should not be construed as limiting the scope of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Mixing 30g of barium nitrate and 150g of water, and heating to 60 ℃ at the speed of 2.0 ℃/min under the condition of stirring speed of 280rpm to obtain a saturated aqueous solution of barium nitrate;
cooling to 0-10 ℃ by 150g of ethanol at the speed of 5 ℃/min;
under the condition of stirring ethanol at 480rpm, controlling the dropping rate to be 6.0g/min, dropping a saturated aqueous solution of barium nitrate into the ethanol, filtering the obtained mixed feed liquid after the dropping is finished, drying a filter cake obtained by filtering at 40-60 ℃, and sieving a dried product with a 200-mesh sieve to obtain the subsieve substance, namely the spheroidal superfine barium nitrate.
Example 2
Mixing 25.65g of barium nitrate and 150g of water, and heating to 50 ℃ at the speed of 1.5 ℃/min under the condition of the stirring speed of 260rpm to obtain a saturated aqueous solution of barium nitrate;
cooling to 0-10 ℃ by 150g of ethanol at a speed of 4 ℃/min;
under the condition of stirring ethanol at the speed of 460rpm, controlling the dropping speed to be 5.8g/min, dropping a saturated aqueous solution of barium nitrate into the ethanol, filtering the obtained mixed feed liquid after the dropping is finished, drying a filter cake obtained by filtering at the temperature of 40-60 ℃, and then sieving a dried product with a 200-mesh sieve to obtain the subsieve fraction, namely the spheroidal superfine barium nitrate.
Example 3
Mixing 21.3g of barium nitrate and 150g of water, and heating to 40 ℃ at the speed of 1.0 ℃/min under the condition of stirring speed of 220rpm to obtain a saturated aqueous solution of barium nitrate;
cooling to 0-10 ℃ by 150g of ethanol at the speed of 3 ℃/min;
under the condition of stirring ethanol at the speed of 420rpm, controlling the dropping speed to be 5.7g/min, dropping a saturated aqueous solution of barium nitrate into the ethanol, filtering the obtained mixed feed liquid after the dropping is finished, drying a filter cake obtained by filtering at the temperature of 40-60 ℃, and then sieving a dried product with a 200-mesh sieve to obtain the subsieve fraction, namely the spheroidal superfine barium nitrate.
Performing particle size detection on the quasi-spherical superfine barium nitrate obtained in the examples 1-3 to obtain particle size distribution diagrams shown in the figures 1-3, wherein the figure 1 is the particle size distribution diagram of the quasi-spherical superfine barium nitrate obtained in the example 1; FIG. 2 is a graph showing a distribution of particle sizes of the spheroidal ultra-fine barium nitrate obtained in example 2; FIG. 3 is a graph showing a distribution of particle sizes of the spheroidal ultrafine barium nitrate obtained in example 3.
The spheroidal ultrafine barium nitrate obtained in examples 1 to 3 was subjected to test analysis, and test items and results are shown in table 1.
TABLE 1 test results of quasi-spherical ultrafine barium nitrate obtained in examples 1 to 3
As can be seen from figures 1 to 3 and table 1, the crystal form of the spheroidal ultrafine barium nitrate provided by the invention has a major-minor axis ratio of 1.01 to 1.04 and a high sphericity; the median particle size is 15.437-17.523 mu m, the product has fine and concentrated particle size and uniform distribution; the purity is 99.2-99.3%, and the purity is high.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A preparation method of sphere-like superfine barium nitrate comprises the following steps:
under the condition of stirring, dropwise adding a saturated aqueous solution of barium nitrate into an anti-solvent, and recrystallizing to obtain the spheroidal superfine barium nitrate; the temperature of the saturated aqueous solution of barium nitrate is higher than that of the anti-solvent.
2. The method according to claim 1, wherein the stirring speed is 400 to 500 rpm.
3. The method according to claim 1, wherein the anti-solvent is ethanol or acetone.
4. The preparation method according to claim 1, wherein the mass ratio of the saturated aqueous solution of barium nitrate to the anti-solvent is (0.5-1): 1.
5. the production method according to claim 1 or 4, wherein the dropping rate is 5.5 to 6.5 g/min.
6. The method according to claim 1, wherein the temperature of the saturated aqueous solution of barium nitrate is 30 to 60 ℃.
7. The method according to claim 1 or 6, wherein the temperature of the antisolvent is 0 to 10 ℃.
8. The spheroidal superfine barium nitrate prepared by the preparation method of any one of claims 1 to 7, wherein the length-to-axis ratio of the spheroidal superfine barium nitrate is less than or equal to 1.05, and the median particle size is less than or equal to 20 μm.
9. The spheroidal superfine barium nitrate of claim 8, wherein the spheroidal superfine barium nitrate has a purity of 98.0% or more and a total content of moisture and volatile components of 0.10 wt.% or less.
10. Use of the spheroidal ultrafine barium nitrate according to any one of claims 8 to 9 as a combustion agent or smoke-forming agent in fireworks, firemen, smoke screens or combustion.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113912653A (en) * | 2021-06-04 | 2022-01-11 | 天津大学 | Method for improving bulk density of beta-nicotinamide mononucleotide crystal powder |
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| CN108946768A (en) * | 2018-07-18 | 2018-12-07 | 中国科学院西安光学精密机械研究所 | Recrystallization method for preparing small-particle nitrate |
| CN110451548A (en) * | 2019-09-23 | 2019-11-15 | 山西北化关铝化工有限公司 | Spherical narrow granularity barium nitrate of one kind and preparation method thereof |
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| CN103936534A (en) * | 2014-05-09 | 2014-07-23 | 北京理工大学 | Idiosyncratic refined HMX (cyclotetramethylene tetranitramine) crystal and preparation method thereof |
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| CN113912653A (en) * | 2021-06-04 | 2022-01-11 | 天津大学 | Method for improving bulk density of beta-nicotinamide mononucleotide crystal powder |
| CN113912653B (en) * | 2021-06-04 | 2024-04-23 | 天津大学 | Method for improving bulk density of beta-nicotinamide mononucleotide crystalline powder |
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