CN108946768A - Recrystallization method for preparing small-particle nitrate - Google Patents
Recrystallization method for preparing small-particle nitrate Download PDFInfo
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- CN108946768A CN108946768A CN201810791869.0A CN201810791869A CN108946768A CN 108946768 A CN108946768 A CN 108946768A CN 201810791869 A CN201810791869 A CN 201810791869A CN 108946768 A CN108946768 A CN 108946768A
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- Prior art keywords
- nitrate
- solvent
- recrystallization method
- crystallization kettle
- little particle
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- 229910002651 NO3 Inorganic materials 0.000 title claims abstract description 30
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 239000002245 particle Substances 0.000 title claims abstract description 22
- 238000000034 method Methods 0.000 title claims abstract description 20
- 238000001953 recrystallisation Methods 0.000 title claims abstract description 16
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims abstract description 29
- 238000002425 crystallisation Methods 0.000 claims abstract description 20
- 230000008025 crystallization Effects 0.000 claims abstract description 20
- 238000003756 stirring Methods 0.000 claims abstract description 16
- 239000004323 potassium nitrate Substances 0.000 claims abstract description 14
- 235000010333 potassium nitrate Nutrition 0.000 claims abstract description 14
- 239000012296 anti-solvent Substances 0.000 claims abstract description 13
- 239000002904 solvent Substances 0.000 claims abstract description 13
- 239000000706 filtrate Substances 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 9
- IWOUKMZUPDVPGQ-UHFFFAOYSA-N barium nitrate Chemical compound [Ba+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O IWOUKMZUPDVPGQ-UHFFFAOYSA-N 0.000 claims abstract description 8
- IIPYXGDZVMZOAP-UHFFFAOYSA-N lithium nitrate Chemical compound [Li+].[O-][N+]([O-])=O IIPYXGDZVMZOAP-UHFFFAOYSA-N 0.000 claims abstract description 8
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims abstract description 8
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 6
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical compound [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims abstract description 5
- 238000001914 filtration Methods 0.000 claims abstract description 4
- 239000004317 sodium nitrate Substances 0.000 claims abstract description 4
- 235000010344 sodium nitrate Nutrition 0.000 claims abstract description 4
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- -1 filtering Substances 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- 229910052792 caesium Inorganic materials 0.000 claims description 2
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims 1
- NLSCHDZTHVNDCP-UHFFFAOYSA-N caesium nitrate Chemical compound [Cs+].[O-][N+]([O-])=O NLSCHDZTHVNDCP-UHFFFAOYSA-N 0.000 abstract description 10
- 238000001035 drying Methods 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- 239000002994 raw material Substances 0.000 description 8
- 239000013078 crystal Substances 0.000 description 5
- 238000009826 distribution Methods 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 4
- 229910052783 alkali metal Inorganic materials 0.000 description 3
- 238000004090 dissolution Methods 0.000 description 3
- 239000003380 propellant Substances 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000012856 packing Methods 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D9/00—Nitrates of sodium, potassium or alkali metals in general
- C01D9/18—Preparation in the form of shaped products, e.g. granules
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D36/00—Filter circuits or combinations of filters with other separating devices
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0004—Crystallisation cooling by heat exchange
- B01D9/0013—Crystallisation cooling by heat exchange by indirect heat exchange
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/02—Crystallisation from solutions
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D15/00—Lithium compounds
- C01D15/10—Nitrates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D17/00—Rubidium, caesium or francium compounds
- C01D17/003—Compounds of alkali metals
-
- 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
- C01F11/44—Concentrating; Crystallisating; Dehydrating; Preventing the absorption of moisture or caking
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Geology (AREA)
- Agronomy & Crop Science (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides a recrystallization method for preparing small-particle nitrate, aiming at the problems of poor appearance, sharp edges and corners, large particle size and the like of the nitrate, and comprising the following steps: 1) completely dissolving nitrate in a solvent, and filtering to obtain filtrate for later use; wherein the nitrate is one of sodium nitrate, potassium nitrate, cesium nitrate, barium nitrate, calcium nitrate and lithium nitrate, and the solvent is water; 2) injecting the anti-solvent into a crystallization kettle, and starting stirring; the anti-solvent is absolute ethyl alcohol or methanol or acetone; the volume of the anti-solvent is 2-5 times of the volume of the solvent; 3) dropwise adding the filtrate into a crystallization kettle, and continuously stirring for crystallization; 4) and filtering, washing and drying the mixture in the crystallization kettle.
Description
Technical field
The present invention relates to raw material disposal technical fields, and in particular to a kind of recrystallization for being used to prepare little particle nitrate
Method.
Background technique
Plasma can reflect or refracted electromagnetic wave, forms radar decoy, plays stealthy effect, and thermotropic electricity
From being a kind of simplest method for generating plasma, alkali metal element ionization energy is minimum in nature, but since it is active
Chemical characteristic, be not readily used for practical operation, therefore alkali metal salt is selected to be used as substitute, cesium nitrate is with fusing point, boiling point, decomposition
The relatively low feature of temperature is a kind of ideal material, and potassium nitrate, sodium nitrate, barium nitrate, lithium nitrate can also serve as
Alkali metal salt is ionized.
Currently, that there are appearances is poor for nitrate available on the market, sharp corners are had, the problems such as granularity is bigger than normal, referring to Fig. 1
Shown in the distribution of existing potassium nitrate raw material granularity.Therefore existing nitrate hot spot easy to form in pyrotechnic compound and propellant, thus
There may be burning or the danger of explosion；In addition degree of packing is influenced, keeps its degree of packing relatively low；Drawbacks described above limits nitric acid
Salt pyrotechnic compound and in terms of application, therefore to nitrate carry out refinement be of great significance.
Summary of the invention
The purpose of the present invention is having sharp corners for nitrate, the defects of granularity is bigger than normal and influence its in pyrotechnic compound and
The application of propellant etc., and then a kind of recrystallization method for being used to prepare little particle nitrate is provided, it is intended to it is nitrate
Application provide raw material support.
To achieve the above object, present invention provide the technical scheme that a kind of knot again for being used to prepare little particle nitrate
Crystal method is characterized in that, comprising the following steps:
1) nitrate is completely dissolved in a solvent, filtering, filtrate is stand-by；Wherein nitrate is sodium nitrate, potassium nitrate, nitre
One of sour caesium, barium nitrate, calcium nitrate and lithium nitrate, solvent are water；
2) anti-solvent is injected into crystallization kettle, opens stirring；Anti-solvent is dehydrated alcohol or methanol or acetone；The body of anti-solvent
Product is 2~5 times of solvent volume；
3) after filtrate added drop-wise being entered crystallization kettle, continue stirring and crystallized；
4) mixture in crystallization kettle is filtered, washed, dried.
Further, in step 2), water temperature is 25~40 DEG C in the collet of crystallization kettle.
Further, the stirring rate in step 2) and step 3) is 300~500rpm.
Further, the mixing time in step 2) is 2~5min；Mixing time in step 3) is 2~3h.
Further, in step 3), the drop rate of filtrate is 20~40mL/min.
Further, the initial concentration of nitrate is 0.23~0.48g/mL, i.e. dissolution 0.23 in every milliliter of solvent~
The nitrate of 0.48g
The invention has the advantages that
1, provided by the present invention for the recrystallization method of preparation little particle nitrate, technological operation is simple, reaction condition
Mildly, securely and reliably, green high-efficient, it is easy to accomplish industrialization；By adjusting technique, the round and smooth fine grained of narrow granularity can be obtained
Crystal.
2, after how much influences recrystallization of anti-solvent addition volume particle size, can be with by the additive amounts of different volumes
The crystal grain for obtaining different-grain diameter, realizes different purposes, solves in pyrotechnic compound and propellant that granularity is single, and density is inclined
It is low, the few problem of explosive payload.
3, selected solvent is water, and anti-solvent is volatile components, especially dehydrated alcohol, and anti-solvent and solvent are all right
Environment is friendly process, by realizing the recycling of tailing to mother liquid evaporation without influence.By the amplification of crystallization kettle, may be implemented
Industrialized production.
4, stirring comes into full contact with its solvent and anti-solvent, and the matching of mixing time and stirring rate makes after its crystallization
Grain surface is rounder and more smooth, and granularity is more uniform.
Detailed description of the invention
Fig. 1 is the particle size distribution figure of potassium nitrate raw material in existing market；
Fig. 2 is the particle size distribution figure using potassium nitrate after recrystallization method of the present invention crystallization.
Specific embodiment
In conjunction with attached drawing and by following two specific embodiment, the present invention is further explained, and the present invention is not limited to following
Embodiment.
Embodiment 1
The present embodiment provides a kind of recrystallization methods for being used to prepare little particle nitrate, comprising the following steps:
1) by 15g cesium nitrate dissolution of raw material in 50mL deionized water, solution is filled into 100mL beaker for use；
2) 100mL dehydrated alcohol is added into the flask of 250mL, flask is fixed on the dress of the electric stirring with water-bath
It sets, water bath with thermostatic control is set as 30 DEG C, and it opens and stirs, after revolving speed 300rpm, 2min,
3) it opens constant flow pump and the filtrate in 100mL beaker, drop rate 20mL/min is added dropwise into flask；To whole drops
After adding, continues stirring 2h and crystallized；
4) mixture in crystallization kettle is filtered, washed, dried, weighed.
Cesium nitrate crystal weight is about 13.4g, and cesium nitrate yield is 89.3%.
Embodiment 2
The present embodiment provides a kind of recrystallization methods for being used to prepare little particle nitrate, comprising the following steps:
1) by 40g potassium nitrate dissolution of raw material in 100mL deionized water, solution is filled into 250mL beaker for use；
2) 400mL dehydrated alcohol is added into the flask of 1000mL, flask is fixed on the electric stirring with water-bath
On device, water bath with thermostatic control is set as 35 DEG C, opens and stirs, after revolving speed 400rpm, 5min；
3) it opens constant flow pump and the filtrate in 250mL beaker, drop rate 30mL/min is added dropwise into flask；To whole drops
After adding, continues stirring 3h and crystallized；
4) mixture in crystallization kettle is filtered, washed, dried, weighed.
Potassium nitrate crystals weight is about 35.8g, and potassium nitrate yield is 89.5%.
Potassium nitrate size distribution after crystallization is shown in Fig. 2.Potassium nitrate median after crystallization is 19.959 μm, particle size range
It is relatively narrow, and potassium nitrate raw material granularity distribution as shown in Figure 1, median be 294.953 μm, particle size range is wider.With raw material phase
Compare, the potassium nitrate granules median after crystallization is smaller, and particle size range narrows, and sphericity is higher, and pattern is rounder and more smooth.
Claims (6)
1. a kind of recrystallization method for being used to prepare little particle nitrate, which comprises the following steps:
1) nitrate is completely dissolved in a solvent, filtering, filtrate is stand-by；Wherein nitrate is sodium nitrate, potassium nitrate, nitric acid
One of caesium, barium nitrate, calcium nitrate and lithium nitrate, solvent are water；
2) anti-solvent is injected into crystallization kettle, opens stirring；Anti-solvent is dehydrated alcohol or methanol or acetone；The volume of anti-solvent is
2~5 times of solvent volume；
3) after filtrate added drop-wise being entered crystallization kettle, continue stirring and crystallized；
4) mixture in crystallization kettle is filtered, washed, dried.
2. the recrystallization method according to claim 1 for being used to prepare little particle nitrate, it is characterised in that；Step 2)
In, water temperature is 25~40 DEG C in the collet of crystallization kettle.
3. the recrystallization method according to claim 2 for being used to prepare little particle nitrate, it is characterised in that；Step 2) and
Stirring rate in step 3) is 300~500rpm.
4. the recrystallization method according to claim 2 or 3 for being used to prepare little particle nitrate, it is characterised in that；Step
2) mixing time in is 2~5min；Mixing time in step 3) is 2~3h.
5. the recrystallization method according to claim 4 for being used to prepare little particle nitrate, it is characterised in that；Step 3)
In, the drop rate of filtrate is 20~40mL/min.
6. the recrystallization method according to claim 5 for being used to prepare little particle nitrate, it is characterised in that；Nitrate
Initial concentration is 0.23~0.48g/mL.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810791869.0A CN108946768A (en) | 2018-07-18 | 2018-07-18 | Recrystallization method for preparing small-particle nitrate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810791869.0A CN108946768A (en) | 2018-07-18 | 2018-07-18 | Recrystallization method for preparing small-particle nitrate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108946768A true CN108946768A (en) | 2018-12-07 |
Family
ID=64497823
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810791869.0A Pending CN108946768A (en) | 2018-07-18 | 2018-07-18 | Recrystallization method for preparing small-particle nitrate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108946768A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112125765A (en) * | 2020-09-25 | 2020-12-25 | 山西北化关铝化工有限公司 | Sphere-like superfine barium nitrate and preparation method and application thereof |
-
2018
- 2018-07-18 CN CN201810791869.0A patent/CN108946768A/en active Pending
Non-Patent Citations (2)
| Title |
|---|
| 丁亚娟: ""超细硝酸钾制备及其热物理性能研究"", 《中国优秀硕士学位论文全文数据库（电子期刊）工程科技I辑》 * |
| 任慧等: "《微纳米含能材料》", 30 April 2015, 北京理工大学出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112125765A (en) * | 2020-09-25 | 2020-12-25 | 山西北化关铝化工有限公司 | Sphere-like superfine barium nitrate and preparation method and application thereof |
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| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20181207 |
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