CN101428826B - Crystallization method for high-purity potassium fluoride - Google Patents
Crystallization method for high-purity potassium fluoride Download PDFInfo
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- CN101428826B CN101428826B CN2008102338271A CN200810233827A CN101428826B CN 101428826 B CN101428826 B CN 101428826B CN 2008102338271 A CN2008102338271 A CN 2008102338271A CN 200810233827 A CN200810233827 A CN 200810233827A CN 101428826 B CN101428826 B CN 101428826B
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- potassium fluoride
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- oslo crystallizer
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Abstract
The invention relates to a crystallization method for high-purity potassium fluoride, which is characterized in that crystallization is performed in an evaporative OSLO crystallizer. The potassium fluoride product prepared by the invention is characterized by large crystal granule and even granularity; the crystal represents an ellipsoid; moisture absorption and agglomeration are unlikely to happen; and the carbon content in the product is smaller than 15 ppm and stable. In addition, the daily output of the evaporative OSLO crystallizer for producing potassium fluoride is higher than 1 t, the daily output of the evaporative OSLO crystallizer is 8-10 times greater than that of an original middle-sized decompression crystallizer; the production cost of potassium fluoride is greatly reduced; and the invention has good economic value and social value and is easy to popularize and apply.
Description
Technical field
The present invention relates to a kind of crystallization method of high-purity potassium fluoride.
Background technology
Potassium monofluoride is mainly used in various alloys, the metal solder fusing assistant; On organic compound generates, be widely used as fluorizating agent, be used to generate Tenate and monofluoroacetamide sterilant on the agricultural; Pharmaceutically be used for making Norxin; Can be used as absorption agent (absorb HF and moisture) in addition, and the raw material of system potassium hydrogen fluoride, also can be used for glass-engraving and food is anticorrosion.Because KF character and crystalline structure characteristic are easy to the moisture absorption, absorbing carbon dioxide generation caking phenomenon, thereby influence its use properties.Therefore its quality index also must reach the purity height, the lattice complete form, and epigranular, good fluidity is difficult for the deliquescence caking.
Before this, the condensing crystal of Potassium monofluoride carries out in concentrating pan.Synthetic good potassium fluoride solution is transported in the concentrating pan with vacuum pump, opens the heating unit heating, make vacuum tightness remain on 80～100KPa, begin to concentrate.Per hour charging 10L concentrates 36h, stops vacuum pump, unloading.Keep the oil temperature at 80～95 ℃, continue to stir 3h, make the crystal grain maturation, stop oil heating and recycle pump, use whizzer to do processed concentrated solution then.In the Potassium monofluoride crystallisation process, the crystal grain of growing up earlier is deposited to the bottom of a pan, very easily with the discharging valve blockage, must just can open with steam heating.The Potassium monofluoride crystal grain that adopts this method to produce is smaller usually, the easy moisture absorption, and size is inhomogeneous, and it is irregular angular that the crystalline profile is, and the foreign matter content instability in the product, carbon content influence the final use properties of product at 5～25ppm.
Summary of the invention
The objective of the invention is to overcome the defective of above-mentioned prior art, provide a kind of Potassium monofluoride crystal of being produced that makes to be elliposoidal, be difficult for the moisture absorption, the foreign matter content in the product further descends and keeps stable, ensures the crystallization method of the high-purity potassium fluoride of the final use properties of product.
For realizing that the technical scheme that goal of the invention of the present invention is taked is:
A kind of crystallization method of high-purity potassium fluoride is characterized in that: crystallization is to carry out in evaporating OSLO crystallizer;
The density of feed liquid reaches 1.620g/cm in evaporating OSLO crystallizer
3The time water of condensation in the emptying surge tank.
Continue material once, 65 ℃～76 ℃ of slurry temperatures per half an hour in crystallisation process;
Vacuum tightness 0.08Mpa～0.09MPa in the control evaporating OSLO crystallizer, 33～38 ℃ of recycle pump out temperatures;
When pulp density reaches 1.625g/cm
3The time the centrifugal material that gets rid of.
Technical characterstic of the present invention is:
(1) selection of nucleation mode and nucleation process control: because the KF product characteristic of the moisture absorption very easily, the preparation number can be counted, even-grained crystal seed is difficult realization, so nucleation has been selected by control solution degree of supersaturation, the nucleus that spontaneous generation is an amount of, the mode of then degree of supersaturation being reduced to the steady district that is situated between.
(2) crystallization operation temperature controlling: the KF Tc is controlled under the temperature more than 65 ℃ carries out.
(3) control of solid-to-liquid ratio: in the practice, the overall average voidage of crystallizer is best at 0.7-0.95.
(4) control of degree of supersaturation: degree of supersaturation is the crystalline impellent, is in the stable degree of supersaturation in the steady district that is situated between, and is the key factor of decision crystallization nucleation and growth speed.Under the stable situation of all other operational conditions, monitor recycle pump and imported and exported the temperature difference, just can control the control of degree of supersaturation well.
The prepared Potassium monofluoride product crystal particle that goes out of the present invention is big, epigranular, and crystal is ellipsoid, is difficult for the moisture absorption and bonding, and the carbon content in the product is less than 15ppm and stable.In addition, the present invention produces the OSLO crystallizer day output of Potassium monofluoride more than 1t, is 8-10 times of original medium-sized decompression crystallizer, and greatly reduces the production cost of Potassium monofluoride, has good economic worth and social value, is easy to apply.
The Potassium monofluoride product index that the present invention produces
Embodiment
Embodiment 1
Synthetic good potassium fluoride solution one batch (2000kg) is sent into the crystallizer internal recycle by feed pump, open heating system for oil and propeller pump, in good time test density.When density reaches 1.620g/cm
3The time water of condensation in the emptying surge tank, per hour continuous material once keeps the liquid level in the evaporator room moderate in the crystallisation process.Keep the outlet oil of heating system for oil warm at 107 ℃, the vacuum tightness of 0.08MPa in the crystallizer, the solution temperature of continuous material is 76 ℃, 33 ℃ of recycle pump out temperatures.Saturated solution axially flows into the crystalline growth section through central downtake and removes degree of supersaturation, and crystal is suspension growth in continuous round-robin mother liquor stream, and particle is grown up the back settling velocity above floating velocity, and macrobead constantly accumulates in the crystallizer bottom.When solution density reaches 1.625g/cm
3After begin the centrifugal material that gets rid of, obtained the qualified Potassium monofluoride product of oarse-grained elliposoidal.
Embodiment 2
Synthetic good potassium fluoride solution one batch (1500kg) is sent into the crystallizer internal recycle by feed pump, open heating system for oil and propeller pump, later in good time test density.When density reaches 1.620g/cm
3The time water of condensation in the emptying surge tank, per hour continuous material once keeps the liquid level in the evaporator room moderate in the crystallisation process.Keep the outlet oil of heating system for oil warm at 110 ℃, the vacuum tightness of 0.08MPa in the crystallizer, the solution temperature of continuous material is 65 ℃, 38 ℃ of recycle pump out temperatures.Saturated solution axially flows into the crystalline growth section through central downtake and removes degree of supersaturation, and crystal is suspension growth in continuous round-robin mother liquor stream, and particle is grown up the back settling velocity above floating velocity, and macrobead constantly accumulates in the crystallizer bottom.Reach 1.625g/cm from solution density
3After begin the centrifugal material that gets rid of, obtained the qualified Potassium monofluoride product of oarse-grained elliposoidal.
Embodiment 3
Synthetic good potassium fluoride solution one batch (1800kg) is sent into the crystallizer internal recycle by feed pump, open heating system for oil and propeller pump, later in good time test density.When density reaches 1.621g/cm
3The time water of condensation in the emptying surge tank, per hour continuous material once keeps the liquid level in the evaporator room moderate in the crystallisation process.Keep the outlet oil of heating system for oil warm at 105 ℃, the vacuum tightness of 0.09MPa in the crystallizer, the solution temperature of continuous material is 69 ℃, 35 ℃ of recycle pump out temperatures.Saturated solution axially flows into the crystalline growth section through central downtake and removes degree of supersaturation, and crystal is suspension growth in continuous round-robin mother liquor stream, and particle is grown up the back settling velocity above floating velocity, and macrobead constantly accumulates in the crystallizer bottom.Reach 1.625g/cm from solution density
3After begin the centrifugal material that gets rid of, obtained the qualified Potassium monofluoride product of oarse-grained elliposoidal.
Embodiment 4
Synthetic good potassium fluoride solution one batch (2150kg) is sent into the crystallizer internal recycle by feed pump, open heating system for oil and propeller pump, later in good time test density.When density reaches 1.620g/cm
3The time water of condensation in the emptying surge tank, per hour continuous material once keeps the liquid level in the evaporator room moderate in the crystallisation process.Keep the outlet oil of heating system for oil warm at 112 ℃, the vacuum tightness of 0.09MPa in the crystallizer, the solution temperature of continuous material is 72 ℃, 37 ℃ of recycle pump out temperatures.Saturated solution axially flows into the crystalline growth section through central downtake and removes degree of supersaturation, and crystal is suspension growth in continuous round-robin mother liquor stream, and particle is grown up the back settling velocity above floating velocity, and macrobead constantly accumulates in the crystallizer bottom.Reach 1.625g/cm from solution density
3After begin the centrifugal material that gets rid of, obtained the qualified Potassium monofluoride product of oarse-grained elliposoidal.
Claims (1)
1. the crystallization method of a high-purity potassium fluoride, it is characterized in that: crystallization is to carry out in evaporating OSLO crystallizer, and the density of feed liquid reaches 1.620g/cm in evaporating OSLO crystallizer
3The time water of condensation in the emptying surge tank, continue material once per half an hour in crystallisation process, 65 ℃～76 ℃ of slurry temperatures, vacuum tightness 0.08MPa～0.09MPa in the control evaporating OSLO crystallizer, 33 ℃～38 ℃ of recycle pump out temperatures are when pulp density reaches 1.625g/cm
3The time centrifugal get rid of material oarse-grained elliposoidal Potassium monofluoride product, carbon content is less than 15ppm in this Potassium monofluoride product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008102338271A CN101428826B (en) | 2008-12-16 | 2008-12-16 | Crystallization method for high-purity potassium fluoride |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008102338271A CN101428826B (en) | 2008-12-16 | 2008-12-16 | Crystallization method for high-purity potassium fluoride |
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| Publication Number | Publication Date |
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| CN101428826A CN101428826A (en) | 2009-05-13 |
| CN101428826B true CN101428826B (en) | 2011-02-09 |
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| CN111498874B (en) * | 2020-02-21 | 2022-10-04 | 天津大学 | Large-particle-size cesium iodide spherical crystal and preparation method thereof |
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Granted publication date: 20110209 Termination date: 20121216 |