CN103818942B - Method for preparing high-purity anhydrous strontium iodide - Google Patents
Method for preparing high-purity anhydrous strontium iodide Download PDFInfo
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- CN103818942B CN103818942B CN201410029571.8A CN201410029571A CN103818942B CN 103818942 B CN103818942 B CN 103818942B CN 201410029571 A CN201410029571 A CN 201410029571A CN 103818942 B CN103818942 B CN 103818942B
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Abstract
The invention relate to a method for preparing high-purity anhydrous strontium iodide. The method comprises the following steps: dropwise adding hydroiodic acid into a reaction vessel containing an aqueous solution containing a strontium compound under stirring until the pH of the solution is 5-6 to obtain an iodide-strontium aqueous solution; regulating the pH value of the iodide-strontium aqueous solution to 7-9 for filtering; after concentrating filtrate to near saturation, quickly lowering the temperature to 0-4 DEG C and precipitating crystal substances; filtering to obtain the crystal substances dissolving in water, and obtaining a purified iodide-strontium aqueous solution; heating the purified strontium iodide aqueous solution to 150-200 DEG C under the flowing inert shielding gas, and preserving heat for 1-30 hours to dehydrate to obtain a SrI2.xH2O white flurry material, wherein x is less than or equal to 1; grinding the white flurry material into powder in an anhydrous and oxygen-free inert atmosphere, and putting in a glass vessel; under vacuum, heating the glass vessel to 350-450 DEG C and preserving heat for 1-20 hours to remove crystal water in the powder, and naturally lowering the temperature to room temperature in the condition of keeping vacuum; heat-sealing the glass vessel in the condition of keeping vacuum.
Description
Technical field
The present invention relates to a kind of preparation method of high-pure anhydrous strontium iodide, more particularly, the present invention relates to the preparation method of a kind of single crystal growing with high-pure anhydrous strontium iodide raw material, belong to haloid material preparation field, particularly crystal growth halide feedstock preparation field.
Background technology
Inorganic scintillator can be used for fast, determine highly enriched uranium sensitively and accurately, the gamma-rays characteristic of weapons-grade plutonium, radioactive source and other special nucleus raw material, verifies, the radiation detection field such as low energy nuclear test and nuclear non-proliferation verification has a wide range of applications at Radionuclides identification, safety inspection, environmental monitoring, chemical and biological weapons.In recent years, increasingly serious along with global Nuclear safety and terrified situation, and the raising of people's Radiation Environment Safety consciousness, also increased day by day to the demand of more high-performance scintillator.At present, a kind of scintillator be most widely used in above-mentioned field is NaI:Tl crystal, but the energy response disproportional of NaI:Tl crystal and energy resolution poor-performing, and as the hypertoxic Tl of activator ion
+, also there is the potential safety hazard that environment is polluted in a large amount of uses of ion.A new generation scintillation material LaBr
3: Ce crystal has good scintillation properties, but this material exists serious cleavage or stress cracking, and melt easily reacts with crucible, and preparation cost is high, also to contain simultaneously and can produce radioactive background
138la isotopic composition, it receives larger restriction in the application in radiation detection field.
As far back as 1969, U.S. Robert Hofstadter just applied for Eu
2+doping strontium iodide (SrI
2: Eu) crystal is as the patent of radiation detection material, but owing to preparing the second-rate of crystal at that time, performance was compared to business-like Tl
+ion doping NaI crystal there is no advantage, and its correlative study is subsequently absorbed in the silence of nearly 40 years.Until 2008, preparing high-quality SrI
2: after Eu crystal, the people such as Nerine Cherepy re-recognize SrI
2: the excellent scintillation properties of Eu.Their research finds, SrI
2: the light output of Eu can reach 120,000ph/MeV, is light output the highest known inorganic scintillator, has splendid energy resolution (<3%), in wider energy region, has good energy linearity.In addition, strontium iodide has lower fusing point, without cleavage, without phase transformation in from melting temperature to room temperature range, very easily adopts falling crucible method to realize mass-producing industrialization preparation.But the preparation of large size strontium iodide crystal faces larger difficulty; the strontium iodide raw material of commercial type must first could use through zone-refine; and batch there is larger cognation in the crystal mass grown and raw material; even if adopt extremely slow cooling rate; the crystal grown also often can ftracture; this not only adds the complicacy of equipment and process, also limit the development of this crystal application layer size (three inch diameters and more than).
It is generally acknowledged, the root of these problems that crystal growth exists is that the purity of raw material is not high enough, and except the content of metallic impurity ion, normal containing water molecules and non-water class oxygenate impurity in raw material, these water moleculess and non-water class are also harmful impurity containing oxygen class impurity for crystal growth.In halogenide Raw, water molecules generally exists with the form of planar water and crystal water, and the oxygenate impurity most importantly oxide compound of the oxidized rear formation of principal constituent or oxyhalogenide.Preparing on source at raw material, avoid the generation of these materials to be the fundamental ways obtaining high pure raw material, is also the inevitable choice improving crystal optics quality and performance.Strontium iodide (SrI
2) be a kind of inorganic salt be made up of strontium and iodine element, belong to ionic compound, anhydrous strontium iodide very easily deliquescence, and turn yellow seeing light or be exposed to easy precipitation elemental iodine in air, and Sr
2+ion is then converted to strontium oxide; In aerobic situation, strontium iodide is heated more easily oxidized, and the anhydrous strontium iodide preparing high-purity, low degree of oxidation and low water content exists larger difficulty always, is also the biggest obstacle that restriction strontium iodide crystal moves towards practical application.
The conventional method of the anhydrous strontium iodide of present preparation mainly contains following two kinds:
Method one: by concentration be 15% ~ 20% hydroiodic acid HI be dropwise added in Strontium carbonate powder and carry out neutralization reaction, be terminal during pH=5.5 ± 0.5, the iodine that of dissociating can be crossed and filter.In heating concentration process, just in case when having a large amount of free-iodine, dropwise can add H
2the S aqueous solution reduces.Continue suction strainer to concentrate, be concentrated into containing strontium iodide about 300 ~ 320g in about 100g solution, place cooling, six water strontium iodides can be separated out.Dry in moisture eliminator after centrifuge dehydration, fully mixed with ammonium iodide by six water strontium iodides, in semi-enclosed Glass tubing, decompression slowly heats up, and melting is dewatered, and can change anhydrous strontium iodide into, and cooling post crystallization is separated out.
Method two: Strontium carbonate powder is added to the water and stirs formation slurry, then hydroiodic acid HI is added gradually in slurry and react with Strontium carbonate powder, form the aqueous solution of strontium iodide, when the pH of solution is 1, solution is heated to 140 DEG C in atmosphere, keeps this temperature for some time, water in solution is evaporated in a large number, evaporation after product is cooled to 5 DEG C, filters the strontium iodide hydrate obtained containing six crystal water, hydrate is separated with solution parent under vacuo; Vacuumize progressively raised temperature to 60 DEG C, 90 DEG C, 150 DEG C and 300 DEG C, all keep for some time at each temperature section.
Wherein, the technical process involved by first method is comparatively complicated, and operational condition is wayward, low conversion rate, and uses ammonium iodide can produce a large amount of HI gas, there is the risk of contaminate environment, is not suitable as technique prepared by mass.Second method technique is comparatively simple, easy and simple to handle, but owing to being direct heating solution to 140 DEG C in atmosphere, the oxidation of strontium iodide is difficult to avoid, and adds to hanker excessive hydrogen iodide gas and directly volatilize, can serious environment pollution; In addition on the one hand, directly concentrated after dissolving containing strontium compound, that generally obtain is the strontium iodide hydrate (SrI containing 6 crystal water
26H
2o), if by the zone heating dehydration under vacuo of this hydrate, due in this hydrate containing a large amount of crystal water, when vacuum hydro-extraction, water molecules is difficult to be extracted out in time, and during dehydration, raw material easily hardens into bulk, often contains I in the middle of this block
2the material such as simple substance and water, these materials become the detrimental impurity in crystal growing process the most at last; Further, for avoiding remaining I
2simple substance and HI gas directly enter vacuum apparatus, and produce corrosion to vacuum apparatus, must set up cold-trap equipment in vacuum-lines, this will add complexity and the equipment cost of preparation technology undoubtedly.Therefore, need badly and find the simple preparation method of a kind of easy handling, technique, to obtain anhydrous strontium iodide raw material that is high-purity, low degree of oxidation, meet pure strontium iodide with doping strontium iodide crystal growth applications to the requirements at the higher level of raw material.
Summary of the invention
The object of the invention is to there are problems to solve in existing high-purity strontium iodide material prepared technology, that as low in productive rate, condition controls is difficult, preparation cost is high and easy generation environmental pollution etc., provides a kind of preparation method of high-pure anhydrous strontium iodide.
At this, the invention provides a kind of preparation method of high-pure anhydrous strontium iodide, comprising:
(1) dropwise adding hydroiodic acid HI to pH value of solution under stirring in the reaction vessel filled containing the strontium compound aqueous solution is 5 ~ 6, obtains the aqueous solution of strontium iodide;
(2) pH value of the aqueous solution of the strontium iodide of gained is adjusted to 7 ~ 9, filters, filtrate is concentrated into nearly saturated rear fast cooling to 0 ~ 4 DEG C with crystallization thing, filters to obtain crystallisate and be dissolved in deionized water, obtains the aqueous solution of strontium iodide after purifying;
(3) aqueous solution of strontium iodide after the purifying of gained is transferred in dewatering container, under the inertia protection gas of flowing, is heated to 150 ~ 200 DEG C, and is incubated 1 ~ 30 hour and dewaters, obtain SrI
2.xH
2the white puff material of O, x≤1;
(4) the white puff material of gained grind into powder in the inert atmosphere of anhydrous and oxygen-free is also loaded in the Glass Containers that can vacuumize;
(5) heat described Glass Containers to 350 ~ 450 DEG C insulation 1 ~ 20 hour under vacuum, to slough the crystal water in the powder of gained, keeping making described powder Temperature fall to room temperature under the state vacuumized; And
(6) to keep under the state that vacuumizes, by described Glass Containers sealing by fusing, obtaining the high-pure anhydrous strontium iodide be sealed in Glass Containers.
The present invention after the completion of reaction, first by pH regulator to 7 ~ 9 to neutralize excessive hydroiodic acid HI, and carry out thermal dehydration again after the strontium iodide be obtained by reacting is carried out purifying, excessive hydroiodic acid HI effectively can be avoided to enter vacuum apparatus at the hydrogen iodide gas concentrated and produce in heat-processed, or enter contaminate environment in air.And concentration process carries out under lesser temps or vacuum, and thermal dehydration process is carried out under protective atmosphere or vacuum condition, effectively can avoid the oxidation of strontium iodide.In addition, thermal dehydration process comprises: first under the inertia protection gas of flowing, most of crystal water is sloughed in heating, obtains only containing the white puff material of a small amount of crystal water; Carry out vacuum high-temperature again and slough remaining a small amount of crystal water.Like this owing to having removed mass crystallization water before vacuum high-temperature dehydration, and only remain a small amount of crystal water, therefore during vacuum hydro-extraction, water molecules is extracted out relatively easily in time, and during dehydration, powder is not easy caking.The present invention has that technique is simple, easy and simple to handle, environmental pollution is little, purity is high, oxidisability is low and be easy to industrialized feature, can be directly used in pure strontium iodide and the doping strontium iodide crystal of growing high-quality.
Preferably, in step (1), described is 30% ~ 60% containing the mass percent containing strontium compound in the strontium compound aqueous solution.Described is at least one in Strontium carbonate powder, strontium oxide and strontium hydroxide containing strontium compound.The described purity containing strontium compound is preferably not less than 99.9%.
Preferably, in step (1), described reaction vessel does not react with strontium iodide and HI acid or introduce the container of impurity, comprises glass, metal and earthenware porcelain receptacle.Be preferably the quartz crucible that purity is not less than 99.99%.
Preferably, in step (2), filtrate is concentrated into and is closely saturatedly concentrated into 50% ~ 70% of filtrate original volume for filtrate.Preferably, in step (2), described concentrated be heated to 100 DEG C ± 2 DEG C in air steam the concentrated or vacuum hydro-extraction of water and concentrate.
Preferably, in step (3), described dewatering container is do not introduce impurity or and SrI in heat-processed
2the container reacted, comprises glass, metal, graphite and vitreous carbon container.Dewatering container preferably has larger contact area with inert gas.
Preferably, in step (3), the inertia protection gas of described flowing is high-purity nitrogen, argon gas and/or helium, and flow velocity is 1 ~ 10L/ minute.
Preferably, in step (3), described heating is speed raised temperature to 150 ~ 200 DEG C with 1 ~ 10 DEG C/min.
Preferably, in step (4), described anhydrous and oxygen-free is that water and oxygen level be not all higher than 1000ppm.Preferably water and oxygen level are all at below 100ppm.
Preferably, in step (5), described Glass Containers is in advance through dehydroxylation and rare HF acid clean.Described Glass Containers is preferably the quartz glass crucibles that purity is not less than 99.99%.
Preferably, in step (5), described vacuum condition be vacuum tightness not higher than 1Pa, be preferably 10
-3below Pa.
Preferably, in step (5), described heating is heated to 350 ~ 450 DEG C stage by stage and is incubated 1 ~ 20 hour; Or rise to 300 ~ 450 DEG C with the temperature rise rate of 1 ~ 10 DEG C/min and be incubated 1 ~ 20 hour.
Accompanying drawing explanation
Fig. 1 is the process flow sheet of high-pure anhydrous strontium iodide preparation method.
Embodiment
Further illustrate the present invention below in conjunction with accompanying drawing and following embodiment, should be understood that accompanying drawing and following embodiment are only for illustration of the present invention, and unrestricted the present invention.
The invention provides the preparation method of high-purity strontium iodide.This preparation method mainly comprises: react containing strontium compound and hydroiodic acid HI the reactions steps generating strontium iodide; The strontium iodide of generation is carried out the purification step that purifying obtains sheet water-containing crystal thing; Remove the most of crystal water in water-containing crystal thing under an inert atmosphere, obtain the first water removal phase of the strontium iodide containing a small amount of crystal water; And under vacuum condition, remove the second water removal phase that remaining a small amount of crystal water obtains anhydrous strontium iodide.
Fig. 1 illustrates the concrete technology schema of the present invention's example.As shown in Figure 1, preparation method of the present invention specifically can comprise the following steps.
(1) add a certain amount of deionized water at reaction vessel, take appropriate adding in this container containing strontium compound, make the mass percent containing strontium compound be 30% ~ 60%.The reaction vessel adopted can be do not react with strontium iodide and HI acid or introduce the container of impurity, such as, can be glass, metal and pottery etc., be preferably the quartz crucible that purity is not less than 99.99%.What adopted can be any one of Strontium carbonate powder, strontium oxide and strontium hydroxide containing strontium compound, also can be the arbitrary proportion mixture of two or three of these materials.These purity containing strontium compound are generally not less than 99.9%.Dropwise (such as adopt reaction titration apparatus) and add hydroiodic acid HI at this container, continuous stirring (such as adopting magnetic stirring apparatus), make containing strontium compound and hydroiodic acid HI generation complete reaction, stop adding hydroiodic acid HI when pH value of solution to 5 ~ 6, obtain the aqueous solution of strontium iodide.
(2) regulating step (1) obtains pH to 7 ~ 9 of the aqueous solution, and the alkali such as ammoniacal liquor can be adopted to regulate.Elimination insolubles wherein, adopts heating or dehydrated under vacuum mode in air the filtrate obtained to be concentrated into closely saturated, when used be 30% ~ 60% containing the mass percent containing strontium compound in the strontium compound aqueous solution time, be concentrated into 50% ~ 70% of filtrate original volume.Wherein heating in air can be such as be heated to 100 DEG C ± 2 DEG C; Dehydrated under vacuum such as can adopt water ring vacuum pump.The reaction vessel filling near saturated solution is positioned in low temperature environment (such as ice cube), make filtrate fast cooling to 0 ~ 4 DEG C, make in solution, to produce plate crystal thing, vacuum filtration makes crystallisate be separated with mother liquor, crystallisate is dissolved in deionized water again, be preferably completely water-soluble to clear state, obtain the aqueous solution of strontium iodide after purifying.
(3) aqueous solution of purifying strontium iodide step (2) obtained is transferred in dewatering container, heats this aqueous solution, slough the main water in the aqueous solution, obtain only containing the white puff material of a small amount of crystal water under the inertia protection gas of flowing.Wherein, the dewatering container adopted can be in heat-processed does not introduce impurity or and SrI
2the container reacted, including but not limited to the container of the materials such as glass, metal, graphite or vitreous carbon.In addition, dewatering container preferably has larger contact area with inert gas.The inertia protection gas of flowing can be high pure nitrogen, high-purity argon gas or high-purity helium, and be preferably high-purity argon gas and high-purity helium, gas flow rate can be 1 ~ 10L/ minute.Described heating such as can adopt the ramp of 1 ~ 10 DEG C/min, raised temperature to 150 ~ 200 DEG C, and is incubated 1 ~ 30 hour.Can be directly be warming up to 150 ~ 200 DEG C; Also can be progressively heat, first be warming up to a certain medium temperature, such as 120 DEG C, and be incubated 2 hours, then be warming up to 150 ~ 200 DEG C.
(4) white fluffy material transfer step (3) obtained enters in glove box, pulverizes wherein in the Glass Containers of last loading vacuum-pumping.The glove box adopted can be inert-atmosphere glove box, and in this glove box, the content of water and oxygen all higher than 1000ppm, should not be preferably the content of water and oxygen all at below 100ppm.The Glass Containers adopted can be through the glass pot of dehydroxylation and rare HF acid clean, and being preferably purity is the quartz glass crucibles of more than 99.9%.
(5) under vacuum, powder described in heating steps (4), progressively slough a small amount of crystal water of residue that step (4) obtains containing in raw material, after water to be crystallized is sloughed completely, keep the state vacuumized to raw material Temperature fall to room temperature, namely obtain anhydrous strontium iodide powder that is high-purity, low degree of oxidation.Described heating can be warming up to 350 ~ 450 DEG C stage by stage, and keeps 1 ~ 20 hour, such as, be progressively warming up to 200 DEG C, 300 DEG C, 450 DEG C, keep 1 ~ 5 hour respectively at each temperature section; Also can be directly with ramp to 350 ~ 450 DEG C of 1 ~ 10 DEG C/min, and keep high temperature 1 ~ 20 hour.Described vacuum condition can be vacuum tightness not higher than 1Pa, preferred vacuum tightness is 10
-3below Pa.
(6) the Glass Containers sealing by fusing will constantly vacuumized, such as, adopt flame welding gun to carry out sealing by fusing, can obtain the high-pure anhydrous strontium iodide be sealed in Glass Containers.This high-pure anhydrous strontium iodide can be preserved so for a long time and not perishable.
The preparation method of anhydrous strontium iodide of the present invention has that technique is simple, easy and simple to handle, equipment requirements is low, oxidisability is low and is easy to advantage prepared by mass-producing, can be directly used in the pure strontium iodide of growth and doping strontium iodide crystal.
Exemplify embodiment below further to describe the present invention in detail.Should understand equally; following examples are only used to further illustrate the present invention; can not be interpreted as limiting the scope of the invention, some nonessential improvement that those skilled in the art's foregoing according to the present invention is made and adjustment all belong to protection scope of the present invention.The processing parameter etc. that following example is concrete is also only an example in OK range, and namely those skilled in the art can be done in suitable scope by explanation herein and select, and do not really want the concrete numerical value being defined in Examples below.
Embodiment 1
(1) in the glass beaker of 250ml, add 5.4 grams of deionized waters, take the Strontium carbonate powder (SrCO that purity is 99.99%
3) raw material 7.38 grams is placed in reaction vessel, dropwise add the hydroiodic acid HI that purity is not less than 99.9%, stirred by magnetic stirring apparatus, make Strontium carbonate powder and hydroiodic acid HI complete reaction, to solution clarification and pH value is 5.5 time, stop adding hydroiodic acid HI;
(2) adopt the mode adding a small amount of ammoniacal liquor, the pH value of this solution is adjusted to 7.5, filter and remove impurity; By the strontium iodide aqueous solution that obtains 100 DEG C ± 2 DEG C stirring heating, when solution is concentrated into initial capacity 2/5, stop heating and glass beaker is put into ice cube immediately, making the temperature of solution in beaker be reduced to 2-3 DEG C fast, in solution, separate out a large amount of plate crystal thing;
(3) crystallisate is separated with mother liquor vacuum filtration, obtains water-containing crystal thing 20.036 grams, these water-containing crystal things are dissolved in 10 grams of water again, obtain the aqueous solution of strontium iodide after purifying;
(4) move in silica glass boat by the above-mentioned aqueous solution, then silica glass boat is placed in tube furnace, tube furnace side connects vacuum pump, and opposite side connects High Purity Nitrogen gas cylinder.First open vacuum pump, valve tube being evacuated to relative pressure is-0.01MPa, and being filled with high-purity argon gas to valve tube boiler tube is pressure-fired, and adopts gasflow clean-up boiler tube 10 times;
(5) close vacuum-pumping valve, close vacuum pump, open boiler tube air discharge cook, adjustment high pure nitrogen flow maintains 2L/min, makes to maintain pressure-fired in valve tube.Tube furnace be warming up to 120 DEG C and keep 3 hours, being then warming up to 200 DEG C, and keeping this temperature 5 hours, the aqueous solution in final silica glass boat is dried to white plates material, closes heating system, makes boiler tube Temperature fall to room temperature;
(6) white plates material is transferred in inert-atmosphere glove box, and wherein by sheet abrasive lapping powdered, then powder is loaded the silica tube of vacuum-pumping, finally silica tube is shifted out glove box; Silica tube is connected with vacuum system, starts to vacuumize, when vacuum tightness is reduced under 0.1Pa, heat to 400 DEG C with the speed of 5 DEG C/min, after this temperature keeps 2h, be reduced to room temperature;
(7) vacuumizing under state, adopting oxyhydrogen flame by silica tube sealing by fusing, namely obtain anhydrous strontium iodide powder.
Embodiment 2
(1) in the glass beaker of 1000ml, 54 grams of deionized waters are added, take purity be 99.99% strontium oxide raw material 51.81 grams be placed in reaction vessel, dropwise add purity higher than 99.9% hydroiodic acid HI carry out neutralization reaction, carry out stirring by magnetic stirring apparatus to make to react completely, stop when being 5.0 to solution ph adding hydroiodic acid HI;
(2) adopt the mode adding a small amount of ammoniacal liquor, the pH value of this solution is adjusted to 7.0, filter and remove impurity; The strontium iodide aqueous solution obtained is loaded in quartz crucible, water ring vacuum pump is adopted to vacuumize 2 hours to quartz crucible, the aqueous solution of strontium iodide is concentrated, the quartz crucible that concentrated solution is housed is put into ice cube immediately, make the temperature of concentrated solution be reduced to 1-2 DEG C fast, in solution, separate out a large amount of plate crystal thing;
(3) plate crystal thing is separated with mother liquor vacuum filtration, obtains water-containing crystal thing about 210 grams, this plate crystal thing is dissolved in 100 grams of water again, obtain the aqueous solution of strontium iodide after purifying;
(4) move in silica glass boat by the above-mentioned aqueous solution, then silica glass boat is placed in tube furnace, tube furnace side connects vacuum pump, and opposite side connects High Purity Nitrogen gas cylinder.First open vacuum pump, valve tube being evacuated to relative pressure is-0.01MPa, and being filled with high-purity argon gas to valve tube boiler tube is pressure-fired, and adopts gasflow clean-up boiler tube 20 times;
(5) close vacuum-pumping valve, close vacuum pump, open boiler tube air discharge cook, adjustment high pure nitrogen flow maintains 5L/min, makes to maintain pressure-fired in valve tube; Tube furnace is warming up to 120 DEG C, and keeps 10 hours, be then warming up to 200 DEG C, and keep this temperature 20 hours, in silica glass boat, the aqueous solution is finally dried to white plates material, closes heating system, makes boiler tube Temperature fall to room temperature;
(6) white plates is transferred in inert atmosphere gloves, and wherein by flap grind into powder, then powder is loaded the silica tube of vacuum-pumping, finally silica tube is shifted out glove box; Silica tube is connected with vacuum system, starts to vacuumize, when vacuum tightness is reduced under 0.1Pa, heat to 450 DEG C with the speed of 2 DEG C/min, keep this temperature to be naturally down to room temperature after 20 hours;
(7) vacuumizing under state, adopting oxyhydrogen flame welding gun by silica tube sealing by fusing, namely obtain anhydrous strontium iodide powder.
Industrial applicability: preparation method's technique of anhydrous strontium iodide of the present invention is simple, easy and simple to handle, equipment requirements is low, oxidisability is low, be easy to mass-producing preparation.Prepared anhydrous strontium iodide directly can be used as the raw material of the pure strontium iodide of growth and doping strontium iodide crystal, and then is applied to the radiation detection such as safety inspection, nuclear weapon inspection field.
Claims (9)
1. a preparation method for high-pure anhydrous strontium iodide, is characterized in that, comprising:
(1) dropwise adding hydroiodic acid HI to pH value of solution under stirring in the reaction vessel filled containing the strontium compound aqueous solution is 5 ~ 6, obtains the aqueous solution of strontium iodide;
(2) pH value of the aqueous solution of the strontium iodide of gained is adjusted to 7 ~ 9, filters, filtrate is concentrated into nearly saturated rear fast cooling to 0 ~ 4 DEG C with crystallization thing, filters to obtain crystallisate and be dissolved in deionized water, obtains the aqueous solution of strontium iodide after purifying;
(3) aqueous solution of strontium iodide after the purifying of gained is transferred in dewatering container, under the inertia protection gas of flowing, is heated to 150 ~ 200 DEG C, and is incubated 1 ~ 30 hour and dewaters, obtain SrI
2xH
2the white puff material of O, x≤1;
(4) the white puff material of gained grind into powder in the inert atmosphere of anhydrous and oxygen-free is also loaded in the Glass Containers that can vacuumize;
(5) heat described Glass Containers to 350 ~ 450 DEG C insulation 1 ~ 20 hour under vacuum, to slough the crystal water in the powder of gained, keeping making described powder Temperature fall to room temperature under the state vacuumized; And
(6) to keep under the state that vacuumizes, by described Glass Containers sealing by fusing, obtaining the high-pure anhydrous strontium iodide be sealed in Glass Containers.
2. preparation method according to claim 1, is characterized in that, in step (1), described is 30% ~ 60% containing the mass percent containing strontium compound in the strontium compound aqueous solution; Described is at least one in Strontium carbonate powder, strontium oxide and strontium hydroxide containing strontium compound.
3. preparation method according to claim 2, is characterized in that, in step (2), filtrate is concentrated into and is closely saturatedly concentrated into 50% ~ 70% of filtrate original volume for filtrate.
4. preparation method according to any one of claim 1 to 3, is characterized in that, in step (2), described concentrated be heated to 100 DEG C ± 2 DEG C in air steam the concentrated or vacuum of water and draw water concentrated.
5. preparation method according to any one of claim 1 to 3, is characterized in that, in step (3), the inertia protection gas of described flowing is high-purity nitrogen, argon gas and/or helium, and flow velocity is 1 ~ 10L/ minute.
6. preparation method according to any one of claim 1 to 3, is characterized in that, in step (3), described heating is speed raised temperature to 150 ~ 200 DEG C with 1 ~ 10 DEG C/min.
7. preparation method according to any one of claim 1 to 3, is characterized in that, in step (4), described anhydrous and oxygen-free is that water and oxygen level be not all higher than 1000ppm.
8. preparation method according to any one of claim 1 to 3, is characterized in that, in step (5), described Glass Containers is in advance through dehydroxylation and rare HF acid clean.
9. preparation method according to any one of claim 1 to 3, is characterized in that, in step (5), described vacuum condition is that vacuum tightness is not higher than 1Pa.
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| CN105778901B (en) * | 2014-12-24 | 2018-11-06 | 有研稀土新材料股份有限公司 | Eu2+Activate high-pure anhydrous halide of alkaline-earth metal and preparation method thereof |
| CN109402724B (en) * | 2017-08-16 | 2020-12-11 | 中国科学院上海硅酸盐研究所 | Non-doped and Eu2+Directional zone-melting growth device and method for doped strontium iodide crystal |
| CN112194204A (en) * | 2020-09-10 | 2021-01-08 | 昆明铂锐金属材料有限公司 | Preparation method of high-purity rhodium triiodide |
| CN114797547B (en) * | 2022-06-07 | 2024-03-12 | 重庆新申新材料股份有限公司 | Liquid feeding device is used in production of high-purity strontium compound, barium compound solution |
| CN116119702A (en) * | 2022-12-27 | 2023-05-16 | 奕瑞新材料科技（太仓）有限公司 | Preparation method of high-purity anhydrous strontium iodide |
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| CN1603235A (en) * | 2004-11-01 | 2005-04-06 | 北京中信国安盟固利新材料技术研究院有限公司 | Method for preparing anhydrous magnesium chloride |
| CN101633514A (en) * | 2008-07-23 | 2010-01-27 | 甘肃稀土新材料股份有限公司 | Preparation method of anhydrous ceric sulfate |
| CN101683994A (en) * | 2008-09-26 | 2010-03-31 | 天津市黎虹化工有限公司 | Production method for preparing white anhydrous magnesium chloride |
| CN103395817A (en) * | 2013-07-31 | 2013-11-20 | 荆门市磊鑫石膏制品有限公司 | Preparation method of high-purity anhydrous calcium sulfate |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1603235A (en) * | 2004-11-01 | 2005-04-06 | 北京中信国安盟固利新材料技术研究院有限公司 | Method for preparing anhydrous magnesium chloride |
| CN101633514A (en) * | 2008-07-23 | 2010-01-27 | 甘肃稀土新材料股份有限公司 | Preparation method of anhydrous ceric sulfate |
| CN101683994A (en) * | 2008-09-26 | 2010-03-31 | 天津市黎虹化工有限公司 | Production method for preparing white anhydrous magnesium chloride |
| CN103395817A (en) * | 2013-07-31 | 2013-11-20 | 荆门市磊鑫石膏制品有限公司 | Preparation method of high-purity anhydrous calcium sulfate |
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