CN103818942A - Method for preparing high-purity anhydrous strontium iodide - Google Patents
Method for preparing high-purity anhydrous strontium iodide Download PDFInfo
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- CN103818942A CN103818942A CN201410029571.8A CN201410029571A CN103818942A CN 103818942 A CN103818942 A CN 103818942A CN 201410029571 A CN201410029571 A CN 201410029571A CN 103818942 A CN103818942 A CN 103818942A
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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 halogenide raw material preparation field for crystal growth.
Background technology
Inorganic scintillator can be used for fast, determines sensitively and accurately the gamma-rays characteristic of highly enriched uranium, weapons-grade plutonium, radioactive source and other special nucleus raw material, has a wide range of applications in radiation detection fields such as Radionuclides identification, safety inspection, environmental monitoring, chemical and biological weapons verification, low energy nuclear test and nuclear non-proliferation verifications.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 high-performance scintillator more.At present, a kind of scintillator being 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
+a large amount of uses of ion, the potential safety hazard that also exists environment to be polluted.The scintillation material LaBr of a new generation
3: Ce crystal has good scintillation properties, but this material exists serious cleavage or stress cracking, melt easily and crucible react, preparation cost is high, also contains simultaneously and can produce radioactive background
138la isotopic composition, its application in radiation detection field has been subject to larger restriction.
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 at that time the second-rate of crystal, performance is than 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 is found, 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%), has good energy linearity in wider energy region.In addition, strontium iodide has lower fusing point, without cleavage, from melting temperature to room temperature range in without phase transformation, very easily adopt 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 selling on the market must first could use through zone-refine; and the larger cognation of batch existence of the crystal mass growing and raw material; even if adopt extremely slow cooling rate; the crystal growing also often can ftracture; this has not only increased the complicacy of equipment and process, has also limited 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, in raw material, often containing water molecules and non-water class oxygenate impurity, 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 most importantly oxide compound or the oxyhalogenide of the oxidized rear formation of principal constituent of oxygenate impurity.Prepare on source at raw material, the generation of avoiding these materials is the fundamental way of obtaining high pure raw material, is also the inevitable choice that improves crystal optics quality and performance.Strontium iodide (SrI
2) be a kind of inorganic salt that formed by strontium and iodine element, belong to ionic compound, very easily deliquescence of anhydrous strontium iodide, and easily separate out elemental iodine and flavescence in seeing light or being exposed to air, and Sr
2+ion is converted to strontium oxide; In aerobic situation, strontium iodide is heated more easily oxidized, and the anhydrous strontium iodide of preparing high-purity, suboxide degree 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 preparation mainly contains following two kinds now:
Method one: the hydroiodic acid HI that is 15%～20% by concentration is dropwise added in Strontium carbonate powder and carries out neutralization reaction, and pH=5.5 ± 0.5 o'clock is terminal, and the iodine that dissociates can remove by filter.In heating concentration process, just in case while having a large amount of free-iodine, can dropwise add H
2the S aqueous solution reduces.Continue suction strainer concentrated, be concentrated in about 100g solution containing strontium iodide 300～320g left and right, place coolingly, can separate out six water strontium iodides.Dry in moisture eliminator after centrifuge dehydration, six water strontium iodides are fully mixed with ammonium iodide, in semi-enclosed Glass tubing, decompression slowly heats up, and melting dehydration, 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 reacted with Strontium carbonate powder, form the aqueous solution of strontium iodide, be 1 o'clock until the pH of solution, solution be heated in air to 140 ℃, keep this temperature for some time, water in solution is evaporated in a large number, evaporation after product is cooled to 5 ℃, and filtration obtains the strontium iodide hydrate that contains six crystal water, and hydrate is separated with solution parent under vacuum; Vacuumize the temperature to 60 ℃ that progressively raises, 90 ℃, 150 ℃ and 300 ℃, all keep for some time at each temperature section.
Wherein, the comparatively complexity of technical process that first method is related, operational condition is wayward, low conversion rate, and use ammonium iodide can produce a large amount of HI gas, and there is the risk of contaminate environment, be 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 ℃ in air, 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 vacuum of this hydrate, owing to containing a large amount of crystal water in this hydrate, in the time of vacuum hydro-extraction, water molecules is difficult to be extracted out in time, and raw material easily hardens into blockly when dehydration, 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; Have again, for avoiding remaining I
2simple substance and HI gas directly enter vacuum apparatus, and vacuum apparatus is produced to corrosion, must in vacuum-lines, set up cold-trap equipment, and this will increase preparation technology's complexity and equipment cost undoubtedly.Therefore, need badly and find a kind of easy handling, the simple preparation method of technique, the anhydrous strontium iodide raw material of, suboxide degree high-purity to obtain, meets pure strontium iodide and the requirements at the higher level of doping strontium iodide crystal growth applications to raw material.
Summary of the invention
The object of the invention is to have problems in order to solve in existing high-purity strontium iodide raw material technology of preparing, as low in productive rate, condition control difficulty, preparation cost is high and easily produce environmental pollution etc., and a kind of preparation method of high-pure anhydrous strontium iodide is provided.
At this, the invention provides a kind of preparation method of high-pure anhydrous strontium iodide, comprising:
(1) be 5～6 to filling containing dropwise adding hydroiodic acid HI to pH value of solution under stirring in the reaction vessel of the strontium compound aqueous solution, obtain the aqueous solution of strontium iodide;
(2) the 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 ℃ 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 mobile inertia protection gas, is heated to 150～200 ℃, and be incubated 1～30 hour and dewater, obtain SrI
2.xH
2the fluffy material of white of O, x≤1;
(4) by fluffy the white of gained material grind into powder packing in the Glass Containers that can vacuumize in the inert atmosphere of anhydrous and oxygen-free;
(5) under vacuum condition, heat described Glass Containers to 350～450 ℃ insulation 1～20 hour, to slough the crystal water in the powder of gained, keeping making described powder naturally cool to room temperature under the state vacuumizing; And
(6) under the state vacuumizing in maintenance, by described Glass Containers sealing by fusing, obtain being sealed in the high-pure anhydrous strontium iodide in Glass Containers.
The present invention is after reaction finishes, first by pH regulator to 7～9 to neutralize excessive hydroiodic acid HI, and the strontium iodide that reaction is obtained carries out carrying out thermal dehydration after purifying again, the hydrogen iodide gas that can effectively avoid excessive hydroiodic acid HI to produce in concentrated and heat-processed enters vacuum apparatus, or enters contaminate environment in atmosphere.And concentration process is to carry out under lesser temps or vacuum, and thermal dehydration process is to carry out under protective atmosphere or vacuum condition, can effectively avoid the oxidation of strontium iodide.In addition, thermal dehydration process comprises: first under mobile inertia protection gas, most of crystal water is sloughed in heating, obtains the only fluffy material of white containing a small amount of crystal water; Carry out again vacuum high-temperature and slough remaining a small amount of crystal water.Like this owing to having removed mass crystallization water before vacuum high-temperature dehydration, and surplus a small amount of crystal water only, therefore water molecules is extracted out relatively easily in time when vacuum hydro-extraction, and powder is not easy caking when dehydration.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 and is not less than 99.9%.
Preferably, in step (1), described reaction vessel is do not react with strontium iodide and HI acid or introduce the container of impurity, comprises glass, metal and earthenware porcelain receptacle.Be preferably purity and be not less than 99.99% quartz crucible.
Preferably, in step (2), filtrate is concentrated into and near is saturatedly concentrated into 50%～70% of filtrate original volume for filtrate.Preferably, in step (2), described concentrated be in air, to be heated to 100 ℃ ± 2 ℃ to steam that water are concentrated or vacuum hydro-extraction is concentrated.
Preferably, in step (3), described dewatering container is in heat-processed, not introduce impurity or and SrI
2the container reacting, comprises glass, metal, graphite and vitreous carbon container.Dewatering container is preferably with inert gas larger contact area.
Preferably, in step (3), described mobile inertia protection gas is high-purity nitrogen, argon gas and/or helium, and flow velocity is 1～10L/ minute.
Preferably, in step (3), described heating is speed rising temperature to 150～200 ℃ with 1～10 ℃/min.
Preferably, in step (4), described anhydrous and oxygen-free is that water and oxygen level be not all higher than 1000ppm.Be preferably water and oxygen level all below 100ppm.
Preferably, in step (5), described Glass Containers passes through dehydroxylation and rare HF acid clean in advance.Described Glass Containers is preferably purity and is not less than 99.99% quartz glass crucibles.
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 to be heated to stage by stage 350～450 ℃ and be incubated 1～20 hour; Or rise to 300～450 ℃ and be incubated 1～20 hour with the temperature rise rate of 1～10 ℃/min.
Accompanying drawing explanation
Fig. 1 is high-pure anhydrous strontium iodide preparation method's process flow sheet.
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 the present invention is described, and unrestricted the present invention.
The invention provides the preparation method of high-purity strontium iodide.This preparation method mainly comprises: react the reactions steps that generates strontium iodide with hydroiodic acid HI containing strontium compound; The strontium iodide of generation is carried out to purifying and obtains the purification step of sheet water-containing crystal thing; Under inert atmosphere, remove the most of crystal water in water-containing crystal thing, obtain containing first of the strontium iodide of a small amount of crystal water step that dewaters; And under vacuum condition, remove remaining a small amount of crystal water and obtain second of the anhydrous strontium iodide step that dewaters.
Fig. 1 illustrates the concrete technology schema of an example of the present invention.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, making containing the mass percent of strontium compound is 30%～60%.The reaction vessel adopting can be do not react with strontium iodide and HI acid or introduce the container of impurity, for example, can be glass, metal and pottery etc., is preferably purity and is not less than 99.99% quartz crucible.What adopt can be any of Strontium carbonate powder, strontium oxide and strontium hydroxide containing strontium compound, can be also two or three arbitrary proportion mixture of these materials.These purity containing strontium compound are generally not less than 99.9%.Dropwise (for example adopt reaction titration apparatus) and add hydroiodic acid HI at this container, constantly stir (for example adopting magnetic stirring apparatus), make, containing strontium compound and hydroiodic acid HI generation complete reaction, to stop adding hydroiodic acid HI until pH value of solution to 5～6 o'clock, obtain the aqueous solution of strontium iodide.
(2) regulating step (1) obtains pH to 7～9 of the aqueous solution, can adopt the alkali such as ammoniacal liquor to regulate.Elimination insolubles wherein, adopts in air under heating or vacuum dewatering type that the filtrate obtaining is concentrated into closely saturated, when the mass percent containing strontium compound is 30%～60% in the strontium compound aqueous solution, is concentrated into 50%～70% of filtrate original volume when used.Wherein in air, heating can be to be for example heated to 100 ℃ ± 2 ℃; Under vacuum, dehydration for example can adopt water ring vacuum pump.The reaction vessel that fills near saturated solution is for example positioned over, in low temperature environment (ice cube), make filtrate fast cooling to 0～4 ℃, make to produce in solution plate crystal thing, vacuum filtration makes crystallisate separate with mother liquor, crystallisate is dissolved in to deionized water again, be preferably completely water-solublely to clear state, obtain the aqueous solution of strontium iodide after purifying.
(3) aqueous solution of purifying strontium iodide step (2) being obtained is transferred in dewatering container, under mobile inertia protection gas, heats this aqueous solution, sloughs the main moisture in the aqueous solution, obtains the only fluffy material of white containing a small amount of crystal water.Wherein, the dewatering container adopting can be and in heat-processed, not introduce impurity or and SrI
2the container reacting, including but not limited to the container of the materials such as glass, metal, graphite or vitreous carbon.In addition, dewatering container is preferably with inert gas larger contact area.Mobile inertia protection gas can be high pure nitrogen, high-purity argon gas or high-purity helium, is preferably high-purity argon gas and high-purity helium, and gas flow rate can be 1～10L/ minute.Described heating for example can adopt the speed of 1～10 ℃/min to heat up, rising temperature to 150～200 ℃, and be incubated 1～30 hour.Can be to be directly warming up to 150～200 ℃; Also can be progressively to heat, first be warming up to a certain medium temperature, for example 120 ℃, and be incubated 2 hours, then be warming up to 150～200 ℃.
(4) white puffy material step (3) being obtained shifts and enters in glove box, pulverizes therein in the last Glass Containers that packs vacuum-pumping into.The glove box adopting can be inert-atmosphere glove box, and in this glove box, the content of water and oxygen all should be higher than 1000ppm, is preferably the content of water and oxygen all below 100ppm.The Glass Containers adopting can be that being preferably purity is more than 99.9% quartz glass crucibles through the glass pot of dehydroxylation and rare HF acid clean.
(5) under vacuum condition, the powder that heating steps (4) is described, 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 state to the raw material vacuumizing naturally to cool to room temperature, obtain anhydrous strontium iodide powder high-purity, suboxide degree.Described heating can be to be warming up to stage by stage 350～450 ℃, and keeps 1～20 hour, for example, be progressively warming up to 200 ℃, 300 ℃, 450 ℃, keeps respectively 1～5 hour at each temperature section; Also can be to be directly warming up to 350～450 ℃ with the speed of 1～10 ℃/min, and keep high temperature 1～20 hour.Described vacuum condition can be vacuum tightness not higher than 1Pa, preferably vacuum tightness is 10
-3below Pa.
(6) by the Glass Containers sealing by fusing constantly vacuumizing, for example adopt flame welding gun to carry out sealing by fusing, can obtain the high-pure anhydrous strontium iodide being sealed in Glass Containers.Can preserve for a long time like this this high-pure anhydrous strontium iodide and not perishable.
The preparation method of anhydrous strontium iodide of the present invention has advantages of that technique is simple, easy and simple to handle, equipment requirements is low, oxidisability is low and be easy to mass-producing and prepares, and can be directly used in the pure strontium iodide of growth and doping strontium iodide crystal.
Further exemplify embodiment below 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 that following example is concrete etc. is only also an example in OK range, and those skilled in the art can be done in suitable scope and be selected by explanation herein, and do not really want to be defined in the below concrete numerical value of example.
Embodiment 1
(1) in the glass beaker of 250ml, add 5.4 grams of deionized waters, take purity and be 99.99% Strontium carbonate powder (SrCO
3) 7.38 grams of raw materials are placed in reaction vessel, dropwise add purity to be not less than 99.9% hydroiodic acid HI, stir by magnetic stirring apparatus, make Strontium carbonate powder and hydroiodic acid HI complete reaction, to solution clarification and pH value be 5.5 o'clock, stop adding hydroiodic acid HI;
(2) adopt the mode that adds 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 obtaining 100 ℃ ± 2 ℃ stirring heating, in the time that solution is concentrated into initial capacity 2/5, stop heating and glass beaker is put into ice cube immediately, making the temperature fast reducing of solution in beaker to 2-3 ℃, in solution, separating out a large amount of plate crystal things;
(3) crystallisate is separated with mother liquor vacuum filtration, obtain 20.036 grams of water-containing crystal things, these water-containing crystal things are dissolved in 10 grams of water again, obtain the aqueous solution of strontium iodide after purifying;
(4) the above-mentioned aqueous solution is moved in silica glass boat, then silica glass boat is placed in to tube furnace, tube furnace one side connects vacuum pump, and opposite side connects High Purity Nitrogen gas cylinder.First open vacuum pump, it is-0.01MPa that being filled with high-purity argon gas to valve tube boiler tube is pressure-fired, and adopts gasflow clean-up boiler tube 10 times that valve tube is evacuated to relative pressure;
(5) close vacuum-pumping valve, close vacuum pump, open boiler tube air discharge cook, adjust high pure nitrogen flow and maintain 2L/min, make to maintain in valve tube pressure-fired.Tube furnace is warming up to 120 ℃ and keep 3 hours, is then warming up to 200 ℃, and keeps this temperature 5 hours, the aqueous solution in final silica glass boat is dried to white plates material, closes heating system, makes boiler tube naturally be cooled to room temperature;
(6) white plates material is transferred in inert-atmosphere glove box, and therein by sheet abrasive lapping powdered, then powder is packed into the silica tube of vacuum-pumping, finally silica tube is shifted out to glove box; Silica tube is connected with vacuum system, starts to vacuumize, be reduced to lower time of 0.1Pa until vacuum tightness, heat to 400 ℃ with the speed of 5 ℃/min, keep being reduced to room temperature after 2h in this temperature;
(7) vacuumizing under state, adopting oxyhydrogen flame by silica tube sealing by fusing, obtaining anhydrous strontium iodide powder.
Embodiment 2
(1) in the glass beaker of 1000ml, add 54 grams of deionized waters, take purity and be 51.81 grams of 99.99% strontium oxide raw materials and be placed in reaction vessel, dropwise add purity to carry out neutralization reaction higher than 99.9% hydroiodic acid HI, being stirred and made to react completely by magnetic stirring apparatus, is to stop adding hydroiodic acid HI at 5.0 o'clock to pH;
(2) adopt the mode that adds 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 obtaining is packed in quartz crucible, adopt water ring vacuum pump to vacuumize 2 hours to quartz crucible, make the aqueous solution of strontium iodide concentrated, the quartz crucible that concentrated solution is housed is put into ice cube immediately, make the temperature fast reducing of concentrated solution to 1-2 ℃, in solution, separate out a large amount of plate crystal things;
(3) plate crystal thing is separated with mother liquor vacuum filtration, obtain approximately 210 grams of water-containing crystal things, this plate crystal thing is dissolved in 100 grams of water again, obtain the aqueous solution of strontium iodide after purifying;
(4) the above-mentioned aqueous solution is moved in silica glass boat, then silica glass boat is placed in to tube furnace, tube furnace one side connects vacuum pump, and opposite side connects High Purity Nitrogen gas cylinder.First open vacuum pump, it is-0.01MPa that being filled with high-purity argon gas to valve tube boiler tube is pressure-fired, and adopts gasflow clean-up boiler tube 20 times that valve tube is evacuated to relative pressure;
(5) close vacuum-pumping valve, close vacuum pump, open boiler tube air discharge cook, adjust high pure nitrogen flow and maintain 5L/min, make to maintain in valve tube pressure-fired; Tube furnace is warming up to 120 ℃, and keeps 10 hours, be then warming up to 200 ℃, 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 naturally be cooled to room temperature;
(6) white plates is transferred in inert atmosphere gloves, and therein by flap grind into powder, then powder is packed into the silica tube of vacuum-pumping, finally silica tube is shifted out to glove box; Silica tube is connected with vacuum system, starts to vacuumize, be reduced to lower time of 0.1Pa until vacuum tightness, heat to 450 ℃ with the speed of 2 ℃/min, keep this temperature after 20 hours, to be naturally down to room temperature;
(7) vacuumizing under state, adopting oxyhydrogen flame welding gun by silica tube sealing by fusing, obtaining 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.The directly raw material with doping strontium iodide crystal as the pure strontium iodide of growth of prepared anhydrous strontium iodide, and then be 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) be 5～6 to filling containing dropwise adding hydroiodic acid HI to pH value of solution under stirring in the reaction vessel of the strontium compound aqueous solution, obtain the aqueous solution of strontium iodide;
(2) the 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 ℃ 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 mobile inertia protection gas, is heated to 150～200 ℃, and be incubated 1～30 hour and dewater, obtain SrI
2xH
2the fluffy material of white of O, x≤1;
(4) by fluffy the white of gained material grind into powder packing in the Glass Containers that can vacuumize in the inert atmosphere of anhydrous and oxygen-free;
(5) under vacuum condition, heat described Glass Containers to 350～450 ℃ insulation 1～20 hour, to slough the crystal water in the powder of gained, keeping making described powder naturally cool to room temperature under the state vacuumizing; And
(6) under the state vacuumizing in maintenance, by described Glass Containers sealing by fusing, obtain being sealed in the high-pure anhydrous strontium iodide 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 near is saturatedly concentrated into 50%～70% of filtrate original volume for filtrate.
4. according to the preparation method described in any one in claims 1 to 3, it is characterized in that, in step (2), described concentrated be in air, to be heated to 100 ℃ ± 2 ℃ steam the concentrated or vacuum of water and draw water concentrated.
5. according to the preparation method described in any one in claim 1 to 4, it is characterized in that, in step (3), described mobile inertia protection gas is high-purity nitrogen, argon gas and/or helium, and flow velocity is 1～10L/ minute.
6. according to the preparation method described in any one in claim 1 to 5, it is characterized in that, in step (3), described heating is speed rising temperature to 150～200 ℃ with 1～10 ℃/min.
7. according to the preparation method described in any one in claim 1 to 6, it 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. according to the preparation method described in any one in claim 1 to 7, it is characterized in that, in step (5), described Glass Containers passes through dehydroxylation and rare HF acid clean in advance.
9. according to the preparation method described in any one in claim 1 to 8, it is characterized in that, in step (5), described vacuum condition is that vacuum tightness is not higher than 1Pa.
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| CN109402724A (en) * | 2017-08-16 | 2019-03-01 | 中国科学院上海硅酸盐研究所 | The undoped and Eu of one kind2+Adulterate the orientation growing by zone melting device and method of iodate strontium 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 |
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| CN114797547A (en) * | 2022-06-07 | 2022-07-29 | 重庆新申新材料股份有限公司 | Liquid adding device for producing high-purity strontium compound and barium compound solution |
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