CN105460965A - Method for preparing anti-caking high-purity electronic-grade strontium nitrate - Google Patents
Method for preparing anti-caking high-purity electronic-grade strontium nitrate Download PDFInfo
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- CN105460965A CN105460965A CN201610063173.7A CN201610063173A CN105460965A CN 105460965 A CN105460965 A CN 105460965A CN 201610063173 A CN201610063173 A CN 201610063173A CN 105460965 A CN105460965 A CN 105460965A
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- DHEQXMRUPNDRPG-UHFFFAOYSA-N strontium nitrate Chemical compound [Sr+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O DHEQXMRUPNDRPG-UHFFFAOYSA-N 0.000 title claims abstract description 78
- 238000000034 method Methods 0.000 title claims abstract description 29
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 claims abstract description 28
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 27
- 238000002425 crystallisation Methods 0.000 claims abstract description 15
- 238000001704 evaporation Methods 0.000 claims abstract description 15
- 230000008020 evaporation Effects 0.000 claims abstract description 15
- 238000000926 separation method Methods 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- 238000002360 preparation method Methods 0.000 claims abstract description 11
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims description 43
- 239000013078 crystal Substances 0.000 claims description 34
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- 239000012043 crude product Substances 0.000 claims description 18
- 210000002966 serum Anatomy 0.000 claims description 18
- 238000003756 stirring Methods 0.000 claims description 18
- JJJBUGDRBSGCTD-UHFFFAOYSA-N [Sr].[N+](=O)(O)[O-] Chemical compound [Sr].[N+](=O)(O)[O-] JJJBUGDRBSGCTD-UHFFFAOYSA-N 0.000 claims description 15
- 238000005054 agglomeration Methods 0.000 claims description 15
- 230000002776 aggregation Effects 0.000 claims description 15
- 239000000706 filtrate Substances 0.000 claims description 14
- 238000001556 precipitation Methods 0.000 claims description 13
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 12
- 230000032683 aging Effects 0.000 claims description 12
- 238000013019 agitation Methods 0.000 claims description 12
- 239000011812 mixed powder Substances 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 12
- 239000002893 slag Substances 0.000 claims description 12
- 238000001291 vacuum drying Methods 0.000 claims description 12
- 239000011521 glass Substances 0.000 claims description 9
- 238000005119 centrifugation Methods 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 7
- 239000006228 supernatant Substances 0.000 claims description 7
- 238000000498 ball milling Methods 0.000 claims description 6
- 239000002131 composite material Substances 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 6
- 239000000376 reactant Substances 0.000 claims description 6
- 238000007873 sieving Methods 0.000 claims description 6
- 229910001220 stainless steel Inorganic materials 0.000 claims description 6
- 239000010935 stainless steel Substances 0.000 claims description 6
- 238000009423 ventilation Methods 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 abstract description 10
- 229910017604 nitric acid Inorganic materials 0.000 abstract description 10
- 229910000018 strontium carbonate Inorganic materials 0.000 abstract description 9
- LEDMRZGFZIAGGB-UHFFFAOYSA-L strontium carbonate Chemical compound [Sr+2].[O-]C([O-])=O LEDMRZGFZIAGGB-UHFFFAOYSA-L 0.000 abstract description 9
- 230000008025 crystallization Effects 0.000 abstract description 8
- 239000012535 impurity Substances 0.000 abstract description 7
- 238000006467 substitution reaction Methods 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 238000001914 filtration Methods 0.000 abstract description 4
- 238000001035 drying Methods 0.000 abstract description 3
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 3
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 abstract description 2
- 239000000920 calcium hydroxide Substances 0.000 abstract description 2
- 229910001861 calcium hydroxide Inorganic materials 0.000 abstract description 2
- 238000001723 curing Methods 0.000 abstract 1
- 239000002244 precipitate Substances 0.000 abstract 1
- 239000000047 product Substances 0.000 description 6
- 206010053567 Coagulopathies Diseases 0.000 description 4
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 4
- 230000035602 clotting Effects 0.000 description 4
- 229910002651 NO3 Inorganic materials 0.000 description 3
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 3
- 239000004973 liquid crystal related substance Substances 0.000 description 3
- 239000002585 base Substances 0.000 description 2
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical compound [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229910052712 strontium Inorganic materials 0.000 description 2
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 2
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- FTNOFNIESZSONM-UHFFFAOYSA-J calcium strontium carbonate sulfate Chemical class S(=O)(=O)([O-])[O-].[Sr+2].C([O-])([O-])=O.[Ca+2] FTNOFNIESZSONM-UHFFFAOYSA-J 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000031068 symbiosis, encompassing mutualism through parasitism Effects 0.000 description 1
Classifications
-
- 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
- C01F11/38—Preparation with nitric acid or nitrogen oxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/10—Solid density
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
- C01P2006/82—Compositional purity water content
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Medicinal Preparation (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method for preparing anti-caking high-purity electronic-grade strontium nitrate and belongs to the technical field of strontium nitrate preparation. Strontianite and witherite are crushed and pulped and then nitric acid is added for reaction, and a nitric acid solution is generated; then, a sodium hydroxide solution is added into the nitric acid solution, and calcium hydroxide precipitate is generated through reaction; then, supernate is collected through centrifugal separation, nitric acid is added, and a filtered solution is obtained through reaction, curing and filtering; finally, the obtained filtered solution is subjected to cooling crystallization, impurity removal, filtering, evaporation crystallization and drying, and the anti-caking high-purity electronic-grade strontium nitrate is obtained. Examples show that operation is easy and convenient, and the isomorphous substitution phenomenon can not occur in the preparation process. Besides, the prepared strontium nitrate is high in purity, low in impurity content, not prone to caking, capable of reducing production and use cost of clients and worthy of large-scale production and application.
Description
Technical field
The invention discloses a kind of preparation method of agglomeration resistance high purity electronic grade nitric acid strontium, belong to strontium nitrate preparing technical field.
Background technology
Strontium nitrate is a kind of white or faint yellow cubic system; Soluble in water, be insoluble to nitric acid and Diluted Alcohol; Being mainly used in liquid crystal glass base, opticglass and fluor industry, is the important additives of liquid crystal substrate glass, plays the effect improving specific refractory power and improve multiple physicochemical property, is one of most important raw material during liquid crystal glass base is produced.
At present, the preparation method of strontium nitrate has carbonation and strontianite, witherite method.
Wherein, (1) carbonation adds concentrated nitric acid and carries out being obtained by reacting corresponding nitrate raw material liquid after referring to and being sized mixing by industrial nitric acid strontium, strontium nitrate product is obtained after removal of impurities, filtration, evaporative crystallization, drying, the product caking phenomenon that existing preparation method obtains is serious, just can use after needing artificial pulverizing, increase production cost;
(2) strontianite, witherite method are reacted after strontianite and witherite respectively broken slurrying with nitric acid, and reaction product obtains product after subsequent filter, removal of impurities, filtration, evaporative crystallization, drying.The method is using strontianite or witherite as starting material, production cost reduces relatively, but due to the reduction of strontianite grade, existence containing impurity such as more symbiosis calcium carbonate Strontium Sulphates in strontianite, containing a large amount of nitrocalcite in solution after nitric acid solution, owing to not taking circulation method, then concentrated degree is higher, to improve the yield of strontium as far as possible, but due to strontium nitrate crystallization in the ca nitrate soln of higher concentration, the phenomenons such as isomorphous substitution can be there is, not only affect the purity of the finished product, and affect the evaporation and crystal process of strontium nitrate, the strontium nitrate crystal grain finally obtained is tiny, dry difficulty and easily luming.
Summary of the invention
The technical problem that the present invention mainly solves: for strontianite conventional at present, witherite method is in the process preparing strontium nitrate, though the yield of strontium nitrate can be improved, but in preparation process, due to strontium nitrate crystallization in the ca nitrate soln of higher concentration, isomorphous substitution phenomenon can be there is, have impact on evaporation and crystal process, cause product purity low, obtained strontium nitrate crystal grain is tiny, and the present situation of easily luming, provide a kind of by strontianite, witherite adds nitric acid reaction after pulverizing slurrying, generate salpeter solution, sodium hydroxide solution is added again subsequently in salpeter solution, reaction generates calcium hydroxide precipitation, pass through centrifugation afterwards, collect supernatant liquor and add nitric acid, through reaction, slaking, filter to get filtrate, the filtrate crystallisation by cooling finally will obtained, removal of impurities filter after evaporative crystallization again, dry, thus obtain the preparation method of agglomeration resistance high purity electronic grade nitric acid strontium.The method is easy and simple to handle, not only can not produce isomorphous substitution phenomenon in preparation process, and obtained strontium nitrate purity is high, foreign matter content is low, prevented from caking, decreases the production and application cost of client, is worth large-scale production and application.
In order to solve the problems of the technologies described above, the technical solution adopted in the present invention is:
(1) 500 ~ 600g height calciostrontianite and 700 ~ 800g witherite is got, pour in crusher and carry out coarse breaking process, process 2 ~ 3min, cross 50 ~ 60 mesh sieves, subsequently the composite grain after sieving is put into high speed ball mill, add the stainless steel abrading-ball pearl that particle diameter is 4 ~ 5mm, ball milling 10 ~ 12min under rotational speed of ball-mill is 500 ~ 600r/min, be milled to granularity <0.08mm, obtain mixed powder, the mixed powder obtained afterwards is poured in container, and adds powder quality 70 ~ 80% clear water wherein, mix, obtain mixed serum;
(2) in mixed serum obtained above, slowly adding mixed serum quality 35 ~ 40% mass concentration is the salpeter solution of 98%, stir with glass stick, standing and reacting at 30 ~ 32 DEG C, be till 2.5 ~ 3.2 until reacting solution pH value, question response terminates, and is 2: 1 ~ 3: 1, adds 0.5M sodium hydroxide solution in reactant by solid-to-liquid ratio, promote temperature to 32 ~ 35 DEG C, Keep agitation is until generate without precipitation;
(3) said mixture is put into whizzer, under the rotating speed of 1100 ~ 1200r/min, centrifugation 10 ~ 20min, removes slag, and gets supernatant liquor, pour in container, at normal temperatures, in container, dripping mass concentration with the speed of 8 ~ 10mL/min is while stirring the salpeter solution of 37%, controls to be added dropwise to complete in 25 ~ 35min, temperature to 100 ~ 105 DEG C are promoted again subsequently with the speed of 5 ~ 10 DEG C/min, Keep agitation reaction 2 ~ 2.5h, question response terminates, slaking 2 ~ 4h;
(4) treat that above-mentioned slaking terminates, material after slaking is carried out solid-liquid separation while hot, remove slag, stay liquid, the filtrate obtained is put into concentration tank, reducing tank internal pressure is 1000 ~ 1100Pa, when being evaporated to that in tank, filtrate volume is 1/3 ~ 1/2 of original volume, stop concentrated, relative density controls at 15 ~ 18Be, dry after crystallisation by cooling, obtain strontium nitrate crude product;
(5) strontium nitrate crude product obtained above is put into distilled water, heating for dissolving at 50 ~ 60 DEG C, after to be dissolved, adding strontium nitrate crude product quality 20 ~ 30% mass concentration is wherein the hydrogen peroxide of 25%, is uniformly mixed, and precipitation 1 ~ 2h, filters, obtain filtered liquid;
(6) filtered liquid obtained above is put into container for evaporation, heated and stirred at 80 ~ 90 DEG C, when to be evaporated to filtered liquid volume be original volume 1/2, stop evaporation, promote temperature to 92 ~ 95 DEG C, stir ageing 1 ~ 2h, preferred 1.5h, treat that ageing terminates, solid-liquid separation, obtain crystal;
(7) crystal obtained above is put into vacuum drying oven, wherein vacuum drying oven vacuum tightness is-0.03 ~ 0.05Mpa, temperature is 110 ~ 130 DEG C, dry until crystal water content be till 0.2 ~ 0.3%, subsequently dried crystal is positioned over ventilation, naturally cool to room temperature, a kind of agglomeration resistance high purity electronic grade nitric acid strontium can be obtained.
The agglomeration resistance high purity electronic grade nitric acid strontium that the present invention obtains is white crystals, and relative density is 2.9, and fusing point is 580 DEG C, and purity is more than 99.85%, and grain diameter is 650 ~ 710 μm, and clotting time reaches more than 200 days.
Principle of the present invention: the present invention first utilizes salpeter solution to extract strontium in high calciostrontianite and witherite, again by adding the calcium impurities in sodium hydroxide removal solution, add salpeter solution subsequently, form polymerize aluminum chloride with aluminum nitrate, finally utilize polymerize aluminum chloride different with strontium nitrate ctystallizing point, pass through evaporative crystallization, dry formation strontium nitrate, operation like this, reduces the possibility of recombine between crystal in operating process, more can not produce isomorphous substitution phenomenon.
The invention has the beneficial effects as follows:
(1) the present invention is easy and simple to handle, and method is unique, reduces the possibility of recombine between crystal, can not produce isomorphous substitution phenomenon, obtained strontium nitrate uniform particle sizes, stable performance in the process of preparation;
(2) the strontium nitrate purity that obtains of the present invention is high, foreign matter content is low, decrease the production and application cost of client, and agglomeration preventing performance improves greatly, and product is stacked and also do not had caking phenomenon in more than 200 days, is worth large-scale production and application.
Embodiment
First 500 ~ 600g height calciostrontianite and 700 ~ 800g witherite is got, pour in crusher and carry out coarse breaking process, process 2 ~ 3min, cross 50 ~ 60 mesh sieves, subsequently the composite grain after sieving is put into high speed ball mill, add the stainless steel abrading-ball pearl that particle diameter is 4 ~ 5mm, ball milling 10 ~ 12min under rotational speed of ball-mill is 500 ~ 600r/min, be milled to granularity <0.08mm, obtain mixed powder, the mixed powder obtained afterwards is poured in container, and adds powder quality 70 ~ 80% clear water wherein, mix, obtain mixed serum; Then in mixed serum obtained above, slowly add mixed serum quality 35 ~ 40% mass concentration is the salpeter solution of 98%, stir with glass stick, standing and reacting at 30 ~ 32 DEG C, be till 2.5 ~ 3.2 until reacting solution pH value, question response terminates, and is 2: 1 ~ 3: 1, adds 0.5M sodium hydroxide solution in reactant by solid-to-liquid ratio, promote temperature to 32 ~ 35 DEG C, Keep agitation is until generate without precipitation; Subsequently said mixture is put into whizzer, under the rotating speed of 1100 ~ 1200r/min, centrifugation 10 ~ 20min, removes slag, and gets supernatant liquor, pour in container, at normal temperatures, in container, dripping mass concentration with the speed of 8 ~ 10mL/min is while stirring the salpeter solution of 37%, controls to be added dropwise to complete in 25 ~ 35min, temperature to 100 ~ 105 DEG C are promoted again subsequently with the speed of 5 ~ 10 DEG C/min, Keep agitation reaction 2 ~ 2.5h, question response terminates, slaking 2 ~ 4h; Treat that above-mentioned slaking terminates, material after slaking is carried out solid-liquid separation while hot, remove slag, stay liquid, the filtrate obtained is put into concentration tank, reducing tank internal pressure is 1000 ~ 1100Pa, when being evaporated to that in tank, filtrate volume is 1/3 ~ 1/2 of original volume, stop concentrated, relative density controls at 15 ~ 18Be, dry after crystallisation by cooling, obtain strontium nitrate crude product; Next strontium nitrate crude product obtained above is put into distilled water, heating for dissolving at 50 ~ 60 DEG C, after to be dissolved, adding strontium nitrate crude product quality 20 ~ 30% mass concentration is wherein the hydrogen peroxide of 25%, is uniformly mixed, precipitation 1 ~ 2h, filter, obtain filtered liquid; Filtered liquid obtained above is put into container for evaporation, heated and stirred at 80 ~ 90 DEG C, when to be evaporated to filtered liquid volume be original volume 1/2, stop evaporation, promote temperature to 92 ~ 95 DEG C, stir ageing 1 ~ 2h, preferred 1.5h, treat that ageing terminates, solid-liquid separation, obtain crystal; Finally crystal obtained above is put into vacuum drying oven, wherein vacuum drying oven vacuum tightness is-0.03 ~ 0.05Mpa, temperature is 110 ~ 130 DEG C, dry until crystal water content be till 0.2 ~ 0.3%, subsequently dried crystal is positioned over ventilation, naturally cool to room temperature, a kind of agglomeration resistance high purity electronic grade nitric acid strontium can be obtained.
Example 1
First 500g height calciostrontianite and 700g witherite is got, pour in crusher and carry out coarse breaking process, process 2min, cross 50 mesh sieves, subsequently the composite grain after sieving is put into high speed ball mill, add the stainless steel abrading-ball pearl that particle diameter is 4mm, ball milling 10min under rotational speed of ball-mill is 500r/min, be milled to granularity <0.08mm, obtain mixed powder, the mixed powder obtained afterwards is poured in container, and adds powder quality 70% clear water wherein, mix, obtain mixed serum; Then in mixed serum obtained above, slowly add mixed serum quality 35% mass concentration is the salpeter solution of 98%, stir with glass stick, standing and reacting at 30 DEG C, be till 2.5 until reacting solution pH value, question response terminates, and is 2: 1, adds 0.5M sodium hydroxide solution in reactant by solid-to-liquid ratio, promote temperature to 32 DEG C, Keep agitation is until generate without precipitation; Subsequently said mixture is put into whizzer, under the rotating speed of 1100r/min, centrifugation 10min, removes slag, and gets supernatant liquor, pour in container, at normal temperatures, in container, dripping mass concentration with the speed of 8mL/min is while stirring the salpeter solution of 37%, is added dropwise to complete in control 25min, temperature to 100 DEG C is promoted again subsequently with the speed of 5 DEG C/min, Keep agitation reaction 2h, question response terminates, slaking 2h; Treat that above-mentioned slaking terminates, material after slaking is carried out solid-liquid separation while hot, remove slag, stay liquid, the filtrate obtained is put into concentration tank, reducing tank internal pressure is 1000Pa, when being evaporated to that in tank, filtrate volume is 1/3 of original volume, stop concentrated, relative density controls at 15Be, dry after crystallisation by cooling, obtain strontium nitrate crude product; Next strontium nitrate crude product obtained above is put into distilled water, heating for dissolving at 50 DEG C, after to be dissolved, adding strontium nitrate crude product quality 20 ~ 30% mass concentration is wherein the hydrogen peroxide of 25%, is uniformly mixed, and precipitation 1h, filters, obtain filtered liquid; Filtered liquid obtained above is put into container for evaporation, heated and stirred at 80 DEG C, when to be evaporated to filtered liquid volume be original volume 1/2, stop evaporation, promote temperature to 92 DEG C, stir ageing 1h, preferred 1.5h, treats that ageing terminates, solid-liquid separation, obtains crystal; Finally crystal obtained above is put into vacuum drying oven, wherein vacuum drying oven vacuum tightness is-0.03Mpa, temperature is 110 DEG C, dry until crystal water content be till 0.2%, subsequently dried crystal is positioned over ventilation, naturally cool to room temperature, a kind of agglomeration resistance high purity electronic grade nitric acid strontium can be obtained.
This case method is unique novel, and final obtained agglomeration resistance high purity electronic grade nitric acid strontium is white crystals, and relative density is 2.9, and fusing point is 580 DEG C, and purity is 99.85%, and grain diameter is 650 μm, and clotting time reaches 200 days.
Example 2
First 55g height calciostrontianite and 750g witherite is got, pour in crusher and carry out coarse breaking process, process 2.5min, cross 55 mesh sieves, subsequently the composite grain after sieving is put into high speed ball mill, add the stainless steel abrading-ball pearl that particle diameter is 4.5mm, ball milling 11min under rotational speed of ball-mill is 550r/min, be milled to granularity <0.08mm, obtain mixed powder, the mixed powder obtained afterwards is poured in container, and adds powder quality 75% clear water wherein, mix, obtain mixed serum; Then in mixed serum obtained above, slowly add mixed serum quality 38% mass concentration is the salpeter solution of 98%, stir with glass stick, standing and reacting at 31 DEG C, be till 2.8 until reacting solution pH value, question response terminates, and is 2.5: 1, adds 0.5M sodium hydroxide solution in reactant by solid-to-liquid ratio, promote temperature to 34 DEG C, Keep agitation is until generate without precipitation; Subsequently said mixture is put into whizzer, under the rotating speed of 1150r/min, centrifugation 15min, removes slag, and gets supernatant liquor, pour in container, at normal temperatures, in container, dripping mass concentration with the speed of 9mL/min is while stirring the salpeter solution of 37%, is added dropwise to complete in control 30min, temperature to 103 DEG C is promoted again subsequently with the speed of 8 DEG C/min, Keep agitation reaction 2.3h, question response terminates, slaking 3h; Treat that above-mentioned slaking terminates, material after slaking is carried out solid-liquid separation while hot, remove slag, stay liquid, the filtrate obtained is put into concentration tank, reducing tank internal pressure is 1050Pa, when being evaporated to that in tank, filtrate volume is 5/12 of original volume, stop concentrated, relative density controls at 17Be, dry after crystallisation by cooling, obtain strontium nitrate crude product; Next strontium nitrate crude product obtained above is put into distilled water, heating for dissolving at 55 DEG C, after to be dissolved, adding strontium nitrate crude product quality 25% mass concentration is wherein the hydrogen peroxide of 25%, is uniformly mixed, and precipitation 1.5h, filters, obtain filtered liquid; Filtered liquid obtained above is put into container for evaporation, heated and stirred at 85 DEG C, when to be evaporated to filtered liquid volume be original volume 1/2, stop evaporation, promote temperature to 94 DEG C, stir ageing 1.5h, preferred 1.5h, treats that ageing terminates, solid-liquid separation, obtains crystal; Finally crystal obtained above is put into vacuum drying oven, wherein vacuum drying oven vacuum tightness is 0.02Mpa, temperature is 120 DEG C, dry until crystal water content be till 0.25%, subsequently dried crystal is positioned over ventilation, naturally cool to room temperature, a kind of agglomeration resistance high purity electronic grade nitric acid strontium can be obtained.
This case method is unique novel, and final obtained agglomeration resistance high purity electronic grade nitric acid strontium is white crystals, and relative density is 2.9, and fusing point is 580 DEG C, and purity is 99.87%, and grain diameter is 680 μm, and clotting time reaches 210 days.
Example 3
First 600g height calciostrontianite and 800g witherite is got, pour in crusher and carry out coarse breaking process, process 3min, cross 60 mesh sieves, subsequently the composite grain after sieving is put into high speed ball mill, add the stainless steel abrading-ball pearl that particle diameter is 5mm, ball milling 12min under rotational speed of ball-mill is 600r/min, be milled to granularity <0.08mm, obtain mixed powder, the mixed powder obtained afterwards is poured in container, and adds powder quality 80% clear water wherein, mix, obtain mixed serum; Then in mixed serum obtained above, slowly add mixed serum quality 40% mass concentration is the salpeter solution of 98%, stir with glass stick, standing and reacting at 32 DEG C, be till 3.2 until reacting solution pH value, question response terminates, and is 3: 1, adds 0.5M sodium hydroxide solution in reactant by solid-to-liquid ratio, promote temperature to 35 DEG C, Keep agitation is until generate without precipitation; Subsequently said mixture is put into whizzer, under the rotating speed of 1200r/min, centrifugation 20min, removes slag, and gets supernatant liquor, pour in container, at normal temperatures, in container, dripping mass concentration with the speed of 10mL/min is while stirring the salpeter solution of 37%, is added dropwise to complete in control 35min, temperature to 105 DEG C is promoted again subsequently with the speed of 10 DEG C/min, Keep agitation reaction 2.5h, question response terminates, slaking 4h; Treat that above-mentioned slaking terminates, material after slaking is carried out solid-liquid separation while hot, remove slag, stay liquid, the filtrate obtained is put into concentration tank, reducing tank internal pressure is 1100Pa, when being evaporated to that in tank, filtrate volume is 1/2 of original volume, stop concentrated, relative density controls at 18Be, dry after crystallisation by cooling, obtain strontium nitrate crude product; Next strontium nitrate crude product obtained above is put into distilled water, heating for dissolving at 60 DEG C, after to be dissolved, adding strontium nitrate crude product quality 30% mass concentration is wherein the hydrogen peroxide of 25%, is uniformly mixed, and precipitation 2h, filters, obtain filtered liquid; Filtered liquid obtained above is put into container for evaporation, heated and stirred at 90 DEG C, when to be evaporated to filtered liquid volume be original volume 1/2, stop evaporation, promote temperature to 95 DEG C, stir ageing 2h, preferred 1.5h, treats that ageing terminates, solid-liquid separation, obtains crystal; Finally crystal obtained above is put into vacuum drying oven, wherein vacuum drying oven vacuum tightness is 0.05Mpa, temperature is 130 DEG C, dry until crystal water content be till 0.3%, subsequently dried crystal is positioned over ventilation, naturally cool to room temperature, a kind of agglomeration resistance high purity electronic grade nitric acid strontium can be obtained.
This case method is unique novel, and final obtained agglomeration resistance high purity electronic grade nitric acid strontium is white crystals, and relative density is 2.9, and fusing point is 580 DEG C, and purity is 99.9%, and grain diameter is 710 μm, and clotting time reaches 220 days.
Claims (1)
1. a preparation method for agglomeration resistance high purity electronic grade nitric acid strontium, is characterized in that concrete operation step is:
(1) 500 ~ 600g height calciostrontianite and 700 ~ 800g witherite is got, pour in crusher and carry out coarse breaking process, process 2 ~ 3min, cross 50 ~ 60 mesh sieves, subsequently the composite grain after sieving is put into high speed ball mill, add the stainless steel abrading-ball pearl that particle diameter is 4 ~ 5mm, ball milling 10 ~ 12min under rotational speed of ball-mill is 500 ~ 600r/min, be milled to granularity <0.08mm, obtain mixed powder, the mixed powder obtained afterwards is poured in container, and adds powder quality 70 ~ 80% clear water wherein, mix, obtain mixed serum;
(2) in mixed serum obtained above, slowly adding mixed serum quality 35 ~ 40% mass concentration is the salpeter solution of 98%, stir with glass stick, standing and reacting at 30 ~ 32 DEG C, be till 2.5 ~ 3.2 until reacting solution pH value, question response terminates, and is 2: 1 ~ 3: 1, adds 0.5M sodium hydroxide solution in reactant by solid-to-liquid ratio, promote temperature to 32 ~ 35 DEG C, Keep agitation is until generate without precipitation;
(3) said mixture is put into whizzer, under the rotating speed of 1100 ~ 1200r/min, centrifugation 10 ~ 20min, removes slag, and gets supernatant liquor, pour in container, at normal temperatures, in container, dripping mass concentration with the speed of 8 ~ 10mL/min is while stirring the salpeter solution of 37%, controls to be added dropwise to complete in 25 ~ 35min, temperature to 100 ~ 105 DEG C are promoted again subsequently with the speed of 5 ~ 10 DEG C/min, Keep agitation reaction 2 ~ 2.5h, question response terminates, slaking 2 ~ 4h;
(4) treat that above-mentioned slaking terminates, material after slaking is carried out solid-liquid separation while hot, remove slag, stay liquid, the filtrate obtained is put into concentration tank, reducing tank internal pressure is 1000 ~ 1100Pa, when being evaporated to that in tank, filtrate volume is 1/3 ~ 1/2 of original volume, stop concentrated, relative density controls at 15 ~ 18Be, dry after crystallisation by cooling, obtain strontium nitrate crude product;
(5) strontium nitrate crude product obtained above is put into distilled water, heating for dissolving at 50 ~ 60 DEG C, after to be dissolved, adding strontium nitrate crude product quality 20 ~ 30% mass concentration is wherein the hydrogen peroxide of 25%, is uniformly mixed, and precipitation 1 ~ 2h, filters, obtain filtered liquid;
(6) filtered liquid obtained above is put into container for evaporation, heated and stirred at 80 ~ 90 DEG C, when to be evaporated to filtered liquid volume be original volume 1/2, stop evaporation, promote temperature to 92 ~ 95 DEG C, stir ageing 1 ~ 2h, preferred 1.5h, treat that ageing terminates, solid-liquid separation, obtain crystal;
(7) crystal obtained above is put into vacuum drying oven, wherein vacuum drying oven vacuum tightness is-0.03 ~ 0.05Mpa, temperature is 110 ~ 130 DEG C, dry until crystal water content be till 0.2 ~ 0.3%, subsequently dried crystal is positioned over ventilation, naturally cool to room temperature, a kind of agglomeration resistance high purity electronic grade nitric acid strontium can be obtained.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108439453A (en) * | 2018-05-31 | 2018-08-24 | 成都市科隆化学品有限公司 | A kind of purification process of strontium nitrate |
| CN116375287A (en) * | 2023-04-28 | 2023-07-04 | 新疆西部合盛硅业有限公司 | Calcium chloride wastewater treatment system and treatment method |
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| DE1592081A1 (en) * | 1967-06-29 | 1972-11-09 | Kalk Chemische Fabrik Gmbh | Process for the production of strontium nitrate from rock phosphate |
| EP0025237A1 (en) * | 1979-08-13 | 1981-03-18 | FMC Corporation | Method for producing strontium nitrate |
| CN101549880A (en) * | 2009-05-06 | 2009-10-07 | 重庆新申世纪化工有限公司 | Preparation method of anti-caking strontium nitrate |
| CN104030333A (en) * | 2014-06-27 | 2014-09-10 | 重庆邮电大学 | Method for joint production of strontium nitrate and barium nitrate from high-calcium strontianite and witherite |
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| DE1592081A1 (en) * | 1967-06-29 | 1972-11-09 | Kalk Chemische Fabrik Gmbh | Process for the production of strontium nitrate from rock phosphate |
| EP0025237A1 (en) * | 1979-08-13 | 1981-03-18 | FMC Corporation | Method for producing strontium nitrate |
| CN101549880A (en) * | 2009-05-06 | 2009-10-07 | 重庆新申世纪化工有限公司 | Preparation method of anti-caking strontium nitrate |
| CN104030333A (en) * | 2014-06-27 | 2014-09-10 | 重庆邮电大学 | Method for joint production of strontium nitrate and barium nitrate from high-calcium strontianite and witherite |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108439453A (en) * | 2018-05-31 | 2018-08-24 | 成都市科隆化学品有限公司 | A kind of purification process of strontium nitrate |
| CN116375287A (en) * | 2023-04-28 | 2023-07-04 | 新疆西部合盛硅业有限公司 | Calcium chloride wastewater treatment system and treatment method |
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