CN111533105A - Preparation method of optical-grade strontium metaphosphate - Google Patents
Preparation method of optical-grade strontium metaphosphate Download PDFInfo
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- CN111533105A CN111533105A CN202010415030.4A CN202010415030A CN111533105A CN 111533105 A CN111533105 A CN 111533105A CN 202010415030 A CN202010415030 A CN 202010415030A CN 111533105 A CN111533105 A CN 111533105A
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- strontium
- metaphosphate
- dihydrogen phosphate
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- 229910052712 strontium Inorganic materials 0.000 title claims abstract description 59
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 36
- 230000003287 optical effect Effects 0.000 claims abstract description 35
- 238000001354 calcination Methods 0.000 claims abstract description 33
- AOKGFBICYSLGKE-UHFFFAOYSA-L strontium;dihydrogen phosphate Chemical compound [Sr+2].OP(O)([O-])=O.OP(O)([O-])=O AOKGFBICYSLGKE-UHFFFAOYSA-L 0.000 claims abstract description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910001868 water Inorganic materials 0.000 claims abstract description 19
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 18
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 15
- 239000000843 powder Substances 0.000 claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- 239000007921 spray Substances 0.000 claims abstract description 11
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000012535 impurity Substances 0.000 claims abstract description 9
- 238000001704 evaporation Methods 0.000 claims abstract description 8
- 229910052751 metal Inorganic materials 0.000 claims abstract description 8
- 239000002184 metal Substances 0.000 claims abstract description 8
- 150000002739 metals Chemical class 0.000 claims abstract description 7
- IATRAKWUXMZMIY-UHFFFAOYSA-N strontium oxide Chemical group [O-2].[Sr+2] IATRAKWUXMZMIY-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000003456 ion exchange resin Substances 0.000 claims abstract description 6
- 229920003303 ion-exchange polymer Polymers 0.000 claims abstract description 6
- UUCCCPNEFXQJEL-UHFFFAOYSA-L strontium dihydroxide Chemical compound [OH-].[OH-].[Sr+2] UUCCCPNEFXQJEL-UHFFFAOYSA-L 0.000 claims abstract description 6
- 229910001866 strontium hydroxide Inorganic materials 0.000 claims abstract description 6
- 150000002500 ions Chemical class 0.000 claims abstract description 4
- 239000003957 anion exchange resin Substances 0.000 claims description 17
- 239000003729 cation exchange resin Substances 0.000 claims description 17
- 238000006243 chemical reaction Methods 0.000 claims description 17
- 239000000463 material Substances 0.000 claims description 9
- 230000035484 reaction time Effects 0.000 claims description 7
- 239000010431 corundum Substances 0.000 claims description 6
- 229910052593 corundum Inorganic materials 0.000 claims description 6
- 229910001252 Pd alloy Inorganic materials 0.000 claims description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 2
- 238000000746 purification Methods 0.000 claims description 2
- 239000010453 quartz Substances 0.000 claims description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 2
- 239000012141 concentrate Substances 0.000 claims 3
- 239000002994 raw material Substances 0.000 abstract description 9
- 239000000087 laser glass Substances 0.000 abstract description 5
- 239000005304 optical glass Substances 0.000 abstract description 3
- 238000005342 ion exchange Methods 0.000 abstract description 2
- 229910052759 nickel Inorganic materials 0.000 description 7
- 229940023913 cation exchange resins Drugs 0.000 description 6
- 229910052804 chromium Inorganic materials 0.000 description 6
- 229910052745 lead Inorganic materials 0.000 description 6
- 229910052748 manganese Inorganic materials 0.000 description 6
- 229910052802 copper Inorganic materials 0.000 description 5
- 229910052742 iron Inorganic materials 0.000 description 5
- 125000005341 metaphosphate group Chemical group 0.000 description 5
- 230000002572 peristaltic effect Effects 0.000 description 4
- 238000005507 spraying Methods 0.000 description 4
- UJPWWRPNIRRCPJ-UHFFFAOYSA-L strontium;dihydroxide;octahydrate Chemical compound O.O.O.O.O.O.O.O.[OH-].[OH-].[Sr+2] UJPWWRPNIRRCPJ-UHFFFAOYSA-L 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 3
- 229910019142 PO4 Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 2
- 235000021317 phosphate Nutrition 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000036760 body temperature Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- -1 ferrous metals Chemical class 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 239000005365 phosphate glass Substances 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/38—Condensed phosphates
- C01B25/44—Metaphosphates
-
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The technical scheme of the invention provides a preparation method of optical grade strontium metaphosphate, which comprises the following steps: reacting a strontium source, phosphoric acid and water in a certain proportion under the conditions of heating and pressurizing to obtain a crude strontium dihydrogen phosphate solution, wherein the strontium source is strontium oxide or strontium hydroxide; adjusting the concentration of the crude strontium dihydrogen phosphate solution, and passing through ion exchange resin at a certain flow rate to remove nonferrous metals and impurity ions; evaporating and concentrating to obtain concentrated solution containing strontium dihydrogen phosphate with concentration of more than 24%; removing free water and structural water in the concentrated solution to obtain strontium metaphosphate intermediate powder; and calcining to obtain the optical grade strontium metaphosphate finished product. The preparation method has strong adaptability to the raw material strontium hydroxide, adopts the mode of removing impurities by an ion exchange method, and combining indirect heating clean spray calcination with high-temperature electric furnace clean calcination, and can prepare high-purity strontium metaphosphate, and all indexes of the strontium metaphosphate meet the requirements of optical glass and laser glass raw materials.
Description
Technical Field
The invention relates to the field of fine inorganic phosphorus chemical industry, in particular to a preparation method of optical-grade strontium metaphosphate.
Background
Metaphosphate is the most stable phosphate among dibasic phosphates, and is a basic raw material for the production of phosphate glass. The high-purity metaphosphate has excellent light transmittance, so that the metaphosphate can be used as an important raw material of laser glass in a high-power laser (such as national scientific engineering-Shenguang plan) and also can be used as an important raw material of some advanced optical equipment such as camera lenses, high-definition cameras, smart phone lenses and mobile phone panel substrates.
The transition metals of Fe, Co, Ni and the like can cause strong absorption of metaphosphate glass in the near ultraviolet to infrared regions, and the optical performance of the glass is influenced. Therefore, the preparation of high purity metaphosphate raw material becomes the key to the manufacture of high performance laser glass.
Disclosure of Invention
In view of the above-mentioned prior art, the technical problem to be solved by the present invention is to provide a method for preparing optical grade strontium metaphosphate.
In order to solve the technical problems, the technical scheme of the invention provides a preparation method of optical grade strontium metaphosphate, which comprises the following steps:
(1) reacting a strontium source, phosphoric acid and water in a certain proportion under the conditions of heating and pressurizing to obtain a crude strontium dihydrogen phosphate solution, wherein the strontium source is strontium oxide or strontium hydroxide;
(2) adjusting the concentration of the crude strontium dihydrogen phosphate solution, and passing through ion exchange resin at a certain flow rate to remove nonferrous metals and impurity ions;
(3) evaporating and concentrating to obtain concentrated solution containing strontium dihydrogen phosphate with concentration of more than 24%;
(4) removing free water and structural water in the concentrated solution to obtain strontium metaphosphate intermediate powder;
(5) and calcining to obtain the optical grade strontium metaphosphate finished product.
Preferably, in the step (1), the molar ratio of the strontium source to the phosphoric acid is 1 (1.97-2.03), the mass ratio of the phosphoric acid to the water is 1 (2.0-3.6), the reaction temperature is 125-145 ℃, the reaction pressure is 0.3-0.55 MPa, and the reaction time is 3-6 h. Further preferably, the molar ratio of the strontium source to the phosphoric acid is 1 (0.985-2.015), the mass ratio of the phosphoric acid to the water is 1 (2.1-2.9), the reaction temperature is 130-140 ℃, the reaction pressure is 0.38-0.47 MPa, and the reaction time is 3.5-5 h.
Preferably, in the step (2), the concentration of the crude strontium dihydrogen phosphate is adjusted to 7 to 17 percent. More preferably, it is 9% to 15%.
Preferably, the ion exchange resin comprises a cation exchange resin and an anion exchange resin, the cation exchange resin comprises 741, D001, IONRESIN IR1200F, IONRESIN1600 and IONRESIN252, and the anion exchange resin comprises 201 × 4, 201 × 7, D201, D406 and D407.
Preferably, the flow rate through the cation exchange resin and the anion exchange resin is 1L/min to 5L/min. More preferably, it is 2L/min to 4L/min.
Preferably, the concentration of the strontium dihydrogen phosphate in the concentrated solution is 24-30%, and more preferably, 26-29%.
Preferably, the concentrated solution is sent to a spray calcining tower for dehydration, wherein the air inlet temperature of the spray calcining tower is 710-800 ℃, the temperature of the upper section of the tower body is 680-760 ℃, the temperature of the middle section of the tower body is 650-730 ℃, the temperature of the lower section of the tower body is 620-700 ℃, the air outlet temperature is 390-465 ℃, and the flow rate of the concentrated solution pumped into the tower body is 6-13L/min. Further, the air inlet temperature is 750-780 ℃, the temperature of the upper section of the tower body is 720-750 ℃, the temperature of the middle section of the tower body is 685-720 ℃, the temperature of the lower section of the tower body is 660-685 ℃, the air outlet temperature is 420-455 ℃, and the flow rate of the concentrated solution pumped into the tower body is 7-11L/min.
Preferably, in order to ensure the product quality, the material contact part of the calcining tower adopts a high-purity alumina lining, the spray head is made of titanium palladium alloy, the heating mode adopts indirect heating, and the air inlet needs to be subjected to multi-stage purification treatment.
The indirect heating is adopted, and the problem that the highest inlet air temperature of a spray calcining tower can only reach 780-800 ℃ (the tower body temperature can only reach 700-.
Preferably, the material is calcined by an electric furnace, a hearth is lined by high-purity corundum or high-purity quartz material, the calcining temperature is 780-860 ℃, and the calcining time is 5-12 h. Furthermore, the calcining temperature of the electric furnace is 800-840 ℃, and the calcining time is 7-10 h.
The preparation method of the optical grade strontium metaphosphate in the technical scheme of the invention has the following beneficial effects:
the adaptability to the raw material strontium hydroxide is strong, the method of removing impurities by an ion exchange method, and combining indirect heating clean spray calcination with high-temperature electric furnace clean calcination can prepare high-purity strontium metaphosphate, and each index meets the requirements of optical glass and laser glass raw materials.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without inventive labor.
Fig. 1 is a flow chart of a method for preparing optical grade strontium metaphosphate according to the technical scheme of the invention.
Detailed Description
The conception, the specific structure and the technical effects of the present invention will be further described with reference to the accompanying drawings to fully understand the objects, the features and the effects of the present invention.
As shown in fig. 1, the method for preparing optical grade strontium metaphosphate in accordance with the present invention comprises the following steps:
(1) reacting a strontium source, such as strontium hydroxide, phosphoric acid and water, in a certain proportion under the conditions of heating and pressurizing to obtain a crude strontium dihydrogen phosphate solution;
(2) adjusting the concentration of the crude strontium dihydrogen phosphate solution (i.e. the concentration adjusting step in fig. 1), and passing through an ion exchange resin at a certain flow rate to remove non-ferrous metals and impurity ions;
(3) evaporating and concentrating to obtain concentrated solution containing strontium dihydrogen phosphate with concentration of more than 24%;
(4) removing free water and structural water in the concentrated solution (namely the clean spray calcination step in figure 1) to obtain intermediate powder of strontium metaphosphate;
(5) and calcining (namely calcining in a clean electric furnace in figure 1) to obtain the finished product of the optical grade strontium metaphosphate.
The following describes in detail the method for preparing optical grade strontium metaphosphate according to the present invention with reference to specific examples.
Example 1
The preparation method of the optical grade strontium metaphosphate of the embodiment specifically comprises the following steps:
(1)200kg of strontium hydroxide octahydrate with the content of 97 percent is added into diluted phosphoric acid blended by 170kg of 85 percent industrial phosphoric acid and 408kg of water, the reaction temperature is controlled to be 133-137 ℃, the reaction pressure is controlled to be 0.35-0.4 MPa, the reaction time is controlled to be 4-5 h, and crude strontium dihydrogen phosphate solution is obtained after the reaction;
(2) the concentration of the crude strontium dihydrogen phosphate solution is adjusted to 12%, and the crude strontium dihydrogen phosphate solution passes through a group of cation exchange resin and anion exchange resin at the flow rate of 4.4L/min, wherein the cation exchange resin adopted in the embodiment of the invention is D001 and IONFERN IR1200F type cation exchange resin, and the anion exchange resin adopted in the embodiment of the invention is 201 × 7 and D406 type anion exchange resin, so that nonferrous metals such as Fe, Mn, Pb, Cr, Cu, Ni, Co and the like and Cl are removed－Sulfate radicals and the like;
(3) evaporating and concentrating to obtain concentrated solution containing 28% of strontium dihydrogen phosphate;
(4) controlling the concentrated solution by a peristaltic pump, spraying the concentrated solution into a calcining tower at a flow rate of 11L/min, and controlling the inlet air temperature of the calcining tower to be 755-780 ℃, the upper section temperature of the tower body to be 725-750 ℃, the middle section temperature of the tower body to be 690-720 ℃, the lower section temperature of the tower body to be 660-685 ℃ and the outlet air temperature to be 420-445 ℃ to obtain 186kg of optical grade strontium metaphosphate powder;
(5) the optical grade strontium metaphosphate intermediate powder is calcined for 6 hours at 840 ℃ in an electric furnace lined with a high-purity corundum material to obtain 174kg of optical grade strontium metaphosphate finished product with the comprehensive yield of 97.1 percent.
Example 2
The preparation method of the optical grade strontium metaphosphate of the embodiment specifically comprises the following steps:
(1) adding 250kg of 98 percent strontium hydroxide octahydrate into dilute phosphoric acid blended by 215.6kg of 85 percent industrial phosphoric acid and 517.4kg of water, controlling the reaction temperature to be 135-139 ℃, the reaction pressure to be 0.37-0.42 MPa and the reaction time to be 4-5 h, and reacting to obtain a crude strontium dihydrogen phosphate solution;
(2) adjusting the concentration of the crude strontium dihydrogen phosphate solution to 13%, and passing through a group of cation exchange resins and anion exchange resins at a flow rate of 4.2L/min, wherein the cation exchange resins adopted by the embodiment of the invention are IONRISI 1600 and IONRISI 252 type cation exchange resins, and the anion exchange resins adopted by the embodiment of the invention are 201 × 4, 201 × 7 and D201 type anion exchange resins, so as to remove nonferrous metals such as Fe, Mn, Pb, Cr, Cu, Ni and Co and Cl－Sulfate radicals and the like;
(3) evaporating and concentrating to obtain concentrated solution containing 27% of strontium dihydrogen phosphate;
(4) controlling the concentrated solution by a peristaltic pump, spraying the concentrated solution into a calcining tower at the flow rate of 12L/min, and controlling the air inlet temperature of the calcining tower to be 760-785 ℃, the temperature of the upper section of the tower to be 733-752 ℃, the temperature of the middle section of the tower to be 697-725 ℃, the temperature of the lower section of the tower to be 668-690 ℃ and the air outlet temperature to be 424-447 ℃ to obtain 234kg of optical-grade strontium metaphosphate powder;
(5) and calcining the optical grade strontium metaphosphate intermediate powder in an electric furnace lined with a high-purity corundum material at 840 ℃ for 6 hours to obtain 219kg of optical grade strontium metaphosphate finished product with the comprehensive yield of 96.5 percent.
Example 3
The preparation method of the optical grade strontium metaphosphate of the embodiment specifically comprises the following steps:
(1)300kg of 96.5 percent strontium hydroxide octahydrate is added into a diluted phosphoric acid blended by 253.2kg of 85 percent industrial phosphoric acid and 607.8kg of water, the reaction temperature is controlled to be 138-142 ℃, the reaction pressure is controlled to be 0.4-0.45 MPa, the reaction time is 4-5 h, and a crude strontium dihydrogen phosphate solution is obtained after the reaction;
(2) adjusting the concentration of the crude strontium dihydrogen phosphate solution to 14%, passing through a group of cation exchange resins and anion exchange resins at a flow rate of 4L/min, wherein the cation exchange resins adopted in the embodiment of the invention are 741, D001 and IONRESIN252 type cation exchange resins, and the anion exchange resins are D406 and D407 type anion exchange resins, so as to remove nonferrous metals such as Fe, Mn, Pb, Cr, Cu, Ni and Co and Cl－Sulfate radicalAnd the like;
(3) evaporating and concentrating to obtain concentrated solution containing 26% of strontium dihydrogen phosphate;
(4) controlling the concentrated solution by a peristaltic pump, spraying the concentrated solution into a calcining tower at the flow rate of 10L/min, and controlling the air inlet temperature of the calcining tower to be 746-770 ℃, the upper section temperature of the tower body to be 717-735 ℃, the middle section temperature of the tower body to be 679-706 ℃, the lower section temperature of the tower body to be 648-673 ℃ and the air outlet temperature to be 405-428 ℃ to obtain 276kg of optical grade strontium metaphosphate powder;
(5) and calcining the optical grade strontium metaphosphate intermediate powder in an electric furnace lined with a high-purity corundum material at 840 ℃ for 6 hours to obtain 257g of the optical grade strontium metaphosphate finished product, wherein the comprehensive yield is 96.1%.
Example 4
The preparation method of the optical grade strontium metaphosphate of the embodiment specifically comprises the following steps:
(1)340kg of strontium hydroxide octahydrate with the content of 97.5 percent is added into dilute phosphoric acid blended by 282.6kg of 85 percent industrial phosphoric acid and 678.4kg of water, the reaction temperature is controlled to be 135-140 ℃, the reaction pressure is controlled to be 0.37-0.42 MPa, the reaction time is 4-5 h, and crude strontium dihydrogen phosphate solution is obtained after the reaction;
(2) the concentration of the crude strontium dihydrogen phosphate solution is adjusted to 10%, the crude strontium dihydrogen phosphate solution passes through a group of cation exchange resin and anion exchange resin at the flow rate of 4.8L/min, the cation exchange resin adopted in the embodiment of the invention is IONRESIN IR1200F and IONRESIN1600 type cation exchange resin, and the anion exchange resin adopted in the embodiment of the invention is 201 × 4 and D406 type anion exchange resin, so as to remove nonferrous metals such as Fe, Mn, Pb, Cr, Cu, Ni, Co and the like and Cl－Sulfate radicals and the like;
(3) evaporating and concentrating to obtain concentrated solution containing 25% of strontium dihydrogen phosphate;
(4) controlling the concentrated solution by a peristaltic pump, spraying the concentrated solution into a calcining tower at the flow rate of 9L/min, and controlling the inlet air temperature of the calcining tower to be 740-760 ℃, the upper section temperature of the tower body to be 715-730 ℃, the middle section temperature of the tower body to be 685-705 ℃, the lower section temperature of the tower body to be 655-673 ℃ and the outlet air temperature to be 403-422 ℃ to obtain 315kg of optical grade strontium metaphosphate powder;
(5) the optical grade strontium metaphosphate intermediate powder is calcined in an electric furnace lined with a high-purity corundum material at 840 ℃ for 6 hours to obtain 298kg of optical grade strontium metaphosphate finished product with the comprehensive yield of 97.4 percent.
The strontium metaphosphate samples prepared in examples 1 to 4 were analyzed, and the results are shown in table 1:
TABLE 1 analysis of strontium metaphosphate samples
As can be seen from Table 1, the strontium metaphosphate prepared in examples 1-4 contains impurities such as Fe2O3The total content of 10 key impurity indexes of Cu, Co, Cr, Mn, Ni, Pb and the like is not more than 5ppm, wherein the total content of Co, Cr, Mn, Ni, Pb and the like is not more than 1ppm, the content of Cu is not more than 0.2ppm, and Fe2O3Content of not more than 2ppm, Cl－The total content of sulfate radicals is not more than 120ppm, the content of SrO is 42 +/-0.5 percent, and P2O5The content is 58 plus or minus 0.5 percent.
In conclusion, the strontium metaphosphate prepared by the preparation method of the technical scheme of the invention has high main content, low impurity content, stable quality and uniform granularity, all indexes meet the index requirements of laser glass and optical glass raw materials, and the preparation method of the optical strontium metaphosphate is efficient, simple and convenient and has low production cost.
While specific embodiments of the present invention have been described in detail above, it will be appreciated that those skilled in the art, upon attaining an understanding of the foregoing may readily produce alterations to, variations of, and equivalents to these embodiments. Therefore, the technical solutions available to those skilled in the art through logic analysis, reasoning and limited experiments based on the prior art according to the concept of the present invention should be within the scope of protection defined by the claims.
Claims (9)
1. A preparation method of optical grade strontium metaphosphate is characterized by comprising the following steps:
(1) reacting a strontium source, phosphoric acid and water in a certain proportion under the conditions of heating and pressurizing to obtain a crude strontium dihydrogen phosphate solution, wherein the strontium source is strontium oxide or strontium hydroxide;
(2) adjusting the concentration of the crude strontium dihydrogen phosphate solution, and passing through ion exchange resin at a certain flow rate to remove nonferrous metals and impurity ions;
(3) evaporating and concentrating to obtain concentrated solution containing strontium dihydrogen phosphate with concentration of more than 24%;
(4) removing free water and structural water in the concentrated solution to obtain strontium metaphosphate intermediate powder;
(5) and calcining to obtain the optical grade strontium metaphosphate finished product.
2. The method for preparing optical grade strontium metaphosphate according to claim 1, wherein in the step (1), the molar ratio of the strontium source to the phosphoric acid is 1 (1.97-2.03), the mass ratio of the phosphoric acid to the water is 1 (2.0-3.6), the reaction temperature is 125-145 ℃, the reaction pressure is 0.3-0.55 MPa, and the reaction time is 3-6 h.
3. The method for preparing optical grade strontium metaphosphate of claim 1, wherein in step (2), the concentration of said crude strontium dihydrogen phosphate is adjusted to 7% -17%.
4. The method of claim 1, wherein the ion exchange resin comprises a cation exchange resin comprising 741, D001, iorreiesin nir1200F, iorrein 1600, iorrein 252, or a combination thereof, and an anion exchange resin comprising 201 x 4, 201 x 7, D201, D406, or a combination thereof.
5. The method of claim 1, wherein the flow rate through the cation exchange resin and the anion exchange resin is 1L/min to 5L/min.
6. The method of claim 1, wherein the concentration of strontium dihydrogen phosphate in the concentrate is from 24% to 30%.
7. The method of claim 1, wherein the optical grade strontium metaphosphate is dehydrated by feeding the concentrate to a spray calcination tower, wherein the spray calcination tower has an inlet air temperature of 710 to 800 ℃, an upper tower section temperature of 680 to 760 ℃, a middle tower section temperature of 650 to 730 ℃, a lower tower section temperature of 620 to 700 ℃, an outlet air temperature of 390 to 465 ℃ and a flow rate of the concentrate into the tower body of 6 to 13L/min.
8. The method for preparing optical-grade strontium metaphosphate of claim 7, wherein the material contact part in the spray calcination tower is made of high-purity alumina lining, the spray head is made of titanium-palladium alloy, the heating mode is indirect heating, and the intake air needs to be subjected to multi-stage purification treatment.
9. The method for preparing optical grade strontium metaphosphate of claim 1, wherein the optical grade strontium metaphosphate is calcined by an electric furnace, the hearth of the electric furnace is lined with high-purity corundum or high-purity quartz material, the calcination temperature is 780-860 ℃, and the calcination time is 5-12 h.
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| CN202010415030.4A CN111533105A (en) | 2020-05-15 | 2020-05-15 | Preparation method of optical-grade strontium metaphosphate |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1761616A (en) * | 2003-03-14 | 2006-04-19 | 日本化学工业株式会社 | High purity metaphosphate and method for production thereof |
| CN1800001A (en) * | 2004-12-31 | 2006-07-12 | 西安交通大学医学院 | Calcium metaphosphorate production process |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1761616A (en) * | 2003-03-14 | 2006-04-19 | 日本化学工业株式会社 | High purity metaphosphate and method for production thereof |
| CN1800001A (en) * | 2004-12-31 | 2006-07-12 | 西安交通大学医学院 | Calcium metaphosphorate production process |
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