CN111362241A - Preparation method of optical-grade barium dihydrogen phosphate - Google Patents
Preparation method of optical-grade barium dihydrogen phosphate Download PDFInfo
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- CN111362241A CN111362241A CN202010415031.9A CN202010415031A CN111362241A CN 111362241 A CN111362241 A CN 111362241A CN 202010415031 A CN202010415031 A CN 202010415031A CN 111362241 A CN111362241 A CN 111362241A
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- dihydrogen phosphate
- barium dihydrogen
- barium
- optical grade
- exchange resin
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- IOPOLWHQYJSKCT-UHFFFAOYSA-L barium(2+);dihydrogen phosphate Chemical compound [Ba+2].OP(O)([O-])=O.OP(O)([O-])=O IOPOLWHQYJSKCT-UHFFFAOYSA-L 0.000 title claims abstract description 84
- 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 38
- 230000003287 optical effect Effects 0.000 claims abstract description 29
- 239000000843 powder Substances 0.000 claims abstract description 24
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 19
- 239000003957 anion exchange resin Substances 0.000 claims abstract description 19
- 239000003729 cation exchange resin Substances 0.000 claims abstract description 19
- 238000001035 drying Methods 0.000 claims abstract description 19
- 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 13
- RQPZNWPYLFFXCP-UHFFFAOYSA-L barium dihydroxide Chemical compound [OH-].[OH-].[Ba+2] RQPZNWPYLFFXCP-UHFFFAOYSA-L 0.000 claims abstract description 12
- 229910001863 barium hydroxide Inorganic materials 0.000 claims abstract description 12
- 239000012535 impurity Substances 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910001868 water Inorganic materials 0.000 claims abstract description 11
- 229910052751 metal Inorganic materials 0.000 claims abstract description 10
- 239000002184 metal Substances 0.000 claims abstract description 10
- 238000005342 ion exchange Methods 0.000 claims abstract description 8
- 150000002739 metals Chemical class 0.000 claims abstract description 8
- 150000002500 ions Chemical class 0.000 claims abstract description 6
- 238000004519 manufacturing process Methods 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims description 19
- 238000006243 chemical reaction Methods 0.000 claims description 16
- 238000001694 spray drying Methods 0.000 claims description 15
- 230000036760 body temperature Effects 0.000 claims description 14
- 229910052804 chromium Inorganic materials 0.000 claims description 9
- 229910052759 nickel Inorganic materials 0.000 claims description 9
- 229910052802 copper Inorganic materials 0.000 claims description 8
- 229910052745 lead Inorganic materials 0.000 claims description 8
- 229910052748 manganese Inorganic materials 0.000 claims description 8
- 229910052742 iron Inorganic materials 0.000 claims description 7
- 230000035484 reaction time Effects 0.000 claims description 7
- 238000009835 boiling Methods 0.000 claims description 5
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 3
- 239000010936 titanium Substances 0.000 claims description 3
- 229910052719 titanium Inorganic materials 0.000 claims description 3
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- 239000000463 material Substances 0.000 claims description 2
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 7
- 239000005304 optical glass Substances 0.000 abstract description 5
- 239000000087 laser glass Substances 0.000 abstract description 3
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 9
- 239000011651 chromium Substances 0.000 description 8
- 239000010949 copper Substances 0.000 description 8
- 239000011133 lead Substances 0.000 description 8
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 7
- 239000011572 manganese Substances 0.000 description 7
- 229940023913 cation exchange resins Drugs 0.000 description 6
- 230000018044 dehydration Effects 0.000 description 5
- 238000006297 dehydration reaction Methods 0.000 description 5
- 229910019142 PO4 Inorganic materials 0.000 description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 4
- 239000010452 phosphate Substances 0.000 description 4
- 238000009461 vacuum packaging Methods 0.000 description 4
- 229910052723 transition metal Inorganic materials 0.000 description 3
- 150000003624 transition metals Chemical class 0.000 description 3
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- LYSTYSFIGYAXTG-UHFFFAOYSA-L barium(2+);hydrogen phosphate Chemical compound [Ba+2].OP([O-])([O-])=O LYSTYSFIGYAXTG-UHFFFAOYSA-L 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000005385 borate glass Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- -1 ferrous metals Chemical class 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000005365 phosphate glass Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 230000026731 phosphorylation Effects 0.000 description 1
- 238000006366 phosphorylation reaction Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000005368 silicate glass Substances 0.000 description 1
- 239000007921 spray Substances 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
- C01B25/32—Phosphates of magnesium, calcium, strontium, or barium
- C01B25/325—Preparation by double decomposition
-
- 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
- C01B25/32—Phosphates of magnesium, calcium, strontium, or barium
- C01B25/327—After-treatment
-
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The technical scheme of the invention discloses a preparation method of optical grade barium dihydrogen phosphate, which comprises the following steps: reacting barium hydroxide, phosphoric acid and water according to a certain proportion to obtain a crude barium dihydrogen phosphate solution; adjusting the concentration of the crude barium dihydrogen phosphate solution, and passing through cation exchange resin and anion exchange resin at a certain flow rate to remove nonferrous metals and impurity ions; dehydrating after ion exchange to obtain barium dihydrogen phosphate intermediate powder; drying the barium dihydrogen phosphate intermediate powder to obtain the optical grade barium dihydrogen phosphate powder. Various indexes of the barium dihydrogen phosphate prepared by the technical scheme of the invention all meet the index requirements of raw materials of optical glass and laser glass, and the preparation method of the optical barium dihydrogen phosphate is efficient, simple and convenient, has low production cost and is suitable for large-scale production.
Description
Technical Field
The invention relates to the field of fine inorganic phosphorus chemical industry, in particular to a preparation method of optical-grade barium dihydrogen phosphate.
Background
Compared with silicate glass and borate glass, the phosphate optical glass has more excellent physical and optical properties, such as large stimulated emission section, low light absorption intensity and good light transmission performance, so that the phosphate optical glass can be used for manufacturing glass hoods of high-power laser systems, high-repetition-rate lasers, precision guidance missiles and cruise missiles, lenses of imaging equipment, lenses of advanced video cameras, digital cameras and the like.
And the high-purity phosphate with the total content of transition metal impurities (iron, copper, cobalt, chromium, manganese, nickel, lead and the like) not more than 5ppm is a basic raw material for preparing high-performance phosphate glass, so that the preparation of the high-purity phosphate has important significance for the national defense industry.
Patent CN201711378807.9 discloses a method for separating out high-purity barium dihydrogen phosphate by using electronic grade phosphoric acid and barium source (barium carbonate or barium hydroxide) through intermediate barium hydrogen phosphate precipitation phosphorylation, the whole process of the method needs to use high-purity raw materials, no chemical purification process exists, the method has raw material limitation, and the product purity is difficult to reach a higher degree (for example, the total amount of transition metal impurities is less than 2 ppm).
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 barium dihydrogen phosphate.
In order to solve the technical problems, the technical scheme of the invention provides a preparation method of optical grade barium dihydrogen phosphate, which comprises the following steps:
(1) reacting barium hydroxide, phosphoric acid and water according to a certain proportion to obtain a crude barium dihydrogen phosphate solution;
(2) adjusting the concentration of the crude barium dihydrogen phosphate solution, and removing nonferrous metals and impurity ions by passing through cation exchange resin and specially selected anion exchange resin at a certain flow rate;
(3) dehydrating after ion exchange to obtain barium dihydrogen phosphate intermediate powder;
(4) drying the barium dihydrogen phosphate intermediate powder to obtain the optical grade barium dihydrogen phosphate powder.
Preferably, in the step (1), the molar ratio of barium hydroxide to phosphoric acid is 1 (1.97-2.03), the mass ratio of phosphoric acid to water is 1 (2.6-4.2), the reaction temperature is 120-140 ℃, the reaction pressure is 0.25-0.5 MPa, and the reaction time is 3-8 h.
Further preferably, the reaction molar ratio of the barium hydroxide to the phosphoric acid is 1 (1.98-2.02), the mass ratio of the phosphoric acid to the water is 1 (3.0-4.0), the reaction temperature is 125-135 ℃, the reaction pressure is 0.3-0.45 MPa, and the reaction time is 4-6 h.
Preferably, the concentration of the crude barium dihydrogen phosphate is 8 to 17 percent, and more preferably, 9 to 15 percent.
Preferably, in the step (2), the concentration of the crude barium dihydrogen phosphate solution is adjusted to 10 to 15%.
Preferably, the cation exchange resin comprises one or more of 001 × 7, 001 × 4, 732, 741, D001 and IONRESINIR120, and the anion exchange resin comprises one or more of D201, D202, D407, 201 × 7 and 201 × 4.
Preferably, in step (2), the cation exchange resin and the anion exchange resin are passed at a flow rate of 1L/min to 5L/min. More preferably, it is 2L/min to 4L/min.
Preferably, the non-ferrous metals include Fe, Mn, Pb, Cr, Cu, Ni and Co, and the impurity ions include Cl－、SO4 2-And the like.
Preferably, in the step (3), the barium dihydrogen phosphate solution is sent to a spray drying tower for dehydration at a flow rate of 5L/min to 13L/min, the inlet air temperature of the spray drying tower is 180 ℃ to 210 ℃, the tower body temperature is 150 ℃ to 180 ℃, and the outlet air temperature is 125 ℃ to 150 ℃.
Further preferably, in the step (3), the flow rate of the barium dihydrogen phosphate solution entering the spray drying tower is 8L/min to 12L/min, the inlet air temperature of the spray drying tower is 185 ℃ to 200 ℃, the tower body temperature is 155 ℃ to 173 ℃, and the outlet air temperature is 130 ℃ to 147 ℃.
Preferably, in the step (4), the optical-grade barium dihydrogen phosphate intermediate powder is dried by using a high-efficiency boiling dryer, wherein the air inlet temperature is 160-185 ℃, the tower body temperature is 140-160 ℃, the air outlet temperature is 115-135 ℃, the single feeding amount is 100 kg-300 kg, the drying time is 1.5 h-4 h, further, the air inlet temperature of the high-efficiency boiling dryer is 167-180 ℃, the tower body temperature is 146-165 ℃, the air outlet temperature is 121-128 ℃, the single feeding amount is 150 kg-250 kg, and the drying time is 2 h-3 h.
In order to ensure the product quality, the material contact part of the high-efficiency boiling dryer adopts a pure aluminum or pure titanium lining and the surface is highly polished, the spray head of the dryer is made of pure titanium, and the air inlet needs to be subjected to multi-stage purification treatment.
The preparation method of the optical grade barium dihydrogen phosphate provided by the technical scheme of the invention has the following beneficial effects: the method has strong raw material adaptability, the main technical indexes meet the optical grade requirement, the total amount of transition metal impurities can be controlled to be below 2ppm, the ultra-pure barium dihydrogen phosphate can be produced, and a high-purity raw material is provided for the industrial production of laser glass and optical glass.
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 barium dihydrogen phosphate 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 barium dihydrogen phosphate according to the present invention comprises the following steps:
(1) reacting barium hydroxide, phosphoric acid and water according to a certain proportion, namely heating and pressurizing reaction in figure 1, to obtain a crude barium dihydrogen phosphate solution;
(2) adjusting the concentration of the crude barium dihydrogen phosphate solution, and passing through cation exchange resin and anion exchange resin at a certain flow rate to remove nonferrous metals and impurity ions;
(3) after ion exchange, dehydrating, namely, performing clean spray drying in figure 1 to obtain barium dihydrogen phosphate intermediate powder;
(4) drying the barium dihydrogen phosphate intermediate powder to obtain the optical grade barium dihydrogen phosphate powder.
The following will describe in detail the method for producing optical grade barium dihydrogen phosphate according to the present invention with reference to specific examples.
Example 1
The preparation method of the optical-grade barium dihydrogen phosphate of the embodiment specifically comprises the following steps:
(1) adding 300kg of 98.5 percent industrial barium hydroxide into dilute phosphoric acid blended by 220.5kg of 85 percent industrial phosphoric acid and 716.5kg of water, controlling the reaction temperature to be 128-132 ℃, the reaction pressure to be 0.35-0.40 MPa, and the reaction time to be 5-6 h, and reacting to obtain a crude barium dihydrogen phosphate solution;
(2) adjusting the concentration of the crude barium dihydrogen phosphate solution to 13%, and passing through a group of cation exchange resin and anion exchange resin at a flow rate of 4L/min, wherein the cation exchange resin adopted by the embodiment of the invention is 001 × 7 type cation exchange resin, and the anion exchange resin comprises D407 type and 201 × 7 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) after ion exchange, the barium dihydrogen phosphate intermediate powder enters a spray drying tower at a rate of 7L/min for dehydration, and the inlet air temperature of the spray drying tower is controlled to be 185-190 ℃, the tower body temperature is controlled to be 155-160 ℃, and the outlet air temperature is controlled to be 130-135 ℃, so that 307kg of barium dihydrogen phosphate intermediate powder is obtained;
(4) the method comprises the steps of adopting clean and efficient fluidized drying of barium dihydrogen phosphate intermediate powder, obtaining 298kg of optical grade barium dihydrogen phosphate finished product under the conditions that the air inlet temperature of an efficient fluidized drying machine is 170-175 ℃, the tower body temperature is 148-152 ℃, the air outlet temperature is 124-128 ℃, the single feeding amount is 200kg, and the drying time is 2.5h, and carrying out vacuum packaging with the yield of 96.0%.
Example 2
The preparation method of the optical-grade barium dihydrogen phosphate of the embodiment specifically comprises the following steps:
(1) adding 400kg of 97% industrial barium hydroxide into dilute phosphoric acid blended by 289.4kg of 85% industrial phosphoric acid and 940.6kg of water, controlling the reaction temperature to be 125-130 ℃, the reaction pressure to be 0.35-0.40 MPa, and the reaction time to be 5-6 h, and reacting to obtain a crude barium dihydrogen phosphate solution;
(2) adjusting the concentration of the crude barium dihydrogen phosphate solution to 15%, passing through a group of cation exchange resins and anion exchange resins at a flow rate of 3.5L/min, wherein the cation exchange resins adopted in the embodiment of the invention are 741 type and D001 type cation exchange resins, and the anion exchange resins are D201 type and 201 × 4 type anion exchange resins, 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) after ion exchange, feeding the barium dihydrogen phosphate into a spray drying tower at 8L/min for dehydration, and controlling the air inlet temperature of the spray drying tower at 189-194 ℃, the tower body temperature at 158-162 ℃ and the air outlet temperature at 133-137 ℃ to obtain 410kg of barium dihydrogen phosphate intermediate powder;
(4) the method comprises the steps of adopting clean and efficient fluidized drying of barium dihydrogen phosphate intermediate powder, obtaining 396kg of optical grade barium dihydrogen phosphate finished product under the conditions that the air inlet temperature of an efficient fluidized drying machine is 172-176 ℃, the tower body temperature is 150-154 ℃, the air outlet temperature is 126-130 ℃, the single feeding amount is 220kg, and the drying time is 3 hours, and carrying out vacuum packaging with the yield of 97.1%.
Example 3
The preparation method of the optical-grade barium dihydrogen phosphate of the embodiment specifically comprises the following steps:
(1) adding 420kg of 97.5 percent industrial barium hydroxide into 305.9kg of diluted phosphoric acid blended by 85 percent industrial phosphoric acid and 994.1kg of water, controlling the reaction temperature to be 130-135 ℃, the reaction pressure to be 0.38-0.45 MPa, and the reaction time to be 6-7 h, and reacting to obtain a crude barium dihydrogen phosphate solution;
(2) the concentration of the crude barium dihydrogen phosphate solution is adjusted to 14%, the crude barium dihydrogen phosphate solution passes through a group of cation exchange resin and anion exchange resin at the flow rate of 4.2L/min, the cation exchange resin adopted in the embodiment of the invention is IONRESIN IR120 type cation exchange resin, the anion exchange resin is D202 type anion exchange resin, and nonferrous metals such as Fe, Mn, Pb, Cr, Cu, Ni, Co and the like and Cl are removed－Sulfate radicals and the like;
(3) after ion exchange, the barium dihydrogen phosphate intermediate powder enters a spray drying tower at a rate of 7.5L/min for dehydration, and the air inlet temperature of the spray drying tower is controlled to be 187-191 ℃, the tower body temperature is controlled to be 157-161 ℃, and the air outlet temperature is controlled to be 132-136 ℃, so that 428kg of the barium dihydrogen phosphate intermediate powder is obtained;
(4) the method comprises the steps of adopting clean and efficient fluidized drying of barium dihydrogen phosphate intermediate powder, wherein the air inlet temperature of an efficient fluidized drying machine is 171-175 ℃, the tower body temperature is 149-153 ℃, the air outlet temperature is 125-129 ℃, the single feeding amount is 240kg, and the drying time is 3h, so that 416kg of optical grade barium dihydrogen phosphate finished products are obtained, and the yield is 97.6 percent after vacuum packaging.
Example 4
The preparation method of the optical-grade barium dihydrogen phosphate of the embodiment specifically comprises the following steps:
(1) adding 330kg of 98 percent industrial barium hydroxide into 241.2kg of 85 percent industrial phosphoric acid and 783.8kg of diluted phosphoric acid blended by water, controlling the reaction temperature to be 135-140 ℃, the reaction pressure to be 0.40-0.45 MPa, and the reaction time to be 4-5 h, and reacting to obtain a crude barium dihydrogen phosphate solution;
(2) the concentration of the crude barium dihydrogen phosphate solution is adjusted to 12%, and the crude barium dihydrogen phosphate solution passes through a group of cation exchange resins and anion exchange resins at the flow rate of 4.6L/min, wherein the cation exchange resins adopted by the embodiment of the invention are 001 × 4 type and 732 type cation exchange resins, and the anion exchange resins adopted by the embodiment of the invention are 201 × 7 type and 201 × 4 type anion exchange resins, 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) after ion exchange, the mixture enters a spray drying tower at 8.5L/min for dehydration, and the inlet air temperature of the spray drying tower is controlled to be 191-196 ℃, the tower body temperature is 161-165 ℃, and the outlet air temperature is controlled to be 136-140 ℃, so that 345kg of barium dihydrogen phosphate intermediate powder is obtained;
(4) the method comprises the steps of adopting clean and efficient fluidized drying of barium dihydrogen phosphate intermediate powder, wherein the air inlet temperature of a high-efficiency fluidized drying machine is 175-179 ℃, the tower body temperature is 153-157 ℃, the air outlet temperature is 129-133 ℃, the single feeding amount is 250kg, and the drying time is 3h, so that 335kg of optical grade barium dihydrogen phosphate finished products are obtained, and the yield is 97.7% after vacuum packaging.
The optical grade barium dihydrogen phosphate samples prepared in examples 1 to 4 were analyzed, and the results are shown in table 1:
TABLE 1 optical grade barium dihydrogen phosphate sample analysis
As can be seen from Table 1, the barium dihydrogen phosphate prepared in examples 1 to 4 includes Fe2O310 key impurity indexes of Cu, Co, Cr, Mn, Ni, Pb and the like, the total content of the impurities 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 150ppm, the BaO content is 46 +/-0.5 percent, and P2O5The content is 43 plus or minus 0.5 percent.
In conclusion, the barium dihydrogen phosphate prepared by the preparation method disclosed by the invention is high in main content, low in impurity content, stable in quality and uniform in granularity, all indexes meet the index requirements of raw materials of optical glass and laser glass, and the preparation method disclosed by the invention is efficient, simple and convenient, low in production cost and suitable for large-scale production.
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 (10)
1. A preparation method of optical grade barium dihydrogen phosphate is characterized by comprising the following steps:
(1) reacting barium hydroxide, phosphoric acid and water according to a certain proportion to obtain a crude barium dihydrogen phosphate solution;
(2) adjusting the concentration of the crude barium dihydrogen phosphate solution, and passing through cation exchange resin and anion exchange resin at a certain flow rate to remove nonferrous metals and impurity ions;
(3) dehydrating after ion exchange to obtain barium dihydrogen phosphate intermediate powder;
(4) drying the barium dihydrogen phosphate intermediate powder to obtain the optical grade barium dihydrogen phosphate powder.
2. The method for preparing optical grade barium dihydrogen phosphate according to claim 1, wherein in step (1), the molar ratio of barium hydroxide to phosphoric acid is 1 (1.97-2.03), the mass ratio of phosphoric acid to water is 1 (2.6-4.2), the reaction temperature is 120-140 ℃, the reaction pressure is 0.25-0.5 MPa, and the reaction time is 3-8 h.
3. The method for preparing optical grade barium dihydrogen phosphate according to claim 1, wherein in step (1), the concentration of the crude barium dihydrogen phosphate is 8% to 17%.
4. The method for preparing optical grade barium dihydrogen phosphate according to claim 1, wherein in step (2), the concentration of the crude barium dihydrogen phosphate solution is adjusted to 10% to 15%.
5. The method of claim 1, wherein the cation exchange resin comprises one or more of 001 × 7, 001 × 4, 732, 741, D001, and IONESIN IR120, and the anion exchange resin comprises one or more of D201, D202, D407, 201 × 7, and 201 × 4.
6. The process for preparing optical grade barium dihydrogen phosphate according to claim 1, wherein in step (2), the flow rate is 1L/min to 5L/min.
7. The process for preparing optical grade barium dihydrogen phosphate according to claim 1,characterized in that the non-ferrous metal comprises at least one of Fe, Mn, Pb, Cr, Cu, Ni and Co, and the impurity ions comprise Cl－And/or SO4 2-。
8. The method for preparing optical grade barium dihydrogen phosphate according to claim 1, wherein in step (3), the barium dihydrogen phosphate solution is dehydrated by feeding it into a spray drying tower at a flow rate of 5L/min to 13L/min, the inlet air temperature of the spray drying tower is 180 ℃ to 210 ℃, the tower body temperature is 150 ℃ to 180 ℃, and the outlet air temperature is 125 ℃ to 150 ℃.
9. The method for preparing optical grade barium dihydrogen phosphate according to claim 1, wherein in step (4), the intermediate powder of optical grade barium dihydrogen phosphate is dried by a high efficiency boiling dryer, wherein the inlet air temperature is 160 ℃ to 185 ℃, the tower body temperature is 140 ℃ to 160 ℃, the outlet air temperature is 115 ℃ to 135 ℃, and the drying time is 1.5h to 4 h.
10. The method of claim 9, wherein the material contact portion of the high efficiency boiling dryer is lined with pure aluminum or pure titanium and polished, and the intake air is purified in multiple stages.
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| 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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