CN107500261B - Aluminum metaphosphate powder for optical glass and preparation method thereof - Google Patents
Aluminum metaphosphate powder for optical glass and preparation method thereof Download PDFInfo
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- CN107500261B CN107500261B CN201710729598.1A CN201710729598A CN107500261B CN 107500261 B CN107500261 B CN 107500261B CN 201710729598 A CN201710729598 A CN 201710729598A CN 107500261 B CN107500261 B CN 107500261B
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- aluminum
- acid
- mixed solution
- optical glass
- metaphosphate powder
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- DHAHRLDIUIPTCJ-UHFFFAOYSA-K aluminium metaphosphate Chemical compound [Al+3].[O-]P(=O)=O.[O-]P(=O)=O.[O-]P(=O)=O DHAHRLDIUIPTCJ-UHFFFAOYSA-K 0.000 title claims abstract description 74
- 239000000843 powder Substances 0.000 title claims abstract description 49
- 239000005304 optical glass Substances 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 11
- 239000011259 mixed solution Substances 0.000 claims description 72
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 38
- 239000000203 mixture Substances 0.000 claims description 32
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 29
- 239000002243 precursor Substances 0.000 claims description 29
- 238000004519 manufacturing process Methods 0.000 claims description 20
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 19
- 229910052751 metal Inorganic materials 0.000 claims description 19
- 239000002184 metal Substances 0.000 claims description 19
- WVDDGKGOMKODPV-UHFFFAOYSA-N Benzyl alcohol Chemical compound OCC1=CC=CC=C1 WVDDGKGOMKODPV-UHFFFAOYSA-N 0.000 claims description 18
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 18
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 18
- 229910052782 aluminium Inorganic materials 0.000 claims description 18
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 16
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- 238000001035 drying Methods 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 14
- 238000006116 polymerization reaction Methods 0.000 claims description 14
- 238000000227 grinding Methods 0.000 claims description 13
- 239000002245 particle Substances 0.000 claims description 13
- 238000007873 sieving Methods 0.000 claims description 13
- 239000002904 solvent Substances 0.000 claims description 13
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 12
- 230000032683 aging Effects 0.000 claims description 12
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 12
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 11
- 239000011574 phosphorus Substances 0.000 claims description 11
- 229910052698 phosphorus Inorganic materials 0.000 claims description 11
- PPQREHKVAOVYBT-UHFFFAOYSA-H dialuminum;tricarbonate Chemical compound [Al+3].[Al+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O PPQREHKVAOVYBT-UHFFFAOYSA-H 0.000 claims description 10
- DLYUQMMRRRQYAE-UHFFFAOYSA-N tetraphosphorus decaoxide Chemical compound O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 claims description 10
- 239000002738 chelating agent Substances 0.000 claims description 9
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 8
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 8
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 8
- XHXFXVLFKHQFAL-UHFFFAOYSA-N phosphoryl trichloride Chemical compound ClP(Cl)(Cl)=O XHXFXVLFKHQFAL-UHFFFAOYSA-N 0.000 claims description 8
- LWIHDJKSTIGBAC-UHFFFAOYSA-K tripotassium phosphate Chemical compound [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 claims description 8
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 6
- 235000019445 benzyl alcohol Nutrition 0.000 claims description 6
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 6
- RGHNJXZEOKUKBD-SQOUGZDYSA-N D-gluconic acid Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C(O)=O RGHNJXZEOKUKBD-SQOUGZDYSA-N 0.000 claims description 5
- 229940118662 aluminum carbonate Drugs 0.000 claims description 5
- BAERPNBPLZWCES-UHFFFAOYSA-N (2-hydroxy-1-phosphonoethyl)phosphonic acid Chemical compound OCC(P(O)(O)=O)P(O)(O)=O BAERPNBPLZWCES-UHFFFAOYSA-N 0.000 claims description 4
- 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 claims description 4
- URDCARMUOSMFFI-UHFFFAOYSA-N 2-[2-[bis(carboxymethyl)amino]ethyl-(2-hydroxyethyl)amino]acetic acid Chemical compound OCCN(CC(O)=O)CCN(CC(O)=O)CC(O)=O URDCARMUOSMFFI-UHFFFAOYSA-N 0.000 claims description 4
- ZUGAOYSWHHGDJY-UHFFFAOYSA-K 5-hydroxy-2,8,9-trioxa-1-aluminabicyclo[3.3.2]decane-3,7,10-trione Chemical compound [Al+3].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O ZUGAOYSWHHGDJY-UHFFFAOYSA-K 0.000 claims description 4
- QPCDCPDFJACHGM-UHFFFAOYSA-N N,N-bis{2-[bis(carboxymethyl)amino]ethyl}glycine Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(=O)O)CCN(CC(O)=O)CC(O)=O QPCDCPDFJACHGM-UHFFFAOYSA-N 0.000 claims description 4
- 229920002125 Sokalan® Polymers 0.000 claims description 4
- HDYRYUINDGQKMC-UHFFFAOYSA-M acetyloxyaluminum;dihydrate Chemical compound O.O.CC(=O)O[Al] HDYRYUINDGQKMC-UHFFFAOYSA-M 0.000 claims description 4
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 claims description 4
- 229940009827 aluminum acetate Drugs 0.000 claims description 4
- -1 aluminum ethylenediamine tetraacetic acid Chemical compound 0.000 claims description 4
- 239000001506 calcium phosphate Substances 0.000 claims description 4
- 229910000389 calcium phosphate Inorganic materials 0.000 claims description 4
- 235000011010 calcium phosphates Nutrition 0.000 claims description 4
- 229960001484 edetic acid Drugs 0.000 claims description 4
- 229910001386 lithium phosphate Inorganic materials 0.000 claims description 4
- MGFYIUFZLHCRTH-UHFFFAOYSA-N nitrilotriacetic acid Chemical compound OC(=O)CN(CC(O)=O)CC(O)=O MGFYIUFZLHCRTH-UHFFFAOYSA-N 0.000 claims description 4
- 229960003330 pentetic acid Drugs 0.000 claims description 4
- FAIAAWCVCHQXDN-UHFFFAOYSA-N phosphorus trichloride Chemical compound ClP(Cl)Cl FAIAAWCVCHQXDN-UHFFFAOYSA-N 0.000 claims description 4
- 239000004584 polyacrylic acid Substances 0.000 claims description 4
- 229910000160 potassium phosphate Inorganic materials 0.000 claims description 4
- 235000011009 potassium phosphates Nutrition 0.000 claims description 4
- 239000001488 sodium phosphate Substances 0.000 claims description 4
- 229910000162 sodium phosphate Inorganic materials 0.000 claims description 4
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 claims description 4
- TWQULNDIKKJZPH-UHFFFAOYSA-K trilithium;phosphate Chemical compound [Li+].[Li+].[Li+].[O-]P([O-])([O-])=O TWQULNDIKKJZPH-UHFFFAOYSA-K 0.000 claims description 4
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 4
- WJQZZLQMLJPKQH-UHFFFAOYSA-N 2,4-dichloro-6-methylphenol Chemical compound CC1=CC(Cl)=CC(Cl)=C1O WJQZZLQMLJPKQH-UHFFFAOYSA-N 0.000 claims description 3
- 229910000505 Al2TiO5 Inorganic materials 0.000 claims description 3
- 239000004254 Ammonium phosphate Substances 0.000 claims description 3
- RGHNJXZEOKUKBD-UHFFFAOYSA-N D-gluconic acid Natural products OCC(O)C(O)C(O)C(O)C(O)=O RGHNJXZEOKUKBD-UHFFFAOYSA-N 0.000 claims description 3
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 3
- 229920002253 Tannate Polymers 0.000 claims description 3
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 3
- MTEWCUZXTGXLQX-AHUNZLEGSA-H [Al+3].[Al+3].[O-]C(=O)\C=C/C([O-])=O.[O-]C(=O)\C=C/C([O-])=O.[O-]C(=O)\C=C/C([O-])=O Chemical compound [Al+3].[Al+3].[O-]C(=O)\C=C/C([O-])=O.[O-]C(=O)\C=C/C([O-])=O.[O-]C(=O)\C=C/C([O-])=O MTEWCUZXTGXLQX-AHUNZLEGSA-H 0.000 claims description 3
- MJWPFSQVORELDX-UHFFFAOYSA-K aluminium formate Chemical compound [Al+3].[O-]C=O.[O-]C=O.[O-]C=O MJWPFSQVORELDX-UHFFFAOYSA-K 0.000 claims description 3
- 229910000148 ammonium phosphate Inorganic materials 0.000 claims description 3
- 235000019289 ammonium phosphates Nutrition 0.000 claims description 3
- ZCLVNIZJEKLGFA-UHFFFAOYSA-H bis(4,5-dioxo-1,3,2-dioxalumolan-2-yl) oxalate Chemical compound [Al+3].[Al+3].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O ZCLVNIZJEKLGFA-UHFFFAOYSA-H 0.000 claims description 3
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 claims description 3
- 239000000174 gluconic acid Substances 0.000 claims description 3
- 235000012208 gluconic acid Nutrition 0.000 claims description 3
- GVALZJMUIHGIMD-UHFFFAOYSA-H magnesium phosphate Chemical compound [Mg+2].[Mg+2].[Mg+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O GVALZJMUIHGIMD-UHFFFAOYSA-H 0.000 claims description 3
- 239000004137 magnesium phosphate Substances 0.000 claims description 3
- 229910000157 magnesium phosphate Inorganic materials 0.000 claims description 3
- 229960002261 magnesium phosphate Drugs 0.000 claims description 3
- 235000010994 magnesium phosphates Nutrition 0.000 claims description 3
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 claims description 3
- 239000011976 maleic acid Substances 0.000 claims description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 3
- 235000011007 phosphoric acid Nutrition 0.000 claims description 3
- 230000000379 polymerizing effect Effects 0.000 claims description 3
- AABBHSMFGKYLKE-SNAWJCMRSA-N propan-2-yl (e)-but-2-enoate Chemical compound C\C=C\C(=O)OC(C)C AABBHSMFGKYLKE-SNAWJCMRSA-N 0.000 claims description 3
- 235000011008 sodium phosphates Nutrition 0.000 claims description 3
- 239000011975 tartaric acid Substances 0.000 claims description 3
- 235000002906 tartaric acid Nutrition 0.000 claims description 3
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 claims description 3
- JOPDZQBPOWAEHC-UHFFFAOYSA-H tristrontium;diphosphate Chemical compound [Sr+2].[Sr+2].[Sr+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O JOPDZQBPOWAEHC-UHFFFAOYSA-H 0.000 claims description 3
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 2
- 229910019142 PO4 Inorganic materials 0.000 claims description 2
- MAQCMFOLVVSLLK-UHFFFAOYSA-N methyl 4-(bromomethyl)pyridine-2-carboxylate Chemical compound COC(=O)C1=CC(CBr)=CC=N1 MAQCMFOLVVSLLK-UHFFFAOYSA-N 0.000 claims description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 2
- 239000010452 phosphate Substances 0.000 claims description 2
- 238000003980 solgel method Methods 0.000 claims description 2
- BDOYKFSQFYNPKF-UHFFFAOYSA-N 2-[2-[bis(carboxymethyl)amino]ethyl-(carboxymethyl)amino]acetic acid;sodium Chemical compound [Na].[Na].OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O BDOYKFSQFYNPKF-UHFFFAOYSA-N 0.000 claims 1
- 238000012216 screening Methods 0.000 claims 1
- 230000008569 process Effects 0.000 abstract description 3
- 239000012535 impurity Substances 0.000 description 12
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 10
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 10
- 238000006243 chemical reaction Methods 0.000 description 8
- 239000002994 raw material Substances 0.000 description 8
- 239000011521 glass Substances 0.000 description 7
- 239000000126 substance Substances 0.000 description 7
- 238000010438 heat treatment Methods 0.000 description 6
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 5
- 229910052804 chromium Inorganic materials 0.000 description 5
- 239000011651 chromium Substances 0.000 description 5
- 229910052802 copper Inorganic materials 0.000 description 5
- 239000010949 copper Substances 0.000 description 5
- 229910052742 iron Inorganic materials 0.000 description 5
- 229910052759 nickel Inorganic materials 0.000 description 5
- 229910017052 cobalt Inorganic materials 0.000 description 4
- 239000010941 cobalt Substances 0.000 description 4
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 4
- 150000002739 metals Chemical class 0.000 description 4
- 238000001514 detection method Methods 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 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 3
- 239000003109 Disodium ethylene diamine tetraacetate Substances 0.000 description 2
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 235000019301 disodium ethylene diamine tetraacetate Nutrition 0.000 description 2
- 239000005303 fluorophosphate glass Substances 0.000 description 2
- 230000004927 fusion Effects 0.000 description 2
- 229910052748 manganese Inorganic materials 0.000 description 2
- 239000011572 manganese Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 239000005365 phosphate glass Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- BAWFMRPQYKKOLX-UHFFFAOYSA-B tetraaluminum;2-[2-[bis(carboxylatomethyl)amino]ethyl-(carboxylatomethyl)amino]acetate Chemical compound [Al+3].[Al+3].[Al+3].[Al+3].[O-]C(=O)CN(CC([O-])=O)CCN(CC([O-])=O)CC([O-])=O.[O-]C(=O)CN(CC([O-])=O)CCN(CC([O-])=O)CC([O-])=O.[O-]C(=O)CN(CC([O-])=O)CCN(CC([O-])=O)CC([O-])=O BAWFMRPQYKKOLX-UHFFFAOYSA-B 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 229920000180 alkyd Polymers 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000013522 chelant Substances 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000001066 destructive effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- RGPUVZXXZFNFBF-UHFFFAOYSA-K diphosphonooxyalumanyl dihydrogen phosphate Chemical compound [Al+3].OP(O)([O-])=O.OP(O)([O-])=O.OP(O)([O-])=O RGPUVZXXZFNFBF-UHFFFAOYSA-K 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000000087 laser glass Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- WVDDGKGOMKODPV-ZQBYOMGUSA-N phenyl(114C)methanol Chemical compound O[14CH2]C1=CC=CC=C1 WVDDGKGOMKODPV-ZQBYOMGUSA-N 0.000 description 1
- 229920000137 polyphosphoric acid Polymers 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000011895 specific detection Methods 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 229910001428 transition metal ion Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
Abstract
The invention discloses aluminum metaphosphate powder for optical glass and a preparation method thereof. The invention has the advantages of simple process, compact steps, less investment, low cost and popularization significance.
Description
Technical Field
The invention belongs to the field of chemistry, and particularly relates to aluminum metaphosphate powder for optical glass and a preparation method thereof.
Background
In the last 90 s of the last century, the Japanese Imperial chemical company first produced aluminum metaphosphate of K-90 as the basic model and K-WHITE94 as the modified model, which was originally used in the anticorrosion field, for example, for manufacturing alkyd anticorrosive paint, and has excellent protection for steel. The british name for aluminum metaphosphate is aluminum metaphosphate, and its chemical formula is Al (PO)3)3. After decades of development, aluminum metaphosphate is applied as a raw material for producing special optical glass, phosphate glass, fluorophosphate glass and laser nuclear fusion glass. The optical glass made of the aluminum metaphosphate has good moisture resistance, low refractive index, large Abbe number, low ultraviolet partial dispersion, and high chemical stability and mechanical strength. The invention discloses a temperature-control step-by-step conversion method for producing electronic-grade aluminum metaphosphate, application number 201110252987.2, which discloses a temperature-control step-by-step conversion method for producing electronic-grade aluminum metaphosphate, comprising the following steps: adding water and phosphoric acid in a weight ratio of 1:1 into a reaction kettle; slowly adding aluminum hydroxide after the reaction is completed, wherein the weight ratio of the added aluminum hydroxide to the phosphoric acid is 1: 2; putting the generated aluminum dihydrogen phosphate into a box, placing the box in a heating furnace, and sealing the heating furnace; heating the heating furnace, and exhausting air to enable the interior of the heating furnace to be in a negative pressure state; and (3) roasting the heating furnace at three steps of temperature control to obtain the high-purity aluminum metaphosphate, taking out the high-purity aluminum metaphosphate, and cooling the aluminum metaphosphate at room temperature. By controlling different temperatures for phosphoric acidThe aluminum dihydrogen is converted step by step to prepare the high-purity electronic grade aluminum metaphosphate, and the method has the characteristics of simple and clear operation steps, high stability and safety of industrial process operation, high purity of the produced aluminum metaphosphate, low production cost, realization of batch production and the like. The invention relates to a high-purity aluminum metaphosphate and a manufacturing method thereof, and the application number is as follows: 200710108995.3, discloses a method for producing high purity aluminum metaphosphate, wherein the high purity aluminum metaphosphate has an impurity concentration of 5ppm or less of each metal element, which is at least one of iron, chromium, nickel, manganese or copper, and the mixture obtained by mixing alumina, aluminum hydroxide or aluminum carbonate with phosphoric anhydride and polyphosphoric acid is placed in a sintering vessel previously coated with aluminum metaphosphate powder and sintered.
An optical glass is a glass that can change the direction of light propagation and can change the relative spectral distribution of ultraviolet, visible, or infrared light. The optical glass in a narrow sense refers to colorless optical glass, and the optical glass in a broad sense also includes colored optical glass, laser glass, quartz optical glass, radiation-resistant glass, ultraviolet infrared optical glass, fiber optical glass, acousto-optic glass, magneto-optic glass and photochromic glass. The optical glass can be used for manufacturing lenses, prisms, reflectors, windows and the like in optical instruments. Components made of optical glass are critical elements in optical instruments. The aluminum metaphosphate for optical glass has strict requirements on the content of impurity metals, for example, iron, chromium, nickel, manganese, copper, cobalt and other transition metal ions contain unpaired electrons, so that the aluminum metaphosphate has abundant colors due to energy transition and has destructive influence on the performance of the aluminum metaphosphate optical glass. In the actual production process, the raw materials and the high-temperature reaction device can also bring impurity metals. In order to obtain the aluminum metaphosphate with low content of impurity metal and high purity, the method adopted by the prior art uses high-purity raw materials and a high-temperature reaction device without introducing the impurity metal, has strict requirements on the raw materials, the process and equipment, is difficult to control and has high production cost. In the prior art, no report that a metal chelating agent is used for removing metal impurities and achieving a good effect in the production of aluminum metaphosphate is found, and no report that a sol-gel-polymerization method is adopted for obtaining high-purity aluminum metaphosphate is found.
Disclosure of Invention
The invention aims to provide aluminum metaphosphate powder for optical glass and a preparation method thereof.
In order to achieve the purpose, the technical scheme of the invention is as follows:
the aluminum metaphosphate powder for optical glass is prepared by dissolving an aluminum source in an alcohol solvent I, dissolving a phosphorus source in an alcohol solvent II, preparing a precursor by a sol-gel method, and polymerizing at high temperature.
Further, the preparation method of the aluminum metaphosphate powder for optical glass comprises the following steps:
A. dissolving an aluminum source in an alcohol solvent I to obtain a mixed solution A, and dissolving a phosphorus source in an alcohol solvent II to obtain a mixed solution B;
B. respectively adding a metal chelating agent into the mixed solution A and the mixed solution B, uniformly mixing the mixed solution A and the mixed solution B, adding phosphoric acid to adjust the pH value of a system to be 0.5-5 to obtain semitransparent sol, and aging and separating to obtain gel;
C. drying, grinding and sieving the gel to obtain a precursor;
D. and carrying out polymerization reaction on the precursor at the temperature of 200-1000 ℃ for 0.5-8 hours to obtain aluminum metaphosphate powder.
Preferably, the aluminum source is one or a mixture of two or more of aluminum hydroxide, aluminum oxide, aluminum carbonate, aluminum nitrate, aluminum sulfate, aluminum chloride, aluminum oleate, aluminum formate, aluminum acetate, aluminum citrate, aluminum ethylenediaminetetraacetate, aluminum tartrate, aluminum tannate, aluminum amino acid, aluminum titanate, aluminum oxalate and aluminum maleate.
More preferably, the aluminum source is one or a mixture of two or more of aluminum hydroxide, aluminum oxide, aluminum carbonate, aluminum sulfate and aluminum chloride.
Preferably, the phosphorus source is one or a mixture of more than two of phosphorus pentoxide, phosphorus trichloride, phosphoric acid, sodium phosphate, ammonium phosphate, potassium phosphate, calcium phosphate, magnesium phosphate, lithium phosphate, strontium phosphate, phosphate and phosphorus oxychloride.
Further preferably, the phosphorus source is one or a mixture of more than two of phosphoric acid, sodium phosphate, ammonium phosphate and potassium phosphate.
Preferably, the alcohol solvent I or the alcohol solvent II is one or a mixture of more than two of methanol, ethanol, propanol, butanol, ethylene glycol, propylene glycol, glycerol and benzyl alcohol.
More preferably, the alcohol solvent I or the alcohol solvent II is one or a mixture of more than two of methanol, ethanol, propanol and benzyl alcohol.
Preferably, the metal chelating agent is one or a mixture of more than two of ethylenediamine tetraacetic acid, disodium ethylenediamine tetraacetic acid, nitrilotriacetic acid, diethylenetriamine pentaacetic acid, citric acid, tartaric acid, maleic acid, gluconic acid, hydroxyethyl ethylenediamine triacetic acid, hydroxyethylidene diphosphonic acid and polyacrylic acid.
More preferably, the metal chelating agent is one or a mixture of more than two of ethylenediamine tetraacetic acid, disodium ethylenediamine tetraacetic acid, citric acid and hydroxyethylidene diphosphonic acid.
Preferably, the mass ratio of the aluminum source to the phosphorus source is 1:9-9: 1.
Preferably, the addition amount of the metal chelating agent is 0.01-2% of the total mass of the phosphorus source and the aluminum source.
Preferably, the gel drying in the step C is carried out under a constant temperature condition, and the temperature is 50-200 ℃.
Preferably, in the step C, the xerogel is ground and sieved, and powder with the particle size of 2-50 μm is screened out, so as to obtain the precursor.
The invention has the beneficial effects that:
the method synthesizes the aluminum metaphosphate by using a sol-gel-polymerization method, and adopts a metal chelating agent for pretreatment to chelate impurity metals without participating in the reaction, so that harmful impurity metals introduced by raw materials and equipment are greatly reduced, the purity of the aluminum metaphosphate is improved, and the defects of the prior art are overcome. The aluminum metaphosphate obtained by the method has low metal content of impurities, wherein the transition metal element: the contents of iron, chromium, nickel, manganese, copper and cobalt are all lower than 3ppm, and the impurity removal rate from the raw materials to the products is more than 90%; the product purity is high, and the particles are uniformly distributed; the aluminum metaphosphate obtained by the method is applied to the production of optical glass such as phosphate glass, fluorophosphate glass, laser nuclear fusion glass and the like, and good performance is obtained.
Detailed Description
The present invention will be described in detail below with reference to specific examples.
Example 1
The preparation method of the aluminum metaphosphate powder for the optical glass comprises the following steps:
A. preparing a mixture of 5kg of aluminum nitrate, 10kg of butanol and 10kg of propylene glycol into a mixed solution A, and preparing a mixture of 5kg of sodium phosphate, 10kg of ethanol and 10kg of benzyl alcohol into a mixed solution B;
B. respectively adding a mixture of 0.02kg of citric acid and 0.03kg of maleic acid into the mixed solution A and the mixed solution B, uniformly mixing the mixed solution A and the mixed solution B, simultaneously dropwise adding phosphoric acid to adjust the pH value of a system to be 4.0 to obtain semitransparent sol, and aging and separating to obtain gel;
C. drying the gel at a constant temperature of 150 ℃ to obtain dry gel, grinding and sieving the dry gel, and collecting a part with the particle size of 2-5 mu m as a precursor; and carrying out polymerization reaction on the precursor at 800 ℃ for 5 hours to obtain aluminum metaphosphate powder.
Example 2
The preparation method of the aluminum metaphosphate powder for the optical glass comprises the following steps:
A. preparing a mixture of 5kg of aluminum hydroxide and 5kg of aluminum ethylene diamine tetraacetate, a mixture of 20kg of propanol and 30kg of glycerol into a mixed solution A, and preparing a mixture of 0.5kg of phosphoric acid and 0.5kg of phosphorus oxychloride and 50kg of ethylene glycol into a mixed solution B;
B. respectively adding 0.08kg of hydroxyethylidene diphosphonic acid into the mixed solution A and the mixed solution B, then uniformly mixing the mixed solution A and the mixed solution B, simultaneously dropwise adding phosphoric acid to adjust the pH value of a system to be 5.0 to obtain semitransparent sol, and aging and separating to obtain gel;
C. drying the gel at a constant temperature of 50 ℃ to obtain dry gel, grinding and sieving the dry gel, and collecting a part with the particle size of 3-12 mu m as a precursor; and carrying out polymerization reaction on the precursor at the temperature of 200 ℃ for 8 hours to obtain aluminum metaphosphate powder.
Example 3
The preparation method of the aluminum metaphosphate powder for the optical glass comprises the following steps:
A. preparing a mixed solution A from a mixture of 5kg of aluminum carbonate and 5kg of aluminum nitrate, 10kg of propylene glycol and 10kg of glycerol, and preparing a mixed solution B from a mixture of 5kg of calcium phosphate and 5kg of magnesium phosphate and 20kg of ethylene glycol;
B. respectively adding a mixture of 0.02kg of tartaric acid and 0.03kg of diethylenetriaminepentaacetic acid into the mixed solution A and the mixed solution B, uniformly mixing the mixed solution A and the mixed solution B, simultaneously dropwise adding phosphoric acid to adjust the pH value of a system to be 2.5 to obtain semitransparent sol, and aging and separating to obtain gel;
C. drying the gel at a constant temperature of 150 ℃ to obtain dry gel, grinding and sieving the dry gel, and collecting a part with the particle size of 10-30 mu m as a precursor; and carrying out polymerization reaction on the precursor at 800 ℃ for 5 hours to obtain aluminum metaphosphate powder.
Example 4
The preparation method of the aluminum metaphosphate powder for the optical glass comprises the following steps:
A. preparing a mixed solution A from a mixture of 8kg of aluminum tannate and 3kg of amino acid aluminum and 30kg of ethanol, and preparing a mixed solution B from a mixture of 6kg of phosphorus trichloride, 10kg of methanol, 5kg of ethylene glycol and 5kg of benzyl alcohol;
B. respectively adding a mixture of 0.05kg of disodium ethylene diamine tetraacetate, 0.02kg of gluconic acid and 0.05kg of nitrilotriacetic acid into the mixed solution A and the mixed solution B, uniformly mixing the mixed solution A and the mixed solution B, simultaneously dropwise adding phosphoric acid to adjust the pH value of a system to be 0.5 to obtain semitransparent sol, and aging and separating to obtain gel;
C. drying the gel at a constant temperature of 80 ℃ to obtain dry gel, grinding and sieving the dry gel, and collecting a part with the particle size of 40-50 mu m as a precursor; and carrying out polymerization reaction on the precursor at 1000 ℃ for 0.5 hour to obtain aluminum metaphosphate powder.
Example 5
The preparation method of the aluminum metaphosphate powder for the optical glass comprises the following steps:
A. preparing a mixture of 3kg of aluminum formate, 3kg of aluminum acetate and 3kg of aluminum citrate and 26kg of propanol into a mixed solution A, and preparing a mixture of 3kg of phosphorus pentoxide, 2kg of phosphorus trichloride and 2kg of calcium phosphate and 37kg of benzyl alcohol into a mixed solution B;
B. respectively adding a mixture of 0.1kg of nitrilotriacetic acid and 0.01kg of polyacrylic acid into the mixed solution A and the mixed solution B, then uniformly mixing the mixed solution A and the mixed solution B, simultaneously dropwise adding phosphoric acid to adjust the pH value of a system to be 3.5 to obtain semitransparent sol, and aging and separating to obtain gel;
C. drying the gel at a constant temperature of 110 ℃ to obtain dry gel, grinding and sieving the dry gel, and collecting a part with a particle size of 25-35 mu m as a precursor; and carrying out polymerization reaction on the precursor at 900 ℃ for 7 hours to obtain aluminum metaphosphate powder.
Example 6
The preparation method of the aluminum metaphosphate powder for the optical glass comprises the following steps:
A. preparing 6kg of aluminum sulfate and 25kg of glycerol into a mixed solution A, and preparing a mixture of 0.5kg of lithium phosphate and 0.5kg of strontium phosphate and 30kg of ethanol into a mixed solution B;
B. respectively adding a mixture of 0.005kg of polyacrylic acid and 0.005kg of hydroxyethyl ethylenediamine triacetic acid into the mixed solution A and the mixed solution B, then uniformly mixing the mixed solution A and the mixed solution B, simultaneously dropwise adding phosphoric acid to adjust the pH value of a system to be 1.5 to obtain semitransparent sol, and aging and separating to obtain gel;
C. drying the gel at constant temperature of 120 ℃ to obtain dry gel, grinding and sieving the dry gel, and collecting a part with the particle size of 30-42 mu m as a precursor; and carrying out polymerization reaction on the precursor at 500 ℃ for 6.5 hours to obtain aluminum metaphosphate powder.
Example 7
The preparation method of the aluminum metaphosphate powder for the optical glass comprises the following steps:
A. preparing 8kg of alumina and 12kg of ethanol into a mixed solution A, and preparing 8kg of phosphorus pentoxide and 16kg of ethylene glycol into a mixed solution B;
B. respectively adding 0.03kg of diethylenetriaminepentaacetic acid into the mixed solution A and the mixed solution B, then uniformly mixing the mixed solution A and the mixed solution B, simultaneously dropwise adding phosphoric acid to adjust the pH value of a system to be 4.5 to obtain semitransparent sol, and aging and separating to obtain gel;
C. drying the gel at a constant temperature of 70 ℃ to obtain dry gel, grinding and sieving the dry gel, and collecting a part with a particle size of 5-12 mu m as a precursor; and carrying out polymerization reaction on the precursor at 750 ℃ for 4.5 hours to obtain aluminum metaphosphate powder.
Example 8
The preparation method of the aluminum metaphosphate powder for the optical glass comprises the following steps:
A. preparing a mixed solution A from a mixture of 6kg of aluminum tartrate and 1kg of aluminum maleate and 18kg of propanol, and preparing a mixed solution B from 3kg of lithium phosphate and 22kg of ethanol;
B. respectively adding 0.0003kg of ethylene diamine tetraacetic acid into the mixed solution A and the mixed solution B, then uniformly mixing the mixed solution A and the mixed solution B, simultaneously dropwise adding phosphoric acid to adjust the pH value of a system to be 2.0 to obtain semitransparent sol, and aging and separating to obtain gel;
C. drying the gel at a constant temperature of 180 ℃ to obtain dry gel, grinding and sieving the dry gel, and collecting a part with a particle size of 10-18 mu m as a precursor; and carrying out polymerization reaction on the precursor at 400 ℃ for 3.5 hours to obtain aluminum metaphosphate powder.
Example 9
The preparation method of the aluminum metaphosphate powder for the optical glass comprises the following steps:
A. preparing a mixed solution A from a mixture of 9kg of aluminum titanate and 1kg of aluminum oxalate and 33kg of benzyl alcohol, and preparing a mixed solution B from 6kg of potassium phosphate and 15kg of methanol;
B. respectively adding 0.009kg of disodium ethylene diamine tetraacetate into the mixed solution A and the mixed solution B, then uniformly mixing the mixed solution A and the mixed solution B, simultaneously dropwise adding phosphoric acid to adjust the pH value of a system to be 3.7 to obtain semitransparent sol, and aging and separating to obtain gel;
C. drying the gel at a constant temperature of 165 ℃ to obtain dry gel, grinding and sieving the dry gel, and collecting a part with a particle size of 15-25 mu m as a precursor; and carrying out polymerization reaction on the precursor at 250 ℃ for 7 hours to obtain aluminum metaphosphate powder.
Example 10
The preparation method of the aluminum metaphosphate powder for the optical glass comprises the following steps:
A. preparing a mixed solution A from a mixture of 3kg of aluminum citrate and 1kg of aluminum acetate and 13kg of glycerol, and preparing a mixed solution B from 7kg of phosphorus oxychloride and 23kg of butanol;
B. respectively adding 0.0008kg of hydroxyethyl ethylene diamine triacetic acid into the mixed solution A and the mixed solution B, then uniformly mixing the mixed solution A and the mixed solution B, simultaneously dropwise adding phosphoric acid to adjust the pH value of a system to be 4.2 to obtain semitransparent sol, and aging and separating to obtain gel;
C. drying the gel at a constant temperature of 105 ℃ to obtain dry gel, grinding and sieving the dry gel, and collecting a part with the particle size of 33-48 mu m as a precursor; and carrying out polymerization reaction on the precursor at 950 ℃ for 3 hours to obtain aluminum metaphosphate powder.
Example 11
The comparative test analysis of the aluminum metaphosphate powder prepared in example 5 and the aluminum metaphosphate powder prepared by the conventional method is carried out, and the specific process is as follows:
1 course of the experiment
1.1 Experimental materials
Control group: mixing phosphoric acid and aluminum hydroxide for reaction, polymerizing at high temperature, and crushing to obtain aluminum metaphosphate powder.
Experimental groups: the aluminum metaphosphate powder prepared in example 5 of the present invention.
1.2 analysis of the physical and chemical Properties of aluminum metaphosphate
And (4) detecting chemical components by using a flame atomic absorption instrument.
Results and discussion
2.1 detection of the physical and chemical Properties of aluminum metaphosphate
The chemical component detection indexes of the aluminum metaphosphate powder comprise the detection of the contents of iron, chromium, nickel, manganese, copper and cobalt, and the specific detection results are shown in table 1:
table 1 impurity metal content and removal rate of aluminum metaphosphate powder obtained by the present invention:
| sample (I) | Iron content | Chromium content | Nickel content | Manganese content | Copper content | Cobalt content |
| Raw materials (control group) | 500ppm | 20ppm | 20ppm | 100ppm | 100ppm | 20ppm |
| Raw materials (experiment group) | 500ppm | 20ppm | 20ppm | 100ppm | 100ppm | 20ppm |
| Product (control group) | 465ppm | 17ppm | 19ppm | 95ppm | 92ppm | 19ppm |
| Product (experiment group) | 2ppm | 1ppm | 2ppm | 2ppm | 2ppm | 1ppm |
| Removal Rate (control group) | 7% | 15% | 5% | 5% | 8% | 5% |
| Removal Rate (Experimental group) | 99.6% | 95% | 90% | 98% | 98% | 95% |
As can be seen from table 1, the removal rate of impurities in the aluminum metaphosphate powder of the present invention is significantly improved compared to the aluminum metaphosphate powder prepared by the conventional method of the control group.
Although the invention has been described in detail hereinabove with respect to a general description, specific embodiments and tests related thereto, it will be apparent to those skilled in the art that modifications and improvements can be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (9)
1. A preparation method of aluminum metaphosphate powder for optical glass is characterized by comprising the following steps: dissolving an aluminum source in an alcohol solvent I, dissolving a phosphorus source in an alcohol solvent II, preparing a precursor by adopting a sol-gel method, and polymerizing at high temperature to obtain the precursor;
the method comprises the following steps:
A. dissolving an aluminum source in an alcohol solvent I to obtain a mixed solution A, and dissolving a phosphorus source in an alcohol solvent II to obtain a mixed solution B;
B. respectively adding a metal chelating agent into the mixed solution A and the mixed solution B, uniformly mixing the mixed solution A and the mixed solution B, adding phosphoric acid to adjust the pH value of a system to be 0.5-5 to obtain semitransparent sol, and aging and separating to obtain gel;
C. drying, grinding and sieving the gel to obtain a precursor;
D. and carrying out polymerization reaction on the precursor at the temperature of 200-1000 ℃ for 0.5-8 hours to obtain aluminum metaphosphate powder.
2. The method for producing an aluminum metaphosphate powder for optical glass as defined in claim 1, wherein: the aluminum source is one or a mixture of more than two of aluminum hydroxide, aluminum oxide, aluminum carbonate, aluminum nitrate, aluminum sulfate, aluminum chloride, aluminum oleate, aluminum formate, aluminum acetate, aluminum citrate, aluminum ethylenediamine tetraacetic acid, aluminum tartrate, aluminum tannate, aluminum amino acid, aluminum titanate, aluminum oxalate and aluminum maleate.
3. The method for producing an aluminum metaphosphate powder for optical glass as defined in claim 1, wherein: the phosphorus source is one or a mixture of more than two of phosphorus pentoxide, phosphorus trichloride, phosphoric acid, sodium phosphate, ammonium phosphate, potassium phosphate, calcium phosphate, magnesium phosphate, lithium phosphate, strontium phosphate, phosphate and phosphorus oxychloride.
4. The method for producing an aluminum metaphosphate powder for optical glass as defined in claim 1, wherein: the alcohol solvent I or II is one or more of methanol, ethanol, propanol, butanol, ethylene glycol, propylene glycol, glycerol and benzyl alcohol.
5. The method for producing an aluminum metaphosphate powder for optical glass as defined in claim 1, wherein: the metal chelating agent is one or a mixture of more than two of ethylene diamine tetraacetic acid, ethylene diamine tetraacetic acid disodium, nitrilotriacetic acid, diethylene triamine pentaacetic acid, citric acid, tartaric acid, maleic acid, gluconic acid, hydroxyethyl ethylene diamine triacetic acid, hydroxy ethylidene diphosphonic acid and polyacrylic acid.
6. The method for producing an aluminum metaphosphate powder for optical glass according to claim 1, wherein: the mass ratio of the aluminum source to the phosphorus source is 1:9-9: 1.
7. The method for producing an aluminum metaphosphate powder for optical glass as defined in claim 1, wherein: the addition amount of the metal chelating agent is 0.01-2% of the total mass of the phosphorus source and the aluminum source.
8. The method for producing an aluminum metaphosphate powder for optical glass as defined in claim 1, wherein: and C, drying the gel in the step C at a constant temperature of 50-200 ℃.
9. The method for producing an aluminum metaphosphate powder for optical glass as defined in claim 1, wherein: and C, grinding and sieving the xerogel, and screening out powder with the particle size of 2-50 mu m to obtain the precursor.
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| CN109133024B (en) * | 2018-09-30 | 2020-07-03 | 广西新晶科技有限公司 | Magnesium-aluminum metaphosphate powder for optical glass and preparation method thereof |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102336401A (en) * | 2011-09-19 | 2012-02-01 | 南京师范大学 | Preparation method of Fe (PO3)3 with high-purity three-dimensional loose porous structure |
| CN102408103A (en) * | 2011-08-30 | 2012-04-11 | 四川明晶光电科技有限公司 | Temperature control stepwise conversion method of producing electronic grade aluminum metaphosphate |
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| CN102408103A (en) * | 2011-08-30 | 2012-04-11 | 四川明晶光电科技有限公司 | Temperature control stepwise conversion method of producing electronic grade aluminum metaphosphate |
| CN102336401A (en) * | 2011-09-19 | 2012-02-01 | 南京师范大学 | Preparation method of Fe (PO3)3 with high-purity three-dimensional loose porous structure |
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