CN104789213B - A kind of rare-earth terbium complex and preparation method thereof - Google Patents
A kind of rare-earth terbium complex and preparation method thereof Download PDFInfo
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- CN104789213B CN104789213B CN201510192188.9A CN201510192188A CN104789213B CN 104789213 B CN104789213 B CN 104789213B CN 201510192188 A CN201510192188 A CN 201510192188A CN 104789213 B CN104789213 B CN 104789213B
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- terbium
- polar solvent
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- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 79
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 44
- 229910052771 Terbium Inorganic materials 0.000 title claims description 41
- GZCRRIHWUXGPOV-UHFFFAOYSA-N terbium atom Chemical compound [Tb] GZCRRIHWUXGPOV-UHFFFAOYSA-N 0.000 title claims description 37
- 238000002360 preparation method Methods 0.000 title description 5
- 238000010668 complexation reaction Methods 0.000 title description 2
- 238000013329 compounding Methods 0.000 claims abstract description 43
- -1 compound rare earth Chemical class 0.000 claims abstract description 41
- 238000000034 method Methods 0.000 claims abstract description 23
- 239000002798 polar solvent Substances 0.000 claims abstract description 21
- 238000003756 stirring Methods 0.000 claims abstract description 11
- 239000006185 dispersion Substances 0.000 claims abstract description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 58
- 150000001875 compounds Chemical class 0.000 claims description 31
- BSYNRYMUTXBXSQ-UHFFFAOYSA-N Aspirin Chemical compound CC(=O)OC1=CC=CC=C1C(O)=O BSYNRYMUTXBXSQ-UHFFFAOYSA-N 0.000 claims description 25
- 229960001138 acetylsalicylic acid Drugs 0.000 claims description 24
- 239000007787 solid Substances 0.000 claims description 20
- 239000002253 acid Substances 0.000 claims description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 13
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 13
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 12
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical group OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 12
- GFISHBQNVWAVFU-UHFFFAOYSA-K terbium(iii) chloride Chemical compound Cl[Tb](Cl)Cl GFISHBQNVWAVFU-UHFFFAOYSA-K 0.000 claims description 12
- 239000002904 solvent Substances 0.000 claims description 10
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical group OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 8
- 238000002425 crystallisation Methods 0.000 claims description 7
- 230000008025 crystallization Effects 0.000 claims description 7
- 238000000695 excitation spectrum Methods 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 7
- 238000002329 infrared spectrum Methods 0.000 claims description 5
- 239000003638 chemical reducing agent Substances 0.000 claims description 4
- 229960004756 ethanol Drugs 0.000 claims description 4
- 230000005284 excitation Effects 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 229940068372 acetyl salicylate Drugs 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 3
- 238000002189 fluorescence spectrum Methods 0.000 claims description 3
- 238000001228 spectrum Methods 0.000 claims description 3
- 150000001217 Terbium Chemical class 0.000 claims description 2
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical group O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 claims description 2
- 230000003595 spectral effect Effects 0.000 claims 2
- 239000000463 material Substances 0.000 abstract description 11
- 150000007529 inorganic bases Chemical class 0.000 abstract description 9
- 239000000126 substance Substances 0.000 abstract description 9
- 238000001556 precipitation Methods 0.000 abstract description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 description 12
- 239000002585 base Substances 0.000 description 10
- 238000006243 chemical reaction Methods 0.000 description 9
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 description 8
- 238000010521 absorption reaction Methods 0.000 description 7
- 230000008859 change Effects 0.000 description 6
- 239000003446 ligand Substances 0.000 description 6
- 150000003839 salts Chemical class 0.000 description 6
- 238000001914 filtration Methods 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 3
- 239000004115 Sodium Silicate Substances 0.000 description 3
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 238000000295 emission spectrum Methods 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 3
- 229910052911 sodium silicate Inorganic materials 0.000 description 3
- 239000002689 soil Substances 0.000 description 3
- NWYRNCMKWHKPAI-UHFFFAOYSA-N C(=O)=O.[Na] Chemical compound C(=O)=O.[Na] NWYRNCMKWHKPAI-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- 229910052692 Dysprosium Inorganic materials 0.000 description 2
- 229910052693 Europium Inorganic materials 0.000 description 2
- 229910052688 Gadolinium Inorganic materials 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- YNPNZTXNASCQKK-UHFFFAOYSA-N Phenanthrene Natural products C1=CC=C2C3=CC=CC=C3C=CC2=C1 YNPNZTXNASCQKK-UHFFFAOYSA-N 0.000 description 2
- SMWDFEZZVXVKRB-UHFFFAOYSA-N Quinoline Chemical compound N1=CC=CC2=CC=CC=C21 SMWDFEZZVXVKRB-UHFFFAOYSA-N 0.000 description 2
- DGEZNRSVGBDHLK-UHFFFAOYSA-N [1,10]phenanthroline Chemical compound C1=CN=C2C3=NC=CC=C3C=CC2=C1 DGEZNRSVGBDHLK-UHFFFAOYSA-N 0.000 description 2
- CUJRVFIICFDLGR-UHFFFAOYSA-N acetylacetonate Chemical compound CC(=O)[CH-]C(C)=O CUJRVFIICFDLGR-UHFFFAOYSA-N 0.000 description 2
- 150000001298 alcohols Chemical class 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 150000001340 alkali metals Chemical class 0.000 description 2
- 229940040526 anhydrous sodium acetate Drugs 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical compound [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 238000000799 fluorescence microscopy Methods 0.000 description 2
- UIWYJDYFSGRHKR-UHFFFAOYSA-N gadolinium atom Chemical compound [Gd] UIWYJDYFSGRHKR-UHFFFAOYSA-N 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 229910052747 lanthanoid Inorganic materials 0.000 description 2
- 150000002602 lanthanoids Chemical class 0.000 description 2
- 238000002386 leaching Methods 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 238000003760 magnetic stirring Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 230000010355 oscillation Effects 0.000 description 2
- FDPIMTJIUBPUKL-UHFFFAOYSA-N pentan-3-one Chemical compound CCC(=O)CC FDPIMTJIUBPUKL-UHFFFAOYSA-N 0.000 description 2
- IOLCXVTUBQKXJR-UHFFFAOYSA-M potassium bromide Chemical compound [K+].[Br-] IOLCXVTUBQKXJR-UHFFFAOYSA-M 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 239000000523 sample Substances 0.000 description 2
- 235000019795 sodium metasilicate Nutrition 0.000 description 2
- ROFVEXUMMXZLPA-UHFFFAOYSA-N Bipyridyl Chemical group N1=CC=CC=C1C1=CC=CC=N1 ROFVEXUMMXZLPA-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910052684 Cerium Inorganic materials 0.000 description 1
- 241000551547 Dione <red algae> Species 0.000 description 1
- 229910052691 Erbium Inorganic materials 0.000 description 1
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 1
- 229910052689 Holmium Inorganic materials 0.000 description 1
- 229910052779 Neodymium Inorganic materials 0.000 description 1
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 1
- 229910052777 Praseodymium Inorganic materials 0.000 description 1
- 229910052773 Promethium Inorganic materials 0.000 description 1
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 description 1
- 229910052772 Samarium Inorganic materials 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- 229910052775 Thulium Inorganic materials 0.000 description 1
- 229910052769 Ytterbium Inorganic materials 0.000 description 1
- 125000000218 acetic acid group Chemical group C(C)(=O)* 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 229910000272 alkali metal oxide Inorganic materials 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 229910001860 alkaline earth metal hydroxide Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 1
- ZMIGMASIKSOYAM-UHFFFAOYSA-N cerium Chemical compound [Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce] ZMIGMASIKSOYAM-UHFFFAOYSA-N 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 150000004292 cyclic ethers Chemical class 0.000 description 1
- 150000003997 cyclic ketones Chemical class 0.000 description 1
- 238000013016 damping Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- RXKJFZQQPQGTFL-UHFFFAOYSA-N dihydroxyacetone Chemical compound OCC(=O)CO RXKJFZQQPQGTFL-UHFFFAOYSA-N 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- UYAHIZSMUZPPFV-UHFFFAOYSA-N erbium Chemical compound [Er] UYAHIZSMUZPPFV-UHFFFAOYSA-N 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000001506 fluorescence spectroscopy Methods 0.000 description 1
- 239000007850 fluorescent dye Substances 0.000 description 1
- WBJINCZRORDGAQ-UHFFFAOYSA-N formic acid ethyl ester Natural products CCOC=O WBJINCZRORDGAQ-UHFFFAOYSA-N 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- KJZYNXUDTRRSPN-UHFFFAOYSA-N holmium atom Chemical compound [Ho] KJZYNXUDTRRSPN-UHFFFAOYSA-N 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- OHSVLFRHMCKCQY-UHFFFAOYSA-N lutetium atom Chemical compound [Lu] OHSVLFRHMCKCQY-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- AHVIPVIHHYMXPY-UHFFFAOYSA-N phenanthrene quinoline Chemical compound N1=CC=CC2=CC=CC=C12.C1=CC=CC=2C3=CC=CC=C3C=CC12 AHVIPVIHHYMXPY-UHFFFAOYSA-N 0.000 description 1
- 239000003495 polar organic solvent Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- VQMWBBYLQSCNPO-UHFFFAOYSA-N promethium atom Chemical compound [Pm] VQMWBBYLQSCNPO-UHFFFAOYSA-N 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 description 1
- 239000001632 sodium acetate Substances 0.000 description 1
- 235000017281 sodium acetate Nutrition 0.000 description 1
- PANBYUAFMMOFOV-UHFFFAOYSA-N sodium;sulfuric acid Chemical compound [Na].OS(O)(=O)=O PANBYUAFMMOFOV-UHFFFAOYSA-N 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- GWYXTVGANSBRNB-UHFFFAOYSA-N terbium(iii) oxide Chemical compound O=[Tb]O[Tb]=O GWYXTVGANSBRNB-UHFFFAOYSA-N 0.000 description 1
- 238000001161 time-correlated single photon counting Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 230000003313 weakening effect Effects 0.000 description 1
- NAWDYIZEMPQZHO-UHFFFAOYSA-N ytterbium Chemical compound [Yb] NAWDYIZEMPQZHO-UHFFFAOYSA-N 0.000 description 1
- PAPBSGBWRJIAAV-UHFFFAOYSA-N ε-Caprolactone Chemical compound O=C1CCCCCO1 PAPBSGBWRJIAAV-UHFFFAOYSA-N 0.000 description 1
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- Luminescent Compositions (AREA)
Abstract
The invention discloses a kind of method preparing compound rare earth compounding, including: weigh inorganic base substance, add polar solvent, dispersion；Add and react under rare-earth salts and part, stirring；It is filtrated to get compound rare earth compounding, is optionally dried, thus obtain compound rare earth compounding.The present invention is not for being easily formed the rare earth complex of precipitation in polar solvent, by using inorganic base substance, polar solvent successfully synthesizes and is extracted compound rare earth compounding, not only the rare earth complex being difficult to precipitate is precipitated out effectively, and reduces the cost of rare-earth luminescent material.
Description
Technical field
The invention belongs to rare earth luminescent material technical field, relate to a kind of novel being combined
Luminescent material, combines rare earth using inorganic base as kernel, extexine particularly to one
The compound rare earth compounding of coordination compound with and preparation method thereof.
Background technology
Rare earth compounding, as a kind of luminescent material, owing to having, emission peak is narrow, amount
Sub-efficiency is high, launch peak position not with the change of part the feature of movement and extensively answered
It is used in luminescence display, fluorescent probe, the field such as false proof.
But, due to rising steadily of rare earth price, rare earth compounding is in some fields
Application receive certain restriction.Certain methods of once reporting document improves rare earth and joins
The luminescent properties of compound, utilizes the terbium doped oxygen of rare earth as in patent CN 102504817 A
Change aluminum fiber, CN 102153576 A utilizes coated with silica rare earth compounding
Method realizes the optimization of rare-earth complexes luminous material performance and the reduction of cost.But,
The absorption affinity that rare earth compounding is attached to nano-silica surface is more weak, at material
The course of processing in be easily separated from and reassemble.Coated with silica rare earth compounding
Although cost can be effectively reduced, but not it is applicable to all of rare earth compounding,
Because major part rare earth compounding has occurred that during hydrolyzing tetraethoxy orthosilane
Decomposition reaction.
On the other hand, some rare earth compounding is relatively big due to dissolubility in polar solvent,
Thus be difficult to be precipitated out.In order to precipitation, the employing second having in prior art occur
Part, but due to the introducing of Ligands, reduce the fluorescence property of rare earth compounding.
Summary of the invention
In order to solve the problems referred to above, present inventor has performed and study with keen determination, found that:
For not being easily formed the rare earth complex of precipitation in polar solvent, by using
Inorganic base substance, successfully synthesizes in polar solvent and is extracted the cooperation of rare earth binary
Thing and the complex of inorganic base substance, on the one hand by introducing cheap inorganic alkaline
Material and reduce the cost of rare-earth luminescent material, on the other hand dilute by be difficult to precipitate
Soil two-element match is precipitated out effectively, thus completes the present invention.
It is an object of the invention to provide following aspect:
First aspect, the present invention provides a kind of method preparing compound rare earth compounding,
It is characterized in that, the method comprises the following steps:
(1) weigh inorganic base substance, add polar solvent, dispersion；
(2) add under rare-earth salts and part, stirring and react；
(3) it is filtrated to get compound rare earth compounding, is optionally dried, thus obtains
Obtain compound rare earth compounding.
Second aspect, the present invention also provides for according to the method system described in above-mentioned first aspect
The compound rare earth compounding obtained.
The present invention described below.
According to the first aspect of the invention, it is provided that one prepares compound rare earth compounding
Method, it is characterised in that the method comprises the following steps:
Step 1, weighs inorganic base substance, adds polar solvent, dispersion.
The alkaline matter used in the present invention is inorganic base substance, generally solid shape
Formula, it can not be completely dissolved in polar solvent, is the most only dispersed in polar solvent
In.
According to the preferred embodiment of the present invention, the inorganic base substance of described solid can
To be common solid base, such as alkali metal or alkaline earth metal hydroxide or salt, excellent
Select the salt of alkali metal or alkaline-earth metal, can be strong acid salt or salt of weak acid, such as sulphuric acid
Sodium, sodium carbonate, sodium acetate or sodium silicate, usually anhydrous form, the most anhydrous
Sodium carbonate, anhydrous sodium sulfate, anhydrous sodium acetate or anhydrous sodium metasilicate, preferably weak acid
Salt, such as natrium carbonicum calcinatum, anhydrous sodium acetate or anhydrous sodium metasilicate, more preferably
Natrium carbonicum calcinatum.
The polar solvent used in the present invention can be polar organic solvent, above-mentioned inorganic
Alkaline matter does not dissolves in wherein, but can dissolve rare earth compounding.
According to the preferred embodiment of the present invention, described polar solvent can be that alcohols is molten
The lower alcohols such as agent such as methanol, ethanol, propanol or butanol, ketones solvent such as acetone, first
The aliphatic ketone such as ethyl ketone, Ketohexamethylene or cyclic ketones, ether solvent such as ether, oxirane etc.
Aliphatic ether or cyclic ethers, and esters solvent such as Ethyl formate, ethyl acetate etc., preferably
Use methanol, ethanol, acetone, Ketohexamethylene, ether, ethyl acetate, more preferably adopt
By ethanol, acetone, ethyl acetate, most preferably use dehydrated alcohol.
Solid base is 0.1:150g/ml～10:150g/ml with the amount ratio of polar solvent,
Preferably 0.5:150g/ml～8:150g/ml, more preferably 1:150g/ml～7:150g/ml,
Such as, in 15ml polar solvent add 0.1g, 0.2g, 0.3g, 0.4g, 0.5g,
0.6g, 0.7g solid base.
In the present invention, the time scattered to system is not particularly limited, making
It is preferred that solid base is dispersed in polar solvent, preferably 5 minutes～2.5 hours, more
It is preferably 10 minutes～2 hours, such as 1 hour.
Step 2, adds and reacts under rare-earth salts and part, stirring.
In the present invention, described rare-earth salts be lanthanide series metal (Ln) such as lanthanum, cerium, praseodymium,
Neodymium, promethium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutecium etc. inorganic
Salt, preferably hydrochlorate, be preferably able to launch fluorescence lanthanide series metal such as terbium, europium,
Dysprosium, the hydrochlorate of gadolinium, particularly preferably terbium chloride.
According to the present invention, described rare-earth salts can be commercial goods, also by oxide system
For obtaining.As a example by terbium chloride, terbia. Diterbium trioxide prepare with strong acid example hydrochloric acid.Tool
For body, weigh terbia. Diterbium trioxide, dissolve, add strong acid and reducing agent, add diluted acid
Clarify to solution.Under heating condition, removing solvent while stirring, epitaxial to be had occurs
And after being paved with liquid level, cooling, crystallization, i.e. prepare product chlorinated terbium, can be dried
Standby.
In the present invention, above-mentioned terbia. Diterbium trioxide can be terbium sesquioxide, it is also possible to be seven
Aoxidize four terbiums, preferably terbium peroxide.
The strong acid that the present invention selects is selected from chloride strong acid, preferably concentrated hydrochloric acid, diluted acid
Selected from chloride diluted acid, preferably dilute hydrochloric acid.
The reducing agent that the present invention selects is preferably hydrogen peroxide, and the mass fraction of hydrogen peroxide is excellent
Elect 30% as.
The solvent of terbia. Diterbium trioxide place liquid-phase system is not specially limited by the present invention, preferably
Use pure water, deionized water and/or distilled water, preferably deionized water.
The inventors discovered that heating can shorten the response time of terbia. Diterbium trioxide and strong acid, and
And make that reaction carries out more abundant, the temperature of reaction is 30 DEG C～100 DEG C, preferably 40 DEG C
～95 DEG C., more preferably 50 DEG C～92 DEG C.
The present invention selects to remove the molten of terbia. Diterbium trioxide place liquid-phase system before cooling, crystallization
Agent, the mode removing solvent is not specially limited by the present invention, any in prior art
A kind of mode removing solvent all can use, such as room temperature volatilization, normal heating, decompression
Distillation etc..
The inventors discovered that having impurity salt in reaction system occurs, under filtercondition,
Can obtain pure crystal, the mode filtered is not specially limited by the present invention, as
Sucking filtration, natural filtration, preferably sucking filtration.
In the present invention, described part (L) can be monodentate ligand, it is also possible to be many
Tooth part, such as bidentate ligand, oxalate denominationby, 2,2'-bipyridyl, 1,10-neighbour is luxuriant and rich with fragrance
Quinoline (phen), diones part such as acetylacetone,2,4-pentanedione (acac), acetylsalicylate from
Son (aspirin) etc., preferably 1,10-neighbour's phenanthrene quinoline (phen), acetylacetone,2,4-pentanedione (acac)
With aspirin radical ion, more preferably aspirin radical ion (aspirin).
Correspondingly, the rare earth compounding of gained can be LnL6(when L is monodentate ligand) or
LnL3(when L is bidentate ligand), such as Tb (aspirin)3。
The system formed for solid base, rare-earth salts and part carries out time of reacting not
It is particularly limited to, preferably 20 minutes～3 hours, more preferably 30 minutes～2.5 hours,
Such as 2 hours.
Step 3, is filtrated to get compound rare earth compounding, is optionally dried, thus
Obtain compound rare earth compounding.
According to the present invention, carry out filtering by the reaction system of step 2 i.e. obtain compound dilute
Soil coordination compound, is preferably dried it, and baking temperature is not specially limited, preferably
Being 50 DEG C～120 DEG C, such as 80 DEG C, drying time is also not specially limited, and preferably 2
Hour～24 hours, such as 12 hours.
According to the present invention, rare earth compounding LnL6Or LnL3(such as Tb (aspirin)3) with
Stronger interaction is there is, therefore, it is possible to have between solid base such as natrium carbonicum calcinatum
The absorption of effect ground is filtered out on solid base surface.Without being bound by any theory,
Its reason may is that the surface molecules carboxylic as alkali Yu part of natrium carbonicum calcinatum granule
Acid reaction so that part furthers with natrium carbonicum calcinatum granule surface molecules spacing, from
And absorption affinity strengthens.Therefore, the rare earth compounding of generation will be strongly adsorbed to as
The solid base particle surfaces such as natrium carbonicum calcinatum, cause the part number with rare-earth ion coordination
Reduce, such as, form Tb (aspirin)x, wherein x < 3.
Compound rare earth compounding is finally prepared, its fluorescence according to said method of the present invention
Spectrum and infrared spectrum have the characteristic peak being different from rare earth compounding.When solid base is
Natrium carbonicum calcinatum, when rare earth compounding is the coordination compound that terbium is formed with acetylsalicylate,
Its fluorescence emission spectrum shows, this compound rare earth compounding wavelength be 420nm,
Emission peak is there is near 550nm, 590nm, 625nm；Its fluorescence excitation spectrum shows,
Excitation spectrum is there is in this compound rare earth compounding in the range of wavelength is 250-350nm
Peak；Infrared spectrum shows, it is 1749cm in wave number-1、881cm-1、702cm-1、
1400-1600cm-1Place's existing characteristics absworption peak.
The preparation method of the compound rare earth compounding provided according to the present invention and corresponding
Compound rare earth compounding, show following beneficial effect:
(1) fluorescence lifetime of this compound rare earth compounding is greatly improved, can conduct
Luminescent material is widely used in display and print field；
(2) method preparing this compound rare earth compounding has started novel synthesis fluorescence
The technology of powder, not only by introducing cheap solid base (such as natrium carbonicum calcinatum)
Reduce the cost of fluorescent material as kernel, and the rare earth precipitated can be difficult to
Coordination compound (coordination compound that formed such as terbium and aspirin (Tb (aspirin) x, wherein
X be 3 or < 3) be effectively precipitated out, beneficially industrialized production；
(3) this compound rare earth compounding and preparation method thereof environmental protection, without environment
Pollute.
Accompanying drawing explanation
Fig. 1 illustrates that the rare earth compounding that embodiment 1-7 obtains is anhydrous at different quality
Sodium carbonate surface formed after emission spectrum figure (λex=334nm)；
Fig. 2 illustrates that the rare earth terbium that natrium carbonicum calcinatum consumption and embodiment 1-7 obtain is joined
The fluorescent emission intensity graph of a relation of compound；
Fig. 3 illustrate rare-earth terbium complex that embodiment 1-7 obtains different quality without
Aqueous sodium carbonate surface formed after exciting light spectrogram (λem=545nm)；
Fig. 4 illustrate rare-earth terbium complex that embodiment 1-7 obtains different quality without
Aqueous sodium carbonate surface formed after infrared spectrogram；
Fig. 5 illustrates the mean fluorecence longevity of the rare-earth terbium complex that embodiment 1-7 obtains
Order the variation relation figure with natrium carbonicum calcinatum consumption；
Fig. 6 a, 6b, 6c, 6d, 6e are shown respectively the dilute of embodiment 1-5 acquisition
Soil terbium coordination compound fluorescence microscopy after different quality natrium carbonicum calcinatum surface is formed
Mirror photo (amplifies 100 times).
Detailed description of the invention
Below by embodiment, the present invention is described in detail, the feature of the present invention and
Advantage will become more apparent from, clearly along with these explanations, but the present invention does not limit
In these exemplary illustrations.
Measuring method
Infrared spectrum measurement:
Use pressing potassium bromide troche in 4000-400cm-1At Fourier transformation infrared spectrometer
(WQF-IR 510) is upper to be measured.
Fluorescence spectrometry:
Use FM4NIR TCSPC fluorescence spectrophotometer (JY company of France), use
The optical filter of 350nm filters off by light produced by light source for instrument.Incidence and transmitting slit
It is 1nm, uses the light damping plate of 10 times to reduce the intensity of light source simultaneously.
Fluorescence lifetime measures:
Use the LED excitation source of 370nm, gather 20000 photons, fluorescence lifetime
Curve uses second order life-span approximating method.
Fluorescence microscopy:
Using Olympus TL4, photographic head model is KP73IX53, exposure intensity
800, amplification 200 times, time of exposure is 2 seconds, and excitation source is 460-530nm
Royal purple light.
Embodiment
In the present embodiment, terbia. Diterbium trioxide used is purchased from Shanghai crystalline substance pure reagent company limited, anhydrous
Ethanol is purchased from upper seamount purchased from Shanghai Zhen Qi chemical reagent company limited, natrium carbonicum calcinatum
Pu Chemical Co., Ltd., aspirin purchased from Beijing Century AudioCodes biotechnology limited
Company.
Embodiment 1
In beaker, weigh 10g terbia. Diterbium trioxide, pour 80ml deionized water into, then toward burning
Slow alternate dropwise addition concentrated hydrochloric acid and hydrogen peroxide in Bei, then drip appropriate hydrochloric acid reaction to molten
Liquid is clarified.Evaporating solvent under the conditions of 90 DEG C while stirring, epitaxial to be had occurs and spreads
After full liquid level, reaction system is cooled down, has mass crystallization to separate out, take out with buchner funnel
Preparing terbium chloride after leaching crystallization, in exsiccator, drying at room temperature is standby.
Weigh 0.1 natrium carbonicum calcinatum to be placed in the beaker of 100mL, add 15mL anhydrous
Ethanol and in ultrasonic instrument sonic oscillation disperse one hour.
Then terbium chloride the most dried for 0.5mmol and 1.5mmol acetyl salicylic are weighed
Acid adds in beaker, and beaker is placed on magnetic stirring apparatus stirring 2h.
Finally obtaining solid sample with buchner funnel sucking filtration, products therefrom is put in baking oven
At a temperature of 80 DEG C, it is dried 12h, obtains compound rare-earth terbium complex finally,
Its sign is shown in following experimental example 1-6.
Embodiment 2-7
Repeat embodiment 1, differ only in and change the quality of natrium carbonicum calcinatum respectively
0.2g, 0.3g, 0.4g, 0.5g, 0.6g, 0.7g, obtain compound rare earth respectively
Its sign of terbium coordination compound is shown in following experimental example 1-6.
Embodiment 8-15
Repeat embodiment 1-7 respectively, differ only in and use commercially available terbium chloride as former
Material, the compound rare-earth terbium complex of final acquisition, its emission spectrum figure, excitation spectrum
Figure, infrared spectrogram, fluorescent microscopy images, fluorescent emission intensity, mean fluorecence
Life experiment result is similar with embodiment 1-7.
Comparative example
Comparative example 1
In beaker, weigh 10g terbia. Diterbium trioxide, pour 80ml deionized water into, then toward burning
Slow alternate dropwise addition concentrated hydrochloric acid and hydrogen peroxide in Bei, then drip appropriate hydrochloric acid reaction to molten
Liquid is clarified.Evaporating solvent under the conditions of 90 DEG C while stirring, epitaxial to be had occurs and spreads
After full liquid level, reaction system is cooled down, has mass crystallization to separate out, take out with buchner funnel
Preparing terbium chloride after leaching crystallization, in exsiccator, drying at room temperature is standby.
Weigh terbium chloride the most dried for 0.5mmol and 1.5mmol aspirin adds
Enter in beaker, add 15mL dehydrated alcohol sonic oscillation dispersion in ultrasonic instrument
One hour, then beaker is placed on magnetic stirring apparatus stirring 2h, but there is no solid
Separate out.
Experimental example
Experimental example 1
Fig. 1 is that the rare earth compounding of embodiment 1-7 acquisition is at different quality natrium carbonicum calcinatum
Emission spectrum figure (λ after upper absorptionex=334nm).
As can be seen from the figure the emission peak of four features of terbium ion, illustrates terbium coordination compound
Form and can effectively absorb ultraviolet light and pass to terbium ion.Sodium carbonate is used
Amount is the sample of 0.2-0.7g, all sees a wide emission peak near 420nm, this
It is belonging to the emission peak of part aspirin.And part aspirin and Tb3+Have extraordinary
Matching, if part and Tb3+All define terbium coordination compound, the emission peak of part
Can't see.This demonstrate some ligands and do not participate in coordination, but with independence
The form of part is adsorbed on sodium carbonate surface, and this is owing to terbium coordination compound needs at carbonic acid
The reason that sodium surface is formed.
Experimental example 2
Fig. 2 is the rare-earth terbium complex that natrium carbonicum calcinatum consumption obtains with embodiment 1-7
Fluorescent emission intensity graph of a relation.It can be seen that along with natrium carbonicum calcinatum consumption
Increase, the fluorescent emission intensity of terbium coordination compound is the most on a declining curve.This be due to
Caused by the decline of the terbium coordination compound density formed on sodium carbonate surface.
Experimental example 3
Fig. 3 is that the rare-earth terbium complex of embodiment 1-7 acquisition is at different quality Carbon Dioxide
Sodium surface formed after exciting light spectrogram (λem=545nm).From the figure, it can be seen that seven
The excitation spectrum diagram shape difference planting product is relatively big, 0.1 and 0.2g natrium carbonicum calcinatum consumption
The excitation spectrum peak shape of obtained product is wider, 0.3-0.7g natrium carbonicum calcinatum consumption gained
Excitation spectrum peak shape to product substantially narrows.This illustrates that different natrium carbonicum calcinatum is used
Measure the structure to terbium coordination compound and there is large effect.
Experimental example 4
Fig. 4 is that the rare-earth terbium complex of embodiment 1-7 acquisition is at different quality Carbon Dioxide
Sodium surface formed after infrared spectrogram.When using 0.1g natrium carbonicum calcinatum as alkali,
It can be seen that mainly terbium coordination compound and part is acetysalicylic in infrared spectrogram
Characteristic absorption peak, peak shape is relatively more sharp-pointed, 1749cm-1Locate strong absworption peak to illustrate to have to join
The acetysalicylic carbonyl of body exists.At 881cm-1And 702cm-1Place does not see bright
Aobvious natrium carbonicum calcinatum characteristic absorption peak, but, at 1400-1600cm-1Place can see
Occurring to the strongest broad peak, this is the characteristic absorption peak of natrium carbonicum calcinatum, and terbium is described
Coordination compound forms complex with natrium carbonicum calcinatum.Along with natrium carbonicum calcinatum consumption
Increase, 1400-1600cm-1The wide strong peak at place becomes increasingly stronger, 881cm-1With 702
cm-1The peak at place also becomes increasingly stronger, and the peak of terbium coordination compound and part is more and more weak.
Experimental example 5
The rare-earth terbium complex that embodiment 1-7 obtains is at different quality natrium carbonicum calcinatum table
Face formed after time lifetime be respectively 1.30ms, 1.48ms, 1.46ms, 1.61ms,
1.41ms, 1.65ms, 1.74ms, Fig. 5 illustrates that the mean fluorecence life-span is with Carbon Dioxide
The variation relation figure of sodium consumption.It can be seen that terbium coordination compound Tb (aspirin)x
The mean fluorecence life-span the most in rising trend with natrium carbonicum calcinatum consumption increase.This says
Understand that the consumption of natrium carbonicum calcinatum have impact on terbium coordination compound Tb (aspirin)xThe fluorescence longevity
Life, indicates along with the consumption of natrium carbonicum calcinatum changes, and terbium coordination compound molecular structure is sent out
Give birth to certain change.Along with increasing of natrium carbonicum calcinatum consumption, distribution is at anhydrous carbon
The TbCl that acid sodium surface reacts3·6H2O and aspirin molecular amounts occurs the most therewith
Change, therefore can cause formed terbium coordination compound Tb (aspirin)xX becoming
Change.Fig. 5 compares Fig. 2 and can be seen that terbium coordination compound Tb (aspirin)xThe mean fluorecence life-span
The biggest, its fluorescent emission intensity can be the most weak.
Experimental example 6
Fig. 6 a, 6b, 6c, 6d and 6e are shown respectively the rare earth terbium that embodiment 1-5 obtains
Coordination compound fluorescent microscopy images after different quality natrium carbonicum calcinatum surface is formed
(amplifying 100 times), correspondence uses 0.1g, 0.2g, 0.3g, 0.4g and 0.5g respectively
Na2CO3Situation.And Na2CO3For being then hardly visible fluorescence during 0.6g and 0.7g.
It can be seen that along with Na2CO3Increasing of consumption, by fluorescence microscope light source
Blue purple light excited produced green fluorescence gradually weakens.It can be seen that nothing
Aqueous sodium carbonate is covered by green fluorescence produced by terbium coordination compound completely, illustrates nothing
Combine closely with Tb (aspirin) x in aqueous sodium carbonate surface.Why fluorescence along with
Increasing and gradually weakening of natrium carbonicum calcinatum consumption, is because natrium carbonicum calcinatum surface
Tb (aspirin) x molecular amounts gradually decreases and causes.But, we can see
Arrive, photo shows Changing Pattern and the fluorescence intensity shown in Fig. 2 of the brightness of fluorescence
Changing Pattern difference is the biggest.This is the optical source wavelength due to fluorescence microscope and transmitting light
Spectrum excitation wavelength used is not caused by the same area.
Above in association with detailed description of the invention and exemplary example, the present invention is carried out in detail
Illustrate, but these explanations can not be interpreted as limitation of the present invention.This area skill
Art personnel understand, without departing from the spirit and scope of the invention, and can be to this
Inventive technique scheme and embodiment thereof carry out multiple equivalencing, modify or improve,
These are within the scope of the present invention.Protection scope of the present invention is wanted with appended right
Ask and be as the criterion.
Claims (8)
1. the method preparing compound rare earth compounding, it is characterised in that the party
Method comprises the following steps:
(1) weigh solid base natrium carbonicum calcinatum, add polar solvent, dispersion；
(2) add under terbium chloride and aspirin, stirring and react；
(3) it is filtrated to get compound rare earth compounding, is dried, thus obtain multiple
Mould assembly rare earth compounding,
The fluorescence emission spectrum of this compound rare earth compounding wavelength be 420nm,
Emission peak is there is near 550nm, 590nm, 625nm；Its fluorescence excitation spectrum is at ripple
Exciting light spectral peak is there is in the range of a length of 250-350nm；Its infrared spectrum in wave number is
1749cm-1、881cm-1、702cm-1、1400-1600cm-1Place's existing characteristics absworption peak.
Method the most according to claim 1, it is characterised in that
In step 1, described polar solvent is methanol, ethanol, acetone, Ketohexamethylene, second
Ether, ethyl acetate；
Solid base is 0.5:150g/ml～8:150g/ml with the amount ratio of polar solvent.
Method the most according to claim 2, it is characterised in that
In step 1, described polar solvent is dehydrated alcohol；
Solid base is 1:150g/ml～7:150g/ml with the amount ratio of polar solvent.
Method the most according to claim 1, it is characterised in that
In step 2, described terbium chloride is prepared with strong acid as follows by terbia. Diterbium trioxide:
Weigh terbia. Diterbium trioxide, dissolve, add strong acid and reducing agent, add diluted acid to molten
Liquid is clarified；Under heating condition, removing solvent while stirring, epitaxial to be had occurs and spreads
After full liquid level, cooling, crystallization, i.e. prepare product chlorinated terbium；
Described terbia. Diterbium trioxide is terbium peroxide；
Described strong acid is dilute hydrochloric acid；
Described reducing agent is hydrogen peroxide.
Method the most according to claim 4, it is characterised in that the matter of hydrogen peroxide
Amount number is 30%.
Method the most according to claim 1, it is characterised in that
In step 2, the system that solid base, terbium chloride are formed with aspirin is carried out instead
The time answered is 20 minutes～3 hours.
Method the most according to claim 6, it is characterised in that
In step 2, the system that solid base, terbium chloride are formed with aspirin is carried out instead
The time answered is 30 minutes～2.5 hours.
8. the compound rare earth prepared according to the method one of claim 1 to 7 Suo Shu
Coordination compound, said method comprising the steps of:
(1) weigh solid base natrium carbonicum calcinatum, add polar solvent, dispersion；
(2) add under terbium chloride and aspirin, stirring and react；
(3) it is filtrated to get compound rare earth compounding, is dried, thus obtain multiple
Mould assembly rare earth compounding, by natrium carbonicum calcinatum and terbium and joining that acetylsalicylate is formed
The fluorescence emission spectrum of the compound rare-earth terbium complex that compound obtains at wavelength is
Emission peak is there is near 420nm, 550nm, 590nm, 625nm；Its fluorescence excitation
Exciting light spectral peak is there is in spectrum in the range of wavelength is 250-350nm；Its infrared spectrum
It is 1749cm in wave number-1、881cm-1、702cm-1、1400-1600cm-1There is spy in place
Levy absworption peak.
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| CN110655915A (en) * | 2018-06-29 | 2020-01-07 | 阜阳师范学院 | Organic-inorganic hybrid rare earth composite fluorescent material and preparation method thereof |
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| CN110734760A (en) * | 2018-07-19 | 2020-01-31 | 阜阳师范学院 | rare earth europium composite fluorescent material using sodium acetate as matrix and preparation method thereof |
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| CN111533659A (en) * | 2020-05-16 | 2020-08-14 | 内蒙古联丰稀土化工研究院有限公司 | Preparation method of acetylsalicylic acid rare earth |
| CN114249651B (en) * | 2021-12-21 | 2024-04-09 | 包头稀土研究院 | Organic rare earth complex microsphere, preparation method thereof and application of ammonia water |
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Address after: 453499 No. 3, Pubei pilot industrial park, Changheng County, Xinxiang, Henan Province Patentee after: Henan Soton New Material Co.,Ltd. Address before: 465450 in vein Industrial Park, south of 312 National Road, Zhaihe Town, Guangshan County, Xinyang City, Henan Province Patentee before: Henan Soton New Material Co.,Ltd. |
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| CP02 | Change in the address of a patent holder | ||
| CP02 | Change in the address of a patent holder |
Address after: 453499 No. 3, Pubei pilot industrial park, Changyuan City, Xinxiang City, Henan Province Patentee after: Henan Soton New Material Co.,Ltd. Address before: 453499 No. 3, Pubei pilot industrial park, Changheng County, Xinxiang, Henan Province Patentee before: Henan Soton New Material Co.,Ltd. |
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| CP02 | Change in the address of a patent holder |