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A kind of highly stable, volatile heteronuclear rare earth chelate and its preparation method and application

A rare earth chelate, highly stable technology, applied in the preparation of aldehyde/ketone chelate, glass manufacturing equipment, manufacturing tools, etc., can solve the problems of poor stability, complicated process, and the concentration of rare earth elements cannot be precisely controlled, and achieve stable Sex-enhancing effects

Active Publication Date: 2022-07-26
HUBEI UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, these rare earth chelate reagents are prepared by regulating the flow rate of carrier gas in different pipelines to release the flow rate of dopant species, and realize the proportioning of different dopants through the flow rate of different dopants. Therefore, the more doping species, the more complicated the process; the longer the doping distance, the greater the difference between the actual ratio of doping species and the initially set ratio concentration, making rare earth chelate The concentration of rare earth elements in the reagent cannot be precisely controlled
Second, Yb(TMHD) is commonly used in fiber doping 3 and Er(TMHD) 3 reagent, although Yb(TMHD) 3 The reagent has extremely high stability, and Er(TMHD) 3 The stability of the reagent is very poor, so how to accurately control the ratio of rare earth elements to achieve one-step sublimation and how to improve the stability of the chelate are currently the bottlenecks encountered, and this patent solves these two problems

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  • A kind of highly stable, volatile heteronuclear rare earth chelate and its preparation method and application
  • A kind of highly stable, volatile heteronuclear rare earth chelate and its preparation method and application
  • A kind of highly stable, volatile heteronuclear rare earth chelate and its preparation method and application

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preparation example Construction

[0029] The embodiments of the present application provide a method for preparing a highly stable and volatile heteronuclear rare earth chelate compound, comprising the following steps:

[0030] S1. After reacting at least two rare earth oxides with an inorganic acid, then adding water to obtain a rare earth salt mixed aqueous solution;

[0031] S2, adding alcohol to the diketone ligand, stirring and then adding an alkali solution to obtain a mixed solution;

[0032] S3, adding the rare earth salt mixed aqueous solution dropwise to the mixed solution, after the reaction, suction filtration to obtain a highly stable and volatile heteronuclear rare earth chelate.

[0033] It should be noted that, in the examples of the present application, the inorganic acids can be hydrochloric acid, nitric acid, boric acid, sulfuric acid, phosphoric acid, etc.; the bases can be triethylamine, ethylenediamine, nicotine, sodium hydroxide, and the like. In the present application, the aqueous sol...

Embodiment 1

[0048] The embodiment of the present application provides a method for preparing a highly stable and volatile heteronuclear rare earth chelate compound, which specifically includes the following steps:

[0049] S1. 34.872g of Yb with a purity of 6N 2 O 3 and 2.082g of Er 2 O 3 Mix, then dropwise add 38g of HPLC-grade nitric acid, react at 80°C, add 200mL of deionized water after 1 hour of reaction, and react to obtain a mixed aqueous solution of rare earth salts;

[0050] S2. Under normal temperature conditions, add 58g of 2,2,6,6-tetramethyl-3,5-heptanedione with a purity greater than 5N into the reactor, then add 200mL of ethanol, stir for 20min, and then add 39g of purity It is 5N sodium hydroxide should be until the liquid becomes clear to obtain a mixture;

[0051] S3, the rare earth salt mixed aqueous solution in S1 is added dropwise to the mixed solution in S2 using a constant pressure funnel, stirred at normal temperature, and reacted for 1 h, and filtered under re...

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Abstract

The invention provides a highly stable and volatile heteronuclear rare earth chelate compound and a preparation method and application thereof. The preparation method of the heteronuclear rare earth chelate comprises: reacting at least two rare earth oxides with an inorganic acid to obtain a mixed aqueous solution of rare earth salts; adding alcohol to diketone ligands to obtain a mixed solution; The heteronuclear rare earth chelate compound is obtained by dropwise adding to the mixed solution for reaction; the preparation method of the present invention utilizes the reaction of the rare earth salt mixed aqueous solution and the diketone ligand mixed solution to directionally synthesize the heteronuclear rare earth ions containing two or more rare earth ions. The nuclear rare earth chelate provides the feasibility of preparing double-clad optical fiber preforms by vapor-phase vapor deposition for realizing multi-species fixed ratio and one-step doping. Compared with the traditional release of dopant species by regulating the flow rate of carrier gas in different pipes To achieve the ratio of different dopants, the preparation method of the present application can precisely control the ratio of doped rare earth elements in one step and improve the unstable bottleneck of erbium rare earth chelate.

Description

technical field [0001] The invention relates to the technical field of rare earth chelate materials, in particular to a preparation method and application of a highly stable and volatile heteronuclear rare earth chelate compound. Background technique [0002] Due to the safety and efficiency of optical fiber communication technology, it has great application prospects in the commercial and military fields. Research on high-power optical fiber communication and fiber laser technology includes key materials, core devices, and systems and equipment. As far as key materials are concerned, the silica fiber (core rod) determines the performance of the fiber, and the doping reagent and process greatly affect the performance of the fiber preform. At present, the output power of the international single-mode fiber laser has reached 20 kilowatts, while that in my country is stable at about 5 kilowatts. The basic optical fiber material and device technology is far behind the advanced ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C45/77C07C49/92C03B37/012
CPCC07C45/77C03B37/012C07C49/92
Inventor 徐海兵黄青青
Owner HUBEI UNIV
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