Lanthanide rare earth-organic polymer precursor, lanthanide rare earth oxide fibers, preparation method and application

A technology of lanthanide rare earths and polymers, which is applied to the chemical characteristics of fibers, textiles and papermaking, etc., can solve the problems of reducing the purity of rare earth oxide nanofiber membranes, affecting the flexibility of fibers, and having many surface defects in fibers, achieving high strength, The effect of increasing content and stabilizing properties

Pending Publication Date: 2020-05-22
SHANDONG UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the flexibility and purity of rare earth oxide fibers are currently the main issues limiting their practical applications.
[0003] Chinese patent document CN101912582A discloses a kind of La 2 o 3 :Tb 3+ The preparation method of the submicron green fluorescent fiber comprises dissolving lanthanum acetate and terbium acetate in water, adding polyethylene oxide whose mass is 1 to 1.2 times the total amount of acetate, and stirring for 4 hours to obtain a spinning solution, which is electrospun and Subsequent heat treatment to obtain La 2 o 3 :Tb 3+ Fiber, the fiber diameter distribution is relatively discrete, and due to the low oxide content in the precursor, a large amount of organic matter is decomposed, resulting in more surface defects on the fiber, which affects the flexibility of the fiber
R. Thangappan et al. used PVA as a structural template to prepare Gd with gadolinium nitrate as a metal source. 2 o 3 Nanofiber (see: Applied Surface Science 261(2012) 770-773), which has good optical properties, but has more pores on the surface, shorter length and poor strength
Chinese patent document CN104153124A discloses a method for preparing a flexible rare earth oxide nanofiber membrane. This method obtains a rare earth nanofiber membrane with good flexibility, but non-rare earth stabilizers and silane coupling agents need to be added during the preparation process, which is extremely difficult. Large reduction in the purity of rare earth oxide nanofibrous membranes

Method used

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  • Lanthanide rare earth-organic polymer precursor, lanthanide rare earth oxide fibers, preparation method and application
  • Lanthanide rare earth-organic polymer precursor, lanthanide rare earth oxide fibers, preparation method and application
  • Lanthanide rare earth-organic polymer precursor, lanthanide rare earth oxide fibers, preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] A kind of preparation method of lanthanum-organic polymer precursor and lanthanum oxide fiber, comprises steps as follows:

[0055] (1) Dissolve 100 grams of anhydrous lanthanum chloride in 600 grams of anhydrous methanol, add 41 grams of acetylacetone to the solution after it is completely dissolved, and after stirring for 2 hours, add 100 grams of triethylamine drop by drop. Then continue to stir for 2 hours to obtain a clear precursor triethylamine solution;

[0056] (2) Transfer the clear solution obtained in (1) into a round-bottomed flask, concentrate under reduced pressure at 38° C. to dry powder, then add 850 grams of acetone to the round-bottomed flask, seal and let stand for 72 hours;

[0057] (3) Filter out the insoluble triethylamine hydrochloride in the round-bottomed flask described in (2), obtain the lanthanum-acetylacetone polymer precursor solution, transfer it to another round-bottomed flask, and dry under reduced pressure at 32°C , to obtain lanthanu...

Embodiment 2

[0062] A kind of preparation method of lutetium-organic polymer precursor and lutetium oxide fiber, comprises steps as follows:

[0063] (1) Dissolve 100 grams of crystalline lutetium chloride in 300 grams of anhydrous methanol, add 38 grams of acetylacetone to the solution after it is completely dissolved, and after stirring for 2 hours, add 77 grams of triethylamine dropwise, after the dropwise addition Continue stirring for 2 hours to obtain a clear precursor triethylamine solution;

[0064] (2) Transfer the clear solution obtained in (1) into a round-bottomed flask, concentrate under reduced pressure at 38°C to dry powder, then add 750 grams of tetrahydrofuran to the round-bottomed flask, seal and let stand for 72 hours;

[0065] (3) Filter out the insoluble triethylamine hydrochloride in the round-bottomed flask described in (2), obtain the lutetium-acetylacetone polymer precursor solution, transfer it to another round-bottomed flask, and dry under reduced pressure at 32°...

Embodiment 3-17

[0070] The preparation steps of Examples 3-17 are the same as those of Example 1, wherein the preparation parameters of the rare earth-organic polymer precursor, the preparation parameters of the spinning solution, and the diameter and purity of the flexible rare earth oxide fibers are shown in Tables 1-3.

[0071] Note: stirring time 1—stirring time after adding ligand; stirring time 2—stirring time after adding triethylamine;

[0072] Drying temperature 1—the drying temperature of the precursor solution containing triethylamine hydrochloride;

[0073] Drying temperature 2—the drying temperature of the precursor solution obtained by filtration after extractant extraction.

[0074] Table 1

[0075]

[0076] Table 2

[0077]

[0078] table 3

[0079]

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Abstract

The invention relates to a lanthanide rare earth-organic polymer precursor, lanthanide rare earth oxide fibers, a preparation method and application. The preparation method comprises: 1) a step of preparing the lanthanide rare earth-organic polymer precursor; 2) a step of preparing precursor fibers by electrostatic spinning, namely a step of dissolving the rare earth-organic polymer precursor serving as a raw material into an organic solvent, adding a spinning aid to obtain a precursor spinning solution, and performing electrostatic spinning on the spinning solution at the voltage of 5-20 kV to obtain the precursor fibers; and 3) a step of carrying out heat treatment on the precursor fibers in air to obtain the lanthanide rare earth oxide fibers. The disclosed fibers are high in purity, high in strength, uniform and adjustable in diameter, good in flexibility, compact in structure and free of defects such as air holes and cracks, and have wide application prospects in the fields of catalysis, illumination, nuclear industry, laser, storage, sensing, display, biomarkers, ceramic materials, refractory materials and the like.

Description

Technical field: [0001] The invention relates to a lanthanide rare earth-organic polymer precursor, a lanthanide rare earth oxide fiber and a preparation method, in particular to a method for preparing a corresponding oxide fiber from a rare earth-organic polymer precursor with a linear polymer structure, belonging to The field of new material technology. Background technique: [0002] Lanthanide rare earth oxides refer to the oxides of 15 elements from lanthanum to lutetium in group IIIB of the periodic table. Because rare earth elements have the characteristics of high electricity price, large radius, rich electronic energy levels, easy polarization, positive correlation between refractive index and polarization intensity, and good thermal stability of rare earth oxides, they are widely used in catalysis, lighting, nuclear industry, laser, storage, etc. , sensing, display, biological markers, ceramic materials and refractory materials have broad application prospects. At...

Claims

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Application Information

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IPC IPC(8): C08G83/00D01F9/10
CPCC08G83/008D01F9/10
Inventor朱陆益谢永帅彭影王新强张光辉许东
OwnerSHANDONG UNIV