Preparation method of rare-earth fluorescent microspheres

A technology of rare earth fluorescence and microspheres, which is applied in the field of preparation of rare earth fluorescent microspheres, can solve the problems of difficulty in maintaining long-term luminescence, poor plasticity, and weak luminescence intensity, and achieve significant luminescence effects, increased luminescence time, and improved luminescence time Effect

Inactive Publication Date: 2015-11-25
JIANGSU ZHENYU ENVIRONMENTAL PROTECTION TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The technical problem mainly solved by the present invention: the plasticity of the products made of the current general fluorescent materials is relatively poor, and the fluorescent materials themselves contain a large amount of harmful substances to the human body, which will increase the incidence of human cancer. In addition, the luminous intensity of the current fluorescent materials is relatively weak, It is difficult to maintain long-term luminescence, and a preparation of rare earth fluorescent microspheres is provided. The method first prepares the monomer refined methyl methacrylate and the initiator refined azobisisobutyronitrile through pretreatment, and uses the coprecipitation method Prepare a ternary complex of rare earth with high luminous intensity with polymerization activity, and then copolymerize it with methyl methacrylate to obtain a kind of high molecular weight rare earth metal copolymer solid material, that is, a rare earth fluorescent microsphere, not only Strong plasticity, no harm to the human body, and long-lasting luminous time, which increases the luminous time by more than 85%

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0021] First, take 100mL methyl methacrylate and put it into a 250mL separatory funnel, wash it three times with 5% sodium hydroxide solution, 30mL each time until it is colorless, then wash it with deionized water until the pH is 7 After drying with anhydrous sodium sulfate for 5 days, refined methyl methacrylate was obtained; then, 50 mL of absolute ethanol was added to a 150 mL Erlenmeyer flask, heated to 50 ° C in a water bath, and then 5 g of azobisisobutyronitrile was added. Vibrate on a shaking table until it is completely dissolved, filter quickly, cool the filtrate until white crystals are precipitated, filter with a Buchner funnel, put the crystals into a vacuum drying oven to dry to obtain refined azobisisobutyronitrile; In a 150mL three-neck flask, add 5mg of europium oxide, 1g of α-methacrylic acid and 50mL of water, heat it in a water bath to 80°C, and pour in condensed water, place it on a magnetic stirrer and stir for 2 hours at a stirring speed of 100r / min to o...

example 2

[0024] First, take 150mL methyl methacrylate and put it into a 250mL separatory funnel, wash it 4 times with 5% sodium hydroxide solution, 35mL each time until it is colorless, then wash it with deionized water until the pH is 7.5 After drying with anhydrous sodium sulfate for 6 days, refined methyl methacrylate was obtained; then, 80 mL of absolute ethanol was added to a 150 mL Erlenmeyer flask, heated to 53°C in a water bath, and 7 g of azobisisobutyronitrile was added. Vibrate on a shaking table until it is completely dissolved, filter quickly, cool the filtrate until white crystals are precipitated, filter with a Buchner funnel, put the crystals into a vacuum drying oven to dry to obtain refined azobisisobutyronitrile; In a 150mL three-necked flask, add 8mg of europium oxide, 1.2g of α-methacrylic acid and 80mL of water, heat it in a water bath to 85°C, and pour in condensed water, place it on a magnetic stirrer and stir for 2.5h at a stirring speed of 150r / min. Obtain α-eur...

example 3

[0027] First, take 200mL methyl methacrylate and put it into a 250mL separatory funnel, wash it with 5% sodium hydroxide solution for 5 times, each time 40mL until it is colorless, then wash it with deionized water until the pH is 8 Finally, dry it with anhydrous sodium sulfate for 7 days to obtain refined methyl methacrylate; then add 100 mL of absolute ethanol to a 150 mL Erlenmeyer flask, put it in a water bath and heat it to 55°C, then add 10 g of azobisisobutyronitrile, Vibrate on a shaking table until it is completely dissolved, filter quickly, cool the filtrate until white crystals are precipitated, filter with a Buchner funnel, and dry the crystals in a vacuum oven to obtain refined azobisisobutyronitrile; In a 150mL three-neck flask, add 10mg of europium oxide, 2g of α-methacrylic acid and 100mL of water, heat it in a water bath to 90°C, pour in condensed water, place it on a magnetic stirrer and stir for 3 hours at a stirring speed of 200r / min to obtain α - Europium ...

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Abstract

The invention relates to a preparation method of rare-earth fluorescent microspheres, belonging to the technical field of fluorescent substance preparation. The method comprises the following steps: carrying out pretreatment to obtain a monomer refined methyl methacrylate and an initiator refined azodiisobutyronitrile, preparing a rare-earth high-luminescent-intensity three-element coordination compound with polymerization activity by a coprecipitation process, copolymerizing the three-element coordination compound with methyl methacrylate to obtain a high-molecular-weight high-polymer rare-earth metal copolymer solid material which is the rare-earth fluorescent microspheres. The example proves that the rare-earth fluorescent microspheres can be used in the aspects of biological detection, fluorescent markers, special-type inks, medical immune detection and cell markers, can not injure the human body, and has stable and efficient luminous emissivity and longer fluorescent lifetime (by 30% or above).

Description

technical field [0001] The invention relates to a preparation method of rare earth fluorescent microspheres, belonging to the technical field of fluorescent powder preparation. Background technique [0002] Fluorescent microspheres refer to solid particles with a diameter ranging from nanometer to micrometer, loaded with fluorescent substances, and can be stimulated by external energy to emit fluorescence. The shape can be any shape, and the typical shape is spherical. The carriers of fluorescent microspheres are mostly organic or inorganic polymer materials, which have a relatively stable morphological structure to stimulate light behavior, and are less affected by external conditions such as solvents, heat, electricity, and magnetism than pure fluorescent compounds. As a new type of carrier material, it has been widely used in the field of biomedicine, such as directional drug delivery in biochemistry and biomedicine, medical latex reagents, biomolecular labeling and traci...

Claims

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Application Information

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IPC IPC(8): C08F220/14C08F230/04C09K11/02C09K11/06
Inventor 郭迎庆林大伟张帆
Owner JIANGSU ZHENYU ENVIRONMENTAL PROTECTION TECH
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