Method for preparing polyphenyl acetylene microballoon spheres

A technology for poly(p-phenylene vinylene) and microspheres is applied in the field of preparation of poly(p-phenylene vinylene) microspheres, which can solve the problems of lack of uniform size microspheres and the like, and achieve the effects of simple production, low energy consumption, and wide application.

Inactive Publication Date: 2013-10-16
HEILONGJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The purpose of the present invention is to solve the problem that existing poly(p-phenylene vinylene) has no microspheres of uniform size in the molding material, and the invention provides a preparation method of poly(p-phenylene vinylene microspheres)

Method used

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  • Method for preparing polyphenyl acetylene microballoon spheres
  • Method for preparing polyphenyl acetylene microballoon spheres
  • Method for preparing polyphenyl acetylene microballoon spheres

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specific Embodiment approach 1

[0014] Specific embodiment one: present embodiment is the preparation method of poly(p-phenylene vinylene vinylene microsphere), and it is realized by following steps: 1, the preparation of disulfide salt: be 1g according to the mass volume ratio of dichloromethylbenzene and tetrahydrofuran: 1.3 ~ 1.6mL, the volume ratio of methanol and tetrahydrofuran is 10:1, weigh dichloromethylbenzene, methanol and tetrahydrofuran respectively, then mix dichloromethylbenzene, methanol and tetrahydrofuran to obtain a mixed solution, and then mix the The temperature of the solution is raised to 50-60°C, then kept at a constant temperature for 6-10 hours, then cooled to room temperature, and then distilled under reduced pressure until the volume is one-third of the original volume, and the concentrated solution is obtained after cooling to room temperature, and then the concentrated solution is used for The acetone at ℃ is reverse-precipitated to obtain a precipitate, and then the precipitate ...

specific Embodiment approach 2

[0026] Specific embodiment 2: The difference between this embodiment and specific embodiment 1 is that in step 1, the reduced-pressure distillation adopts a rotary evaporator and is carried out in a constant temperature water bath at 30° C. to 40° C. Other steps and parameters are the same as those in Embodiment 1.

specific Embodiment approach 3

[0027] Specific embodiment 3: The difference between this embodiment and specific embodiment 1 or 2 is that in step 1, the specific operation steps of reprecipitating the concentrated solution with acetone at 0-5°C are as follows: take acetone at 0-5°C into the container, Then use a pipette to add the concentrated solution dropwise to the acetone at 0-5°C, stir, and filter to obtain a precipitate, wherein the volume ratio of the dropwise amount of the concentrated solution to the acetone at 0-5°C is 1: 10-15. Other steps and parameters are the same as those in Embodiment 1 or Embodiment 2.

[0028] In this embodiment, preferably, 10-15 mL of the concentrated solution is added dropwise to 150 mL of acetone at 0-5° C. for reverse precipitation. Only take 10-15mL of the concentrated solution each time until the concentrated solution is reverse-precipitated completely.

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Abstract

The invention discloses a method for preparing polyphenyl acetylene microballoon spheres, relates to a method for preparing a fluorescent polymer microballoon sphere material and solves the problem of no microballoon spheres with uniform sizes in a forming material of the existing polyphenyl acetylene. The method comprises the following steps of: preparing double-sulfonium salt from benzyl bichloride, methanol and tetrahydrofuran; then after mixing the double-sulfonium salt and methanol, adding sodium hydroxide to perform reaction; after neutralizing by hydrochloric acid, dialyzing and concentrating to obtain aqueous solution of a polyphenyl acetylene precursor; filling the aqueous solution and silicone oil into a microflow control system; pushing the aqueous solution and the silicone oil into a rotary atmometer to obtain liquid beads; curing the liquid beads to obtain the polyphenyl acetylene microballoon spheres; or adding silica particles into the aqueous solution of the polyphenyl acetylene precursor to obtain aqueous solution of a composite precursor so as to prepare the composite microballoon spheres obtained by compounding polyphenyl acetylene with the silica particles. The monodisperse polyphenyl acetylene microballoon spheres with consistent appearances and uniform sizes are prepared and the gap that in the prior art, the preparation of the polyphenyl acetylene microballoon spheres cannot be realized is filled. The microballoon spheres can be applied to the fields of a photoelectric display material and a luminescent device.

Description

technical field [0001] The invention relates to a preparation method of a fluorescent polymer microsphere material, in particular to a preparation method of polyp-phenylene vinylene (PPV) microspheres. Background technique [0002] As a conjugated polymer, polyphenylene vinylene has very good photoluminescence and electroluminescence properties as well as good photoelectric and nonlinear optical properties. This series of excellent properties makes it widely used in real life. So far, scientists have improved some of their properties to realize their applications in various fields. Generally speaking, few studies have been conducted on the influence of the luminescent properties of nanomaterials composed of conjugated polymer poly(phenylene vinylene, abbreviated as PPV) and inorganic nanoparticles. There is even less work to prepare this polymer into spherical particles, and there is no literature on the preparation of composite microspheres of this polymer and inorganic n...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08J3/12C08L65/00
Inventor 孙立国赵冬梅汪成王彦杰王明强张艳红
Owner HEILONGJIANG UNIV
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