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CN-122011436-A - Polyphenyl ether filler, and preparation method and application thereof

CN122011436ACN 122011436 ACN122011436 ACN 122011436ACN-122011436-A

Abstract

The invention relates to a polyphenyl ether filler, a preparation method and application thereof, and the preparation method comprises the following steps of S1, dissolving poly-2, 6-diphenyl polyphenyl ether in a mixed solution composed of an aprotic polar solvent and organic amine to obtain a polymer solution, S2, dropwise adding concentrated hydrochloric acid into the polymer solution in the step S1, stirring, standing in an environment of-10 ℃, precipitating to obtain a polymer precipitate, S3, adding methanol into a system completely precipitated in the step S2, stirring, filtering, and drying a filtering product to obtain the polyphenyl ether filler, wherein the mass ratio of the poly-2, 6-diphenyl polyphenyl ether, the aprotic polar solvent, the organic amine, the concentrated hydrochloric acid and the methanol is 10-60:30-130:1-4:3-6:20-500. The method greatly simplifies the operation flow, reduces the equipment investment and the production cost, overcomes the problems of rapid and random precipitation of products caused by adding a large amount of poor solvent, ensures that the obtained polyphenyl ether filler has regular morphology, forms a large amount of micropores with uniform structure on the surface, and is suitable for being used as chromatographic filler.

Inventors

  • XU CHEN
  • ZHANG TIANSHU
  • WANG YING
  • LI HONGWEI
  • CHEN WULIAN
  • FANG YUTING

Assignees

  • 上海安谱实验科技股份有限公司
  • 辽宁省农产品及兽药饲料产品检验检测院

Dates

Publication Date
20260512
Application Date
20260324

Claims (8)

  1. 1. The preparation method of the polyphenyl ether filler is characterized by comprising the following steps of: S1, taking poly (2, 6-diphenyl-polyphenyl ether), dissolving the poly (2, 6-diphenyl-polyphenyl ether) in a mixed solution composed of an aprotic polar solvent and an organic amine, and stirring the mixture at a rotating speed of 80-250 r/min for 0.5-5 hours at a temperature of 40-100 ℃ to obtain a polymer solution; S2, dropwise adding concentrated hydrochloric acid into the polymer solution in the step S1 at a constant speed of 5-10 mL/min at a stirring speed of 80-250 revolutions per minute, standing in an environment of-10 ℃ after the dropwise adding is finished, and precipitating to obtain polymer precipitate; s3, adding methanol into the system completely precipitated in the step S2, stirring, filtering, and drying the filtered product to obtain the polyphenyl ether filler; The mass ratio of the poly (2, 6-diphenyl-poly (phenylene oxide), the aprotic polar solvent, the organic amine, the concentrated hydrochloric acid and the methanol is 10-60:30-130:1-4:3-6:20-500; the aprotic polar solvent is one of hexamethylphosphoric triamide, N-methylpyrrolidone and N, N-dimethylacetamide; the organic amine is triethylamine or tetramethyl ethylenediamine.
  2. 2. The method according to claim 1, wherein in step S2, the standing time is 5 to 120 hours.
  3. 3. The method of claim 1, wherein in step S3, the polyphenylene ether filler is further sieved using a vibratory sieving machine.
  4. 4. A polyphenylene ether filler, characterized in that it is prepared according to the preparation method of any one of claims 1 to 3.
  5. 5. The polyphenylene ether filler according to claim 4, wherein the polyphenylene ether filler has a specific surface area of 80 to 130 cm3/g.
  6. 6. The polyphenylene ether filler according to claim 4, wherein the polyphenylene ether filler has a particle size of 35 to 100 mesh.
  7. 7. The polyphenylene ether filler according to claim 4, wherein the polyphenylene ether filler has a number average molecular weight of 15 to 20 ten thousand.
  8. 8. Use of the polyphenylene ether filler according to any one of claims 4 to 6 in chromatographic techniques.

Description

Polyphenyl ether filler, and preparation method and application thereof Technical Field The application relates to the technical field of chromatographic packing, in particular to a polyphenyl ether packing and a preparation method and application thereof. Background The polyphenylene ether polymer synthesized by taking the poly-2, 6-diphenyl-phenyl-ether resin as a precursor has low dielectric constant, excellent thermal stability, good anti-adhesion property, excellent mechanical property and higher dimensional stability, and is often used as engineering structural materials and insulating plastics. In addition, the poly (2, 6-diphenyl ether) resin has remarkable adsorption capacity to organic compounds, especially organic solvents, so that the poly (2, 6-diphenyl ether) resin can be widely applied to the fields of chromatographic separation, environmental pollution control and the like as a commercial adsorption material. Internationally, thermal desorption filler Tenax-TA produced by Buchem corporation, netherlands has been widely adopted and is listed by the U.S. Environmental Protection Agency (EPA) and the National Institute of Occupational Safety and Health (NIOSH) as the designated adsorbent medium for a number of standard analytical methods. The existing method for preparing the poly (2, 6-diphenyl-polyphenyl ether) filler is to add a poor solvent into a reaction liquid to separate out solids. For example, patent cn201410840831.X discloses a method for preparing poly (2, 6-diphenyl) polyphenylene ether spherical particles, which comprises the steps of fully mixing a good solvent solution of poly (2, 6-diphenyl) p-phenylene ether with a poor solvent to form a poly (2, 6-diphenyl) p-phenylene ether suspension, adding the suspension into a hardening solvent to harden, precipitating, filtering, and drying to obtain poly (2, 6-diphenyl) p-phenylene ether spherical particles. However, the method requires peristaltic pumps and special hardening processors, and has high equipment requirements and complicated preparation process. Patent CN03803170.1 discloses a method for precipitating polyphenylene ether particles by rotating a stirring blade to circulate a mixed liquid comprising a good solvent, a poor solvent and polyphenylene ether particles, adding a polyphenylene ether solution to the mixed liquid from a solution supply port at the same time, and adding a poor solvent from a poor solvent supply port, thereby further precipitating polyphenylene ether particles. This method requires precipitation of polyphenylene ether particles using a large amount of poor solvent, and is not suitable for preparing poly (2, 6-diphenyl-polyphenylene ether) having a more rigid structure. The existing preparation method of the polyphenyl ether chromatographic packing has the problems of difficult precipitation of products in poor solvents, complex preparation process, high equipment requirement and the like, and the obtained packing has small surface area, uneven pore structure and unsatisfactory physical form. Disclosure of Invention Based on the above, the application aims to provide a preparation method of polyphenyl ether chromatographic packing, which has the advantages of easy product forming, simple operation, low cost and easy industrial production. In order to achieve the above object, the present application provides a method for preparing polyphenylene ether filler, comprising the steps of: S1, taking poly (2, 6-diphenyl-polyphenyl ether), dissolving the poly (2, 6-diphenyl-polyphenyl ether) in a mixed solution composed of an aprotic polar solvent and organic amine, and stirring at a rotating speed of 80-250 rpm to obtain a polymer solution; S2, dropwise adding concentrated hydrochloric acid into the polymer solution in the step S1 at a constant speed of 5-10 mL/min at a stirring speed of 80-250 revolutions per minute, standing in an environment of-10 ℃ after the dropwise adding is finished, and precipitating to obtain polymer precipitate; s3, adding methanol into the system completely precipitated in the step S2, stirring, filtering, and drying the filtered product to obtain the polyphenyl ether filler; the mass ratio of the poly (2, 6-diphenyl-polyphenylene ether), the aprotic polar solvent, the organic amine, the concentrated hydrochloric acid and the methanol is 10-60:30-130:1-4:3-6:20-500. Preferably, in step S1, stirring is performed at 35-100 ℃ for 0.5-5 hours. More preferably, in step S2, the standing time is 5 to 120 hours. Preferably, the aprotic polar solvent is one of hexamethylphosphoric triamide, N-methylpyrrolidone, and N, N-dimethylacetamide. More preferably, the organic amine is triethylamine or tetramethyl ethylenediamine. Preferably, in step S3, the polyphenylene ether filler is also sieved using a vibratory sieving machine. The application also provides a polyphenyl ether filler, which is prepared by the method of any one of the above. Preferably, the specific surface area of the polyphenyl