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CN-118812247-B - Preparation method of fuse ceramic tube

CN118812247BCN 118812247 BCN118812247 BCN 118812247BCN-118812247-B

Abstract

The invention relates to the technical field of alumina ceramics, and discloses a preparation method of a fuse ceramic tube. Compared with the ceramic tube made of the traditional alumina ceramic material, the ceramic tube of the fuse has excellent toughness and is not easy to be fragile, and the preparation method comprises the following five steps of 1) synthesizing functional monomers containing phosphate, 2) synthesizing HNTs coated by organic silicon, 3) synthesizing HNTs@organic silicon/COF with hydroxyl on the surface, 4) carrying out surface modification on HNTs@organic silicon/COF, then reacting with polysilazane to synthesize reinforcing filler, and 5) taking the reinforcing filler, alumina, glass fiber and silane coupling agent as raw materials, and carrying out ball milling, presintering and sintering to obtain the ceramic tube.

Inventors

  • FANG HAOJIE
  • HE YIWEN
  • ZHANG XIAOYUN
  • ZHANG GUOXIU
  • FANG MEILING
  • LIU JIANPING
  • Zeng xiong

Assignees

  • 湖南省美程陶瓷科技有限公司

Dates

Publication Date
20260505
Application Date
20240731

Claims (7)

  1. 1. The preparation method of the ceramic tube of the fuse is characterized by comprising the following steps: Stirring and mixing chloroplatinic acid in isopropanol uniformly, marking the mixture as a catalyst solution, stirring diethyl allyl phosphate, toluene and the catalyst solution for 1h at 45-55 ℃, heating to 70 ℃, slowly dropwise adding tetramethyl tetrahydrocyciotetrasiloxane under the condition of nitrogen, continuously reacting for 5-8h at 80 ℃ after the dropwise adding is finished, adding active carbon, stirring for 5h at room temperature after the reaction is finished, filtering, and steaming in a rotary mode to obtain a functional monomer; step A2, adding halloysite nanotubes into ethanol, dispersing uniformly, adding tetraethoxysilane, gamma-aminopropyl triethoxysilane and a functional monomer, stirring for 20min, adding deionized water, stirring at 30-40 ℃ for reaction for 3-5h, heating to 115-125 ℃ for continuous reaction for 3-5h, and after the reaction is finished, carrying out suction filtration and drying to obtain HNTs@organosilicon; Step A3, adding 2, 5-diamino-1, 4-dihydroxybenzene dihydrochloride and triethylamine into N, N-dimethylformamide, dispersing uniformly, then adding cyanuric chloride and HNTs@organosilicon for 30min, transferring to an autoclave, reacting for 12h at 120 ℃, washing and drying after the reaction is finished to obtain HNTs@organosilicon/COF; Step A4, uniformly stirring and dispersing HNTs@organic silicon/COF and triethylamine in N, N-dimethylformamide, adding acryloyl chloride under the ice water bath condition, raising the temperature to 30-40 ℃ and stirring for reacting for 2-3 hours, after the reaction is finished, carrying out suction filtration, collecting a product, uniformly stirring and dispersing the product, polysilazane and a Kanster platinum catalyst in toluene, and carrying out stirring and reacting for 3-5 hours under the condition that the temperature is 60-70 ℃ C, pH is 1-2, and carrying out suction filtration and drying to obtain the reinforcing filler; And step A5, mixing reinforcing filler, alumina, glass fiber, a silane coupling agent and ethanol, ball milling for 5 hours at a rotating speed of 200-400rpm, raising the system temperature to 90-100 ℃, maintaining the temperature for 12 hours, transferring into a mould, sintering for 1-2 hours at 40-45MPa and 1000-1100 ℃, sintering for 2 hours at 1450-1550 ℃, and cooling to room temperature to obtain the fuse ceramic tube.
  2. 2. The method for preparing a ceramic tube for a fuse according to claim 1, wherein the dosage ratio of allyl diethyl phosphate, toluene, catalyst solution, tetramethyl tetra-hydro-cyclotetrasiloxane and activated carbon in the step A1 is 0.041-0.1mol:20-40mL:5-8g:1mol:1-2g.
  3. 3. The method for preparing a ceramic tube for a fuse according to claim 2, wherein the mass ratio of chloroplatinic acid to isopropanol in the catalyst solution is 0.1:100.
  4. 4. The method for preparing a ceramic tube for a fuse according to claim 1, wherein the dosage ratio of halloysite nanotube, ethanol, ethyl orthosilicate, gamma-aminopropyl triethoxysilane, functional monomer and deionized water in the step A2 is 2-4 g/50 mL/2-3 g/0.5-1.5 g/0.3-0.6 g/10 mL.
  5. 5. The method for preparing a ceramic tube for a fuse according to claim 1, wherein the 2, 5-diamino-1, 4-dihydroxybenzene dihydrochloride, triethylamine, N-dimethylformamide, cyanuric chloride and HNTs@organosilicon are used in the amount ratio of 0.1-0.2mol:15mL:200mL:0.05-0.1mol:0.5-1.2g in the step A3.
  6. 6. The method for preparing a ceramic tube for a fuse according to claim 1, wherein the HNTs@organosilicon/COF, triethylamine, N-dimethylformamide and acryloyl chloride in the step A4 are used in an amount ratio of 1-3g:1-2mL:100mL:5-10mL, and the product, polysilazane, a Karster platinum catalyst and toluene are used in an amount ratio of 0.5-1.5g:10-30g:0.01-0.03g:200mL.
  7. 7. The method for preparing a ceramic tube for a fuse according to claim 1, wherein the mass ratio of reinforcing filler, alumina, glass fiber, silane coupling agent and ethanol in the step A5 is 3-6:25:1-2:0.05-0.15:25.

Description

Preparation method of fuse ceramic tube Technical Field The invention relates to the technical field of alumina ceramics, in particular to a preparation method of a fuse ceramic tube. Background The fuse is a component for protecting a circuit, and is widely used in various electronic equipment such as televisions, refrigerators, air conditioners, washing machines and the like, and the common fuse comprises a tubular shell, an in-tube fuse, a copper cap, a pin wire and external integrally encapsulated epoxy resin. Most of the tubular shell materials are made of glass or ceramic materials, wherein the glass tube has the defects of poor heat conductivity, poor heat dissipation effect and fragility, and therefore, the tubular shell materials have certain limitations in practical application. The aluminum oxide ceramic material is used for preparing the shell, so that the problems of poor heat conductivity and poor heat dissipation effect of the glass tube can be solved, but when the aluminum oxide ceramic material is impacted by external force, the tube body is broken due to poor toughness of the aluminum oxide ceramic material. The toughening mechanism of the alumina ceramic material mainly comprises three aspects of bridging mechanism, pulling mechanism and crack deflection, so that researchers can further improve the toughness of the material by utilizing the synergistic effect among the three mechanisms, so that the material has excellent toughness, and crushing caused by poor toughness is avoided. Disclosure of Invention In order to solve the technical problems, the invention provides a preparation method of a fuse ceramic tube. The aim of the invention can be achieved by the following technical scheme: a preparation method of a fuse ceramic tube comprises the following steps: Stirring and mixing chloroplatinic acid in isopropanol uniformly, marking the mixture as a catalyst solution, stirring diethyl allyl phosphate, toluene and the catalyst solution for 1h at 45-55 ℃, heating to 70 ℃, slowly dropwise adding tetramethyl tetrahydrocyciotetrasiloxane under the condition of nitrogen, continuously reacting for 5-8h at 80 ℃ after the dropwise adding is finished, adding active carbon, stirring for 5h at room temperature after the reaction is finished, filtering, and steaming in a rotary mode to obtain a functional monomer; A2, adding Halloysite Nanotubes (HNTs) into ethanol, dispersing uniformly, adding tetraethoxysilane, gamma-aminopropyl triethoxysilane and a functional monomer, stirring for 20min, adding deionized water, stirring at 30-40 ℃ for reaction for 3-5h, heating to 115-125 ℃ for continuous reaction for 3-5h, and after the reaction is finished, carrying out suction filtration and drying to obtain HNTs@organosilicon; Step A3, adding 2, 5-diamino-1, 4-dihydroxybenzene dihydrochloride and triethylamine into N, N-dimethylformamide, dispersing uniformly, then adding cyanuric chloride and HNTs@organosilicon for 30min, transferring to an autoclave, reacting for 12h at 120 ℃, washing and drying after the reaction is finished to obtain HNTs@organosilicon/COF; Step A4, uniformly stirring and dispersing HNTs@organic silicon/COF and triethylamine in N, N-dimethylformamide, adding acryloyl chloride under the ice water bath condition, raising the temperature to 30-40 ℃ and stirring for reacting for 2-3 hours, after the reaction is finished, carrying out suction filtration, collecting a product, uniformly stirring and dispersing the product, polysilazane and a Kanster platinum catalyst in toluene, and carrying out stirring and reacting for 3-5 hours under the condition that the temperature is 60-70 ℃ C, pH is 1-2, and carrying out suction filtration and drying to obtain the reinforcing filler; Step A5, mixing reinforcing filler, alumina, glass fiber, silane coupling agent and ethanol, ball milling for 5 hours at a rotating speed of 200-400rpm, raising the temperature of the system to 90-100 ℃, maintaining the temperature for 12 hours, transferring into a mould, sintering for 1-2 hours at 40-45MPa and 1000-1100 ℃, sintering for 2 hours at 1450-1550 ℃, and cooling to room temperature to obtain the fuse ceramic tube; further, in the step A1, the dosage ratio of the diethyl allyl phosphate, toluene, the catalyst solution, the tetramethyl tetrahydrocyclotetrasiloxane and the activated carbon is 0.041-0.1mol:20-40mL:5-8g:1mol:1-2g, and the mass ratio of chloroplatinic acid to isopropanol in the catalyst solution is 0.1:100; Further, in the step A2, the dosage ratio of the halloysite nanotube, ethanol, tetraethoxysilane, gamma-aminopropyl triethoxysilane, functional monomer and deionized water is 2-4g:50mL:2-3g:0.5-1.5g:0.3-0.6g:10mL; Further, in the step A3, the dosage ratio of the 2, 5-diamino-1, 4-dihydroxybenzene dihydrochloride, triethylamine, N-dimethylformamide, cyanuric chloride and HNTs@organosilicon is 0.1-0.2mol:15mL:200mL:0.05-0.1mol:0.5-1.2g; Further, in the step A4, the dosage ratio of HNTs@organosilicon/CO