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CN-122011678-A - Preparation method of LED lamp bead rubber sleeve

CN122011678ACN 122011678 ACN122011678 ACN 122011678ACN-122011678-A

Abstract

The invention discloses a preparation method of an LED lamp bead rubber sleeve, which comprises the steps of weighing 100-120 parts of functionalized resin, 5-10 parts of modified boron nitride, 1-3 parts of modified additive, 10-15 parts of triethylene tetramine and 0.1-0.3 part of ammonium persulfate, uniformly mixing the raw materials and injecting the raw materials into a die, heating and preserving heat to prepare the LED lamp bead rubber sleeve, wherein epoxy groups on the functionalized resin react with the triethylene tetramine to form a grid structure when the raw materials are mixed and heated, and under the action of ammonium persulfate, double bonds on a side chain of the functionalized resin, double bonds on the modified boron nitride and double bonds on the modified additive are subjected to free radical polymerization, so that a compact interpenetrating network is formed by the molecular structure, the glass transition temperature is improved, and meanwhile, the main chain is polysiloxane, so that the prepared rubber sleeve has a good high-temperature oxidation resistant effect, and a hindered amine structure on the modified additive can continuously capture and neutralize free radicals which cause thermal oxidation of the epoxy resin.

Inventors

  • ZHAO RUSHUANG

Assignees

  • 吉安华翌电子有限公司

Dates

Publication Date
20260512
Application Date
20260311

Claims (8)

  1. 1. The preparation method of the LED lamp bead rubber sleeve is characterized by comprising the following steps of: Step A1, D-glucose is dissolved in deionized water, and is stirred and added with hexagonal boron nitride, and is stirred to prepare pretreated boron nitride, and pretreated boron nitride, ethanol and deionized water are mixed and stirred and added with methacryloxypropyl trimethoxy silane for reaction to prepare modified boron nitride; A2, mixing the modified epoxy resin, cis-5-dodecenoic acid, hydroquinone and dimethylbenzene, introducing nitrogen for protection, stirring, adding pyridinium p-toluenesulfonate, and reacting to obtain functional resin; Step A3, mixing and stirring cyanuric chloride and anhydrous acetone, adding 1,2, 6-pentamethylpiperidinol, sodium hydroxide aqueous solution and tetrabutylammonium bromide for reaction, heating, adding allyl alcohol and hydroquinone, and continuing to react to obtain a modified additive; And step A4, weighing the following raw materials, by weight, 100-120 parts of functionalized resin, 5-10 parts of modified boron nitride, 1-3 parts of modified additive, 10-15 parts of triethylene tetramine and 0.1-0.3 part of ammonium persulfate, uniformly mixing the raw materials, injecting the mixture into a mold, and heating and preserving heat to obtain the LED lamp bead rubber sleeve.
  2. 2. The method for preparing the LED lamp bead gum cover according to claim 1, wherein the dosage ratio of D-glucose solution, deionized water and hexagonal boron nitride in the step A1 is 15g:20mL:3g, and the dosage of methacryloxypropyl trimethoxysilane is 5% of the mass of the pretreated boron nitride.
  3. 3. The method for preparing the LED lamp bead rubber sleeve according to claim 1, wherein the molar ratio of the hydroxyl group on the modified epoxy resin to the cis-5-dodecenoic acid in the step A2 is 1:1.
  4. 4. The method for preparing the LED lamp bead gum cover according to claim 1, wherein the amount of cyanuric chloride, 1,2, 6-pentamethylpiperidinol, aqueous sodium hydroxide solution, tetrabutylammonium bromide and allyl alcohol in the step A3 is 1mol:2mol:500mL:0.03mol:1mol.
  5. 5. The method for preparing the LED lamp bead rubber sleeve according to claim 1, wherein the modified epoxy resin comprises the following steps: Step B1, mixing thioglycerol, triethylamine and anhydrous dichloromethane, introducing nitrogen for protection, stirring, adding trityl chloride, heating for reaction to obtain modified glycerol, mixing and stirring the modified glycerol and tetrahydrofuran, adding sodium hydride, stirring for treatment, heating, adding 1, 3-dichloro-2-propanol for reaction, cooling, adding sodium hydroxide aqueous solution for reaction, and obtaining a modifier; Step B2, mixing the intermediate with anhydrous dichloromethane, introducing nitrogen for protection, stirring, adding trimethylsilicon iodine, reacting to obtain a modifier, mixing lithium dimethylvinylsilanol with tetrahydrofuran, introducing nitrogen for protection, stirring, adding tetramethylcyclotetrasiloxane, heating for reaction, adding tetrachlorosilane, and continuing to react to obtain branched polysiloxane; And B3, mixing branched polysiloxane, a modifier, benzophenone and DMF (dimethyl formamide) for ultraviolet irradiation reaction to obtain pretreated epoxy resin, mixing the pretreated epoxy resin, allyl alcohol, a Kadster catalyst and DMF, introducing nitrogen for protection, and reacting to obtain the modified epoxy resin.
  6. 6. The method for preparing the LED lamp bead gum cover according to claim 5, wherein the molar ratio of the thioglycerol, the triethylamine and the triphenylmethyl chloride in the step B1 is 1:1:1, and the dosage ratio of the modified glycerol, the sodium hydride, the 1, 3-dichloro-2-propanol and the sodium hydroxide aqueous solution is 1mmol:2 mmol:15mL.
  7. 7. The method of claim 5, wherein the molar ratio of the intermediate to the trimethylsilyl iodide in the step B2 is 1:1.2, and the molar ratio of the dimethyl vinyl silanol lithium, the tetramethyl cyclotetrasiloxane and the Si-Cl bond on the tetrachlorosilane is 1:3:1.
  8. 8. The method for preparing the LED lamp bead rubber sleeve according to claim 5, wherein the molar ratio of the branched polysiloxane to the modifier in the step B3 is 1:4, and the molar ratio of Si-H bonds to allyl alcohol on the pretreated epoxy resin is 1:1.

Description

Preparation method of LED lamp bead rubber sleeve Technical Field The invention relates to the technical field of gum cover preparation, in particular to a preparation method of an LED lamp bead gum cover. Background The performance and lifetime of led as a new generation solid state light source are not only dependent on the chip itself, but also related to the packaging protection material. The LED lamp bead rubber sleeve, namely the packaging colloid, is a key material directly coated on the periphery of the LED chip and has multiple core functions of protecting the chip and a circuit, leading out heat, optically matching, insulating protection, resisting environmental corrosion and the like. Epoxy resins are widely used for conventional LED packages, and are mainstream due to excellent adhesion, high insulation, easy workability, and low cost. However, as the LED technology is developed to high power, high brightness and small size, and the application field is expanded to the fields of high requirements such as outdoor illumination, automobile headlights and the like, the inherent defects of the conventional epoxy resin are increasingly prominent, and particularly, the conventional epoxy resin faces serious challenges on the long-term thermal oxidative aging performance. Research shows that the conventional epoxy resin is easy to oxidize and degrade molecular chains under the action of long-term heat and ultraviolet light, and is characterized by colloid yellowing, light transmittance reduction, brittleness increase and interface layering, and finally LED light output attenuation, color temperature drift and even failure are caused. Disclosure of Invention The invention aims to provide a preparation method of an LED lamp bead rubber sleeve, which solves the problem that the LED lamp bead rubber sleeve is poor in heat resistance and ageing resistance at the present stage. The aim of the invention can be achieved by the following technical scheme: the preparation method of the LED lamp bead rubber sleeve specifically comprises the following steps: Dissolving D-glucose in deionized water, stirring and adding hexagonal boron nitride at the rotation speed of 200-300r/min and the temperature of 25-30 ℃, stirring for 2-3 hours to obtain pretreated boron nitride, uniformly mixing the pretreated boron nitride, ethanol and deionized water, stirring and adding methacryloxypropyl trimethoxysilane at the rotation speed of 150-200r/min and the temperature of 75-80 ℃ to react for 5-7 hours to obtain modified boron nitride; A2, mixing the modified epoxy resin, cis-5-dodecenoic acid, hydroquinone and dimethylbenzene, introducing nitrogen for protection, stirring at the rotating speed of 150-200r/min and the temperature of 70-80 ℃ and adding pyridinium p-toluenesulfonate for reaction for 6-8 hours to obtain functional resin; Step A3, mixing cyanuric chloride and anhydrous acetone, stirring and adding 1,2, 6-pentamethylpiperidinol, sodium hydroxide aqueous solution and tetrabutylammonium bromide at the rotating speed of 200-300r/min and the temperature of 0-5 ℃ for reacting for 2-3 hours, heating to 40-50 ℃, continuing to react for 4-6 hours, heating to 80-90 ℃, adding allyl alcohol and hydroquinone, and continuing to react for 3-5 hours to obtain a modified additive; And step A4, weighing the following raw materials, by weight, 100-120 parts of functionalized resin, 5-10 parts of modified boron nitride, 1-3 parts of modified additive, 10-15 parts of triethylene tetramine and 0.1-0.3 part of ammonium persulfate, uniformly mixing the raw materials, injecting the mixture into a die, carrying out heat preservation treatment for 1-1.5h at 60-70 ℃, then heating to 110-120 ℃, and carrying out heat preservation treatment for 6-8h to obtain the LED lamp bead rubber sleeve. Further, the dosage ratio of D-glucose solution, deionized water and hexagonal boron nitride in the step A1 is 15g:20mL:3g, and the dosage of methacryloxypropyl trimethoxysilane is 5% of the mass of the pretreated boron nitride. Further, the molar ratio of hydroxyl groups to cis-5-dodecenoic acid on the modified epoxy resin in the step A2 is 1:1, the dosage of hydroquinone is 0.05-0.1% of the mass of cis-5-dodecenoic acid, and the dosage of pyridine p-toluenesulfonate is 3% of the mass of cis-5-dodecenoic acid. Further, the amount of cyanuric chloride, 1,2, 6-pentamethylpiperidinol, aqueous sodium hydroxide solution, tetrabutylammonium bromide and allyl alcohol in the step A3 is 1mol:2mol:500mL:0.03mol:1mol, the amount of hydroquinone is 0.05% of the mass of allyl alcohol, and the mass fraction of the aqueous sodium hydroxide solution is 20%. Further, the modified epoxy resin comprises the following steps: Step B1, mixing thioglycerol, triethylamine and anhydrous dichloromethane, introducing nitrogen for protection, stirring and adding trityl chloride at the rotation speed of 150-200r/min and the temperature of 0-5 ℃, heating to 20-25 ℃, reacting for 2-3 hours