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CN-122011036-A - Epoxy resin and preparation method thereof, glue composition and packaging adhesive film

CN122011036ACN 122011036 ACN122011036 ACN 122011036ACN-122011036-A

Abstract

In order to improve the high light transmittance, long-acting ultraviolet aging resistance and permanent high reliability of the flame-retardant epoxy resin packaging material, the invention provides epoxy resin, wherein the chemical formula of the epoxy resin is shown as formula 1: In formula 1, any two of R 1 -R 6 are selected from glycidyl ether, and the rest are selected from H.

Inventors

  • KONG BEIBEI
  • ZHOU SHAOHONG
  • WU JIAHUA
  • HAN JIHUI
  • ZHENG HAITING

Assignees

  • 广州慧谷新材料科技股份有限公司

Dates

Publication Date
20260512
Application Date
20260213

Claims (10)

  1. 1. An epoxy resin is characterized in that the chemical formula of the epoxy resin is shown as formula 1: The method comprises the steps of (1), In formula 1, any two of R 1 -R 6 are selected from glycidyl ether, and the rest are selected from H.
  2. 2. The epoxy resin of claim 1, wherein each R 1 、R 4 is independently selected from the group consisting of epoxypropyl ethers.
  3. 3. The method for producing an epoxy resin according to claim 1 or 2, comprising the steps of: dissolving hexachlorocyclotriphosphazene and phenol in a first solvent, adding an acid binding agent, and reacting to generate dichloro-tetra (phenoxy) cyclotriphosphazene; Dissolving dichloro-tetra (phenoxy) cyclotriphosphazene in a second solvent, adding hydroquinone and an acid binding agent for reaction to generate bis (4-hydroxy phenoxy) -tetra (phenoxy) cyclotriphosphazene; Dissolving bis (4-hydroxyphenoxy) -tetra (phenoxy) cyclotriphosphazene, epichlorohydrin and a catalyst in a third solvent for reaction, and carrying out ring opening etherification to obtain a solution containing an intermediate; And adding an alkali solution into the solution containing the intermediate to react to obtain the epoxy resin shown in the formula 1.
  4. 4. The method according to claim 3, wherein the mole ratio of hexachlorocyclotriphosphazene to phenol is 1:4 to 1:4.2, and/or, The mol ratio of the dichloro-tetra (phenoxy) cyclotriphosphazene to the benzenediol is 1:2-1:2.2, and/or, The molar ratio of the bis (4-hydroxyphenoxy) -tetra (phenoxy) cyclotriphosphazene to the epichlorohydrin is 1:2-1:8.
  5. 5. The method of preparing according to claim 3, wherein the step of generating dichloro-tetra (phenoxy) cyclotriphosphazene further comprises: Dissolving hexachlorocyclotriphosphazene and phenol in a first solvent, adding an acid binding agent, reacting for 3-4 hours at the temperature of minus 10-0 ℃, and then heating to 30-40 ℃ for reacting for 16-20 hours.
  6. 6. A method of preparation according to claim 3, wherein the acid binding agent comprises triethylamine; The catalyst comprises one or more of tetrabutylammonium bromide, tetraoctylammonium bromide and benzyl triethyl ammonium chloride, and/or, The alkali solution comprises one or two of sodium hydroxide solution and potassium hydroxide solution, and the mass concentration of the alkali solution is 20% -30%.
  7. 7. A glue composition comprising a bisphenol a epoxy resin, a curing agent and a functional epoxy resin, wherein the functional epoxy resin is an epoxy resin as defined in claim 1 or 2.
  8. 8. The glue composition according to claim 7, comprising the following components, by weight, 55-70 parts of bisphenol A epoxy resin, 20-30 parts of functional epoxy resin and 20-40 parts of curing agent.
  9. 9. The glue composition of claim 7, further comprising 5-15 parts of an epoxy diluent, 0.2-2 parts of a coupling agent, 0.2-2 parts of an antioxidant, and 0.2-2 parts of an ultraviolet absorber.
  10. 10. An encapsulating adhesive film, characterized in that the encapsulating adhesive film comprises the glue composition according to any one of the claims 7-9.

Description

Epoxy resin and preparation method thereof, glue composition and packaging adhesive film Technical Field The invention relates to the technical field of optical cement, in particular to epoxy resin, a preparation method thereof, a glue composition and a packaging adhesive film. Background The epoxy resin is widely applied to LED packaging by virtue of excellent performance, but with the development of Mini/Micro LED display technology, the packaging material needs to meet high optical transparency, for example, the light transmittance is generally more than 90% at 550 nm wavelength, the haze is lower than 2% so as to ensure the definition and brightness of a display picture, the epoxy resin has excellent ultraviolet aging resistance so as to ensure the service life exceeding 50000 hours and avoid yellowing and performance degradation, and meanwhile, the epoxy resin also needs to have permanent and reliable high flame retardant level, for example, the UL-94V-0 standard is met, and the flame retardant performance is not attenuated and not migrated in long-term use. The existing mainstream flame retardant modification scheme has obvious defects that the high addition amount of the flame retardant can seriously damage the light transmittance and mechanical strength of the material, for example, the light transmittance can be reduced from 90% to below 70% by adding 20% of aluminum hydroxide, and the small molecular flame retardant is easy to migrate and separate out, so that the haze is increased and the flame retardant durability is reduced. While the DOPO-based reactive flame retardant scheme improves the migration problem, the flame retardant efficiency is lower, the phosphorus content of 2-4% is generally needed, the synergistic effect is lacked, meanwhile, the molecular structure of the DOPO-based reactive flame retardant scheme is easy to cause that the light transmittance is difficult to break through 91%, yellowing occurs under ultraviolet light, and the long-acting aging-resistant requirement cannot be met. Therefore, there is a need for an epoxy resin encapsulation material that combines high light transmittance, long-term uv aging resistance, and permanent high reliability flame retardance. Disclosure of Invention The invention aims to provide epoxy resin, a preparation method thereof, a glue composition and an encapsulation adhesive film, so as to solve the problem that the flame retardance, the transparency, the reliability and the processability of the encapsulation adhesive film cannot be balanced in the prior art. The technical scheme adopted by the invention for solving the technical problems is as follows: in a first aspect, the present invention provides an epoxy resin having a chemical formula shown in formula 1: The method comprises the steps of (1), In formula 1, any two of R 1-R6 are selected from glycidyl ether, and the rest are selected from H. Alternatively, each R 1、R4 is independently selected from the group consisting of epoxypropyl ethers. In a second aspect, the present invention provides a method for preparing the epoxy resin, comprising the steps of: dissolving hexachlorocyclotriphosphazene and phenol in a first solvent, adding an acid binding agent, and reacting to generate dichloro-tetra (phenoxy) cyclotriphosphazene; Dissolving dichloro-tetra (phenoxy) cyclotriphosphazene in a second solvent, adding hydroquinone and an acid binding agent for reaction to generate bis (4-hydroxy phenoxy) -tetra (phenoxy) cyclotriphosphazene; Dissolving bis (4-hydroxyphenoxy) -tetra (phenoxy) cyclotriphosphazene, epichlorohydrin and a catalyst in a third solvent for reaction, and carrying out ring opening etherification to obtain a solution containing an intermediate; And adding an alkali solution into the solution containing the intermediate to react to obtain the epoxy resin shown in the formula 1. Optionally, the mole ratio of hexachlorocyclotriphosphazene to phenol is 1:4-1:4.2, and/or, The mol ratio of the dichloro-tetra (phenoxy) cyclotriphosphazene to the benzenediol is 1:2-1:2.2, and/or, The molar ratio of the bis (4-hydroxyphenoxy) -tetra (phenoxy) cyclotriphosphazene to the epichlorohydrin is 1:2-1:8. Optionally, the step of generating dichloro-tetra (phenoxy) cyclotriphosphazene further comprises: Dissolving hexachlorocyclotriphosphazene and phenol in a first solvent, adding an acid binding agent, reacting for 3-4 hours at the temperature of minus 10-0 ℃, and then heating to 30-40 ℃ for reacting for 16-20 hours. Optionally, the acid binding agent comprises triethylamine; the catalyst comprises one or more of tetrabutylammonium bromide, tetraoctylammonium bromide and benzyl triethyl ammonium chloride, and/or, The alkali solution comprises one or two of sodium hydroxide solution and potassium hydroxide solution, and the mass concentration of the alkali solution is 20% -30%. In a third aspect, the present invention provides a glue composition comprising bisphenol a epoxy resin, a curing a