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CN-122011713-A - High-performance LCP resin and preparation method thereof

CN122011713ACN 122011713 ACN122011713 ACN 122011713ACN-122011713-A

Abstract

The present invention discloses a high-performance LCP resin and its preparation method, which relates to the technical field of LCP resin. The present invention uses p-hydroxybenzoic acid, p-tert-butylcatechol, and 5-vinylisophthalic acid as key monomers to synthesize LCP base resins with side chains containing double bonds and tertiary butyl groups. These resins are then melt extruded with ene terminated polyarylesters to produce high-performance LCP resins. By introducing high steric hindrance side groups and reactive double bonds into the macromolecular chains and forming micro crosslinked structures with ene terminated polyarylesters during processing, the excessive orientation of the molecular chains is effectively suppressed, anisotropy is reduced, melt strength and processability are significantly improved, and the resulting resin combines high mechanical properties and improved toughness, making it particularly suitable for preparing high-performance LCP materials.

Inventors

  • FAN AIMIN
  • FAN YULIN

Assignees

  • 红钰电子材料(无锡)有限公司

Dates

Publication Date
20260512
Application Date
20260311

Claims (9)

  1. 1. A method for preparing a high performance LCP resin, comprising the steps of: (1) Mixing a monomer mixture comprising p-hydroxybenzoic acid, p-tert-butylcatechol and 5-vinyl isophthalic acid with acetic anhydride and magnesium acetate, and carrying out a first polymerization reaction under the protection of inert gas to obtain a prepolymer; (2) The LCP resin, the polyarylate and the auxiliary agent are mixed and are subjected to melt extrusion to obtain the high-performance LCP resin.
  2. 2. The method for preparing a high-performance LCP resin according to claim 1, wherein the mass ratio of p-hydroxybenzoic acid, p-tert-butylcatechol, 5-vinylisophthalic acid, acetic anhydride, and magnesium acetate in step (1) is 650-970:105-230:230-422:1110-1130:0.07-0.09.
  3. 3. The method for preparing a high-performance LCP resin according to claim 1, wherein the first polymerization reaction in step (1) is performed by heating the reaction system to 140-150 ℃ under the protection of nitrogen for 2-3 hours, then heating to 350-360 ℃ at a constant speed within 2-3 hours, and continuing the reaction at 350-360 ℃ for 0.5-1 hour, and the second polymerization reaction is performed under the conditions of 330-340 ℃ and 40Pa of vacuum degree for 10 hours.
  4. 4. The method of claim 1, wherein the polyarylate in step (2) is an enary polyarylate.
  5. 5. The method of claim 1, wherein the auxiliary agent in step (2) is an initiator.
  6. 6. The method for preparing a high performance LCP resin according to claim 5, wherein the initiator is a peroxide thermal initiator selected from one or more of t-butyl peroxypivalate, t-butyl peroxy-2-ethylhexanoate, t-butyl hydroperoxide, di-t-butyl peroxide, di-t-amyl peroxide, t-butyl peroxymaleate, t-butyl peroxybenzoate, t-butyl peroxyoctopamoate, bis (3-methoxybutyl) peroxydicarbonate, bis (ethoxyhexyl) peroxydicarbonate, 1, 3-tetramethylbutyl peroxyneodecanoate, bis (4-t-butylcyclohexyl) peroxydicarbonate, and diisopropyl peroxydicarbonate.
  7. 7. The method for preparing a high performance LCP resin according to claim 1, wherein the polyarylate is added in the amount of 1-10% by mass of the LCP resin in the step (2), and the initiator is added in the amount of 0.01-0.05% by mass of the total mass of the LCP resin and the polyarylate.
  8. 8. The method for producing a high-performance LCP resin according to claim 1, wherein said melt extrusion in step (2) is performed by a twin screw extruder.
  9. 9. A high performance LCP resin made according to the preparation method of any one of claims 1 to 8.

Description

High-performance LCP resin and preparation method thereof Technical Field The invention relates to the technical field of LCP resins, in particular to a high-performance LCP resin and a preparation method thereof. Background Liquid Crystal Polymers (LCPs) are a class of specialty high performance engineering plastics that remain in a partially ordered structure in the molten or solution state. Because of their high molecular chains being easily oriented in the flow direction during processing, LCPs exhibit excellent mechanical properties, dimensional stability, heat resistance, chemical resistance, and extremely low dielectric constants and dielectric losses, and are therefore widely used in the fields of electronics and electrical, high frequency communications, precision instruments, aerospace, and the like, especially as key materials for 5G communications, high speed connectors, integrated circuit packages, and high frequency substrate films. However, while possessing the above advantages, conventional wholly aromatic LCP has some inherent limitations, which severely restrict its application in precision parts such as high performance films. First, the high degree of orientation of the LCP molecular chains during melt processing can result in significant differences in the mechanical, thermal expansion, etc. properties of the article in the flow direction versus the perpendicular direction, i.e., strong anisotropies. This anisotropy makes LCP films prone to deformation, warpage and even cracking during subsequent processing or use due to uneven stress distribution, and it is difficult to obtain products with uniform thickness and balanced properties. Secondly, the crystallization speed of LCP is faster, the rigidity of molecular chains is large, entanglement is less, the melt strength is generally lower, the melt is easy to break in the processing processes of film blowing, film drawing and the like, the processing window is narrow, the film forming process is difficult to control, and the preparation of high-quality films is limited. Furthermore, although LCP has high strength and modulus, it generally has low elongation at break, which is manifested as brittle material characteristics, and toughness is to be improved. In addition, to improve specific properties, it is sometimes necessary to introduce bulky side groups, but this is often accompanied by a decrease in crystallinity of the material and a loss of mechanical properties, and how to effectively regulate its aggregation state structure, improve processability and anisotropy while maintaining inherent high properties of LCP is a major challenge in the current LCP material development. In view of the above problems, improvements are generally made in the prior art by methods such as modification by copolymerization, addition of fillers, or blending with other polymers. For example, the crystallization behavior is regulated by introducing monomers of different structures for copolymerization to break the regularity of molecular chains, or the mechanical properties are enhanced and the anisotropy is reduced by adding inorganic fillers and fibers. However, these methods tend to have limited effectiveness or present new problems in that simple copolymerization modification may significantly reduce the heat resistance and rigidity of the material, and the addition of fillers may increase the material density, affect the processing flowability, and may impair its excellent dielectric properties. Particularly for the application of high-frequency films with extremely high requirements, how to realize the precise regulation and control of LCP chain structures, orientation behaviors and interface interactions in the molecular level, thereby synchronously improving the processability, the anisotropism and the comprehensive mechanical properties of the LCP chain structures, and still being a technical problem to be solved in the industry. Therefore, the novel LCP resin and the preparation method thereof are developed, so that the novel LCP resin can effectively inhibit excessive orientation, improve melt strength, widen processing window, improve anisotropy and enhance toughness on the basis of retaining excellent intrinsic properties of LCP, such as high heat resistance, low dielectric property and the like, and has important practical significance for promoting the application of LCP materials in high-end fields, such as high-performance films and the like. The present invention has been made in this context. Disclosure of Invention The invention aims to provide a high-performance LCP resin and a preparation method thereof, which are used for solving the problems in the prior art. In order to solve the technical problems, the invention provides a preparation method of high-performance LCP resin, which comprises the following steps: (1) Mixing a monomer mixture comprising p-hydroxybenzoic acid, p-tert-butylcatechol and 5-vinyl isophthalic acid with acetic