Soluble flame-retardant wholly aromatic copolyester with low dielectric constant and low dielectric loss as well as preparation method and application of soluble flame-retardant wholly aromatic copolyester

A low dielectric constant, dielectric constant technology, applied in the direction of one-component copolyester rayon, additive processing, etc., can solve the problem of difficult to solve the vertical anisotropy of the film and interlayer peeling, limited application, product Single form and other problems, to achieve the effects of excellent anti-droplet resistance, expansion of processing methods, and reduction of bulk density

Pending Publication Date: 2022-08-05
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the rigid rod-like structure of all-aromatic polyester will cause the polymer to be oriented during melt processing, and it is difficult to solve the problems of vertical anisotropy and interlayer peeling of the film.
Therefore, most of this type of polyester is still used as boards and fibers at present, and the product form is single, which greatly limits its application.

Method used

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  • Soluble flame-retardant wholly aromatic copolyester with low dielectric constant and low dielectric loss as well as preparation method and application of soluble flame-retardant wholly aromatic copolyester
  • Soluble flame-retardant wholly aromatic copolyester with low dielectric constant and low dielectric loss as well as preparation method and application of soluble flame-retardant wholly aromatic copolyester
  • Soluble flame-retardant wholly aromatic copolyester with low dielectric constant and low dielectric loss as well as preparation method and application of soluble flame-retardant wholly aromatic copolyester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0089] 1560g of 4-hydroxybenzoic acid, 701g of [1,1'-biphenyl]-3,5-diol, 0.15g of N-methylimidazole and 1537g of acetic anhydride were added to the reaction kettle, and the temperature was raised to 130°C under nitrogen atmosphere. After acylation reaction for 2 h, the product was washed with pure water until the pH value was close to neutral, and dried to constant weight to obtain acylated compound; then, acylated compound, 739g 2-methoxyterephthalic acid and 0.15 g of 2-methoxyterephthalic acid were added to the reactor. g N-methylimidazole, and gradually heated to 360 °C at a heating rate of 0.5 °C / min under normal pressure, reacted for 0.5 h, and then melted and polycondensed under the condition of low vacuum of 10 Pa for 0.5 h, and filled the reaction kettle with Nitrogen, extruding the melt, and cooling with water, the target copolyester can be obtained.

[0090] The dielectric constant of the copolyester is 4.5; the dielectric loss is 0.05; the limiting oxygen index is ...

Embodiment 2

[0092] Add 2085g of 4'-hydroxyl-[1,1'-biphenyl]-4-carboxylic acid, 451g of 5-methoxy-[1,1'-biphenyl]-3,4'-diol into the reaction kettle , 464g of 2-(tert-butyl)terephthalic acid, 0.15g of p-toluenesulfonic acid and 1207g of acetic anhydride were heated to 130°C under nitrogen atmosphere for acylation reaction for 2h, then 0.15g of N-methylimidazole was added, and Under normal pressure, the temperature was gradually raised to 320°C at a heating rate of 0.5°C / min, reacted for 0.5h, then melted and polycondensed for 0.5h under a low vacuum of 10Pa, filled with nitrogen in the reaction kettle, extruded the melt, and cooled with water. , the target copolyester can be obtained.

[0093] The dielectric constant of the copolyester is 4.2; the dielectric loss is 0.03; the limiting oxygen index is 30%; the vertical combustion grade is V-0; Amide, N,N-dimethylacetamide, tetrahydrofuran, γ-butyrolactone, ethylene glycol monobutyl ether, triethylene glycol, ethanolamine and other solvents...

Embodiment 3

[0095] 75g of 4-hydroxybenzoic acid, 1333g of 5-phenoxyisophthalic acid, 565g of phosgene and 6g of N,N-dimethylformamide were added to the reaction kettle, and the temperature was gradually raised to 60°C under stirring for 5h. pressure distillation, washing, drying to constant weight to obtain acid chloride; acid chloride is dissolved in toluene to prepare 0.1wt% organic phase solution A, 1592g 2-fluoro-3",5"-dimethyl-[1 ,1':3',1"-terphenyl]-4,5'-diol and 343 g of sodium hydroxide were dissolved in water to prepare 0.1 wt% aqueous solution B. The above organic solution A was quickly poured into water In the phase solution B, under the stirring condition of 2000rpm, the stirring reaction was continued for 100 minutes, and the whole aromatic copolyester prepolymer was obtained after suction filtration, washing and drying; The polyester prepolymer and 0.15g N-methylimidazole are then gradually heated up to 280°C at a heating rate of 0.5°C / min, and then reacted under a low vacuu...

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Abstract

The soluble low-dielectric-constant low-dielectric-loss flame-retardant wholly-aromatic copolyester is composed of structural units represented by I, II and III, the mole percent of II and the mole percent of III are the same, I + II + III is equal to 100 mole percent, I is larger than or equal to 0 mole percent and smaller than or equal to 90 mole percent, II is larger than or equal to 5 mole percent and smaller than or equal to 50 mole percent, III is larger than or equal to 5 mole percent and smaller than or equal to 50 mole percent, the dielectric constant of the soluble low-dielectric-constant low-dielectric-loss flame-retardant wholly-aromatic copolyester is 1.5-4.5, and the dielectric loss of the soluble low-dielectric-constant low-dielectric-loss flame-retardant wholly-aromatic copolyester is 0.0008-0.050. The limit oxygen index is 28-50%; the vertical combustion grade of UL-94 is V-0 grade; the compound can be completely or partially dissolved in conventional solvents such as N-methyl pyrrolidone, N, N-dimethylformamide, N, N-dimethylacetamide and the like. The invention also discloses a preparation method and application of the compound. The copolyester disclosed by the invention not only can obviously enhance the dissolving capacity of the copolyester in a conventional organic solvent, but also can effectively reduce the dielectric constant and the dielectric loss, can obtain excellent flame retardance and molten drop resistance, can be directly used as a high polymer material, and can also be used as a flame-retardant molten drop-resistant additive.

Description

technical field [0001] The invention belongs to the technical field of soluble low dielectric constant and low dielectric loss flame retardant all-aromatic copolyester and its preparation and application. Specifically, the present invention relates to a novel soluble, low dielectric constant, low dielectric loss, flame retardant all-aromatic copolyester containing twisted, bulky rigid structural units and a method for preparing the same. This kind of copolyester effectively reduces the packing density of molecular chains through the large-volume rigid twisted structure, thereby effectively improving the dielectric properties and solubility of the material, and the rigid twisted structure significantly improves the carbon-forming ability of the copolyester, giving the copolyester Polyester good flame retardant properties. Background technique [0002] Fully aromatic polyester refers to thermoplastic special engineering plastics with aromatic rings and ester bonds on the main...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/60C08G63/682C08G63/78C08G63/79C08G63/80C08L67/00D01F6/84B33Y70/00C08J5/18
CPCC08G63/605C08G63/682C08G63/78C08G63/79C08G63/80C08L67/00D01F6/84B33Y70/00C08J5/18C08J2367/00
Inventor 王玉忠张诗雨付腾龚岳郭德明汪秀丽
Owner SICHUAN UNIV
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