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Thermotropic flame-retardant anti-dripping aromatic liquid crystal copolyester material and preparation method thereof

An anti-droplet and aromatic technology, applied in the field of polyester materials, can solve the problems of high melting point of phosphorus-based flame-retardant polyester, generation of molten droplets, generation of harmful gases, etc., achieve low melting processing temperature, simple preparation process, and widely used The effect of applying the foreground

Active Publication Date: 2021-01-22
ZHEJIANG HENGYI PETROCHEMICAL RES INST CO LTD +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In order to solve the technical problems of the high melting point of phosphorus-based flame-retardant polyesters in the prior art, the generation of molten droplets and harmful gases during combustion, the present invention provides a thermotropic flame-retardant and anti-droplet aromatic liquid crystal copolyester material and its preparation method

Method used

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  • Thermotropic flame-retardant anti-dripping aromatic liquid crystal copolyester material and preparation method thereof
  • Thermotropic flame-retardant anti-dripping aromatic liquid crystal copolyester material and preparation method thereof
  • Thermotropic flame-retardant anti-dripping aromatic liquid crystal copolyester material and preparation method thereof

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preparation example Construction

[0050] A method for preparing a thermotropic flame-retardant and droplet-resistant aromatic liquid crystal copolyester material, comprising the steps of:

[0051] (1) According to the molar ratio of 10 ~ 40: 10 ~ 40: 80 ~ 20: 100 ~ 500: 2 ~ 8, the whole aromatic diphenol monomer, the whole aromatic diacid monomer, and the terminal carboxyl A and terminal AB type fully aromatic monomers of hydroxyl B, polyester particles, active end group compounds, and an appropriate amount of acetic anhydride (50-100% in molar weight relative to the total amount of hydroxyl groups in the raw material) and catalyst (the molar weight is the total molar weight of raw materials) 0.1-0.5% of the amount) into the reactor; under the protection of inert gas, the acetylation reaction is carried out at 120-150° C. for 30-60 minutes.

[0052] (2) Raise the temperature to 300-340° C. at a heating rate of 0.5-1.5° C. / min, and transesterify for 1-3 hours.

[0053] (3) Further reacting for 10-30 minutes un...

Embodiment 1

[0064] Preparation of thermotropic flame retardant anti-droplet aromatic liquid crystal copolyester material: add 4 in a 250 ml three-neck round bottom flask at a molar ratio of 100:80:20:800:1000:80:80:1800:4, 4'-dihydroxybiphenyl, terephthalic acid, 2,6-naphthalene dicarboxylic acid, p-hydroxybenzoic acid, PET particles, N-(3-carboxyphenyl)-4-phenylethynylphthaloyl Amine, N-(3-hydroxyphenyl)-4-phenylethynylphthalimide, and acetic anhydride and potassium acetate. The flask was fitted with a sealed glass paddle stirrer, a nitrogen inlet tube and an insulated distillation head. A moderate nitrogen flow was introduced, and the reaction mixture was acetylated at 120°C for 30 minutes in a quicksand bath, and then the temperature was raised to 340°C at a rate of 1.5°C / min for 1 hour of transesterification. At this point, the reaction system was slowly evacuated to a vacuum degree of 1 mbar and the temperature was set to 300° C. for 10 min. The opaque melt was cooled to room tempe...

Embodiment 2

[0066] Preparation of thermotropic flame retardant and anti-droplet aromatic liquid crystal copolyester material: Add p-benzene in a 250 ml three-neck round bottom flask at a molar ratio of 200:160:40:600:5000:20:20:1200:36 Diphenol, terephthalic acid, 1,7-naphthalene dicarboxylic acid, 6-hydroxy-2-naphthoic acid, PBT particles, 3-ethynylaniline, 2-(3-ethynylphenyl)-1,3-di Oxyisoindole-5-carboxylic acid, as well as acetic anhydride and zinc acetate. The flask was fitted with a sealed glass paddle stirrer, a nitrogen inlet tube and an insulated distillation head. A moderate nitrogen flow was introduced, and the reaction mixture was acetylated at 150°C for 60 minutes in a quicksand bath, and then the temperature was raised to 320°C at a rate of 1.5°C / min for 3 hours of transesterification. At this point, the reaction system was slowly evacuated to a vacuum degree of 3 mbar and the temperature was set to 320° C. for 30 min. The opaque melt was cooled to room temperature and the...

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Abstract

The invention relates to the field of polyester materials, and discloses a thermotropic flame-retardant anti-dripping aromatic liquid crystal copolyester material and a preparation method thereof. Thepreparation method comprises the following steps of: (1) carrying out acetylation reaction on a wholly aromatic diphenol monomer, a wholly aromatic diacid monomer, an AB-type wholly aromatic monomerwhich contains a terminal carboxyl group A and a terminal hydroxyl group B, an active terminal group compound, polyester particles, acetic anhydride and a catalyst at 120-150 DEG C under the protection of inert gas; (2) heating to 300-340 DEG C, and carrying out transesterification; (3) further performing the reaction at the temperature of 300-320 DEG C and under 1-3 mbar; and (4) cooling in an inert gas atmosphere, grinding an obtained product into powder, and carrying out polycondensation reaction under the conditions of 200-260 DEG C and 1-3 mbar to obtain a target product. The thermotropicflame-retardant anti-dripping aromatic liquid crystal copolyester material has the advantages of low melting point, anti-dripping performance and no generation of harmful gas during combustion.

Description

technical field [0001] The invention relates to the field of polyester materials, in particular to a thermotropic flame-retardant anti-droplet aromatic liquid crystal copolyester material and a preparation method thereof. Background technique [0002] As a widely used high polymer material, semi-aromatic polyester has been widely used in civil and industrial fields due to its high strength, high modulus, and low water absorption characteristics. Polyester fiber, also known as polyester, occupies most of the chemical fiber industry. The types of polyesters that have been marketed include PET, PBT, PTT and so on. Because the polymer will undergo reactions such as oxidation and degradation at high temperatures, once it is burned, it is easy to form a fire, which will seriously affect the safety of people's lives and properties. Therefore, it is of great significance to improve the flame retardancy of polyester materials. [0003] The more mature polyester flame retardant mod...

Claims

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Application Information

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IPC IPC(8): C08G63/685C08G63/78C09K19/38
CPCC08G63/685C08G63/78C09K19/3809
Inventor 管清宝钟硕圃游正伟刘可方哲城
Owner ZHEJIANG HENGYI PETROCHEMICAL RES INST CO LTD
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