Continuous preparation method for semi-aromatic polyamide

A technology for semi-aromatic polyamide and prepolymer, which is applied in the field of continuous preparation of semi-aromatic polyamide and achieves the effects of high product yield, stable process and rich variety.

Active Publication Date: 2013-12-11
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, the industrial production of semi-aromatic polyamides usually involves putting materials into a reactor to obtain semi-aromatic polyamide resins through polycondensation. For example, US2002183479A1 reported that polybutylene terephthalamide / hexamethylenediamine copolymer was synthesized by solid-state polycondensation (PA4T / 6T), but this kind of method can only be produced by batch method

Method used

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  • Continuous preparation method for semi-aromatic polyamide
  • Continuous preparation method for semi-aromatic polyamide
  • Continuous preparation method for semi-aromatic polyamide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Mix 20g / hour of phosphoric acid and semi-aromatic polyamide prepolymer (prepared by weight ratio of terephthalic acid: adipic acid: hexamethylenediamine = 83:73:116) 2500g / hour and feed it from the reaction extruder Feed port is added, benzoic acid 5g / hour and dispersion material 300g / hour are mixed and then added from the auxiliary feed port, and reacted and extruded at a temperature of 300°C, a screw speed of 180rpm and a vacuum of 0.07MPa; the extruded product is drawn, cooled, After pelletizing and drying, a semi-aromatic polyamide resin was obtained, with a yield of 96%, and intrinsic viscosity [η]=2.3dL·g -1 .

Embodiment 2

[0044]Mix pyrophosphoric acid 1g / hour and semi-aromatic polyamide prepolymer (prepared by weight ratio of hexamethylenediamine terephthalate:caprolactam=141:59) 1000g / hour and add it from the main feeding port of the reaction extruder , 1 g / hour of p-toluic acid and 100 g / hour of dispersion material are mixed and added from the auxiliary feeding port, and reacted and extruded at a temperature of 330 ° C, a screw speed of 10 rpm and a vacuum of 0.09 MPa; the extruded product is drawn, cooled, After pelletizing and drying, a semi-aromatic polyamide resin was obtained with a yield of 97% and an intrinsic viscosity [η]=1.9dL·g -1 .

Embodiment 3

[0046] Polyphosphoric acid 50g / hour and semi-aromatic polyamide prepolymer (by 4,4'-(4-thioether benzoic acid)-triphenylphosphine oxide: decyl diamine: cycloheptanolactam=582:172: 46 weight ratio preparation) 5000g / hour mixed and added from the main feeding port of the reaction extruder, m-toluic acid 10g / hour and dispersion material 500g / hour mixed and added from the auxiliary feeding port, at a temperature of 320 ° C, Reactive extrusion at a screw speed of 200rpm and a vacuum of 0.07MPa; the extrudate was drawn, cooled, pelletized and dried to obtain a semi-aromatic polyamide resin with a yield of 88% and an intrinsic viscosity [η]=1.6dL·g -1 .

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Abstract

The invention discloses a continuous preparation method for semi-aromatic polyamide. The method is characterized by comprising the following steps that: 1 to 50 parts by weight of a catalyst per hour and 1000 to 5000 parts by weight of a semi-aromatic polyamide prepolymer per hour are mixed and then added into a reaction extruder through a main feeding inlet of the extruder; 1 to 10 parts by weight of a molecular weight regulator per hour and 100 to 500 parts by weight of a dispersing material per hour are mixed and then added through an auxiliary feeding inlet; then reactive extrusion is carried out under the conditions of a temperature of 280 to 330 DEG C, a screw rotation speed of 10 to 200 rpm and a vacuum degree of 0.04 to 0.09 MPa; and traction, cooling, granulation and drying are carried out on obtained extrudate so as to obtain semi-aromatic polyamide resin.

Description

technical field [0001] The invention relates to a continuous preparation method of semi-aromatic polyamide, which belongs to the field of polymer synthesis. Background technique [0002] Semi-aromatic polyamide is a polyamide polymer material whose molecular main chain contains both aromatic segments and aliphatic segments. It has excellent heat resistance and molding processability, and is widely used in electronic appliances, automobile industry and daily heat-resistant products, etc. field. [0003] At present, the industrial production of semi-aromatic polyamides usually involves putting materials into a reactor to obtain semi-aromatic polyamide resins through polycondensation. For example, US2002183479A1 reported that polybutylene terephthalamide / hexamethylenediamine copolymer was synthesized by solid-state polycondensation (PA4T / 6T), but this kind of method can only be produced by batch method. The previous work of the present invention has published the invention pa...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08L77/00C08G69/28C08G69/36C08G69/42
Inventor 杨杰瞿兰张美林龙盛如张刚王孝军严永刚
Owner SICHUAN UNIV
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