Method for preparing semi-aromatic polyamide

A semi-aromatic polyamide, CH2 technology, applied in the field of semi-aromatic polyamide preparation, can solve the problems of high melting point of semi-aromatic polyamide, low product molecular weight, long process time, etc., achieve process stability, high product yield, good repeatability

Active Publication Date: 2012-07-04
潍坊三力本诺化学工业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] U.S. Patent US2002183479A1 has reported polybutylene terephthalamide/hexamethylenediamine copolymer (PA4T/6T) by solid-phase polycondensation, but the process time is long, energy consumption is high, and the molecular weight of the product obtained by simple solid-state polycondensation is not hig

Method used

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  • Method for preparing semi-aromatic polyamide
  • Method for preparing semi-aromatic polyamide
  • Method for preparing semi-aromatic polyamide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Add 272g of monomers (83g of terephthalic acid, 73g of adipic acid, 116g of hexamethylenediamine), 5g of phosphoric acid and 100g of deionized water into the reactor, and raise the temperature to 100°C under the protection of nitrogen, and react for 0.5h; closed reaction Heat up to 220°C within 0.5h, react for 2h; exhaust gas, vacuumize to 0.09MPa, fill nitrogen to 0.5MPa, react at 270°C for 1h, repeat the above exhaust, vacuumize, inflate and react 2 time; cooling and discharging, the solid is pulverized, washed with deionized water, and dried, then added to the reaction extruder, and reacted and extruded at a temperature of 310 ° C and a vacuum of 0.08 MPa for 8 minutes to obtain a high molecular weight semi-aromatic polyamide resin. 95%, intrinsic viscosity [η] = 2.1dL·g -1 .

Embodiment 2

[0041] Add 200g of monomer (141g of hexamethylenediamine terephthalate, 59g of caprolactam), 1g of pyrophosphoric acid and 50g of deionized water into the reactor, and under the protection of nitrogen, heat up to 80°C and react for 1h; close the reactor, and Heat up to 200°C within 1h, react for 5h; exhaust gas, vacuumize to 0.07MPa, fill with argon to 1.5MPa, react at 220°C for 2h, repeat the above exhaust, vacuumize, inflate and react 4 times; cool down After discharging, the solid was pulverized, washed with deionized water, and dried, then added to a reaction extruder, and carried out reaction extrusion at a temperature of 260°C and a vacuum of 0.09MPa for 30 minutes to obtain a high molecular weight semi-aromatic polyamide resin with a yield of 92%. Intrinsic viscosity [η] = 1.5dL·g -1 .

Embodiment 3

[0043]800 g of monomer (582 g of 4,4'-(4-thioetherbenzoic acid)-triphenylphosphine oxide, 172 g of decanediamine, 46 g of enantholactam), 10 g of polyphosphoric acid and 200 g of deionized water were added to the reactor Under the protection of nitrogen, heat up to 90°C and react for 1 hour; close the reactor, heat up to 250°C within 0.5 hours, and react for 4 hours; exhaust gas, vacuumize to 0.08MPa, fill helium to 0.8MPa, React at 280°C for 1 hour, repeat the above exhaust, vacuum, gas and reaction operations once; cool down and discharge, the solid is crushed, washed with deionized water, dried and then added to the reaction extruder. MPa is carried out reaction extrusion 1min, obtains high molecular weight semi-aromatic polyamide resin, productive rate 85%, intrinsic viscosity number [η]=1.0dL·g -1 .

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Abstract

The invention discloses a method for preparing semi-aromatic polyamide. The method is characterized by comprising the following steps of: adding 200 to 800 parts of monomer, 1 to 10 parts of catalyst and 50 to 200 parts of deionized water into a reactor, and reacting at the temperature of between 200 and 250 DEG C for 2 to 5 hours; exhausting gas, vacuumizing until the vacuum degree is 0.07 to 0.09MPa, filling inert gas until the vacuum degree is 0.5 to 1.5MPa, reacting at the temperature of between 220 and 280 DEG C for 1 to 2 hours, and repeating gas exhausting, vacuumizing, gas filling and reacting operation for 1 to 4 times; and reducing the temperature, discharging, grinding a solid, washing, drying, adding into a reactive extruder, and performing reactive extrusion at the temperature of between 260 and 320 DEG C and the vacuum degree of 0.07 to 0.09MPa for 1 to 30 minutes to obtain high molecular weight semi-aromatic polyamide resin with the intrinsic viscosity [eta] of 1.0 to 2.5dL.g<-1>, the melting point Tm of 280 to 330 DEG C and the initial thermal decomposition temperature Td of 420 to 440 DEG C.

Description

technical field [0001] The invention relates to a preparation method of semi-aromatic polyamide, which belongs to the field of polymer synthesis. Background technique [0002] With the development of science and technology, various application fields, especially the automobile manufacturing industry and the electronics industry, have higher and higher requirements for structural materials, and ordinary nylon (PA66, PA6) is close to its performance limit; therefore, a class of polyamides containing aromatic rings Amides have been greatly developed in recent years. For example, fully aromatic polyamides have excellent mechanical strength and thermal properties, but they are difficult to be processed by traditional methods (Rao, Y.; Waddon, A.J.; Farris, R.J.Structure-property relation in poly(p-phenylene terephthalamide) (PPTA) fibers.Polymer 2001, 42, 5937-5946); while semi-aromatic polyamides (such as PA6T, PA9T, etc.) have both high strength and high modulus, excellent heat...

Claims

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Application Information

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IPC IPC(8): C08G69/26C08G69/28C08G69/42C08G69/40
Inventor 杨杰张美林龙盛如瞿兰张目张刚王孝军严永刚
Owner 潍坊三力本诺化学工业有限公司
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