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Preparation method of oxygen absorptivity polyamide resin composition and oxygen absorptivity polyamide resin composition oblained by said method

A technology of polyamide resin and composition, which is applied in the field of preparing oxygen-absorbing polyamide resin composition with stable quality, can solve the problems of unoptimized, increased process and the like

Inactive Publication Date: 2003-09-24
MITSUBISHI GAS CHEM CO INC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method requires further steps, so it is not preferable

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0085] A jacketed 2-liter reaction tank (pressure resistance 1 MPa) equipped with a shrinker, a total shrinker, a dropping funnel, a nitrogen gas introduction tube, a stirring paddle, a stirring device with a torque meter, and a strand die was used. . In this retort, add adipic acid 585.4g (4.006mol), then add sodium hypophosphite monohydrate 0.3377g and make the phosphorus atomic concentration in the polyamide resin composition of final gained reach 3.2 * 10 -3 (mmol / g), add cobalt acetate tetrahydrate 0.8345g, make cobalt atomic concentration reach 3.4 * 10 -3 (mmol / g), the gaseous phase in the reaction tank is replaced with nitrogen with a purity of more than 99% by volume, so that the concentration of oxygen is less than 0.1% by volume.

[0086] The ratio (P / Co) of the concentrations of phosphorus atoms and cobalt atoms was 0.94.

[0087] Then, the temperature was continuously raised to 170°C while stirring for about 30 minutes under normal pressure and nitrogen flow, an...

Embodiment 2

[0092] Add sodium hypophosphite monohydrate 0.0169g, make the phosphorus atomic concentration in the polyamide resin composition reach 1.6 * 10 -4 (mmol / g), add cobalt acetate tetrahydrate 0.8345g, make the concentration of cobalt reach 3.4 * 10 -3 (mmol / g), and polyamide resin composition E2 was synthesized in the same manner as in Example 1.

[0093] The ratio of the concentrations of phosphorus atoms and cobalt atoms was 0.05. The obtained polyamide resin composition E2 had a terminal amino group concentration of 43.2 μeq / g, a terminal carboxyl group concentration of 82.5 μeq / g, and a number average molecular weight of 15,900.

[0094] In addition, the time from the time point of completion of dropping m-xylylenediamine to the stop of stirring was 36 minutes.

[0095] Then, the oxygen absorbing capacity of the obtained polyamide resin composition E2 was measured in the same manner as in Example 1. The results are shown in Table 1.

Embodiment 3

[0097] Add sodium hypophosphite monohydrate 0.5065g, make the phosphorus atom concentration in the polyamide resin composition reach 4.8 * 10 -3 (mmol / g), add cobalt acetate tetrahydrate 1.2518g, make the concentration of cobalt reach 5.1 * 10 -3 (mmol / g), and polyamide resin composition E3 was synthesized in the same manner as in Example 1.

[0098] The ratio of the concentrations of phosphorus atoms and cobalt atoms was 0.94. The obtained polyamide resin composition E3 had a terminal amino group concentration of 44.6 μeq / g, a terminal carboxyl group concentration of 81.0 μeq / g, and a number average molecular weight of 15,900.

[0099] In addition, the time from the time when the dropwise addition of m-xylylenediamine was completed to the stop of stirring was 28 minutes.

[0100] Then, the oxygen absorbing capacity of the obtained polyamide resin composition E3 was measured in the same manner as in Example 1. The results are shown in Table 1.

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Abstract

A method for producing an oxygen-absorbing polyamide resin composition comprising polycondensing a diamine component containing 70 mol% or more of m-xylylenediamine and a dicarboxylic acid component containing 50 mol% or more of adipic acid in the presence of a phosphorus compound, When preparing the polyamide resin composition, before the polycondensation reaction starts or during the reaction, a compound containing one or more metal atoms selected from Group VIII transition metals, manganese, copper and zinc of the periodic table of elements is added to the reaction system or Complex compound, the ratio (P / M) of the phosphorus atomic concentration P (mmol / g) of the phosphorus compound in the polyamide resin composition to the metal atomic concentration M (mmol / g) is 0.02 to 1.0, and the polycondensation reaction is carried out .

Description

technical field [0001] The present invention relates to a method for preparing a polyamide resin composition having an oxygen absorbing function and an oxygen-absorbing polyamide resin composition obtained by the method. More specifically, it relates to a method for producing an oxygen-absorbing polyamide resin composition with stable quality, which is characterized in that a compound containing a metal atom selected from Group VIII transition metals, manganese, copper and zinc of the periodic table of elements is added in a set ratio Or complexes and phosphorus compounds for polycondensation. And the oxygen-absorbing polyamide resin composition obtained by this method. technical background [0002] Some metal cans or glass bottles that have been used as packaging containers that block the ingress of external oxygen and provide excellent storage stability for the contents have been replaced by plastics made of gas-barrier thermoplastic resins in terms of processability and ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B32B27/34C08G69/04C08G69/26C08G69/28
CPCB32B27/34C08G69/04C08G69/265C08G69/28
Inventor 大泷泉二平松宗大郎
Owner MITSUBISHI GAS CHEM CO INC
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