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Polyamide resin and preparation method thereof

A polyamide resin and diamine technology, which is applied in the field of polyamide resin and its manufacturing, can solve the problems of poor melt retention stability, no improvement in relative viscosity, and decrease in viscosity of polyoxamide resin.

Active Publication Date: 2015-11-25
TORAY ADVANCED MATERIALS RES LAB CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Also, in the polyoxamide PA62 / 2-M52 resin described in Patent Document 1 (WO2011 / 136263), the relative viscosity of the polyoxamide resin having a melting point above 280° C. has not been improved (relative viscosity is lower than 2.05) , and the viscosity of the polymer will drop significantly during melt processing
In addition, although the polyoxamide PA52 resin described in Patent Document 2 (Japanese Unexamined Patent Application No. 2011-236387) has improved its viscosity by using a specific solid-state polymerization method, its poor melt retention stability will lead to melt processing. Among them, the viscosity of polyoxamide resin decreased significantly

Method used

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  • Polyamide resin and preparation method thereof
  • Polyamide resin and preparation method thereof
  • Polyamide resin and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 8

[0092] Injection molding temperature: 310°C (Example 8, Comparative Examples 5-7)

[0093] 270°C (comparative example 8)

[0094] 295°C (comparative example 9)

[0095] Mold temperature: 130°C (Example 8, Comparative Examples 5-7)

[0096] 80 (comparative example 8)

[0097] 90°C (comparative example 9)

[0098] Test piece: length 64mm×width 12.7mm×thickness 3.0mm

[0099] Bending performance test equipment: AG-IS-20KN (SHIMAZU)

[0100] (7) Saturated water absorption at 23°C

[0101] The polyamide resin is hot-pressed into a film at a temperature of melting point + 20°C, and rapidly cooled in ice water. The thickness of the sample is 0.1-0.5mm (50mm*50mm). The sample was immersed in water at 23°C to a constant weight and weighed (W1), and then the sample was vacuum-dried at 100°C to a constant weight and weighed (W2). Calculate water absorption (%)=100*(W1-W2) / W2.

[0102] Abbreviation description:

[0103] DN4: 1,4-butylene diamine, DN5: 1,5-pentanediamine, DN6: 1,6...

Embodiment 1

[0115] The three-necked flask (500ml) was first purged with nitrogen for 15 minutes, and then a certain nitrogen flow was maintained. Toluene (300 ml) and DPO (24.22 g, 0.100 mol) were added to the three-necked flask, followed by stirring and raising the temperature to 70°C. After DPO was completely dissolved in toluene at 70°C, DN5 (10.73 g, 0.105 mol) was added to the system, then the temperature was raised to 130°C, and the reaction was refluxed for 1 hour. This is followed by filtration and washing, followed by drying in a vacuum oven at 100°C for 12 hours. The relative viscosity of the obtained prepolymer was 1.49.

[0116] Feed 2.00 g of the obtained prepolymer into a glass test tube with a diameter of 19 mm, then replace it with nitrogen for 5 times, then reduce the pressure of the system to below 300 Pa, and then place it in a metal bath at 280 ° C for post-polymerization React for 1.5 hours. Polymer properties are in Table 1.

Embodiment 2

[0118] The preparation method of prepolymer is identical with embodiment 1,

[0119] Take 2.00 g of the obtained prepolymer and feed it into a glass test tube with a diameter of 19 mm, then replace it with nitrogen for 5 times, then reduce the pressure of the system to below 300 Pa, and then place it in a metal bath at 325 ° C for post-polymerization React for 0.5 hours. Polymer properties are in Table 1.

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Abstract

The invention relates to polyamide resin and a preparation method thereof. The polyamide resin has excellent melting retention stability, low hydroscopicity and excellent mechanical properties. A degree of polymerization of polyamide resin can be improved by the preparation method in short time. The polyamide resin is prepared by condensation of at least diacid and diamine components. A use ratio of diphenyl oxalate to diacid is in a range of 20-100mol%, a use ratio of C4-C12 aliphatic diamine to diamine is in a range of 4-12mol%, sulfuric acid with a concentration of 96% is used as a solvent, and relative viscosity A of a polyamide resin solution with a concentration of 0.01g / ml at a temperature of 25 DEG C is in a range of 2.35-6.00. The polyamide resin can be used for resin molded products such as automobile parts, electrical parts, mechanical parts, household articles, transaction articles, buildings and physical articles, fibers or films.

Description

technical field [0001] The present invention relates to a polyamide resin capable of increasing the degree of polymerization in a short period of time and having excellent properties in terms of melt retention stability, low water absorption and mechanical properties, and a method for producing the same Background technique [0002] Crystalline polyamide resins represented by nylon 6 and nylon 66 are widely used as fibers for clothing, industrial materials, or general-purpose engineering plastics due to their excellent characteristics and ease of melt molding. However, another On the one hand, problems such as changes in physical properties due to water absorption, deterioration in acids, high-temperature alcohols, and hot water have also been pointed out, and there are demands for polyamide resins with better dimensional stability, chemical resistance, and heat resistance. is improving. In the field of electrical and electronic parts, along with the development of surface ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G69/26C08G69/28
Inventor 曹晓秀陈毕文陈圣典何勇加藤公哉
Owner TORAY ADVANCED MATERIALS RES LAB CHINA
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