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Xylylenediamine composition and method for producing polyamide resin

A technology of polyamide resin and xylylenediamine, which is applied in the field of manufacture of xylylenediamine composition and polyamide resin, can solve problems such as mechanical properties and transparency reduction, and achieve improved molding processability, high transparency, The effect of increasing strength

Active Publication Date: 2017-10-10
MITSUBISHI GAS CHEM CO INC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Furthermore, when the dispersion state of the crystal nucleating agent and the like in the polyamide resin becomes uneven, there is a possibility that the mechanical properties and transparency of the molded article formed from the composition containing the polyamide resin will decrease.

Method used

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  • Xylylenediamine composition and method for producing polyamide resin
  • Xylylenediamine composition and method for producing polyamide resin
  • Xylylenediamine composition and method for producing polyamide resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment

[0105] Hereinafter, although an Example demonstrates this invention in more detail, this invention is not limited to these. In addition, in this Example, various measurements were performed by the following methods.

[0106]

[0107] Accurately weigh 0.2 g of polyamide resin, stir and dissolve in 20 ml of 96% sulfuric acid at 20-30°C. After complete dissolution, quickly take out 5 ml of the solution to a Cannon-Fenske type viscometer, and place it in a constant temperature bath at 25° C. for 10 minutes, then measure the falling time (t). In addition, the falling time (t) of 96% sulfuric acid itself was also measured in the same manner. 0 ). by t and t 0 The relative viscosity was calculated according to the following formula.

[0108]Relative viscosity = t / t 0

[0109]

[0110] Regarding the number average molecular weight of the polyamide resin, first, a sample was dissolved in a phenol / ethanol mixed solvent and a benzyl alcohol solvent, and the carboxyl end group c...

manufacture example 1

[0123] Production Example 1 (production of 2,6-bis(aminomethyl)pyridine)

[0124] Into a 100 mL autoclave, 2,6-bis(chloromethyl)pyridine / methanol / ammonia=1 / 25 / 100 mol% was charged at a ratio of 2,6-bis(chloromethyl)pyridine / methanol / ammonia=1 / 25 / 100 mol%, and the reaction was carried out at a pressure of 2 MPaG and a temperature of 60° C. for 2 hours. After the reaction, the precipitate was recovered by filtration, an aqueous sodium hydroxide solution was added to the recovered product, and then extracted with toluene, and the solvent was distilled off by a decompression evaporator to obtain 2,6-bis(aminomethyl)pyridine (purity 99%).

Embodiment 1

[0126] (Preparation of xylylenediamine composition)

[0127] A xylylenediamine composition was prepared so that the content of 2,6-bis(aminomethyl)pyridine would be 0.004 parts by mass relative to 100 parts by mass of m-xylylenediamine.

[0128] (Manufacture of polyamide resin)

[0129] 10 kg (68.43 mol) of adipic acid (manufactured by Rhodia Co., Ltd.) was put into a reaction vessel equipped with a stirrer, partial condenser, total condenser, thermometer, dropping funnel, nitrogen introduction pipe, and strand die, and nitrogen replacement was fully carried out. Afterwards, the system was further heated and melted to 170° C. while stirring under a small amount of nitrogen gas flow. Add 9.273 kg of the xylylenediamine composition obtained as described above (containing 68.08 mol of m-xylylenediamine) dropwise into the molten adipic acid while stirring, and discharge the generated condensation water out of the system , while continuously raising the internal temperature to 24...

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Abstract

A xylylenediamine composition comprising xylylenediamine and a pyridine compound (A) having at least one substituent comprising an amino group, the content of the pyridine compound (A) relative to 100 parts by mass of xylylenediamine is 0.001 to 0.1 parts by mass; and [2] a method for producing a polyamide resin comprising a pyridine compound (A) having at least one substituent containing an amino group, a diamine containing xylylenediamine (wherein, not Including the step of introducing (diamine) corresponding to the aforementioned pyridine compound (A) and dicarboxylic acid into the reaction system to carry out polycondensation reaction, the introduction amount of the pyridine compound (A) is 0.001 to 100 parts by mass of xylylenediamine 0.1 parts by mass.

Description

technical field [0001] The present invention relates to a method for producing a xylylenediamine composition and a polyamide resin. Background technique [0002] Xylylenediamine is a compound useful as a raw material for polyamide resins, an epoxy resin curing agent, and a raw material for isocyanate compounds. Polyamide resins using xylylenediamine as a main diamine component have excellent mechanical properties such as strength and elastic modulus, and are therefore useful as various molding materials. In addition, since they are excellent in gas barrier properties such as oxygen gas and carbon dioxide gas, the above-mentioned polyamide resins are also useful as packaging materials. [0003] When a polyamide resin is used as a molding material, it is known to increase the crystallization rate by adding a crystallization nucleating agent to the polyamide resin in order to improve the molding processability of the polyamide resin (Patent Document 1). In addition, in order ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G69/28
CPCC08G69/28C08G69/26C08L77/06C08K5/0083C08K5/17C08K5/3432C08G69/265C08G59/50C08G59/5053C08G69/30
Inventor 中村宜史山田元杤原健也篠原克巳三田寺淳山本崇史
Owner MITSUBISHI GAS CHEM CO INC
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