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Manufacturing method of polyamide

A manufacturing method, polyamide technology, applied in the field of polyamide, can solve problems such as undisclosed temperature, achieve the effect of increasing commodity value, easy adjustment, and high industrial utilization value

Active Publication Date: 2017-12-01
MITSUBISHI GAS CHEM CO INC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, it is disclosed that the upper limit of the reaction liquid temperature is preferably 35° C. or lower than the melting point of polyamide, but the specific temperature is not disclosed, and even if it is maintained at this temperature, only polyamide with high yellowness can be obtained.

Method used

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  • Manufacturing method of polyamide
  • Manufacturing method of polyamide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057]Into a jacketed 50-liter stainless steel reaction tank equipped with a partial condenser, a total condenser, a stirrer, a nitrogen gas inlet pipe, and a diamine dropping port through which temperature-adjusted oil flows, accurately weighed 15.000 kg of adipic acid (purity: 99.85wt%) was fed as powder and fully replaced with nitrogen. The oil at 300°C was poured into the jacket to start heating up, and the adipic acid was melted while stirring to form a uniform flow state. During this period, supply of nitrogen gas into the reaction tank was started, and the pressure in the reaction tank was increased to 0.3 MPaG. When heated to 190° C., while stirring the molten adipic acid, 13.909 kg of mixed xylylenediamine (purity: 99.95 wt%) containing 70 mol% m-xylylenediamine and 30 mol% p-xylylenediamine were consumed. Add dropwise over 2 hours. During the dropwise addition of the diamine component, until the molar ratio (diamine component / dicarboxylic acid component) in the rea...

Embodiment 2

[0059] During the dropwise addition of the diamine component until the molar ratio (diamine component / dicarboxylic acid component) in the reaction mixture reaches 0.8, in addition to raising the temperature of the reaction mixture with 253°C as the upper limit and maintaining it in a molten state, It carried out similarly to Example 1. The obtained polyamide had a melting point of 258° C. and a number average molecular weight of 16,000. As shown in Table 1, the yellowness (YI) of the obtained polyamide pellets was -6 at the beginning of taking out, -5 after 20 minutes, and -5 after 40 minutes. Almost no increase in YI over time was confirmed, and a color tone was obtained. Good polyamide.

Embodiment 3

[0061] During the dropwise addition of the diamine component until the molar ratio (diamine component / dicarboxylic acid component) in the reaction mixture reaches 0.8, in addition to raising the temperature of the reaction mixture with 255°C as the upper limit and maintaining it in a molten state, It carried out similarly to Example 1. The obtained polyamide had a melting point of 258° C. and a number average molecular weight of 16,000. As shown in Table 1, the yellowness (YI) of the obtained polyamide pellets was -6 at the beginning of taking out, -6 after 20 minutes, and -4 after 40 minutes. Almost no increase in YI over time was confirmed, and the color tone was obtained. Good polyamide.

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Abstract

The present invention provides a method for producing polyamide having improved color tone and favorable quality polyamide, which is characterized in that mixed xylylenediamine containing p-xylylenediamine is used as a diamine component together with two In the method of producing polyamide having a melting point of 255°C or higher by polycondensation of carboxylic acid components using a batch reaction device, the reaction mixture is heated to a temperature above the melting point while maintaining a molten state under a pressure of 0.1 MPaG or higher. When adding the diamine component dropwise to the molten dicarboxylic acid component, keep the temperature of the reaction mixture below 255°C until the molar ratio of the reaction mixture (diamine component / dicarboxylic acid component) reaches 0.8, and when the dropwise addition is completed, The temperature of the reaction mixture is above the melting point of the aforementioned polyamide.

Description

technical field [0001] The present invention relates to a method of polycondensing a dicarboxylic acid component and a diamine component including p-xylylenediamine in a batch reaction tank to produce a polyamide having a melting point of 255° C. or higher. Background technique [0002] Patent Document 1 discloses a method in which a dicarboxylic acid and a diamine are directly mixed and the polycondensation reaction is carried out under normal pressure, and the temperature of the reaction system containing the raw material mixture is raised while the temperature of the reaction is set to be equal to or higher than the melting point of the dicarboxylic acid. Keep the reaction in a substantially uniform molten state, and raise the temperature of the reaction system to a temperature above 30°C lower than the melting point of the copolyamide to be produced before the reaction rate reaches 95%, without losing fluidity in the system and controlling The reaction temperature is suc...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G69/28
CPCC08G69/28C08G69/265C08G69/26
Inventor 宗安邦明木村优也篠原克巳杤原健也黑濑英之
Owner MITSUBISHI GAS CHEM CO INC
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