Method for preparing semi-aromatic nylon

A semi-aromatic and nylon technology, applied in the field of polymer material synthesis, can solve the problems of semi-aromatic nylon, such as the difficulty of discharging, and achieve the effects of saving equipment investment, convenient discharging, and low solvent toxicity

Active Publication Date: 2010-07-07
青岛智库生物技术有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In order to achieve the purpose of the present invention, we adopt the solvothermal method to synthesize semi-aromatic nylon by polymerizing aromatic dibasic acid and aliphatic diamine under relatively mild conditions. At the same time, the synthesized semi-aromatic nylon is in the form of powder , to solve the difficult problem of semi-aromatic nylon discharge

Method used

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  • Method for preparing semi-aromatic nylon
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  • Method for preparing semi-aromatic nylon

Examples

Experimental program
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Effect test

Embodiment 1

[0035] Weigh according to the mass ratio of dodecyl diamine and water as 1:10, mix well, heat to 90°C, after the dodecyl diamine dissolves, add terephthalic acid while stirring until the solution The pH value of the solution reached 7.2, and then continued to stir for 3 hours, then cooled to room temperature and kept stirring for 2 hours, filtered and dried to obtain white powder PA12T salt.

[0036] Put the prepared PA12T salt and absolute ethanol in a ratio of 1g / mL into a stainless steel polymerization kettle, replace the air in the kettle with carbon dioxide for 3 times, then gradually heat up to 205°C under stirring, and control the pressure inside the kettle at 2.8MPa , after keeping the pressure for 1 hour, slowly release the gas to make the pressure in the kettle drop to normal pressure within 2 hours, then raise the temperature to 215°C, continue the reaction for 3 hours, and obtain a white powdery PA12T product with an intrinsic viscosity of 1.72 dL / g. The infrared ...

Embodiment 2

[0038] Weigh according to the mass ratio of tridecyl diamine and water as 1:5, mix evenly, heat to 70°C, after the tridecyl diamine dissolves, add terephthalic acid while stirring until the solution The pH value of the solution reached 7.3, and then continued to stir for 2 hours, then cooled to room temperature and kept stirring for 5 hours, filtered and dried to obtain white powder PA13T salt.

[0039] Add the prepared PA13T salt and acetone into a stainless steel polymerization kettle at a ratio of 2g / mL, replace the air in the kettle with high-purity nitrogen for 3 times, then gradually heat up to 190°C under stirring, and control the pressure inside the kettle at 2.0MPa , after holding the pressure for 3 hours, slowly release the gas to make the pressure in the kettle drop to normal pressure within 3 hours, then raise the temperature to 220°C, continue the reaction for 5 hours, and obtain a white powdery PA13T product with an intrinsic viscosity of 1.85 dL / g. The infrared...

Embodiment 3

[0041] Weigh according to the mass ratio of hexamethylenediamine and water as 1:2, mix well, heat to 55°C, after the hexamethylenediamine dissolves, add terephthalic acid while stirring until the pH value of the solution reaches 7.7 , and then continued to stir for 1 hour, then cooled to room temperature and kept stirring for 2 hours, and obtained white powder PA6T salt after suction filtration and drying.

[0042] Add the prepared PA6T salt and methanol into a stainless steel polymerization kettle at a ratio of 3 g / mL, replace the air in the kettle with high-purity argon for 3 times, then gradually heat up to 230°C under stirring, and control the pressure inside the kettle at 3.0 MPa, after holding the pressure for 5 hours, slowly release the gas to reduce the pressure in the kettle to normal pressure within 2 hours, then raise the temperature to 270°C, continue the reaction for 5 hours, and discharge to obtain a white powdery PA6T product. The intrinsic viscosity of the prod...

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Abstract

The invention discloses a method for preparing semi-aromatic nylon and belongs to the technical field of macromolecular material synthesis. The method comprises the following steps: (1) uniformly mixing aliphatic diamine and water of which the weight is two to ten times that of the aliphatic diamine, heating the mixture to the temperature of between 50 and 90 DEG C, adding aromatic diacid into the mixture with stirring till a pH value of the solution reaches 7.0-7.7, continuously stirring for 1 to 5 hours, cooling the solution to room temperature, continuously stirring the solution for 1 to 5 hours again, and filtering and drying to obtain nylon salt for later use; and (2) adding the prepared nylon salt and a solvent to a polymerization kettle in a certain mixture ratio (0.5 to 3.0 g/mL), raising the temperature to between 190 and 230 DEG C under the protection of inert gas, keeping the pressure in the kettle between 2.0 and 3.0 MPa, discharging gas after 1 to 5 hours to make the pressure in the kettle reduced to normal pressure within 1 to 5 hours, raising the temperature to between 210 and 270 DEG C, and continuing to react for 1 to 5 hours, and discharging to obtain a powdery semi-aromatic nylon product. The method has mild reaction condition and low energy consumption; the product is easy to mold and machine; and the method solves the difficult problem of difficult discharging of the semi-aromatic nylon, and is applicable to industrialized production.

Description

technical field [0001] The invention relates to a semi-aromatic preparation method, which belongs to the technical field of polymer material synthesis. In particular, it relates to a method for preparing semi-aromatic nylon powder by solvothermal method. Background technique [0002] With the rapid development of contemporary science and technology, the market demand for heat-resistant resins is getting higher and higher. In recent years, in order to adapt to the development trend of product miniaturization, precision and low cost, the electronics industry often adopts the process of mounting and connecting semiconductor chips and electronic components on integrated circuit plates, so that surface mount technology (SMT) has been rapidly developed. promotion and popularization. The European Union implemented the RoHS&WEEE directive on July 1, 2006 [Introduction to the EU RoHS Directive, Power Supply Technology Application, 2007 (2), 65], which requires that the lead content...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G69/26C08G69/28
Inventor 刘民英赵清香付鹏李召朋王玉东
Owner 青岛智库生物技术有限公司
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