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Semi-aromatic polyamide and preparation method thereof

A semi-aromatic and polyamide technology, which is applied in the field of semi-aromatic polyamide preparation, can solve the problems of uncontrollable molecular weight of semi-aromatic polyamide, difficulty in meeting the requirements of industrialized large-scale production, irregular distribution of molecular segments, etc. The process is green and environmentally friendly, the production cost is low, and the reaction is easy to control.

Active Publication Date: 2017-09-22
ZHEJIANG NHU SPECIAL MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The polyester polycondensation method uses macromolecular polyester resins as raw materials, resulting in uncontrollable molecular weight of the target product semi-aromatic polyamide, difficulty in molecular chain growth in the later stage, wide molecular weight distribution, irregular distribution of molecular segments, and single and impure products. It is difficult to meet the requirements of industrialized mass production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0058]30Kg of solid hexamethylenediamine with a content of more than 99.7% was completely dissolved in a water bath at 65°C and added to the stirring polymerization reactor, then the stirring was started, 15Kg deionized water was added to the reactor, and 24.50Kg was added to the reactor. of terephthalic acid, 14.38Kg of adipic acid, 590.7g of acetic acid, 130.3g of sodium hypophosphite, 194.4g of polydimethylsiloxane, and then added 2.5Kg of deionized water to the reactor, using After 3 times of nitrogen replacement, the temperature began to rise. When the temperature rose to 130 °C, the exhaust valve on the reactor was opened to exhaust for 2 minutes, and then the temperature continued to rise. The temperature was raised to 220°C within 1.5 hours, the temperature was maintained at 220°C for 10 min, and then the reaction temperature was continued to rise to 240°C. During the heating process, when the reaction pressure reached 2.0MPa, the exhaust valve was opened to discharge ...

Embodiment 2

[0062] The preparation steps of Example 1 were repeated, except that the tackifying method of the prepolymer was changed to solid-phase polymerization. Under the conditions of nitrogen atmosphere and 250°C, solid-phase polymerization was carried out for 8 hours to obtain light yellow semi-aromatic polyamide resin. Its intrinsic viscosity is 0.89dL / g, glass transition temperature is 94.76℃, melting point is 316.07℃, melting enthalpy is 52.53J / g, decomposition temperature is 424℃, and molecular weight distribution is 3.7.

Embodiment 3

[0064] 30Kg of solid hexamethylenediamine with a content of more than 99.7% was completely dissolved in a water bath at 65 ° C and added to the stirring polymerization reactor, then the stirring was started, 15Kg deionized water was added to the reactor, and 24.75Kg was then added to the reactor. terephthalic acid, 16.50Kg isophthalic acid, 606.5g benzoic acid, 157.9g sodium hypophosphite, 195.1g polydimethylsiloxane, then add 2.81Kg deionized water in the reactor After 3 times of nitrogen replacement, the temperature rises. When the temperature rises to 130 °C, open the exhaust valve on the reactor to exhaust for 2 minutes, and then continue to heat up. The temperature was raised to 230°C within 1.5 hours, the temperature was maintained at 230°C for 10 min, and then the reaction temperature was continued to rise to 250°C. During the heating process, when the reaction pressure reached 2.50MPa, the exhaust valve was opened to discharge the steam to keep the pressure constant at...

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Abstract

The invention discloses semi-aromatic polyamide and a preparation method thereof. The preparation method comprises the following steps that (a), dicarboxylic acid and diamine are subjected to a neutralization reaction with water as the solvent, and a semi-aromatic polyamide salt solution is formed; (b), the semi-aromatic polyamide salt solution obtained in the step (a) is further subjected to warming, polycondensation of the solution is promoted by continuous drainage, and after prepolymerization of the solution, semi-aromatic polyamide prepolymer is obtained; (c), the semi-aromatic polyamide prepolymer obtained in the step (b) is subjected to a viscosity-enhancing reaction, and the semi-aromatic polyamide is obtained. According to the preparation method, the aggregate-level dicarboxylic acid and diamine are adopted, so that the operational process is simplified; a diamine online separation recovery device is used for conducting separation and recycling on the diamine in a prepolymerization process, so that the volatilization loss of the diamine along with water vapor is effectively reduced, and pollution generation is avoided; the molar ratio of the diamine to the dicarboxylic acid in the prepolymerization process is kept, so that the yield coefficient is increased, and the product with stable quality is obtained.

Description

technical field [0001] The invention relates to the field of polyamide materials, in particular to a preparation method of semi-aromatic polyamide. Background technique [0002] Since its industrialization, polyamide has been widely used in clothing due to its excellent mechanical properties and good electrical properties, as well as its excellent heat resistance, wear resistance, chemical resistance and self-lubricating properties, as well as good processing properties. In the field of fibers and industrial materials, and as a general engineering plastic, it is also widely used in the automotive, electrical and electronic fields. However, the general polyamides are dimensionally unstable due to the easy absorption of water, and have insufficient heat resistance. With the development of science and technology, the requirements for materials in the electrical and electronic industry and other fields are getting higher and higher. For polyamides used in these fields, high he...

Claims

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Application Information

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IPC IPC(8): C08G69/26C08G69/28C08G69/30
Inventor 宋恩峰张琴吴笑笑洪文刚周贵阳邓杭军
Owner ZHEJIANG NHU SPECIAL MATERIALS
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