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A method for detecting the prepolymerization temperature of nylon salt

A nylon salt and nylon technology is applied in the field of detecting nylon salt prepolymerization temperature, which can solve the problems of wasting raw materials, long research period, product quality depends on quality and structure, etc., and achieves the effect of increasing molecular weight and avoiding volatilization

Active Publication Date: 2017-01-04
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

If the selected prepolymerization temperature is low, the nylon salt will not react completely during the prepolymerization process. During the subsequent temperature rise polymerization process, the unprepolymerized nylon salt will also lose the short carbon chain diamine component, and will eventually reduce Molecular Weight of Nylon Products
In addition, there are problems such as waste of raw materials, long research cycle, and product quality depending on the quality and structure of the polymerization kettle to study the polymerization process conditions of nylon salt directly through the polymerization kettle.

Method used

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  • A method for detecting the prepolymerization temperature of nylon salt
  • A method for detecting the prepolymerization temperature of nylon salt
  • A method for detecting the prepolymerization temperature of nylon salt

Examples

Experimental program
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Effect test

Embodiment 1

[0023] 1. Determine the prepolymerization temperature of nylon salt

[0024](1) Preparation of nylon salt: Add 24kg of dodecanedibasic acid produced by fermentation into the neutralization tank, then add 5 times the mass of ethanol solvent, heat while stirring until the temperature reaches 70°C, and add 11.6kg of Dissolve hexamethylenediamine in 2 times the mass of ethanol at 70°C, gradually add the ethanol solution of hexamethylenediamine dropwise to the neutralization tank, maintain the stirring rate at 100r / min, and control the reaction temperature at 72°C until the neutralization tank When the pH value of the inner solution reaches 6.5, stop adding the ethanol solution of hexamethylenediamine, keep warm for 0.5 hours, and slowly cool to room temperature. After the nylon salt is precipitated, the material is put into a centrifuge, and 32.5kg of nylon 612 salt is obtained after separation. Yield 91.5%.

[0025] (2) Pretreatment of nylon salt: Take 60g of dry white powdery n...

Embodiment 2

[0031] 1. Determine the polymerization temperature of nylon salt

[0032] (1) Preparation of nylon salt: Add 26.5kg of tridecanedibasic acid produced by fermentation into the neutralization tank, then add 5 times the mass of ethanol solvent, heat while stirring until the temperature reaches 75°C, and add 11.6 Dissolve kg of hexamethylenediamine in 2 times the mass of ethanol at 75°C, gradually add the ethanol solution of hexamethylenediamine dropwise to the neutralization tank, maintain the stirring rate at 100r / min, and control the reaction temperature at 75°C until neutralization When the pH value of the solution in the kettle reaches 6.0, stop adding the ethanol solution of hexamethylenediamine dropwise, keep warm for 1.0 hour, and slowly cool to room temperature. After the nylon salt is precipitated, the material is put into a centrifuge, and 34.4kg of nylon 613 salt is obtained after separation. The salt yield is 90%.

[0033] (2) Pretreatment of nylon salt: Take 70g of ...

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Abstract

The invention discloses a method for detecting a prepolymerization temperature of a nylon salt. The method comprises the following steps: (1) adding white powder-shaped nylon salt prepared by condensation polymerization between binary acid and diamine into distilled water according to a ratio of (1:1)-(1:2), heating to the temperature of 60-80 DEG C so as to dissolve the nylon salt, and maintaining the temperature so as to completely volatilize the distilled water, thereby obtaining a transparent nylon salt sample; (2) taking the dried nylon salt sample, preparing a sheet by adopting a KBr method, wherein the mass ratio of the sample to KBr is (1:100)-(1:300), the thickness of the sample sheet is 0.3-0.6mm, and the baseline infrared transmittance is higher than 85 percent; and (3) detecting the heated amidation of the nylon salt under a constant rate by adopting an in-situ transmission infrared spectrum, thereby obtaining the prepolymerization temperature of the nylon salt. According to the method disclosed by the invention, the structural change of the nylon salt in the polymerization process can be really monitored, the optimal prepolymerization temperature is obtained, volatilization of short carbon chain diamine components is avoided, the molar ratio of the diamine and binary acid is guaranteed, and the molecular weight of a polyamide product is improved.

Description

technical field [0001] The invention relates to a method for detecting the prepolymerization temperature of nylon salt. Background technique [0002] Polyamide (PA, commonly known as nylon) was the first resin developed by DuPont in the United States for fiber, and it was industrialized in 1939. In the 1950s, the development and production of injection molding products began to replace metals to meet the requirements of lightweight and cost-reducing downstream industrial products. Polyamide has good comprehensive properties, including mechanical properties, heat resistance, wear resistance, chemical resistance and self-lubricating properties, low friction coefficient, certain flame retardancy, easy processing, suitable for glass fiber and Other fillers are filled and modified to improve performance and expand application range. [0003] There are many varieties of PA, including PA6, PA66, PA11, PA12, PA46, PA610, PA612, PA1010, etc., as well as many new varieties such as s...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N25/00G01N25/02
Inventor 李澜鹏白富栋王艳张全乔凯王领民
Owner CHINA PETROLEUM & CHEM CORP