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A kind of preparation method of long carbon chain semi-aromatic nylon salt

A technology of semi-aromatic nylon and long carbon chain, which is applied to the preparation of long carbon chain semi-aromatic nylon salt and the field of preparing long carbon chain semi-aromatic nylon salt, can solve the problem that high-quality nylon salt cannot be prepared and the molecular weight of polymer product is not high. , uncontrollable molar ratio of products, etc., to achieve the effect of smaller surface tension, shorter reaction time and less harm to human body

Active Publication Date: 2016-02-03
ZHENGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When the above method is used to prepare long carbon chain semi-aromatic nylon salts with water as a solvent, when the ratio of the raw materials aromatic dibasic acid (amine) and aliphatic dibasic acid (acid) in the reaction system is large, the resulting salt Rapid crystallization, and the unreacted and undissolved aromatic dibasic acid (or amine) will be coated in the crystal of the salt, so that the coated aromatic dibasic acid (or amine) cannot participate in the formation Salt reaction, and then cause the salt to contain aromatic dibasic acid (amine), so that the molar ratio of the product is uncontrollable, and high-quality nylon salt cannot be prepared, resulting in low molecular weight and poor performance of the polymerized product

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Add 30.53kg of decanediamine, 29.47kg of terephthalic acid and 43.73kg of water into the reaction kettle, and stir at a speed of 20r / min. Under the protection of carbon dioxide inert gas, heat up to 140°C and stir at a speed of 20r / min. Under the protection of carbon dioxide inert gas, the pressure in the kettle is 0.4MPa, the pH value of the solution is adjusted to 7.3 with decanedidiamine, and stirred for 50 minutes. Rapidly cool down until nylon salt is precipitated, then cool down to room temperature at a rate of 20°C / h, centrifuge, and dry to obtain nylon 10T salt. The resulting nylon salt yield was 92%. Polymerization was carried out using the resulting 10T salt to obtain a polymer having a melting point of 315°C.

Embodiment 2

[0029] Add 29.08kg of undecanediamine, 25.92kg of terephthalic acid and 41.35kg of water into the reaction kettle, and stir at a speed of 200r / min. Under the protection of carbon dioxide inert gas, heat up to 145° C., the pressure inside the kettle is 0.4 MPa, adjust the pH value of the solution to 7.3 with undecyl diamine, and stir for 60 minutes. Rapidly lower the temperature until nylon salt is precipitated, then lower the temperature to room temperature at a rate of 30°C / h, centrifuge, and dry to obtain nylon 11T salt. The resulting nylon salt yield was 92%.

Embodiment 3

[0031] Add 35.48 kg of dodecyl diamine, 29.47 kg of terephthalic acid and 43.73 kg of water into the reaction kettle, and stir at a speed of 100 r / min. Under the protection of nitrogen inert gas, the temperature was raised to 150° C., the pressure inside the kettle was 0.5 MPa, the pH value of the solution was adjusted to 7.2 with dodecyl diamine, and the mixture was stirred for 70 minutes. Rapidly cool down until nylon salt is precipitated, then cool down to room temperature at a rate of 40°C / h, centrifuge, and dry to obtain nylon 12T salt. The resulting nylon salt yield was 93%. Polymerization was carried out using the resulting 12T salt to obtain a polymer having a melting point of 310°C.

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Abstract

The invention discloses a preparation method of a long-carbon-chain semi-aromatic nylon salt, belonging to the technical field of synthesis of high polymer materials. The preparation method comprises the following steps: (1) adding long-carbon-chain aliphatic diamine and aromatic binary acid or aromatic diamine and long-carbon-chain aliphatic binary acid into water according to a molar ratio of 1: 1, and uniformly stirring in an autoclave, wherein the mass fraction of the reactants is 20-80 percent; (2) under the protection atmosphere of inert gas, heating to 100-200 DEG C, preserving the pressure in the autoclave to 0.2-2Mpa, then adding a proper amount of corresponding diamine or binary acid to adjust the pH value of the solution, and when the pH value of the solution is 7.0-7.5, preserving heat for 0-5 hours and beginning to cool; (3) cooling at 5-50 DEG C / h, and when the temperature is reduced to room temperature, centrifugally separating to obtain the long-carbon-chain semi-aromatic nylon salt; (4) adding the centrifugally separated filtrate into the step (1) for recycling. According to the preparation method disclosed by invention, the molar ratio of the binary acid to the diamine can be accurately controlled, and the prepared semi-aromatic nylon salt is high in purity; in addition, the long-carbon-chain semi-aromatic nylon salt is prepared with water as a medium, the preparation method is simple to operate, the raw materials can be sufficiently reacted, and the salifying efficiency is high; the preparation method is environment-friendly and low in cost.

Description

technical field [0001] The invention relates to a preparation method of a long carbon chain semi-aromatic nylon salt, which belongs to the technical field of polymer material synthesis. In particular, it relates to a method for preparing long carbon chain semi-aromatic nylon salt with water as a solvent. Background technique [0002] It is usually distinguished according to the chemical reaction of nylon preparation, which can be divided into two categories: one is made by ring-opening polymerization of amino acid or lactam, usually called AB nylon; the other is made by polycondensation of dibasic acid and diamine Made, commonly known as AABB type nylon. Making dibasic acid and dibasic amine into nylon salt is the most commonly used method to prepare AABB type nylon. This method can effectively control the molar ratio of dibasic acid and dibasic amine, thereby controlling the molecular weight of nylon. [0003] Nylon 66 is the earliest and most important nylon species so f...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C209/00C07C211/09C07C211/51C07C213/08C07C217/90C07C51/41C07C55/21C07C55/02C07C63/28C07C63/24C07C65/24C07C63/15C07C63/333C07C63/331C07C63/38C07C317/44C07C315/04C08G69/26
Inventor 刘民英赵清香付鹏贾汝峰崔喆
Owner ZHENGZHOU UNIV