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Preparation method of carboxyl-terminated diamide

A technology of carboxyl-terminated diamides and diamine diacid salts, which is applied in the preparation of carboxyl-terminated diamides and the field of preparation of carboxyl-terminated diamides. It can solve the problems of high production costs and complicated process, and achieve slow activity and simple reaction process. , Improve the effect of hydrophilicity

Inactive Publication Date: 2021-02-12
DONGHUA UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In summary, the existing amide preparation technology exists, the process is complicated, the production cost is high, and the amount of three wastes (waste water, waste gas and solid waste) is large

Method used

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  • Preparation method of carboxyl-terminated diamide
  • Preparation method of carboxyl-terminated diamide

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preparation example Construction

[0032] A kind of preparation method of carboxyl-terminated diamide, such as reaction formula 1 or reaction formula 2, diamine diacid salt (structural formula is I), dibasic acid (structural formula is II or IV) and non-polar organic solvent (toluene, One or more of xylene and trimethylbenzene) are mixed and reacted, and the generated water is removed by azeotropic distillation while reacting to obtain a carboxyl-terminated diamide; wherein, the molar ratio of diamine diacid salt to dibasic acid is 1 :1~2, the ratio of the volume of the nonpolar organic solvent to the mass of the diamine diacid salt is 1~10:1 (mL / g), the reaction temperature is 10~30°C higher than the boiling point of the nonpolar organic solvent, and the reaction The time is 12-20 hours, and the azeotropic distillation adopts an oil-water separation device. The temperature of the azeotropic distillation is higher than the boiling point of the non-polar organic solvent, and the time of the azeotropic distillatio...

Embodiment 1

[0036] A kind of preparation method of carboxyl-terminated diamide, diamine diacid salt (structural formula is ), dibasic acid (structural formula is ) mixed with a non-polar organic solvent (xylene) to react, carry out azeotropic distillation to remove the generated water while reacting, and obtain the carboxyl-terminated diamide; wherein, the molar ratio of the diamine diacid salt to the dibasic acid is 1:1.5, the ratio of the volume of non-polar organic solvent to the mass of diamine diacid salt is 6:1 (mL / g), the reaction temperature is 160°C, the reaction time is 18h, and the azeotropic distillation adopts an oil-water separation device. The temperature of azeotropic distillation is 160°C, and the time of azeotropic distillation is 18h;

[0037] After the reaction is completed, use an alcoholic organic solvent (ethanol) for purification. The specific process is: firstly mix the reacted mixture with an alcoholic organic solvent at a temperature of 65°C, cool to normal te...

Embodiment 2

[0047] A kind of preparation method of carboxyl-terminated diamide, diamine diacid salt (structural formula is ), dibasic acid (structural formula is ) mixed with a non-polar organic solvent (toluene) to react, and carry out azeotropic distillation to remove the generated water while reacting to obtain a carboxyl-terminated diamide; wherein, the molar ratio of diamine diacid salt to dibasic acid is 1 : 1.4, the ratio of the volume of the non-polar organic solvent to the mass of the diamine diacid salt is 6:1 (mL / g), the reaction temperature is 150°C, the reaction time is 16h, and the azeotropic distillation adopts an oil-water separation device. The temperature of boiling distillation is 150°C, and the time of azeotropic distillation is 16h;

[0048] After the reaction is completed, use an alcoholic organic solvent (ethanol) for purification. The specific process is: firstly mix the reacted mixture with an alcoholic organic solvent at a temperature of 65°C, cool to normal t...

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Abstract

The invention relates to a preparation method of carboxyl-terminated diamide, which comprises the following steps: mixing diamine diacid salt, binary acid (aliphatic binary acid or aromatic binary acid) and a non-polar organic solvent, reacting, and carrying out azeotropic distillation at the temperature higher than the boiling point of the non-polar organic solvent to remove water in the product,thereby obtaining the carboxyl-terminated diamide. The molar ratio of the diamine diacid salt to the binary acid is 1:(1-2). The preparation method of the carboxyl-terminated diamide is simple in process and mild in condition; and the carboxyl-terminated diamide can be used as a modifier for polyester reaction, thereby avoiding the phenomenon of color change caused by reaction with byproducts inthe polyester copolymerization process.

Description

technical field [0001] The invention belongs to the technical field of preparation of amide monomers, and relates to a method for preparing carboxyl-terminated diamides, in particular to a method for preparing carboxyl-terminated diamides by reacting diamine diacids with aliphatic dibasic acids or aromatic dibasic acids Methods. Background technique [0002] Amide salts are stable, can be transported without any special precautions, and are easy to store. They are widely used as industrially important substances, and their application to the synthesis of polyester as a hydrophilic modifier is also an important research direction. However, because the exposed ammonium radicals in the organic ammonium salts are prone to side reactions with the polyester copolymerization process and produce discoloration, this phenomenon greatly affects the application of amide salts. It is very necessary to protect the ammonium root with carboxylate group and develop the reaction to generate ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C231/02C07C233/36C07C233/40C08G63/91
CPCC07C231/02C08G63/91C07C233/36C07C233/40
Inventor 王学利孙莉娜黄莉茜俞建勇郭娟子胡红梅朱瑞淑刘修才
Owner DONGHUA UNIV
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