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Method for preparing polyamide

A technology for polyamide and pre-polycondensation, applied in the field of preparation of polyamide 5X, can solve the problems of low molecular weight, reduced polyamide yield, complexity, etc., and achieve the effects of reduced emissions, good mechanical properties, and reduced energy consumption

Inactive Publication Date: 2016-08-24
CATHAY R&D CENT CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Yet no matter be which kind of polycondensation method, all there is following problem: 1) precondensation effect is not good, can only obtain the prepolymer with lower molecular weight, has increased the time of follow-up polymerization and energy consumption
2) There is more water in the entire polymerization process system, and the existence of more water will increase the tendency of reverse reaction, which is not good for polyamide polymerization, and the water removal process is not only difficult but also complicated
In addition, there is a large amount of water in the low-concentration nylon salt solution, and the process of removing water also requires a lot of heat energy, which greatly increases the energy consumption of the reaction system; at the same time reduces the yield of each batch of polyamide

Method used

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  • Method for preparing polyamide

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preparation example Construction

[0020] The invention provides a method for preparing polyamide, comprising: preparing the polyamide by precondensing and polycondensing a raw material solution with a concentration of 75 to 100 wt% by weight; wherein, the raw material solution is 1, Nylon salt solution formed by 5-pentanediamine and dibasic carboxylic acid, or a mixture of 1,5-pentanediamine and dibasic carboxylic acid with a total concentration of 75 to 100 wt %; the dibasic carboxylic acid is selected from One or more of aliphatic dibasic acids.

[0021] The weight percentage concentration of raw material solution among the present invention refers to in nylon salt solution, and nylon salt accounts for the weight percentage in nylon salt solution, is expressed as with formula: m 尼龙盐 / m 尼龙盐溶液 ×100%; or in the mixed solution of 1,5-pentanediamine and dicarboxylic acid, the total mass of 1,5-pentanediamine and dicarboxylic acid accounts for the mass percentage of the mixed solution.

[0022] The obtained poly...

Embodiment 1

[0046] (1) After mixing 1,5-pentanediamine and adipic acid at a molar ratio of 1:1.02, they are fed into the salt-forming reactor at a flow rate of 1500kg / hr for salt-forming reaction. The salt-forming temperature is 80°C and the pressure is 0.15 MPa, prepare 1,5-pentamethylenediamine adipate solution of 80wt% (nylon salt accounts for the mass percentage of nylon salt solution);

[0047] (2) The 1,5-pentamethylenediamine adipate solution prepared in step (1) is pumped into a concentration tank for concentration through a supply pump at a temperature of 150°C and a pressure of 0.2MPa to obtain 90wt% of 1,5- Concentrated solution of pentamethylenediamine adipate;

[0048] (3) The above-mentioned concentrated solution of 1,5-pentamethylenediamine adipate was pumped to a parallel tubular reactor for prepolymerization. The prepolymerization temperature was 260°C, the prepolymerization pressure was 1 MPa, and the prepolymerization time was 45 minutes. get prepolymer;

[0049] (4) ...

Embodiment 2

[0054] (1) After mixing 1,5-pentamethylenediamine and adipic acid at a molar ratio of 1:1.03, add 100ppm (relative to the weight of 1,5-pentamethylenediamine adipate) of Bruggemann H10 (Bruggolen H10 produced by Bruggolen, Germany) carries out a salt-forming reaction with a salt-forming temperature of 80°C and a pressure of 0.15MPa to make 75wt% 1,5-pentamethylenediamine adipate solution;

[0055] (2) The 1,5-pentamethylenediamine adipate solution prepared in step (1) is pumped to the concentration tank for concentration, the temperature is 160°C, the pressure is 0.3MPa, and 90wt% of 1,5 - concentrated solution of pentamethylenediamine adipate;

[0056] (3) Send the above-mentioned 1,5-pentamethylenediamine adipate concentrated solution to a parallel tubular reactor through a supply pump for prepolymerization. The prepolymerization temperature is 260°C, the pressure is 3MPa, and the time is 50min to obtain a prepolymer. ;

[0057] (4) Lead the prepolymer into a continuous re...

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Abstract

The invention provides a method for preparing polyamide. The method comprises the steps that a raw material solution with the weight percent concentration being 75 wt% to 100 wt% is subjected to a pre-polycondensation reaction and a polycondensation reaction, and polyamide is prepared, wherein the raw material solution is a nylon salt solution prepared from 1,5-pentamethylene diamine and dicarboxylic acid, or a mixture solution of 1,5-pentamethylene diamine and dicarboxylic acid with the total concentration being 75 wt% to 100 wt%. Dicarboxylic acid is one or more selected from aliphatic dibasic acids. Polyamide prepared from the method is good in physical and mechanical performance. Volatilization of 1,5-pentamethylene is obviously inhibited in the whole preparation process, therefore, energy consumption is reduced, cost is reduced, and meanwhile emissions to the environment are reduced.

Description

technical field [0001] The invention relates to a preparation method of polyamide, in particular to a preparation method of polyamide 5X produced by the reaction of 1,5-pentanediamine and dibasic carboxylic acid. Background technique [0002] In the prior art, polyamide polymerization methods can generally be divided into heating polycondensation method and interfacial polycondensation method. For example: Document 1 (Bacon Ke, A.W.Sisko, Differential thermal analysis of highpolymers.III.Polyamides, Journal of Polymer Science, Volume 50, No. 153, Pages 87-98, March 1961) discloses a thermal polycondensation method . However, according to reports (J. Polym. Sci. 50, 87, 1961; Macromolecules, 30, 8540, 1998), compared with the interfacial polycondensation method, the polyamide obtained has a low melting point and poor heat resistance. shortcoming. On the other hand, the process of the interfacial polycondensation method is very complicated, and it is difficult to apply it i...

Claims

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Application Information

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IPC IPC(8): C08G69/28
Inventor 秦兵兵胡定军郑毅刘驰刘修才
Owner CATHAY R&D CENT CO LTD
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