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Caprolactam compound and preparation method and application thereof, and polylactic acid composition

A technology of caprolactam and amidation reaction, applied in the field of polymer chemistry, can solve the problems of agglomeration, dispersion and unevenness, achieve good compatibility, overcome agglomeration and uneven dispersion, and improve crystallization performance

Active Publication Date: 2018-05-01
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to provide a new caprolactam compound and its preparation method and application and polylactic acid composition. The caprolactam compound can overcome the problem of agglomeration or inhomogeneous dispersion of traditional nucleating agents in polylactic acid, effectively improve polylactic acid Crystallization properties of the composition

Method used

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  • Caprolactam compound and preparation method and application thereof, and polylactic acid composition
  • Caprolactam compound and preparation method and application thereof, and polylactic acid composition
  • Caprolactam compound and preparation method and application thereof, and polylactic acid composition

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preparation example Construction

[0027] In a second aspect, the present invention also provides a method for preparing a caprolactam compound, wherein the method includes:

[0028] A, the compound shown in formula (2) is carried out acid chloride reaction with thionyl chloride;

[0029] B, carrying out amidation reaction with the compound shown in the reaction product of step a and formula (3);

[0030]

[0031] Among them, R is hydrogen or C 1 -C 6 straight-chain or branched-chain alkyl groups.

[0032] In the present invention, preferably, R is hydrogen or C 1 -C 6 straight-chain alkyl; more preferably, R hydrogen or C 1 -C 3 straight chain alkyl; most preferably, R is hydrogen or methyl.

[0033] The present invention is not particularly limited to the consumption of the compound shown in formula (2) and thionyl chloride, preferably, the molar ratio of the consumption of the compound shown in formula (2) and the consumption of thionyl chloride is 0.05- 0.5:1, more preferably 0.1-0.2:1.

[0034]...

Embodiment approach

[0046] In the present invention, the method may further include a step of purifying the obtained product after the amidation reaction is completed. According to a specific embodiment of the present invention, the purification method includes: after the amidation reaction is completed, the solvent is removed, and the reaction product of the amidation reaction is dissolved in chloroform, and then the catalyst and unreacted raw materials are removed by water extraction .

[0047] In the third aspect, the present invention also provides the caprolactam compound prepared by the above method. The caprolactam compound does not contain a benzene ring structure, and has no new negative impact on the environment after degradation.

[0048] In the fourth aspect, the present invention also provides the use of the caprolactam compound described in the present invention as a nucleating agent. As a nucleating agent, the caprolactam compound can overcome the problems of agglomeration and un...

preparation example 1

[0062] Mix 0.1 mol of compound 1 (having the structure shown in formula (2), wherein R is hydrogen) with 0.5 mol of thionyl chloride, add 0.5 ml of catalyst DMF to the resulting mixture, and at 90 ° C, acid chloride reaction After 4 hours, DMF was removed by distillation under reduced pressure to obtain the intermediate product Z1.

[0063] 0.5mol of α-aminocaprolactam (with the structure shown in formula (3)) was dissolved in 20mlDMF, and 0.5mol catalyst triethylamine was added; intermediate product Z1 was dissolved in 10mlDMF, and the mixture containing intermediate product Z1 and DMF Slowly add dropwise to the mixture formed by α-aminocaprolactam, DMF and triethylamine, and perform amidation reaction at 0°C for 12 hours. After the DMF solvent is removed by pressurization, the product is dissolved in chloroform and removed by water extraction. catalyst and unreacted raw materials, and the resulting mixture was dried to remove chloroform to obtain caprolactam compound A1.

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Abstract

The invention discloses a caprolactam compound and a preparation method and application thereof, and a polylactic acid composition, belonging to the field of high polymer chemistry. The caprolactam compound has a structure as shown in a formula (1) which is described in the specification. In the formula, R is hydrogen or C1-6 straight-chain or branched-chain alkyl group. The caprolactam compound does not contain a phenyl ring structure, so the caprolactam compound has no negative influence on environment after degradation. The caprolactam compound has good compatibility with polylactic acid; and when the caprolactam compound is applied as a nucleating agent to polylactic acid, the problems of agglomeration and nonuniform dispersion of traditional nucleating agents in polylactic acid can beovercome, and the crystallization performance of the polylactic acid composition can be effectively improved.

Description

technical field [0001] The invention relates to the field of polymer chemistry, in particular to a caprolactam compound, a preparation method and application thereof, and a polylactic acid composition. Background technique [0002] Polylactic acid (PLA) is a polymer with excellent biocompatibility and can be prepared from renewable resource crops. The most prominent advantage is biodegradability, which can be completely degraded in the natural environment to generate carbon dioxide and water. It has the characteristics of not polluting the environment. Polylactic acid has good mechanical properties, thermoplasticity, fiber formation, and high transparency. It is suitable for making polylactic acid products by various processing methods such as blow molding and thermoplastic. It is easy to process and is defined by the industry as the most promising development in the new century. New Materials. [0003] Although polylactic acid has extraordinary mechanical properties, its ...

Claims

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Application Information

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IPC IPC(8): C07D493/04C08L67/04C08K5/3412
CPCC07D493/04C08K5/3412C08L2205/24C08L67/04
Inventor 计文希许宁祝桂香张龙贵李娟殷建军
Owner CHINA PETROLEUM & CHEM CORP
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