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Preparation method of polycaprolactone crystal

A polycaprolactone and crystal technology, which is applied in the field of polycaprolactone crystal preparation, can solve the problems of severe crystallization conditions and great influence on the performance of PCL films, and achieves the effect of a simple method.

Pending Publication Date: 2022-05-27
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the conditions for epigenetic crystallization are harsh, and the post-treatment has a great influence on the performance of PCL thin films

Method used

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  • Preparation method of polycaprolactone crystal

Examples

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preparation example Construction

[0025] The invention provides a method for preparing polycaprolactone crystals, which comprises the steps of: preparing a polycaprolactone-polyvinyl chloride blend film; and forming a polycaprolactone crystal. A detailed description is given below.

[0026]

[0027] Polycaprolactone, polyvinyl chloride and a solvent are formed into a blending solution. Specifically, polycaprolactone and polyvinyl chloride are mixed with a solvent to obtain a blended solution.

[0028] The solvent is tetrahydrofuran or 2-methyltetrahydrofuran, preferably, the solvent is tetrahydrofuran. In the blend solution, the total mass fraction of polycaprolactone and polyvinyl chloride is 4.5-5.5 wt %, preferably 4.7-5.3 wt %, and more preferably 5.0-5.3 wt %.

[0029] In the blended solution, the mass ratio of polycaprolactone and polyvinyl chloride is 70-80:20-30, preferably 70-75:20-30; more preferably 70-75:25-30. This facilitates the formation of polycaprolactone crystals in which a-axis orienta...

preparation example 1-

[0054] Preparation Example 1 - Preparation of Polycaprolactone-PVC Blended Film

[0055] (1) Disperse polycaprolactone and polyvinyl chloride with a mass ratio of 70:30 in tetrahydrofuran, and stir at a stirring rate of 600 r / min at 40° C. for 6 h to obtain a total of polycaprolactone and polyvinyl chloride. The mass fraction is 5wt% of the blended solution.

[0056] (2) Spread the above blended solution evenly in a 75ml petri dish; dry it in a vacuum drying oven, dry at 35°C and a vacuum of 0.1MPa for 48h, and gently peel off the blended film from the petri dish , to obtain a polycaprolactone-polyvinyl chloride blend film with a thickness of 100 μm. The above-mentioned polycaprolactone-polyvinyl chloride blend film was passed through a dumbbell-shaped stretch spline die and a pneumatic punching machine to form a dumbbell-shaped polycaprolactone-polyvinyl chloride blend film.

Embodiment 1

[0058] The dumbbell-shaped polycaprolactone-polyvinyl chloride blend film obtained in Preparation Example 1 was fixed on a stretching machine and placed in an infrared spectrometer for scanning; then the dumbbell-shaped polycaprolactone-polyvinyl chloride film was The blended film was heated to 100°C at a heating rate of 20°C / min and kept for 20min;

[0059] The dumbbell-shaped polycaprolactone-polyvinyl chloride blend film was cooled with liquid nitrogen, and rapidly cooled to 40°C at a cooling rate of 60°C / min;

[0060] Immediately, the polycaprolactone-polyvinyl chloride blend film was stretched at 40 °C with a stretching rate of 100 μm / s and a stretching ratio of 4, and isothermally crystallized at 40 °C for 750 min to obtain polycaprolactone crystals.

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Abstract

The invention discloses a preparation method of a polycaprolactone crystal, which comprises the following steps: (1) heating a polycaprolactone-polyvinyl chloride blended film to 80-110 DEG C at a heating rate of 10-30 DEG C / min, and keeping the temperature for 10-30 minutes; wherein the polycaprolactone-polyvinyl chloride blended film is not attached to the substrate subjected to induced orientation; (2) cooling the polycaprolactone-polyvinyl chloride blended film obtained in the step (1) to 35-45 DEG C at a cooling rate of 55-65 DEG C / min; and (3) stretching and crystallizing the polycaprolactone-polyvinyl chloride blended film obtained in the step (2) at 35-45 DEG C at a stretching rate of 90-110 [mu] m / s and a stretching ratio of 3.5-5.5, so as to obtain the polycaprolactone crystal in which only a-axis orientation and b-axis orientation coexist. According to the invention, the polycaprolactone crystal with specific orientation can be obtained.

Description

technical field [0001] The invention relates to a preparation method of polycaprolactone crystals. Background technique [0002] Polycaprolactone (PCL) is a semi-crystalline aliphatic polyester with a single crystal form. Due to its good biocompatibility and degradability, it can be used in drug controlled release carriers, packaging materials and surgical sutures, etc., and has received extensive attention. However, there are still relatively few crystal studies on PCL. [0003] CN108084477A discloses a preparation method of a polymer oriented film. (1) The first polymer oriented film is prepared by melt stretching method, and the first polymer oriented film is attached to the substrate; (2) The second polymer blend solution is attached to the first polymer by spin coating method On the oriented film, a second polymer film is formed, and then heat treatment is performed to obtain a polymer oriented film with parallel lamellae. The above method needs to prepare the first...

Claims

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Application Information

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IPC IPC(8): B29D7/01C08L67/04C08L27/06C08J5/18B29K67/00B29K27/06
CPCB29D7/01C08J5/18B29K2067/00B29K2027/06C08J2367/04C08J2427/06
Inventor 李慧慧万茹茹闫寿科
Owner BEIJING UNIV OF CHEM TECH