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Polycaprolactone-based polyamide composite material and preparation method thereof

A technology based on polyamide and polycaprolactone, which is applied in the field of polycaprolactone-based polyamide composite materials and its preparation, can solve problems such as limiting the application range of materials, unpleasant odor of materials, and affecting the mechanical properties of materials

Active Publication Date: 2020-06-02
HUNAN JUREN CHEM NEW MATERIAL TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Due to its good biocompatibility and biodegradability, polycaprolactone is widely used in degradable plastics, tissue engineering devices, drug packaging and carriers, green coatings, environmentally friendly hot melt adhesives and other fields, and it is currently the most promising One of the environmentally friendly materials, however, the melting point of polycaprolactone is around 59 ° C ~ 60 ° C, the lower melting point greatly limits the scope of application of the material
Moreover, in the traditional preparation process of polycaprolactone, some cyclic or linear oligomers will inevitably be produced due to the "bite back" of the chain segment. The existence of these oligomers will not only make the material smell bad smell, and will affect the mechanical properties of the material

Method used

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Examples

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preparation example Construction

[0024] The invention provides a kind of preparation method of polycaprolactone-based polyamide composite material, comprises the following steps:

[0025] (1) After mixing ε-caprolactone, alcohols end-capping agent and tin catalyst, carry out prepolymerization reaction to obtain ε-caprolactone prepolymer;

[0026] (2) carry out polymerization reaction after mixing caprolactam, acidic end-capping agent and water, obtain caprolactam prepolymer;

[0027] The steps (1) and (2) are not in chronological order;

[0028] (3) After mixing the ε-caprolactone prepolymer, the caprolactam prepolymer and the catalyst, carry out a copolymerization reaction to obtain a polycaprolactone-based polyamide composite material;

[0029] The catalyst is n-butyl titanate and / or antimony trioxide;

[0030] The mass ratio of the ε-caprolactone prepolymer to the caprolactam prepolymer is 1~9:1~9;

[0031] The temperature of the copolymerization reaction is 100-250°C, and the time is 2h-16h.

[0032] ...

Embodiment 1

[0047] 100 parts by mass of ε-caprolactone, 1 part by mass of ethanol, and 0.001 parts by mass of tin catalyst (stannous octoate and tetraethyltin) previously vacuum-dried to remove water were added to the polymerization kettle, and the rotating speed was adjusted to 100 rpm, and nitrogen was purged at 0.5 After one hour, the temperature was adjusted to 140° C., and the product was taken out after 6 hours of reaction. After the product was pulverized, dried, and extracted with THF, the solid was collected to obtain an ε-caprolactone prepolymer.

[0048] Add 100 parts by mass of caprolactam, 5 parts by mass of adipic acid, and 1 part by mass of water that have been vacuum-dried in advance to remove water, respectively, into the polymerization kettle, adjust the rotation speed to 80rmp, purse with nitrogen for 0.5h, adjust the temperature to 240°C, and take it out after 10h of reaction The product, the product is pulverized, dried, extracted with water, and the solid is collected...

Embodiment 2

[0056] 100 parts by mass of ε-caprolactone, 1 part by mass of ethylene glycol, and 0.05 parts by mass of tin catalyst (methyl tin trichloride and tin tetrachloride) that were previously vacuum-dried to remove water were added to the polymerization kettle together, and the rotating speed was adjusted to 100rpm, nitrogen purging for 0.5h and then adjust the temperature to 140°C. After reacting for 6h, the product was taken out. After the product was pulverized, dried and extracted with tetrahydrofuran, the solid was collected to obtain ε-caprolactone prepolymer.

[0057] Add 100 parts by mass of caprolactam, 5 parts by mass of adipic acid, and 5 parts by mass of water, which have been vacuum-dried and dehydrated, respectively into the polymerization kettle, adjust the rotation speed to 80rmp, purse with nitrogen for 0.5h, adjust the temperature to 220°C, and take it out after 10h of reaction The product, the product is pulverized, dried, extracted with water, and the solid is col...

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Abstract

The invention relates to the field of high polymer materials, and provides a polycaprolactone-based polyamide composite material and a preparation method thereof. The preparation method comprises thefollowing steps of: mixing epsilon-caprolactone, an alcohol end-capping reagent and a tin catalyst, and carrying out prepolymerization reaction to obtain an epsilon-caprolactone prepolymer; mixing caprolactam, an acidic end-capping reagent and water, and carrying out polymerization reaction to obtain a caprolactam prepolymer; and then mixing the epsilon-caprolactone prepolymer, the caprolactam prepolymer and a catalyst, and carrying out copolymerization reaction to obtain the polycaprolactone-based polyamide composite material. The polycaprolactone-based polyamide composite material prepared by the preparation method disclosed by the invention has the characteristics of proper melting point, low oligomer content, and high tensile strength and elongation at break; results of embodiments show that the melting point of the polycaprolactone-based polyamide composite material is 80-200DEG C, the mass content of the oligomer is 1.27%-3.56%, the tensile strength is 38MPa-60MPa, and the elongation at break is 1270%-1890%.

Description

technical field [0001] The invention relates to the field of polymer materials, in particular to a polycaprolactone-based polyamide composite material and a preparation method thereof. Background technique [0002] Due to its good biocompatibility and biodegradability, polycaprolactone is widely used in degradable plastics, tissue engineering devices, drug packaging and carriers, green coatings, environmentally friendly hot melt adhesives and other fields, and it is currently the most promising One of the environmentally friendly materials, however, the melting point of polycaprolactone is around 59°C to 60°C, and the lower melting point greatly limits the application range of the material. Moreover, in the traditional preparation process of polycaprolactone, some cyclic or linear oligomers will inevitably be produced due to the "bite back" of the chain segment. The existence of these oligomers will not only make the material smell bad smell, and will affect the mechanical ...

Claims

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Application Information

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IPC IPC(8): C08G69/44
CPCC08G69/44
Inventor 易春旺龚彩红
Owner HUNAN JUREN CHEM NEW MATERIAL TECH CO LTD
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