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Preparation method of aliphatic polyester amide containing short polyamide segment

A technology of polyamide segment and polyester amide, which is applied in the field of biodegradable polyester amide with high molecular weight and short polyamide segment, which can solve the problem of monomer volatilization loss, affecting the ratio of raw materials, low content of polyester amide amide bonds, etc. problem, to achieve the effect of simple method and mild condition

Inactive Publication Date: 2011-06-01
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the polycondensation of dibasic acid and diamide diol is not easy to control the feeding ratio, and it is easy to cause volatilization loss of monomers under high temperature and high vacuum, which affects the ratio of raw materials, so it is difficult to obtain high molecular weight polymers
[0006] Chinese patents CN 1,310,194A (2001), CN 1,124,304C (2003), CN 101,020,746A (2007) reported the preparation of high molecular weight polyester amide with diisocyanate or bisoxazoline extended chain aliphatic polyester prepolymer, but The polyester amides prepared by this method have a low amide bond content, and the thermal and mechanical properties are not significantly improved compared with the corresponding aliphatic polyesters

Method used

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  • Preparation method of aliphatic polyester amide containing short polyamide segment
  • Preparation method of aliphatic polyester amide containing short polyamide segment
  • Preparation method of aliphatic polyester amide containing short polyamide segment

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] 1) Preparation of polyamide oligomer (PA): Weigh 60.0 parts of caprolactam, 6.5 parts of ethanolamine, 8.0 parts of distilled water and 0.13 parts of phosphorous acid in parts by weight, and reflux at 150°C for 7-9 days under nitrogen protection. hour, then gradually raise the temperature to 200°C for polycondensation reaction, collect 70-80% of the generated water, switch to a decompression device, and use a water pump to gradually depressurize and react for 2-3 hours to obtain an intrinsic viscosity of 0.12dL / g and an acid value It is a PA oligomer with 3.12 mgKOH / g and a hydroxyl value of 175.31 mgKOH / g.

[0052] 2) Preparation of polyester amide prepolymer (PEA): Weigh 20.0 parts of PA prepolymer prepared in step 1) and 4.7 parts of adipic acid in parts by weight, and heat up to 200°C under the protection of nitrogen for normal pressure reaction 3 hours, then use a decompression device, first use a water pump to depressurize gradually for 3 hours, then use an oil pu...

Embodiment 2

[0055] Take by weight 30.0 parts of the PEA prepolymer prepared in step 2) of Example 1, 1.1 parts of 1,4-phenyl-bis(2-oxazoline), 0.18 parts of carbonyl biscaprolactam, in nitrogen atmosphere Under protection, it was reacted at 200° C. under normal pressure for 1.5 hours, and then reacted in a 2 mmHg decompression system for 0.5 hours. The intrinsic viscosity of the obtained polymer was 0.67 dL / g.

Embodiment 3

[0057] 1) Preparation of polyester amide prepolymer (PEA): take by weight 20.0 parts of PA prepolymer prepared in step 1) in Example 1, 4.65 parts of adipic acid, and heat up to 200 under the protection of nitrogen. ℃ normal pressure reaction for 3 hours, and then switch to a decompression device, first use a water pump to gradually decompress the reaction for 3 hours, then use an oil pump to depressurize, and react in a 2mmHg decompression system for 2 hours to obtain an acidic acid with an intrinsic viscosity of 0.22dL / g. A PEA prepolymer having a value of 42.25 mgKOH / g and a hydroxyl value of 23.43 mgKOH / g.

[0058] 2) Take by weight 60.0 parts of the PEA prepolymer prepared in step 1 of Example 3, 1.9 parts of 1,4-phenyl-bis(2-oxazoline), and 3.2 parts of carbonyl biscaprolactam. The reaction was carried out at 200°C under normal pressure for 1.5 hours under the protection of 200°C, and then in a 2 mmHg decompression system for 0.5 hours. The intrinsic viscosity of the obt...

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Abstract

The invention discloses a preparation method of aliphatic polyester amide containing a short polyamide segment, which comprises the following steps: polymerizing cyclic lactam or amino acid with alkamine to prepare a polyamide oligomer; carrying out melt polycondensation on the polyamide oligomer, aliphatic dibasic acids and diatomic alcohols to prepare a polyester amide prepolymer with a carboxyl-terminated and hydroxyl-terminated structure; and carrying out chain extension on the polyester amide prepolymer by using diacyl dilactam or carbonyl dilactam and dioxazoline chain extender to prepare the biodegradable polyester amide containing a short polyamide segment, of which the inherent viscosity is 0.37-0.74 dL / g. The invention has the characteristics of simple method, mild conditions, high efficiency and the like.

Description

technical field [0001] The present invention relates to a preparation method of aliphatic polyester amide, in particular to a preparation method of polyester amide using aliphatic dibasic acid, dibasic alcohol and polyamide oligomers as raw materials, especially two steps of polycondensation and chain extension A method for preparing a biodegradable polyester amide with a high molecular weight and a short polyamide segment with an intrinsic viscosity of 0.37-0.74 dL / g. Background technique [0002] Polyesteramide (PEA) is a new type of biodegradable polymer material. Compared with aliphatic polyester, due to the introduction of amide groups and the formation of hydrogen bonds between amide groups, the polymer has better mechanical properties and strength, while the presence of ester bonds endows the material with good biodegradability, making it have a wide range of application prospects. [0003] U.S. Patent US 0,065,314 (2005) reported that adipic acid, 1,4-butanediol, ca...

Claims

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Application Information

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IPC IPC(8): C08G69/44
Inventor 赵京波刘诗乐杨万泰
Owner BEIJING UNIV OF CHEM TECH
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