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Preparation method of aliphatic polyester amide with urea bond

A polyester amide and aliphatic diamine technology, applied in the field of polyester amide, can solve the problems of monomer volatilization loss, low polyester amide bond content, difficult control of feed ratio, etc., and achieve mild conditions, cheap and easy raw materials The effect

Inactive Publication Date: 2015-10-28
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
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 amides by 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 with urea bond
  • Preparation method of aliphatic polyester amide with urea bond
  • Preparation method of aliphatic polyester amide with urea bond

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] 1) Preparation of amino-terminated hydroxyurea monomer (HAU): Dissolve 39.6 parts of octanediamine in 50ml of N,N-dimethylformamide (DMF), raise the temperature to 160°C; weigh 60.4 parts by weight A portion of 2-oxazolidinone was dissolved in 50ml of DMF, and added dropwise to the above-mentioned octyldiamine solution; after the dropwise addition, the reaction was continued for 5 hours, cooled to room temperature, a white solid was precipitated, filtered under reduced pressure, and a white solid was obtained , the measured hydroxyl value is 487.05mgKOH / g, and its molecular weight is 230.36, which is consistent with the theoretical molecular weight of 231.

[0043] 2) Preparation of polyester amide prepolymer with urea bonds: 69.3 parts of HAU monomer prepared in step 1), 145.6 parts of sebacic acid, 27.1 parts of 1,4-butanediol were weighed in parts by weight, 0.48 parts of phosphorous acid, 0.24 parts of stannous chloride, under the protection of nitrogen, heat up to ...

Embodiment 2

[0046] 1) Preparation of polyester amide prepolymer with urea bonds: Weigh 11.6 parts of HAU monomer prepared in step 1) in Example 1, 141.6 parts of sebacic acid, 1,4-butanediol in parts by weight 58.6 parts, 0.42 parts of phosphorous acid, 0.21 parts of stannous chloride, under the protection of nitrogen, heat up to 160 ° C, slowly heat up to 200 ° C within 2 hours, and then switch to a decompression device, first use a water pump to gradually decompress the reaction After 2.5 hours, the oil pump was used to reduce the pressure to 3mmHg and react for 3 hours to obtain a PrePEAU prepolymer with an intrinsic viscosity of 0.26dL / g, an acid value of 39.19mgKOH / g, and a hydroxyl value of 32.01mgKOH / g.

[0047] 3) Weigh 51.5 parts of PrePEAU prepolymer prepared in step 2), 3.9 parts of 1,4-phenyl-bis(2-oxazoline), 4.9 parts of adipyl biscaprolactam, catalyst chlorinated chlorinated 0.12 parts of tin and 0.003 parts of p-toluenesulfonic acid were reacted at 200°C under normal press...

Embodiment 3

[0049] 1) Preparation of polyester amide prepolymer with urea bonds: Weigh 23.1 parts of HAU monomer prepared in step 1) in Example 1, 131.5 parts of sebacic acid, 1,4-butanediol in parts by weight 49.5 parts, 0.41 parts of phosphorous acid, 0.20 parts of stannous chloride, under the protection of nitrogen, raise the temperature to 160°C, slowly raise the temperature to 200°C within 2 hours, then switch to a decompression device, and first use a water pump to gradually depressurize the reaction After 2.5 hours, the oil pump was used to reduce the pressure to 3 mmHg and react for 3 hours to obtain a PrePEAU prepolymer with an intrinsic viscosity of 0.29 dL / g, an acid value of 31.13 mgKOH / g, and a hydroxyl value of 45.76 mgKOH / g.

[0050] 2) Weigh 50.9 parts of PrePEAU prepolymer prepared in step 1), 3.1 parts of 1,4-phenyl-bis(2-oxazoline), 6.9 parts of adipyl biscaprolactam, and chlorinate the catalyst 0.12 parts of stannous and 0.003 parts of p-toluenesulfonic acid were react...

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Abstract

The invention relates to a preparation method of aliphatic polyester amide with urea bond, and belongs to the technical field of polyester amide. According to the invention, urea monomer with terminal amino and terminal hydroxyl is subjected to melt polycondensation with aliphatic dicarboxylic acid and glycol. Amide content is changed through changing the ratio of the urea monomer with terminal amino and terminal hydroxyl to the dicarboxylic acid and glycol. With the method, a series of polyester amide prepolymers with the urea bond and with both Polyester amide structures are prepared. Chain-extending is carried out with diacyl bislactam and bisoxazoline chain extender, such that biodegradable polyester amide comprising urea bond is prepared. Characteristic viscosity of the product at 30 DEG C is 0.38-0.72dL / g.

Description

technical field [0001] The invention belongs to the technical field of polyester amides, and relates to a method for preparing an aliphatic polyester amide with a urea bond, in particular to an aliphatic dibasic acid, a diol, and an amino-terminated hydroxyl monomer with a urea bond. Raw Materials Synthesis of aliphatic polyester amides with urea linkages. technical background [0002] Polyurea has good thermal stability and has excellent properties in terms of tensile strength, modulus, elongation, flexibility, wear resistance, aging resistance, and corrosion resistance. Polyurea is mainly synthesized by two methods: 1) polymerization of isocyanate and diamine; 2) reaction polymerization of diisocyanate and water. Yeh et al. used polytetrahydrofuran as the soft segment, and reacted MDI with ethylenediamine to obtain the polyurea hard segment, forming a polyurea elastomer with good toughness. Unal et al. used diisocyanate and trifunctional amine to prepare polyurea. As the...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G69/44
Inventor 赵京波刘毅兰杨万泰
Owner BEIJING UNIV OF CHEM TECH
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