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A kind of preparation method of hyperbranched polyamide ester rare earth complex

A technology of rare earth complexes and polyesteramides, which is applied in the field of preparation of hyperbranched polyamide ester rare earth complexes, and can solve problems such as application research is still in its initial state

Inactive Publication Date: 2011-12-28
FUJIAN NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the current research on hyperbranched polyesteramides mainly focuses on the synthesis method, performance and structural characterization, and the application research is still in its infancy, especially the research on hyperbranched polyesteramides and metal coordination functionalization. no report

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] The raw materials are maleic anhydride, diethanolamine, lanthanum oxide and acetic acid.

[0025] (1) Synthesis of hydroxyl-terminated hyperbranched polyamide ester

[0026]Under the protection of nitrogen, put 21.028g of 0.2mol diethanolamine and 19.612g of 0.2mol maleic anhydride into a 250mL reactor equipped with a water separator, stir and mix, and heat to 60-65°C to make the Melt the butenedioic anhydride, continue to stir to further mix the two reactants evenly; then, evacuate to maintain the vacuum of the system at 0.080MPa, and heat the temperature of the reaction system to rise rapidly to 125°C, maintain a constant temperature and allow the reactants to undergo co-condensation reaction. Control the continuous stirring, and the by-product water vapor can be seen quickly. When the reaction system is very viscous after 8 hours of reaction, it is ventilated and ventilated, and the material is cooled to obtain a light yellow product of hydroxyl-terminated hyperbran...

Embodiment 2

[0035] The raw materials are maleic anhydride, diethanolamine, lanthanum carbonate and acetic acid.

[0036] (1) Synthesis of hydroxyl-terminated hyperbranched polyamide ester

[0037] The synthesis steps are the same as in Example 1 (1), except that the vacuum degree of the system is maintained at 0.085 MPa during vacuuming, the constant temperature is 135° C., and the yield is 91.5%.

[0038] (GPC method, water as solvent, polyvinyl alcohol as standard)

[0039] FT-IR (ATR method, cm -1 ): 3406, 1728, 1680, 1637, 1265, 1168, 1048.

[0040] 13 C NMR (D 2 O, δppm): 178.8, 178.6, 175.4, 175.3, 175.1, 68.7, 64.3, 62.5, 54.7-49.0, 31.8-27.6.

[0041] (2) Synthesis of hyperbranched polyamide ester lanthanum complexes

[0042] Fully dissolve 0.1 mol of the hydroxyl-terminated hyperbranched polyamide ester obtained in (1) in 50 mL of acetic acid, add 0.001 mol of lanthanum carbonate, and perform a reflux reaction at a temperature of 180° C. After 2 hours, stop the reflux re...

Embodiment 3

[0046] The raw materials are succinic anhydride, diethanolamine, samarium oxide and acetic acid.

[0047] (1) Synthesis of carboxyl-terminated hyperbranched polyamide ester

[0048] Put 10.514g of 0.1mol diethanolamine and 10.008g of 0.1mol succinic anhydride into a 250mL reactor equipped with a water separator, stir and mix, heat to 120-125°C to melt succinic anhydride, and continue stirring to make The two reactants were further mixed evenly; then, the vacuum was maintained at 0.070MPa, and the temperature of the reaction system was rapidly raised to 230°C by heating at the same time, and the reactants were allowed to undergo co-condensation reaction while maintaining a constant temperature. Continuous stirring is controlled, and the by-product water vapor can be seen rapidly. After reacting for 6 hours, start to measure the acid value of the polymer product; when the acid value is less than 25mg KOH g -1 Ventilate and ventilate from time to time to maintain the normal pre...

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Abstract

The invention relates to a method for preparing a hyperbranched polyamide ester rare earth complex, which is characterized in that the hyperbranched polyamide ester rare earth complex is a chelate of rare earth ions and hyperbranched polyamide ester, and the rare earth ion and hyperbranched polyamide ester The molar ratio is 1:1-100. Preparation method: dissolve hyperbranched polyamide ester resin in organic carboxylic acid, add rare earth oxide or rare earth carbonate, reflux reaction at 80-280°C for 1 minute-24 hours, and maintain the vacuum degree of the system at 0.001-0.098MPa , the organic carboxylic acid and by-product water are distilled off, and the product is dried to obtain a hyperbranched polyamide ester rare earth complex. The hyperbranched polyamide ester rare earth complex prepared by the present invention integrates the excellent optical, electrical, and magnetic properties of rare earths with the unique multi-molecular cavity, high chemical reactivity, and low viscosity properties of hyperbranched polymers. Coordination cross-linking agents, luminescent materials, and electromagnetic materials have broad application prospects.

Description

technical field [0001] The invention belongs to the field of polymer materials, and relates to a preparation method of a hyperbranched polymer rare earth complex, in particular a hyperbranched polyamide ester rare earth complex. Background technique [0002] Rare-earth complexes of organic polymers combine the properties of easy molding and processing of organic substances with good optical, thermal, and electrical properties of inorganic substances, and have unique functions and application effects in the fields of optical, electrical, magnetic, and catalytic materials. In recent years, related studies, especially highly branched polymer rare earth complexes, have stimulated great research interest. [0003] Highly branched polymers (Highly branched polymers) are considered to be the fourth type of emerging polymer materials after linear, branched, and cross-linked polymers. According to the incompleteness of the structure, it can be divided into two categories: hyperbranc...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G69/48C08G69/44
CPCC08G83/005
Inventor 陈庆华陈荣国房小明刘欣萍肖荔人黄宝铨许兢钱庆荣
Owner FUJIAN NORMAL UNIV