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Preparation method of hyperbranched polyesteramide resin by using microwave synthesis

A technology for polyamide ester and microwave synthesis, which is applied in the field of preparing hyperbranched polyamide ester and can solve the problems of slow reaction rate, uneven heating and high energy consumption

Inactive Publication Date: 2012-03-28
FUJIAN NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method of the invention has the characteristics of no need for organic solvents, uniform heating, and high reaction rate. It is not only greener than the traditional solution method, but also can overcome the shortcomings of the conventional hot melting method, such as high energy consumption, uneven heating, and slow reaction rate.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Hyperbranched polyamide ester resin was prepared with maleic anhydride and diethanolamine as reactants.

[0020] Take 0.100 mol 9.806 g of maleic anhydride and 0.105 mol 11.040 g of diethanolamine in a three-necked flask equipped with a decompression-distillation device, mechanically stir and mix evenly to form a mixed reactant; pass nitrogen protection into the system; The three-neck flask was placed in a microwave heating environment, and was heated by a microwave with a power of 100 W for 65 minutes to melt the mixed reactants and undergo a co-condensation reaction. Cooling, the yellow glass-like hyperbranched polyamide ester resin that obtains productive rate is 96.9%.

[0021] The characterization data of hyperbranched polyamide ester resin are as follows:

[0022] = 2846 g / mol (GPC method, water as solvent, polyvinyl alcohol as standard)

[0023] FT-IR (KBr,cm -1 ): 3415, 1732, 1680, 1648, 1460, 1213, 1165, 1054.

[0024] 1 H NMR (D 2 O, δ ppm): 4.4–4.1, 3...

Embodiment 2

[0028] Hyperbranched polyamide ester resin was prepared with maleic anhydride and diethanolamine as reactants.

[0029] Take 0.100 mol 9.806 g of maleic anhydride and 0.101 mol 10.619 g of diethanolamine in a three-necked flask equipped with a decompression-distillation device, mechanically stir and mix evenly to form a mixed reactant; pass nitrogen protection into the system; The three-neck bottle is placed in a microwave heating environment, and the microwave with a power of 450 W is used to heat for 1 min to melt the mixed reactants and undergo co-condensation reaction, and at the same time carry out a decompression (vacuum degree of 0.080 MPa) distillation to distill the by-product water; cool , the yield is 94.8% yellow glass-like hyperbranched polyamide ester resin.

[0030] The characterization data of hyperbranched polyamide ester resin are as follows:

[0031] = 8846 g / mol (GPC method, water as solvent, polyvinyl alcohol as standard)

[0032] FT-IR (KBr,cm -1 ): ...

Embodiment 3

[0037] Hyperbranched polyamide ester resin was prepared by using succinic anhydride and diisopropanolamine as reactants.

[0038] Take 0.100 mol 10.008 g of succinic anhydride and 0.101 mol 13.452 g of diisopropanolamine in a three-necked flask equipped with a decompression-distillation device, mechanically stir and mix evenly to form a mixed reactant; place the three-necked flask in microwave heating In an environment with a power of 300 W, the microwave was used to heat for 24 minutes to melt the mixed reactants and undergo co-condensation reaction. At the same time, the by-product water was distilled under reduced pressure (vacuum degree of 0.085 MPa); cooling yielded 95.5 % light yellow glassy hyperbranched polyamide ester resin.

[0039] The characterization data of hyperbranched polyamide ester resin are as follows:

[0040] = 3761 g / mol (GPC method, water is used as solvent, and polyvinyl alcohol is used as standard).

[0041] FTIR (KBr,cm -1 ): 3440, 1730, 1650, 1...

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Abstract

The present invention relates to a preparation method of hyperbranched polyesteramide resin by using microwave synthesis, which is characterized by uniformly mixing the reagents of mono-anhydride and polyhydramine, or the reagents of carboxyl substituted mono-anhydride and mono-hydramine, or the reagents of polyanhydride and mono-hydramine in mole ratio, performing the copolycondensation under the condition of microwave radiation and decompression to remove the by-product of water continuously through distillation, stopping the microwave radiation before the gelatinization of the system and cooling to obtain the hyperbranched polyesteramide resin. The hyperbranched polyesteramide resin is prepared with the vacuum degree of 0.0 to 0.096 MPa, the microwave radiation power of 5 to 500 W and the reaction time of 0.5 to 90 min. The method of the invention has the characteristics of organic solvent free, uniform heating and rapid reaction speed, and is more environment friendly compared with the traditional solution method, and overcomes the disadvantages of high power consumption, uneven heating and slow reaction speed in the traditional thermal fusion method. The invention can saves time and production cost, and enhances the production efficiency.

Description

technical field [0001] The invention relates to a method for preparing hyperbranched polyamide ester, in particular to a method for preparing hyperbranched polyamide ester resin by microwave synthesis. Background technique [0002] At present, the most mature process for preparing hyperbranched polyamide ester with commercial raw material monomers mainly includes traditional solution method and conventional hot melt polycondensation method. [0003] The preparation method of hyperbranched polyesteramide disclosed in Chinese patent "02145101.X" (hyperbranched polyesteramide and its preparation method) is a typical representative of solution synthesis of hyperbranched polyesteramide. Its main features are: in an aprotic solvent, let the raw material monomers react at low temperature to form AB x ( x ≥2) type intermediate monomer, and then let AB under the condition of high temperature and reduced pressure x Polycondensation of intermediate monomers into polymers. This meth...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G69/44
Inventor 陈庆华陈荣国房小明肖荔人刘欣萍许兢钱庆荣
Owner FUJIAN NORMAL UNIV