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Preparation method of hydroxyl-terminated hyperbranched polyurethane

A technology of hydroxyl-terminated hyperbranching and polyurethane, which is applied in the field of hyperbranched polymers, can solve the problems that it is difficult to obtain high-purity hyperbranched polymers, the purity of hyperbranched molecules is difficult to guarantee, and the number of branch growth needs to be increased. Improved stability and good controllability

Inactive Publication Date: 2013-02-27
ANHUI UNIVERSITY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the number of molecular branching and growth of each generation of molecules needs to be improved by using oligomer diol as the starting molecule
Industrial oligomer diol is a polymer with a certain molecular weight distribution range, it is difficult to have pure oligomer diol, so the purity of hyperbranched molecules made from oligomer diol as a starter is difficult to guarantee
Not only that, the process adopted in this patent is a method of directly mixing and heating diisocyanate and oligomer diol. From the principle of polycondensation reaction, it can be known that this method has many side reactions, and it is difficult to obtain hyperbranched polymers with high purity.

Method used

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  • Preparation method of hydroxyl-terminated hyperbranched polyurethane
  • Preparation method of hydroxyl-terminated hyperbranched polyurethane
  • Preparation method of hydroxyl-terminated hyperbranched polyurethane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] The target molecular structure formula of the first-generation hydroxyl-terminated hyperbranched polyurethane is as follows:

[0023]

[0024] The synthesis operation steps are as follows:

[0025] Take 4 grams of trimethylolpropane (TMP) and dissolve it in 20 grams of N,N-dimethylformamide (DMF) to obtain a hydroxyl-terminated small molecule polyol solution. Get 19.88 grams of isophorone diisocyanate (IPDI) and heat it to 85°C, add it to the hydroxyl-terminated small molecule polyol solution and stir for 6 hours to obtain the first generation of hyperbranched prepolymer a 1 . 43.88 grams of the first generation hyperbranched prepolymer a 1 and 23.5 grams of diethanolamine were cooled to 10°C, and the heat preservation and blending reaction was carried out for 6 hours. The obtained product was separated and purified with acetone aqueous solution with a mass fraction of 10%, and then vacuum-dried to obtain the first-generation hydroxyl-terminated hyperbranched polyu...

Embodiment 2

[0028] The target molecular structure formula of the first-generation hydroxyl-terminated hyperbranched polyurethane is as follows:

[0029]

[0030] The synthesis operation steps are as follows:

[0031] Dissolve 4 g of trimethylolpropane (TMP) in 20 g of N,N-dimethylacetamide (DMAC) to obtain a hydroxyl-terminated small molecule polyol solution. Heat 20.46 grams of 4,4'-dicyclohexylmethane diisocyanate (HMDI) to 90°C, add it into the hydroxyl-terminated small molecule polyol solution and stir for 4 hours to obtain the first-generation hyperbranched prepolymer a 1 . 44.46 grams of the first generation hyperbranched prepolymer a 1 and 18.5 grams of diethanolamine were cooled to 15°C, and the heat preservation, blending and stirring reaction was carried out for 6 hours, and the obtained product was separated and purified with water and then vacuum-dried to obtain the first-generation hydroxyl-terminated hyperbranched polyurethane A of a colorless transparent solid 1 .

Embodiment 3

[0033] The target molecular structure formula of the first-generation hydroxyl-terminated hyperbranched polyurethane is as follows:

[0034]

[0035] The synthesis operation steps are as follows:

[0036] Take 3 grams of 1,4-butanediol (BDO) and dissolve it in 20 grams of N,N-dimethylformamide (DMF) to obtain a hydroxyl-terminated small molecule polyol solution. Heat 11.78 grams of isophorone diisocyanate (IPDI) to 80°C, add the hydroxyl-terminated small molecule polyol solution and stir for 6 hours to obtain the first-generation hyperbranched prepolymer a 1 . 34.78 grams of the first generation hyperbranched prepolymer a 1 and 17 grams of diethanolamine were cooled to 10°C, and the heat preservation and blending reaction was carried out for 6 hours. The obtained product was separated and purified with a 5% ether aqueous solution and then vacuum-dried to obtain the first-generation hydroxyl-terminated hyperbranched polyurethane A of a colorless transparent solid. 1 .

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Abstract

The invention relates to a preparation method of hydroxyl-terminated hyperbranched polyurethane. The operation steps include that 1 hydroxyl-terminated micromolecule polyhydric alcohol is dissolved in a non-proton organic solvent to obtain a hydroxyl-terminated micromolecule polyhydric alcohol solution; 2 the temperature of diisocyanate is raised to 70-90 DEG C, the hydroxyl-terminated micromolecule polyhydric alcohol solution is added, catalyst is added, and a reaction is conducted to obtain first generation hyperbranched prepolymer a1; and 3 the temperature of the first generation hyperbranched prepolymer a1 and di-alkanolamine is reduced to 0-15 DEG C, the temperature is kept, a reaction is conducted after blending, and products are separated and purified through precipitator and vacuum-dried to obtain first generation hydroxyl-terminated hyperbranched polyurethane A1. A synthesizing process is good in controllability, and the synthesized hyperbranched polyurethane is high in purity and neat in structure, contains large amount of terminated hydroxyl and is suitable for being used as a biological medicine carrier, a cross-linking agent, a viscosity modifier, a thermosetting material curing agent, a phase solubilizer, a rheological agent, thixotrope, a nucleating agent and the like.

Description

technical field [0001] The invention belongs to the technical field of hyperbranched polymers, and in particular relates to a preparation method of hyperbranched polyurethane. Background technique [0002] Hyperbranched polymers have aroused the interest of scientists from all over the world because of their unique molecular structure, easy solubility, large number of terminal groups, difficult molecular chain entanglement, and low solution viscosity. Polyurethane has been widely used in many fields in modern society, including foam plastics, rubber, coatings, adhesives, etc. Compared with traditional polyurethanes, hyperbranched polyurethanes not only have better viscosity, solubility and film-forming properties, but also have special properties. Functional application. Such as solid-solid phase change energy storage materials, polymer electrolyte materials, shape memory materials, viscosity modifiers, curing agents for thermosetting materials, phase solubilizers, rheologi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G18/32C08G18/10C08G18/24
Inventor 许戈文王继印熊潜生陶灿满德龙
Owner ANHUI UNIVERSITY
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