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Method for preparing aqueous polyurethane/nano titanium dioxide hybrid material

A nano-titanium dioxide and water-based polyurethane technology is applied in the preparation field of polyurethane emulsion modification, which can solve the problems of unresearched emulsion stability, difficulty in ensuring practical application of materials, and complicated steps, and achieves sufficient raw material sources, good mechanical properties, and preparation. simple craftsmanship

Inactive Publication Date: 2010-12-22
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the steps of this method are cumbersome, and the stability of the emulsion has not been studied, so it is difficult to ensure the practical application of the material

Method used

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  • Method for preparing aqueous polyurethane/nano titanium dioxide hybrid material

Examples

Experimental program
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Effect test

Embodiment 1

[0013] In a container equipped with a stirring device, add dehydrated ethanol, whose consumption accounts for 56% of the total substance by volume, and a certain amount of n-butyl titanate (TBT), hydrochloric acid, distilled water and dehydrated ethanol (volume ratio followed by (10:2:1:10) mixed solution was added into the container, and stirred at room temperature for 1 h to obtain a homogeneous clear solution, that is, to obtain TBT sol.

[0014] Add 30g of polyoxypropylene glycol (referred to as polyether polyol N-220) and 5g of dimethylol propionic acid (DMPA) in a 500mL four-necked bottle equipped with a stirrer, reflux condenser, thermometer and feeding device Add 3g of N-methylpyrrolidone (NMP) as a solvent, heat the system to 70°C, add 20g of toluene diisocyanate (TDI), add dropwise catalyst 1g of dibutyltin dilaurate (T-12), and react for 6 hours, Raise the temperature of the system to 90°C (if the viscosity of the system is too high, a certain amount of acetone can ...

Embodiment 2

[0016] In a container equipped with a stirring device, add dehydrated ethanol, whose consumption accounts for 56% of the total substance by volume, and a certain amount of n-butyl titanate (TBT), hydrochloric acid, distilled water and dehydrated ethanol (volume ratio followed by (10:2:1:10) mixed solution was added into the container, and stirred at room temperature for 1 h to obtain a homogeneous clear solution, that is, to obtain TBT sol.

[0017]Add 10g of N-220 and 5g of DMPA into a 500mL four-neck flask equipped with a stirrer, reflux condenser, thermometer and feeding device, add 1g of NMP solvent, raise the temperature of the system to 50°C, add 20g of TDI, and dropwise add 0.2g Catalyst T-12, after 2 hours of reaction, raise the temperature of the system to 70°C (if the system viscosity is too high, add a certain amount of acetone), continue the reaction for 6 hours, then cool down to 40°C, add 2g of triethylamine, and react for 20 minutes , 50g of water was added drop...

Embodiment 3

[0019] In a container equipped with a stirring device, add dehydrated ethanol, whose consumption accounts for 56% of the total substance by volume, and a certain amount of n-butyl titanate (TBT), hydrochloric acid, distilled water and dehydrated ethanol (volume ratio followed by (10:2:1:10) mixed solution was added into the container, and stirred at room temperature for 1 h to obtain a homogeneous clear solution, that is, to obtain TBT sol.

[0020] Add 10g of difunctional polyether polyol GE-210 (industrial product, hydroxyl value 56mg KOH / g) and 1.8g of DMPA into a 500mL four-necked bottle equipped with a stirrer, reflux condenser, thermometer and feeding device , add 1g of NMP solvent, raise the temperature of the system to 60°C, add 10g of isophorone diisocyanate (IPDI), add dropwise 0.1g of catalyst T-12, raise the temperature of the system to 80-85°C, (if the system viscosity is too high , a certain amount of acetone can be added), continue to react for 4 hours, cool dow...

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Abstract

The invention discloses a method for preparing an aqueous polyurethane / nano titanium dioxide hybrid material and relates to a preparation technology of a modified polyurethane emulsion. The method comprises the following steps of: (1) preparing TBT (Tributyltin) sol; (2) adding polyalcohol and isocyanate which are used as raw material monomers, adding a hydrophilic chain extender, heating up the system to 30-80 DEG C by using N-polyvinyl pyrrolidone as a solvent and then adding a catalyst; (3) after the mixture reacts of 1-6 hours, heating up the system to 60-100 DEG C; continuing to make the mixture react for 1-6 hours, and then cooling to 20-60 DEG C; adding triethylamine used as a salt forming agent, and making the mixture react for 10-60 minutes; dispersing with water by using ethanediamine as a chain extender to obtain an aqueous polyurethane emulsion; maintaining the temperature to 20-50 DEG C, adding a small quantity of gamma-epoxypropyl trimethoxy silane and stirring for 10-90 minutes; adding the TBT sol to the system and dropwise adding a small quantity of hydrochloric acid; and persistently stirring for 12-48 hours to obtain the aqueous polyurethane / nano titanium dioxide hybrid material. The properties such as the weather resistance, the mechanical property, the coating transparency, and the like of the hybrid material are greatly improved.

Description

Background technique [0001] The invention relates to a preparation technology of polyurethane emulsion modification, in particular to a preparation method of water-based polyurethane / nano-titanium dioxide hybrid material. Background technique [0002] Polyurethane is widely used in coatings, finishing agents, elastomers, Printing and dyeing auxiliaries, adhesives and other fields. However, there are still some problems in its actual use. For example, with the increasingly stringent environmental protection regulations and the gradual enhancement of people's environmental awareness, the environmentally friendly water-based polyurethane with water as the dispersion medium has become the direction of polyurethane resin development and research in recent years. , but its high temperature resistance, initial viscosity, chemical resistance and water resistance are poor, which limits its popularization and application. In recent years, more and more studies on polyurethane have f...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G18/12C08G18/66C08K9/06C08K3/22C01G23/053
Inventor 邱凤仙吴冬梅许和平杨冬亚
Owner JIANGSU UNIV
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