Preparation method of water-based polyurethane/nano-silicon dioxide composite emulsion

A nano-silica, water-based polyurethane technology, applied in the field of polymer chemistry, can solve the problems of water resistance, solvent resistance, chemical resistance, wear resistance, hardness and other unsatisfactory overall performance, to solve pollution and damage , Eliminate pollution and improve performance

Inactive Publication Date: 2010-09-29
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The object of the present invention is to provide a kind of preparation method of aqueous polyurethane/nano-silica composite emulsion, to overcome the unsatis

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Embodiment 1: 1) Preparation of nano-silica sol:

[0023] Take 15 parts by mass of ethyl tetrasilicate, 15 parts of absolute ethanol, and 1 part of octadecyltrimethylammonium chloride, mix and stir evenly, and when heated to 45°C, drop into the reaction system Add a mixed solution of 5 parts by mass of double-distilled water and 15 parts of absolute ethanol, adjust the pH to 9 with hydrochloric acid solution, and keep stirring at 45°C for 1.5 hours to obtain nano-silica sol;

[0024] 2) Preparation of water-based polyurethane emulsion:

[0025] First, 30.77 parts by mass of polyoxypropylene diol with a relative molecular mass of 1000 was added to the dry reactor, and the reactor was heated to 80°C, and then 43.58 parts of isophorone diisocyanate and 0.45 Part of the catalyst dibutyltin dilaurate was added to the reactor, and polymerized at 80°C for 3.5 hours to form a polyurethane prepolymer;

[0026] Then, 6.27 parts of hydrophilic chain extender sodium ethylenediami...

Embodiment 2

[0030] Embodiment 2: 1) Preparation of nano silica sol:

[0031] According to the number of parts by mass, take 25 parts of ethyl tetrasilicate, 17 parts of absolute ethanol, and 2 parts of octadecyltrimethylammonium chloride, mix and stir evenly, and when heated to 35 ° C, drop into the reaction system Add a mixed solution of 6 parts by mass of double-distilled water and 17 parts of absolute ethanol, adjust the pH to 7.5 with hydrochloric acid solution, and keep stirring at 35°C for 2.5 hours to obtain nano-silica sol;

[0032] 2) Preparation of water-based polyurethane emulsion:

[0033] First, 35.15 parts by mass of polytetrahydrofuran diol with a relative molecular mass of 1000 were added to the dry reactor, and the reactor was heated to 90°C, and then 41.13 parts of toluene isophorone diisocyanate and 0.4 Part of the catalyst dibutyltin dilaurate was added to the reactor, and polymerized at 90°C for 1 hour to form a polyurethane prepolymer;

[0034] Then, 7.5 parts of h...

Embodiment 3

[0038] Embodiment 3: 1) Preparation of nano silica sol:

[0039] Take 20 parts by mass of tetraethyl orthosilicate, mix and stir evenly with 16 parts of absolute ethanol and 1.5 parts of octadecyltrimethylammonium chloride, heat it to 40°C, and drop it into the reaction system Add a mixed solution of 5.5 parts by mass of double-distilled water and 17 parts of absolute ethanol, adjust the pH to 8.5 with hydrochloric acid solution, and keep stirring at 40°C for 2 hours to obtain nano-silica sol;

[0040] 2) Preparation of water-based polyurethane emulsion:

[0041] First, 35.64 parts by mass of polycaprolactone diol with a relative molecular mass of 1000 are added to the dry reactor, and the reactor is heated to 85°C, and then 42.6 parts of hexamethylene diisocyanate and 0.43 parts of catalyst dibutyltin dilaurate were added to the reactor, and polymerized at 85°C for 2.5 hours to form a polyurethane prepolymer;

[0042] Then, 6.13 parts of hydrophilic chain extender dimethylo...

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PUM

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Abstract

The invention relates to a preparation method of a water-based polyurethane/nano-silicon dioxide composite emulsion, which comprises the following steps: uniformly mixing and stirring ethyl orthosilicate, absolute ethyl alcohol and octadecyl trimethyl ammonium chloride for reacting to obtain nano-silicon dioxide sol; heating polyglycol, and then, adding diisocyanate and dibutyltin dilaurate for reacting to form polyurethane prepolymer; adding a hydrophilic chain extender and a cross-linking agent into the polyurethane prepolymer for carrying out chain extending reaction, adding organic base for regulating the pH value to be 7.0-8.0, and then, adding deionized water to obtain 30% of water-based polyurethane emulsion; and mixing the nano-silicon dioxide sol and the water-based polyurethane emulsion in a water bath, and carrying out ultrasonic treatment to obtain the water-based polyurethane/nano-silicon dioxide composite emulsion. Harmful solvents and emulsifying agents do not need to be added in the preparation process of the invention, thereby solving the problems of polluting environment and injuring operators.

Description

technical field [0001] The invention belongs to the field of macromolecular chemistry, in particular to a preparation method of water-based polyurethane / nano silicon dioxide composite emulsion. Background technique [0002] In recent years, as the hazards of volatile organic compounds (VOC) have been increasingly recognized by the world, more and more countries and regions have formulated corresponding policies and standards to limit the emission of VOC, making water-based coatings developed rapidly. Waterborne polyurethane coatings are non-flammable, non-toxic, low pollution, easy to store, easy to use, have the advantages of low temperature resistance and good flexibility, and have become an important research direction in the field of polyurethane research. In recent years, water-based polyurethane resins have been successfully used in leather finishing, paper coating, chemical building materials, automobile coating and other fields, and have good market prospects. There...

Claims

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Application Information

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IPC IPC(8): C08L75/04C08L75/08C08L75/06C08K3/36C08J3/03C09D175/04C09D175/08C09D175/06
Inventor 赖小娟沈一丁王磊赵静杨燕
Owner SHAANXI UNIV OF SCI & TECH
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