Polyurethane based fluorescent whitening agent and preparation method thereof

A fluorescent whitening agent and polyurethane-based technology, applied in the direction of organic dyes, can solve the problems of low fluorescence quantum yield, poor light resistance, heat resistance, reduced whitening effect and use effect, etc., and achieve high fluorescence quantum yield , Easy film formation, excellent whitening effect

Inactive Publication Date: 2016-08-24
ANHUI UNIVERSITY OF ARCHITECTURE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When treating materials with small molecule fluorescent whitening agents, due to the disadvantages of low fluorescence quantum yield, poor light resistance and heat resistance, the whitening effect and use effect are reduced

Method used

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  • Polyurethane based fluorescent whitening agent and preparation method thereof
  • Polyurethane based fluorescent whitening agent and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] in N 2 Under protection, add 100 g, 0.1 mol of polycaprolactone diol into a four-necked flask equipped with a stirrer, a condenser, and a thermometer, heat to 110° C., and dehydrate for 2 hours under a vacuum of 0.1 MPa.

[0052] Cool down to 90°C, add 50g, 0.2mol of 4,4-diphenylmethane diisocyanate MDI, 20ml of dioxane and 0.02g of stannous octoate, and react at 90°C for 3 hours.

[0053] Then add 10 g, 0.011 mol of fluorescent whitening agent 85 (12224-16-7), and raise the temperature to 90°C for 6 hours.

[0054] Cool down to 70°C, add 10g, 0.075mol dimethylolpropionic acid,

[0055] Add 0.45g, 0.005mol 1,4-butanediol, react at 50°C for 1 hour, react for 2 hours, cool down to 30°C, add 100ml of acetone to dilute.

[0056] Add 9.9g, 0.09mol triethylamine and g1 Tween-20, stir at high speed for 30min.

[0057] Transfer to an emulsification tank, add 500ml of deionized water for high-speed emulsification for 30 minutes, and finally distill the emulsion under reduced ...

Embodiment 2

[0060] in N 2 Under protection, add 100 g, 0.1 mol of polytetrahydrofuran diol into a four-necked flask equipped with a stirrer, condenser, and thermometer, heat to 110° C., and dehydrate for 2 hours under a vacuum of 0.1 MPa.

[0061] Cool down to 90°C, add dropwise 44.5g, 0.2mol of isophorone diisocyanate, 20ml of N-methylpyrrolidone and 0.02g of dibutyltin dilaurate, and react at 90°C for 3 hours.

[0062] Then add 10.6g, 0.011mol fluorescent whitening agent 71 (16090-02-1), and raise the temperature to 90°C for 6h.

[0063] Cool down to 70°C, add 10g, 0.075mol dimethylol propionic acid, react for 2 hours,

[0064] Then add 0.53g, 0.005mol diethylene glycol, and react at 60°C for 1 hour,

[0065] Cool down to 30°C, add 100ml acetone to dilute.

[0066] Add 9.9g, 0.09mol triethylamine and 1g nonylphenol polyoxyethylene ether, and stir at high speed for 30min.

[0067] Transfer to an emulsification tank, add 500ml of deionized water for high-speed emulsification for 30 mi...

Embodiment 3

[0070] in N 2 Under protection, add 100 g, 0.1 mol polyoxypropylene diol to a flask equipped with a thermometer, a stirrer, a reflux condenser and a dropping funnel, heat to 110 ° C, and dehydrate for 1.5 h under a vacuum of 0.1 MPa.

[0071] Cool down to 90°C, add dropwise 34.8g, 0.2mol toluene diisocyanate, 20ml methyl ethyl ketone and 0.02g stannous octoate, and react at 90°C for 3 hours.

[0072] Then add 10 g, 0.011 mol of fluorescent whitening agent 85 (12224-16-7), and raise the temperature to 90°C for 6 hours.

[0073] Cool down to 60°C, add 9g, 0.075mol N-methyldiethanolamine, react for 2 hours,

[0074] Then add 0.32g, 0.005mol ethylene glycol, and react at 60°C for 1 hour.

[0075] Cool down to 30°C, add 100ml acetone to dilute.

[0076] Add 4.5g, 0.09mol acetic acid and 1g octylphenol polyoxyethylene ether, and stir at high speed for 30min.

[0077] Transfer to an emulsification tank, add 300ml of deionized water for high-speed emulsification for 30 minutes, an...

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Abstract

The invention discloses a polyurethane based fluorescent whitening agent and a preparation method thereof. The preparation method includes the steps that polymer polyalcohol is heated, vacuum dewatering is conducted for 1-2 hours, nitrogen gas is introduced for cooling, and diisocyanate, solvent and a catalyst are added for a reaction; then, an organic small molecular fluorescent whitening agent body is added, a reaction is conducted, and polyurethane prepolymer with the fluorescent whitening agent body is prepared; water-based chain extender is added into the polyurethane prepolymer, and a reaction is conducted; then, solvent is added to dilute the mixture to certain viscosity, a salt-forming agent is added, and a polyurethane ionomer is formed; the polyurethane ionomer is transferred into an emulsification reactor, then emulgator and water are added, then solvent removal is conducted, and water-based polyurethane based fluorescent whitening emulsion is obtained. The polyurethane based fluorescent whitening agent has the advantages of being high in fluorescence quantum yield, resistant to light, resistant to heat, resistant to washing, resistant to wear, resistant to migration, resistant to wet processing, prone to film formation, capable of being processed and the like and further has the advantages of being good in whitening effect, convenient to use, low in cost, free of toxin, environmentally friendly and the like.

Description

technical field [0001] The invention relates to a polymer fluorescent whitening agent, in particular to a polyurethane-based fluorescent whitening agent and a preparation method thereof. Background technique [0002] Fluorescent whitening agent is a fluorescent substance that can absorb ultraviolet light and emit blue or purple-blue light. When small-molecule fluorescent whitening agents are used to treat materials, due to the disadvantages of low fluorescence quantum yield, poor light resistance and heat resistance, the whitening effect and use effect are reduced. [0003] Polymeric fluorescent whitening agent is formed by polymerizing fluorescent monomers and other monomers. After polymerization, the structure of the chromophoric group of the fluorescent monomer remains unchanged, and its fluorescent whitening performance is still maintained; the covalent bond between the chromophore and the polymer chain The existence of bonds can significantly improve the structural sta...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G18/66C08G18/48C08G18/42C08G18/32C08G18/34C08G18/12C09B69/10
CPCC08G18/12C08G18/0814C08G18/0823C08G18/4277C08G18/4825C08G18/4854C08G18/6633C08G18/6666C09B69/10C08G18/348C08G18/3206C08G18/3275
Inventor 胡先海丁运生程从亮刘瑾陈建利
Owner ANHUI UNIVERSITY OF ARCHITECTURE
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