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A kind of preparation method of tetramercaptosilsesquioxane modified waterborne polyurethane color fixing agent

A technology of silsesquioxane and water-based polyurethane, which is applied in dyeing, textiles and papermaking, etc., can solve the problems affecting the stability of emulsion, thermal stability, etc., to improve the color fastness to rubbing, long-term use, good The effect of suspension performance

Active Publication Date: 2020-12-11
SHEYANG TIANYUAN CHEM IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chinese Patent Publication No. CN101824135A reports the preparation and application of a blocked cationic water-based polyurethane color fixing agent. The method obtains the target product through polyurethane prepolymerization, blocking agent capping, acid neutralization, and ionization reaction. The method of active groups retains part of the active groups so that they can release the active groups to react with the fabric during high-temperature baking, and improve the adhesion of polyurethane to the fabric, but the existence of active groups will affect the stability of the emulsion, especially the thermal stability.
Although the preparation method of mercapto-functionalized silsesquioxane is disclosed in the prior art, such as Yuan Gang et al. 4) and Zhang Lei et al. "Synthesis and Characterization of Mercapto-functionalized Silsesquioxanes" "Journal of Beijing University of Chemical Technology (Natural Science Edition", Volume 36, No. 6) both disclose the preparation of Mercapto-functionalized Silsesquioxanes , but the prior art does not have any reports on the use of mercaptosilsesquioxane to modify polyurethane to improve the effect of polyurethane color fixing agent

Method used

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  • A kind of preparation method of tetramercaptosilsesquioxane modified waterborne polyurethane color fixing agent
  • A kind of preparation method of tetramercaptosilsesquioxane modified waterborne polyurethane color fixing agent
  • A kind of preparation method of tetramercaptosilsesquioxane modified waterborne polyurethane color fixing agent

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Experimental program
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Effect test

Embodiment 1

[0025] Synthesis of tetramercaptosilsesquioxane modified waterborne polyurethane (tetramercaptosilsesquioxane accounts for 0.5% of the total mass of polyol, diisocyanate and chain extender)

[0026] (1) Preparation of tetramercaptosilsesquioxane: 19.6g of 3-mercaptopropyltrimethoxysilane (Guangzhou Shuangtao Fine Chemical Co., Ltd.) and 27.64g of octyltriethoxysilane (Suzhou Siloso New Material Co., Ltd. company) into a flask equipped with magnetic stirring and a condenser, while adding 100ml of concentrated hydrochloric acid and 1200ml of methanol. The mixture was reacted at 90°C for 36 hours under stirring, then cooled to remove methanol solvent, the crude product was washed with cold methanol several times to remove excess oligomeric silsesquioxane, and dried in vacuum to obtain viscous liquid tetramercapto silsesquioxane alkyl.

[0027] (2) Synthesis of tetramercaptosilsesquioxane-modified water-based polyurethane: add 100g polyethylene glycol 1000, 31.32g toluene diisocy...

Embodiment 2

[0029] Synthesis of tetramercaptosilsesquioxane modified waterborne polyurethane (tetramercaptosilsesquioxane accounts for 0.8% of the total mass of polyol, diisocyanate and chain extender)

[0030] (1) Preparation of tetramercaptosilsesquioxane: Add 19.6g of 3-mercaptopropyltrimethoxysilane and 27.64g of octyltriethoxysilane into a flask equipped with a magnetic stirrer and a condenser, and simultaneously add 100ml concentrated hydrochloric acid and 1200ml methanol. The mixture was reacted at 90°C for 36 hours under stirring, then cooled to remove methanol solvent, the crude product was washed with cold methanol several times to remove excess oligomeric silsesquioxane, and dried in vacuum to obtain viscous liquid tetramercapto silsesquioxane alkyl.

[0031] (2) Synthesis of tetramercaptosilsesquioxane-modified water-based polyurethane: add 100g polyethylene glycol 1000, 31.32g toluene diisocyanate, 52.5g 1-methyl-2-pyrrolidone to a four-necked flask, at 70°C React at low te...

Embodiment 3

[0033] Synthesis of tetramercaptosilsesquioxane modified waterborne polyurethane (tetramercaptosilsesquioxane accounts for 1% of the total mass of polyol, diisocyanate and chain extender)

[0034](1) Preparation of tetramercaptosilsesquioxane: Add 19.6g of 3-mercaptopropyltrimethoxysilane and 27.64g of octyltriethoxysilane into a flask equipped with a magnetic stirrer and a condenser, and simultaneously add 100ml concentrated hydrochloric acid and 1200ml methanol. The mixture was reacted at 90°C for 36 hours under stirring, then cooled to remove methanol solvent, the crude product was washed with cold methanol several times to remove excess oligomeric silsesquioxane, and dried in vacuum to obtain viscous liquid tetramercapto silsesquioxane alkyl.

[0035] (2) Synthesis of tetramercaptosilsesquioxane-modified water-based polyurethane: add 100g polyethylene glycol 1000, 31.32g toluene diisocyanate, 52.5g 1-methyl-2-pyrrolidone to a four-necked flask, at 70°C React at low tempe...

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Abstract

The invention relates to a method for preparing a waterborne polyurethane coloring stabilizer modified with tetramercapto silsesquioxane. The method includes mixing and reacting oligomer polyol and diisocyanate to obtain a prepolymer; then adding a hydrophilic chain extender, reacting the mixture to further increase the molecular weight of the prepolymer, then adding self-prepared tetramercapto silsesquioxane to increase the crosslinking degree of the system, finally adding a neutralizing agent, adding water after the reaction is finished, and stirring and emulsifying the reaction solution toobtain waterborne polyurethane emulsion modified with tetramercapto silsesquioxane. The tetramercapto silsesquioxane is adopted to introduce a cagelike structure into the system, and is adopted as crosslinking points to allow the waterborne polyurethane to have denser network distribution. The polyurethane emulsion as a coloring stabilizer can effectively cover the dye to improve coloring stabilizing performance. The emulsion system has good stability.

Description

technical field [0001] The invention relates to the technical field of color-fixing agents, in particular to a method for preparing a tetramercaptosilsesquioxane-modified water-based polyurethane color-fixing agent. Background technique [0002] In recent years, water-based polyurethane color fixing agent has attracted people's attention. It has the advantages of safety, non-toxicity, and pollution-free. In addition to color fixing, it can also bring some additional surface properties to the fabric. The network structure can cover the dye and cover the water-soluble group of the dye, and bind and seal the dye in the form of a transparent thin layer, the color fastness to washing will be greatly improved, and its color fixing effect is not only suitable for water-soluble dyes, It also has a good effect on disperse dyes. [0003] However, pure water-based polyurethane has many disadvantages, such as poor film-forming properties, poor adhesion to fabrics, poor water resistance...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G18/66C08G18/61C08G18/48C08G18/34C08G18/10D06P5/08
CPCC08G18/0823C08G18/10C08G18/4825D06P5/08C08G18/61C08G18/348
Inventor 刘国峰李春荣陈刚王成慧李维智
Owner SHEYANG TIANYUAN CHEM IND CO LTD
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