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Preparation method of fluorine/silicone co-modified waterborne polyurethane

A technology of co-modification of waterborne polyurethane, applied in textiles and papermaking, etc., can solve the problems of reducing the surface energy of polyurethane, affecting the water solubility and long-term storage stability of waterborne polyurethane, poor waterproof and antifouling ability, etc.

Inactive Publication Date: 2019-08-16
嘉兴禾大科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the addition of hydrophilic monomers, ordinary water-based polyurethane has poor waterproof and anti-fouling ability.
Modification with pure silicone can improve the hydrophobicity of polyurethane to a certain extent and reduce the surface energy of polyurethane, but its antifouling and waterproof ability can only be improved to a limited extent.
Simple organic fluorine modification can also reduce the surface energy of polyurethane to a large extent, but to achieve higher waterproof and antifouling ability, more organic fluorine needs to be added, and adding too much will affect the water solubility and long-term storage of waterborne polyurethane Stability, and the production cost is also greatly increased
Chinese patent application 201010115181.4 introduces a single-component silicon / fluorine modified water-based polyurethane resin and its preparation method, and Chinese patent application 201310368406.0 introduces a silicon-fluorine double-modified water-based polyurethane emulsion and its preparation method. The above two documents introduce Most of them are silicon-fluorine-modified water-based polyurethanes used in architectural emulsions and coatings, and silicon-fluorine-modified water-based polyurethanes used in textile fabrics have not been reported yet.

Method used

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  • Preparation method of fluorine/silicone co-modified waterborne polyurethane
  • Preparation method of fluorine/silicone co-modified waterborne polyurethane

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preparation example Construction

[0009] The preparation method of this fluorosilicon co-modified waterborne polyurethane comprises the steps:

[0010] (1) Add diisocyanate, polymer diol, dihydroxy silicone oil, hydrophilic chain extender, and catalyst dibutyltin dilaurate into the reaction kettle, and stir at 50-70°C for 90-120 minutes to obtain a prepolymer;

[0011] (2) Add acetone to the prepolymer obtained in the previous step to dilute, then add a small molecule fluorine-substituted alcohol, a small molecule diol, and a crosslinking agent, and continue the reaction at 50-70°C for 90-120 minutes;

[0012] (3) Lower the reaction temperature to 30-40°C, add a neutralizer and stir evenly; add a diamine chain extender and water, emulsify at high speed, and remove acetone under reduced pressure to obtain fluorosilicone co-modified waterborne polyurethane.

[0013] In the preparation method of this fluorosilicon co-modified water-based polyurethane, the diisocyanate, polymer diol, dihydroxy silicone oil, hydrop...

Embodiment 1

[0020] Raw materials with the following weights are used: 17.5kg isophorone diisocyanate (the content in the diisocyanate is below 800ppm), 45kg polytetrahydrofuran diol-2000, 7.5kg dihydroxy silicone oil-1000, 4.5kg dimethylolpropane, 0.2 kg dibutyltin dilaurate, 0.7kg hexafluoroisopropanol, 0.7kg butanediol, 5kg trimethylolpropane, 4kg triethylamine, 5kg ethylenediamine, 145kg water and 20kg acetone.

[0021] Prepared by following steps:

[0022] Step 1: Add isophorone diisocyanate, polytetrahydrofuran diol-2000, dihydroxysilicone oil-1000, dimethylolpropane, and dibutyltin dilaurate into the reaction kettle, and stir at 60°C for 90 minutes to obtain a prepolymer .

[0023] Step 2: add acetone to the prepolymer obtained in step 1 for dilution, add octafluoropentanol, butanediol, and trimethylolpropane, and continue the reaction at 60° C. for 90 minutes.

[0024] Step 3: Lower the reaction temperature to 30°C, add neutralizing agent triethylamine and stir for 20 minutes; ad...

Embodiment 2

[0026] The following weights of raw materials are used: 18kg toluene diisocyanate (the content of diisocyanate is less than 600ppm), 47kg polyether N220, 7.5kg dihydroxy silicone oil-1000, 4kg dimethylolpropane, 0.2kg dibutyltin dilaurate, 0.7 kg octafluoropentanol, 0.65 kg butanediol, 4.8 kg trimethylolpropane, 4.2 kg triethylamine, 5.2 kg ethylenediamine, 145 kg water and 20 kg acetone.

[0027] Prepared by following steps:

[0028] Step 1: Add toluene diisocyanate, polyether N220, dihydroxy silicone oil-1000, dimethylolpropane, and dibutyltin dilaurate into the reaction kettle, and stir at 50°C for 120 minutes to obtain a prepolymer.

[0029] Step 2: Add acetone to the prepolymer obtained in Step 1 for dilution, add octafluoropentanol, butanediol, and trimethylolpropane, and continue the reaction at 50° C. for 120 minutes.

[0030] Step 3: Lower the reaction temperature to 30°C, add neutralizing agent triethylamine and stir for 20 minutes; add ethylenediamine and water, em...

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Abstract

A preparation method of the fluorine / silicone co-modified waterborne polyurethane comprises the following steps: (1) adding diisocyanate, polymer dihydric alcohol, dihydroxy silicone oil, a hydrophilic chain extender and a catalyst dibutyltin dilaurate into a reaction kettle, and stirring all the components at 50-70 DEG C for 90-120 minutes to obtain a prepolymer; (2) adding acetone into the obtained prepolymer to dilute the prepolymer, then adding micromolecular fluorine substituted alcohol, micromolecular dihydric alcohol and a cross-linking agent, and continuously performing the reaction at50-70 DEG C for 90-120 minutes; (3) reducing the temperature of the reactant to 30-40 DEG C, adding a neutralizer triethylamine, and uniformly stirring the reactant; and (4) adding a diamine chain extender and water, carrying out high-speed emulsification, and finally carrying out reduced pressure suction filtration to remove acetone so as to obtain the product. Due to the adoption of a fluorine / silicone co-modification process, the waterproof and antifouling properties of the obtained waterborne polyurethane can be improved by more than 30%, and the waterborne polyurethane has good stabilityand lower production cost.

Description

technical field [0001] The invention relates to the field of polyurethane synthesis, and relates to a preparation method of fluorosilicon co-modified waterborne polyurethane. Background technique [0002] Water-based polyurethane uses water as a solvent, which is non-toxic, environmentally friendly, and has the advantages of convenient processing and use. Therefore, it has a wide range of uses in fabric coating and leather top coating. However, due to the addition of hydrophilic monomers, ordinary water-based polyurethane has poor waterproof and anti-fouling capabilities. Modification with pure silicone can improve the hydrophobicity of polyurethane to a certain extent and reduce the surface energy of polyurethane, but its antifouling and waterproof ability can only be improved to a limited extent. Simple organic fluorine modification can also reduce the surface energy of polyurethane to a large extent, but to achieve higher waterproof and antifouling ability, more organic ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G18/66C08G18/48C08G18/32C08G18/61C08G18/28D06N3/14
CPCC08G18/2885C08G18/48C08G18/4825C08G18/4854C08G18/61C08G18/6674C08G18/6677C08G18/6685D06N3/146
Inventor 薛振华武锦锋钟名国朱叶佳
Owner 嘉兴禾大科技有限公司
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