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Preparation method for silicofluoride-contained polyurethane water repellent finishing agent

A water-repellent finishing, polyurethane technology, applied in fiber processing, textiles and papermaking, etc., can solve the problems of high brittleness and high cost, and achieve the effect of improving brittleness, easy operation and wide application prospects.

Active Publication Date: 2012-10-03
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to provide a preparation method of silicon-fluorine-containing polyurethane water-repellent finishing agent to solve the problem of high cost and high brittleness caused by increasing the fluorine content of fluorine-containing polyurethane to improve water resistance, oil resistance and antifouling performance. technical problem

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] (1) 1mol diphenylmethane diisocyanate (MDI) and 0.3mol perfluoroalkylethanol (F(C 2 f 4 ) 6 C 2 h 4 OH) was dissolved in 150g N, N-dimethylformamide (DMF) and added to the reaction kettle to fully dissolve, nitrogen gas was introduced, and the reaction was stirred at 40°C for 2h under the protection of nitrogen gas, and the stirring speed was 80rpm; the remaining in the reaction system The number of moles of isocyanate groups contained in isocyanate is 1.7mol;

[0035] (2) Add 0.25mol polybutylene adipate diol (Mn=1000) and 1g dibutyltin dilaurate to the reaction kettle under the protection of nitrogen at 50°C and stir for 2h at a stirring speed of 100rpm to obtain the prepared Polymer R1; the number of moles of isocyanate groups contained in the remaining isocyanate in the reaction system is 1.2mol;

[0036](3) 0.4mol terminal hydroxypropyl polysiloxane (HO-PDMS) (Mn=2000) was dissolved in tetrahydrofuran to obtain a solution with a mass fraction of 30%, and then ...

Embodiment 2

[0040] (1) 1mol toluene diisocyanate (TDI) and 0.35mol perfluoroalkylethanol (F(C 2 f 4 ) 8 C 2 h 4 OH) was dissolved in 100g N, N-dimethylacetamide (DMAc) and added to the reaction kettle to fully dissolve, nitrogen gas was introduced, and the reaction was stirred at 80°C for 2h under the protection of nitrogen gas, and the stirring speed was 180rpm; the remaining The number of moles of isocyanate groups contained in the isocyanate is 1.65mol;

[0041] (2) Add 0.3 mol of polytetrahydrofuran diol (PTMG, Mn=1000), 0.8 g of N, N-dimethylcyclohexylamine in the reaction kettle under the protection of nitrogen at 80°C for 2 hours, and the stirring speed is 200 rpm to obtain Prepolymer R1; the number of moles of isocyanate groups contained in the remaining isocyanate in the reaction system is 1.05mol;

[0042] (3) Dissolve 0.35 mol terminal hydroxypropyl polysiloxane (HO-PDMS) (Mn=2000) in N-methylpyrrolidone to obtain a solution with a mass fraction of 80%, and then add 1 g of...

Embodiment 3

[0046] (1) Dissolve 1 mol of 1,6-hexamethylene diisocyanate (HDI) and 0.4 mol of N-ethyl perfluorooctyl sulfonamide in ethanol in 100 g of ethyl acetate and add them to the reaction kettle to fully dissolve, and then pass in nitrogen gas, under the protection of nitrogen gas Stir the reaction at 50°C for 1 hour at a stirring speed of 100 rpm; the isocyanate group contained in the remaining isocyanate in the reaction system is 1.6 mol;

[0047] (2) Add 0.4mol polyoxypropylene diol (Mn=1000) and 0.5g triethylamine in the reaction kettle under the protection of nitrogen at 65°C and stir for 2h at a stirring speed of 120rpm to obtain the prepolymer R1; The isocyanate group contained in the remaining isocyanate in the system is 0.8mol;

[0048] (3) 0.25mol terminal hydroxypropyl polysiloxane (HO-PDMS) (Mn=2000) was dissolved in N-methylpyrrolidone to obtain a solution with a mass fraction of 50%, and then 0.5g triethylamine was added, Add it dropwise to prepolymer R1 at a speed of...

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Abstract

The invention provides a preparation method for silicofluoride-contained polyurethane water repellent finishing agent, which is characterized in that the preparation method comprises the following specific steps that isocyanate and alcohol with fluoride are dissolved in a solvent, and the isocyanate and the alcohol with fluoride are mixed for reaction under protection of nitrogen; prepolymer R1 is obtained by adding at least one of polyether diol and polyester diol with a catalyst into the reaction system of the first step; organic oxosilane is dissolved in the solvent, the catalyst is added for obtaining organic oxosilane solution, and prepolymer R2 is obtained by adding the organic oxosilane solution into the prepolymer R1 which is obtained from the second step in a dropping way; and diol or diamine is used as chain extender to be added into the prepolymer R2 which is obtained from the third step, finally, small-molecule alcohol is added and mixed with isocyanate remained in the reaction system to be carried out reaction and end capping, and silicofluoride-contained polyurethane is obtained. The silicofluoride-contained polyurethane provided by the invention can be used as fabric finishing agent, leather coating agent, self-cleaning paint additive and the like, and has the advantages of remarkable finishing properties of water and oil repelling.

Description

technical field [0001] The invention relates to a preparation method of a silicon-fluorine-containing polyurethane water-repellent finishing agent, which belongs to the field of chemical auxiliary agents. Background technique [0002] With the development of social economy and technology, people have more and more demands for high-quality, multi-functional materials, especially in the fields of textile leather finishing, coatings, construction, automobiles and papermaking, etc. The pollution effect requirements are getting higher and higher. Due to its excellent thermal stability, weather resistance and chemical inertness, as well as unique properties such as low surface free energy and low coefficient of friction, fluorine-containing polyurethane exhibits outstanding water and oil repellency and anti-adhesion properties. Fluorine-containing polyurethane finishing agents can not only be used for fabric finishing, but also have important applications in veneer carpets, wall ...

Claims

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Application Information

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IPC IPC(8): C08G18/66C08G18/38C08G18/61C08G18/12D06M15/657
Inventor 丁彬王家林斯阳胡娟平崔玲潇俞建勇
Owner DONGHUA UNIV
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