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Preparation method of organosilicon-modified amphoteric polyurethane aqueous dispersion

A polyurethane water dispersion and silicone technology, applied in the direction of polyurea/polyurethane coatings, coatings, etc., can solve the problems of pH sensitivity in the application environment, achieve easy control of the production process, increase the application range, and avoid severe exothermic phenomena Effect

Inactive Publication Date: 2016-03-30
INST OF QUALITY STANDARDS & TESTING TECH FOR AGRO PROD OF SHANDONG ACADEMY OF AGRI SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the polyurethane water dispersion system researched and applied is limited to single anion and cationic polyurethane water dispersions, and most of the research reports on organic silicon-modified waterborne polyurethane are anionic. Large limitations, especially sensitive to the pH of the application environment

Method used

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  • Preparation method of organosilicon-modified amphoteric polyurethane aqueous dispersion
  • Preparation method of organosilicon-modified amphoteric polyurethane aqueous dispersion
  • Preparation method of organosilicon-modified amphoteric polyurethane aqueous dispersion

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Example 1 (cationic silicone content=14.1%, COOH%=1.3%, NCO / OH=2.86:1)

[0031]

[0032] 1. Synthesis of cationic silicone:

[0033] Equilibrium reaction: using trifluoromethanesulfonic acid as a catalyst, tetramethyldihydrosiloxane and octamethylcyclotetrasiloxane (D 4 ) for polymerization reaction, nitrogen protection is used during the reaction process, the reaction temperature is 65° C., and the reaction time is 20 h to obtain α,ω-bissilylhydrogen-terminated polysiloxane. The molar ratio of the above two reactants in the equilibrium reaction depends on the molecular weight of the final product or the silicon hydrogen content. According to the above reaction formula, the molecular weight design formula (taking tetramethyldihydrogensiloxane as the end-capping agent, the dosage is 1mol as an example) is as follows, the design molecular weight of polysiloxane=the molecular weight of the end-capping agent (134)+D 4 Molecular weight (296)×D 4 The amount of substance...

Embodiment 2

[0055] Example 2 (cationic silicone content=21.3%, COOH%=1.44%, NCO / OH=2.5:1)

[0056]

[0057] 1. Synthesis of cationic silicone:

[0058] Hydroxyl protection: at room temperature, first add hexamethyldisilazane dropwise to glycerol, raise the temperature of the reaction system to 90-120°C, and continue to react at this temperature for 4-8 hours, stop the reaction, and distill it off under reduced pressure Excessive hexamethyldisilazane to obtain 1,3-bis(trimethylsilyl)oxyl-2-propanol, and the molar ratio of feeding in the hydroxyl protection reaction process is: glycerol:hexamethyldisilazane Alkane=1:1~1.1.

[0059]Alkylation reaction: At room temperature, slowly add 1,3-bis(trimethylsilyl)oxy-2-propanol dropwise to the tetrahydrofuran solution containing sodium hydride, start stirring and slowly raise the temperature to 40-60°C for reaction 2h until no hydrogen gas is generated; after cooling the reaction system to 0°C, start stirring and slowly add allyl bromide dropw...

Embodiment 3

[0084] Example 3 (cationic silicone content=24.4%, COOH%=1.34%, NCO / OH=2.5:1)

[0085]

[0086] Prepolymerization: In a three-necked flask equipped with a stirrer and a thermometer, add 250g diphenylmethane diisocyanate, 75g cationic silicone (M) of structure (I) n =1500) and 50 g of cationic silicone (M n=1000), heated up to 70°C and reacted for 1.2h; then added 100g of polyether diol (M n =2000), the reaction was continued for 1.5h at the same temperature. Add 22.2g of dimethylolbutyric acid into the reaction system, react at 70°C for 1h, then add 6.20g of ethylene glycol and react at 70°C for 1h, then use the standard di-n-butylamine back titration method to analyze the prepolymer The content of isocyanate group, when the content of isocyanate group reaches the theoretical value of 11.83%, the reaction is terminated, and the main chain contains tertiary sulfonium group, ether group, urethane group, carboxyl group and polysiloxane segment, and the side chain contains po...

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Abstract

The invention discloses a preparation method of organic silicon modified amphiprotic polyurethane aqueous dispersion. The method comprises the following steps of: performing reaction on dihydroxyl alkyl-terminated organic silicon containing a tert-sulfonium group and polyisocyanates to introduce cationic organic silicon into a polyurethane structure; performing reaction on a hydrophilic chain extender, a general chain extender and the organic silicon modified polyurethane prepolymer to introduce an anionic group into the polyurethane structure; finally, dispersing the reaction type organic silicon modified polyurethane prepolymer into water by an acetone method through self-emulsification. The compounded organic silicon modified amphiprotic polyurethane aqueous dispersion molecule contains the hydrophilic cation tert-sulfonium group and the hydrophilic anionic carboxyl group, so that stable dispersion of the final product can be formed in an acid or alkali medium, and the application range of polyurethane aqueous dispersion is widened.

Description

technical field [0001] The invention relates to a method for preparing an aqueous silicone-modified amphoteric polyurethane dispersion, specifically a polysiloxane block or (and) graft-modified structure and a cationic hydrophilic group. The preparation method of the amphoteric polyurethane aqueous dispersion of group and anionic hydrophilic group. Background technique [0002] Due to its environmental friendliness, water-based polyurethane has made considerable progress in related fields since its inception, and is widely used in medical materials, electronic materials and chemical materials, but it also encounters problems that restrict its application. Since most of the synthesized waterborne polyurethanes are linear dispersion products, coupled with the existence of hydrophilic groups in the molecular chain segments, the water resistance of the waterborne polyurethane coating film is poor. Research data show that linking silicone to polyurethane molecules can greatly im...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G18/61C08G18/12
CPCC08G18/0833C08G18/12C08G18/4009C08G18/4018C08G18/61C08G18/6607C08G18/6625C08G18/6674C08G18/6692C09D175/06C09D175/08C08G18/3228C08G18/3275
Inventor 邬元娟张萌张树秋郭栋梁郭长英梁京芸邓立刚李腾
Owner INST OF QUALITY STANDARDS & TESTING TECH FOR AGRO PROD OF SHANDONG ACADEMY OF AGRI SCI
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