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Method for preparing organosilicon modified cationic waterborne polyurethane

A water-based polyurethane and organosilicon technology, applied in the field of preparation of organosilicon-modified cationic water-based polyurethane, can solve the problems of acceleration, difficult control of synthesis process, complicated process and the like

Inactive Publication Date: 2014-08-13
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

In the above-mentioned preparation methods of silicone-modified cationic water-based polyurethanes, N-methyldiethanolamine is used to react with isocyanate groups to prepare prepolymers containing tertiary amine groups. However, tertiary amine groups can be used as catalysts to accelerate the process of preparing water-based polyurethanes. The reaction between the isocyanate group and the hydroxyl group makes the system exothermic violently during the reaction process, and the synthesis process is difficult to control
Therefore, the process of cationic water-based polyurethane prepared by this route is relatively complicated, and sometimes the emulsified product is not stable enough, so it brings difficulties to industrial production.

Method used

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  • Method for preparing organosilicon modified cationic waterborne polyurethane
  • Method for preparing organosilicon modified cationic waterborne polyurethane
  • Method for preparing organosilicon modified cationic waterborne polyurethane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0062] Silicone with hydroxyl groups at both ends and epoxy groups at the side groups (R 1 =A 1 , R 2 =B 1 , m=5, n=8, M n =2000) synthetic technical route:

[0063] Hydroxyl protection reaction (molar ratio of allyl alcohol: hexamethyldisilazane = 2: 1.1)

[0064] In a 1L three-necked flask, slowly add 355.2g of hexamethyldisilazane to 232.3g of allyl alcohol dropwise at room temperature. After the dropwise addition, raise the temperature of the reaction system to 100°C and continue the reaction at this temperature After 6 hours, the reaction stopped. Atmospheric pressure distillation collected fractions at 98-100°C to obtain 447.5 g of allyloxytrimethylsilane with a yield of 86%.

[0065] Hydrosilylation reaction (molar ratio allyloxytrimethylsilane: tetramethyldisiloxane: chloroplatinic acid = 2.4: 1: 3.1 × 10 -4 )

[0066] In a 1L four-necked bottle, add allyloxytrimethylsilane 312.5g, 50mL toluene and chloroplatinic acid 3.1×10 -4 mol of isopropanol solution, aft...

Embodiment 2

[0073] Embodiment 2 A kind of preparation method of organosilicon modified cationic waterborne polyurethane

[0074] Prepolymerization

[0075] In a reaction flask equipped with a stirrer and a thermometer, add 174g of toluene diisocyanate and 100g of organosilicon (R 1 =A 1 , R 2 =B 1 , m=5, n=8, M n =2000), heated up to 70°C and reacted for 0.5h; then added 200g polyether diol (M n =800), the reaction was continued for 0.5h at the same temperature.

[0076] Chain extension and capping reactions

[0077] Add 12.4g of ethylene glycol into the reaction system, react at 70°C for 0.5h, and use the standard di-n-butylamine back titration method to analyze the isocyanate group content in the prepolymer. When the isocyanate group content reaches the theoretical value of 8.63 %, add 74g monohydroxy glycidyl ether (R 5 = H, M n =74) Terminate the reaction to obtain a silicone-modified polyurethane whose main chain contains ether bonds, urethane bonds and polysiloxane segments...

Embodiment 3

[0083] Embodiment 3 A kind of preparation method of organosilicon modified cationic waterborne polyurethane

[0084] Prepolymerization

[0085] In a reaction flask equipped with a stirrer and a thermometer, add 222g of isophorone diisocyanate and 150g of organosilicon (R 1 =A 1 , R 2 =B 8 , m=9, n=2, M n =1500), heated up to 70°C and reacted for 0.5h; then added 250g of polyether glycol (M n =1000), the reaction was continued for 0.5h at the same temperature.

[0086] Chain extension and capping reactions

[0087] Add 6.2g of ethylene glycol into the reaction system, react at 70°C for 0.5h, and then use the standard di-n-butylamine back titration method to analyze the isocyanate group content in the prepolymer. When the isocyanate group content reaches the theoretical value of 7.35 %, add 114.4g monohydroxy glycidyl ether (R 5 =OHCH 2 ,M n =104) terminate the reaction to obtain a silicone-modified polyurethane containing ether bonds, urethane bonds and polysiloxane s...

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Abstract

The invention discloses a method for preparing organosilicon modified cationic waterborne polyurethane. The method comprises the steps: firstly, reacting organosilicon (of which the two terminals contain hydroxyalkyl groups and side groups contain epoxy groups) with polyisocyanate, so as to introduce a principal chain of organosilicon into a polyurethane structure; next, reacting an ordinary chain extender and mono-hydroxyl glycidyl ether (or mono-hydroxyl glycidyl ester or a mixture of the mono-hydroxyl glycidyl ether and the mono-hydroxyl glycidyl ester at any ratio) with the organosilicon modified polyurethane prepolymer; then, adding an organic amine compound (or an organophosphorus compound or organosulfur compound) and organic acid into organosilicon modified polyurethane diluted with butanone, so as to carry out ionization reaction; finally, dispersing the ionized organosilicon modified polyurethane into water through self-emulsifying, distilling at reduced pressure so as to remove butanone, thus obtaining the organosilicon modified cationic waterborne polyurethane.

Description

technical field [0001] The invention relates to a method for preparing organosilicon-modified cationic water-based polyurethane, in particular to a method for preparing organosilicon-modified water-based polyurethane in which cationic hydrophilic groups are used as side groups of polysiloxane chain segments. 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 polysiloxane segments into polyurethane molecules can greatly improve the water resistance ...

Claims

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Application Information

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IPC IPC(8): C08G18/65C08G18/61C08G18/48C08G18/42C08G18/44C08G18/12C08G77/38
CPCC08G18/0809C08G18/0814C08G18/12C08G18/4009C08G18/4018C08G18/44C08G18/4825C08G18/61C08G18/664C08G18/6674C08G18/831C08G77/38C08G18/3206
Inventor 邬元娟张萌张树秋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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