Preparation method for siloxane-terminated organosilicon block polyurethane prepolymer

A polyurethane prepolymer, polyurethane prepolymerization technology, applied in the direction of polyurea/polyurethane adhesives, adhesive types, adhesives, etc., to achieve the effects of easy marketization, good elasticity, and improved heat resistance

Active Publication Date: 2012-08-15
INST OF APPLIED CHEM JIANGXI ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, polyurethane sealants and silicone sealants have been widely used in the engineering field due to their excellent performance. However, their respective chemical structures and physical properties Determining their lack of certain performance, so that their use functions are subject to certain restrictions
Polyurethane sealant (referred to as PU glue) has high strength, tear resistance, puncture resistance, oil resistance and medium corrosion resistance, but its terminal NCO group is very sensitive to moisture, improper handling will easily affect the storage stability of the system, and the long-term stable storage of the product is difficult During curing, the released carbon dioxide may cause pores in the sealing layer. The deep curing speed is slow and the surface is easy to stick. Primers are generally required for bonding with the surface of non-porous base materials such as glass and metal. Long-term moisture resistance and heat aging resistance poor
Silicone sealant cures quickly, does not foam, and can be stably bonded to non-porous surfaces such as glass and metal. The adhesive layer has good heat and aging resistance, but its biggest disadvantage is poor pollution resistance. The joints are seriously polluted, which affects the appearance, and has disadvantages such as poor paintability, poor tear strength, and insufficient oil resistance.

Method used

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  • Preparation method for siloxane-terminated organosilicon block polyurethane prepolymer
  • Preparation method for siloxane-terminated organosilicon block polyurethane prepolymer
  • Preparation method for siloxane-terminated organosilicon block polyurethane prepolymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Add 200.0g of hydroxyl-terminated polyethylene oxide with an average molecular weight of 4500~6000 into a four-neck flask equipped with a thermometer, condenser, stirring device and vent tube, and raise the temperature to 80°C in a water bath within 30 minutes, and the vacuum degree is 0.09MPa Stir under the conditions, vacuum degassing for 1 hour, cool down to 50°C, stop stirring and vacuumize; then add 40.0g hydroxyl-terminated silicone oil, 30.0g toluene diisocyanate (TDI), 12.0g castor oil and 100.0g cyclohexanone, Under the protection of pure nitrogen, slowly heat the above-mentioned materials to 60°C, and when the polyether is completely melted and becomes liquid, add 0.5 g of stannous octoate as a catalyst, and reflux at 90°C for 4 hours to obtain a silicone with an NCO terminal group -Polyurethane polymer, then add 16.0g 3-aminopropyltrimethoxysilane and 0.1g catalyst stannous octoate, continue to stir and react for 1h; detect-When the NCO group content value is ...

Embodiment 2

[0036] Add 260.0g of hydroxyl-terminated polypropylene oxide with an average molecular weight of 5000~6000 into a four-necked flask equipped with a thermometer, condenser, stirring device and vent pipe, and raise the temperature to 80°C in a water bath within 30min, with a vacuum of 0.09MPa Under stirring, vacuum degassing for 1h, cooling down to 50°C, stopping stirring and vacuuming; then adding 50.0g hydroxyl-terminated silicone oil, 60.0g diphenylmethane 4,4'-diisocyanate (MDI), 10.6g castor oil and 80.0 g N-methylpyrrolidone, under the protection of high-purity nitrogen, slowly heat the above-mentioned materials to 70°C, and when the polyester is completely melted and becomes liquid, add 4.0g of dibutyltin dilaurate as a catalyst, and reflux at 90°C 5h, the obtained silicone-polyurethane polymer with NCO terminal group; then add 25.0g 3-(2-aminoethyl)aminopropyl trimethoxysilane and catalyst 1.0g dibutyltin dilaurate, continue to stir the reaction 1.5h; detection - when th...

Embodiment 3

[0038] Add 260.0g of phthalic anhydride polyester polyol with an average molecular weight of 4500~6000 into a four-necked flask equipped with a thermometer, condenser, stirring device and vent pipe, and heat up to 80°C in a water bath within 30min, under the condition of a vacuum of 0.09MPa Stirring, vacuum degassing for 1h, cooling down to 50°C, stopping stirring and vacuuming; then adding 46.6g hydroxyl-terminated silicone oil, 50.0g xylylene diisocyanate (XDI), 8.8g castor oil and 68g cyclohexanone, in Under the protection of high-purity nitrogen, slowly heat the above-mentioned materials to 80°C, and when the polyester and polyether are all melted and become liquid, then add 3.0g of stannous octoate as a catalyst, and reflux at 90°C for 6 hours to obtain the terminal group: Organosilicon-polyurethane polymer of NCO, then add 30.0g 3-phenylpropyltrimethoxysilane and catalyst 2.0g dibutyltin dilaurate, continue to stir and react for 1.2h; when the detection-NCO group content ...

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Abstract

The invention discloses a preparation method for siloxane-terminated organosilicon block polyurethane prepolymer. The method includes the following steps: polyester polyol or polyether polyol, hydroxy-terminated silicone oil, castor oil and the like are dripped into aromatic or aliphatic diisocyanate, so that organosilicon block polyurethane prepolymer is obtained; and afterwards, under organic tin catalyst, siloxane with activated hydrogen is added into the organosilicon block polyurethane prepolymer to react, so that the stable siloxane-terminated organosilicon block polyurethane prepolymer is obtained. The cured film of the prepolymer prepared by the method has the advantages of high elasticity, low-temperature flexibility, high water resistance, high adhesive force, high wear resistance and high aging resistance. The siloxane-terminated organosilicon block polyurethane prepolymer can be widely applied in sealing or coating materials for environment protection, buildings, electronics and other industries and other fields.

Description

[0001] technical field [0002] The invention relates to a method for preparing a siloxane-terminated organosilicon block polyurethane prepolymer, belonging to the technical field of organosilicon new materials. Background technique [0003] At present, polyurethane sealants and silicone sealants have been widely used in the engineering field due to their excellent performance. Subject to certain restrictions. Polyurethane sealant (referred to as PU glue) has high strength, tear resistance, puncture resistance, oil resistance and medium corrosion resistance, but its terminal NCO group is very sensitive to moisture, improper handling will easily affect the storage stability of the system, and the long-term stable storage of the product is difficult During curing, the released carbon dioxide may cause pores in the sealing layer. The deep curing speed is slow and the surface is easy to stick. Primers are generally required for bonding with the surface of non-porous base mat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G18/78C08G18/67C08G18/61C09J175/14
Inventor 陈衍华游胜勇谌开红曾国屏程斌
Owner INST OF APPLIED CHEM JIANGXI ACAD OF SCI
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