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A kind of modified siloxane-terminated polyurethane sealant and preparation method thereof

A polyurethane sealant, hydroxyl-terminated polyurethane technology, applied in the direction of polyurea/polyurethane adhesives, adhesives, non-polymer adhesive additives, etc., can solve the problems of high viscosity and low tensile strength of sealants, and achieve Fast cure, increased modulus and tensile strength, increased effect of cross-linked network sites

Active Publication Date: 2020-05-22
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The sealant does not contain heavy metal catalysts, is high temperature resistant, non-toxic and environmentally friendly, and has good elasticity and bonding performance; however, due to the addition of a large amount of inorganic fillers in the obtained sealant, the viscosity of the sealant is relatively high, although the mechanical properties of the sealant are reinforced by adding fillers. performance, but the single polyether raw material makes its tensile strength still small

Method used

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  • A kind of modified siloxane-terminated polyurethane sealant and preparation method thereof
  • A kind of modified siloxane-terminated polyurethane sealant and preparation method thereof
  • A kind of modified siloxane-terminated polyurethane sealant and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] 1) Preparation of hydroxyl-terminated polyurethane prepolymer

[0037] Raw material composition (unit, g)

[0038]

[0039] According to the above ratio, 40g of polybutadiene diol 2000 and 60g of polyglycerol 4000 were added to a stirred four-neck flask, heated to 120°C, and dehydrated under vacuum for 2h until no bubbles were generated in the flask. Cool down to about 60°C, install the stirring, and seal the reaction vessel. Add 3.32g of 2,4-toluene diisocyanate (accounting for 80wt%) and the mixture of 2,6-toluene diisocyanate (accounting for 20wt%) and 0.05g of the first catalyst tri(dioctyl)phosphoric acid successively in the reaction vessel For zirconium, feed nitrogen into the flask to isolate the air, seal the reaction vessel again, react at 60°C for 1.5h, then raise the temperature to 90°C, and react for 3h. Sampling and measuring the NCO content of the mixture every 30 minutes until the NCO content reacted completely. Stop the reaction, cool down to obtai...

Embodiment 2

[0055] 1) Preparation of hydroxyl-terminated polyurethane prepolymer

[0056] Composition mass (unit, g)

[0057]

[0058] According to the above ratio, 90g of polybutadiene diol 1000 and 60g of polyglycerol 6000 were added to a stirred four-neck flask, heated to 120°C, and dehydrated under vacuum for 2h until no bubbles were generated in the flask. Cool down to about 60°C, install the stirring, and seal the reaction vessel. Then add 3.98g of 2,4-toluene diisocyanate (80%) and 1.01g of 2,6-toluene diisocyanate (20%) mixture and 0.12g of the first catalyst tris (dioctyl) phosphoric acid in the reaction vessel For zirconium, feed nitrogen into the flask to isolate the air, seal the reaction vessel again, react at 60°C for 1.5h, then raise the temperature to 90°C, and react for 3h. Sampling and measuring the NCO content of the mixture every 30 minutes until the NCO content reacted completely. Stop the reaction, cool down to obtain the hydroxyl-terminated polyurethane prepol...

Embodiment 3

[0073] 1) Preparation of hydroxyl-terminated polyurethane prepolymer

[0074] Composition mass (unit, g)

[0075]

[0076] According to the above ratio, 32g of polybutadiene diol 5000 and 48g of polyglycerol 2000 were added to a stirred four-necked flask, heated to 120°C, and dehydrated under vacuum for 2h until no bubbles were generated in the flask. Cool down to about 60°C, install the stirring, and seal the reaction vessel. Then add 2.12g of 2,4-toluene diisocyanate (80%) and 0.54g of 2,6-toluene diisocyanate (20%) mixture and 0.06g of the first catalyst three (dioctyl) successively in the reaction vessel For zirconium phosphate, feed nitrogen into the flask to isolate the air, seal the reaction vessel again, react at 60°C for 1.5h, then raise the temperature to 90°C, and react for 3h. Sampling and measuring the NCO content of the mixture every 30 minutes until the NCO content reacted completely. Stop the reaction, cool down to obtain the hydroxyl-terminated polyureth...

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Abstract

The invention discloses a modified siloxane-terminated polyurethane sealant and a preparation method thereof. The preparation method comprises the following steps: reacting polyether polyol with polyisocyanates to obtain a hydroxy-terminated polyurethane prepolymer; reacting amino siloxane with isocyanate to obtain hydroxy-terminated polyurethane prepolymer; reacting the hydroxy-terminated prepolymer with isocyanate-terminated siloxane to obtain siloxy-terminated polyurethane; reacting a plasticizer, a catalyst, dried inorganic filler and the siloxy-terminated polyurethane; stirring at high speed for 60-90 minutes at the temperature of 60-75 DEG C under a vacuum condition; and cooling to the room temperature and discharging, packing and sealing under vacuum to obtain the siloxane-terminated polyurethane sealant. The prepared siloxane-terminated polyurethane sealant has good stability and large modulus and stretching strength, is high in curing rate at a normal temperature, and can be firmly combined to base materials such as metal and glass without primer.

Description

technical field [0001] The invention relates to the technical field of sealants for automobile windshields, in particular to a silane-modified polyurethane sealant and a preparation method thereof. Background technique [0002] Isocyanate-terminated polyurethane prepolymers can be modified to improve or increase their basic properties by capping the isocyanate groups of the prepolymer with organosilanes. Its characteristic unit structure carbamate (-NH-CO-) alternately contains hard segments and soft segments, endowing polyurethane materials with a multi-phase structure, so polyurethane materials generally have good flexibility and wear resistance, and high strength . Polyurethane prepolymers are widely used in adhesives, coatings and sealants. However, when the isocyanate-terminated polyurethane is cured, it will react with moisture in the air to generate bubbles and even cracks, which will affect the mechanical properties of the polyurethane itself. [0003] Organosilic...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09J175/14C09J11/04C09J11/06
CPCC08K2003/2241C08K2003/265C09J11/04C09J11/06C09J175/14C08K5/12C08K3/26C08K3/22C08K3/04
Inventor 傅和青郭明杰胡恒逢
Owner SOUTH CHINA UNIV OF TECH