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Silane terminated polyurethane oligomer and its preparation method

A polyurethane oligomer and silane-terminated technology, which is applied in the field of modified polyurethane, can solve the problems of difficult synthesis process, difficult thick coating process, easy occurrence of gel and the like, and achieves convenient construction, simple and easy preparation conditions, and easy availability of raw materials. Effect

Active Publication Date: 2014-07-09
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to prepare a kind of active secondary amino silane and use it to carry out capping modification to polyurethane prepolymer, while retaining the main chain of polyurethane, make the end group change from isocyanate group to siloxyl group, solve the current problem The synthesis process of silane-modified polyurethane is not easy to operate, it is prone to gelation, and the traditional one-component isocyanate-terminated polyurethane product releases CO when it is cured. 2 Disadvantages such as easy foaming and difficult thick coating process

Method used

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  • Silane terminated polyurethane oligomer and its preparation method
  • Silane terminated polyurethane oligomer and its preparation method
  • Silane terminated polyurethane oligomer and its preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] (1) Preparation of secondary aminosilane A: In terms of parts by mass, put 22.14 parts of γ-aminopropyltriethoxysilane in the reaction flask, and then according to the molar ratio of 1:1, slowly Add 22.03 parts of γ-(2,3-glycidoxy)propylmethyldimethoxysilane dropwise, and then control the system to stir and react at 20°C for 12 hours to obtain secondary aminosilane A;

[0045] (2) Dehydrate and degas 17 parts of polyether polyol (N220, Foshan Shunde Xingzhou Synthetic Materials Co., Ltd.) at 110°C under vacuum for 4 hours, then cool down to 70°C, and then add 3 parts of 1,6-hexyl Diol, 12 parts of xylene, 9 parts of TDI, and 0.2 parts of dibutyltin dilaurate were added to polyether polyol N220, and high-purity nitrogen was introduced as a reaction protection gas, stirred evenly, and then kept at 80°C for 4 hours. One-step synthesis of isocyanate-terminated polyurethane prepolymers;

[0046] (3) React the isocyanate-terminated polyurethane prepolymer synthesized in step...

Embodiment 2

[0050] (1) Preparation of secondary aminosilane B: In terms of mass fraction, put 22.14 parts of γ-aminopropylmethyldiethoxysilane in the reaction flask, and then according to the molar ratio of 1:1, under the condition of stirring Slowly add 29.04 parts of γ-methacryloxypropyltriethoxysilane dropwise, and then control the system to stir and react at 60°C for 168 hours to obtain secondary aminosilane B;

[0051] (2) Dehydrate and degas 17 parts of polyether polyol (N220, Foshan Shunde Xingzhou Synthetic Materials Co., Ltd.) at 110°C for 3 hours, then cool down to 70°C, and then add 2.25 parts of 1,4-butyl Diol, 12 parts of butyl acetate, 9 parts of TDI, and 0.4 parts of dibutyltin dilaurate were added to polyether polyol N220, and high-purity nitrogen gas was introduced as a reaction protection gas, stirred evenly, and then kept at 85°C for 3.5 h, Synthesis of isocyanate-terminated polyurethane prepolymer by one-step method;

[0052] (3) react the isocyanate-terminated polyur...

Embodiment 3

[0055] (1) Preparation of secondary aminosilane C: in terms of mass fraction, put 17.93 parts of γ-aminopropyltrimethoxysilane in the reaction flask, and slowly dropwise under the condition of stirring according to the molar ratio of 1:1 Add 24.83 parts of γ-methacryloxypropyltrimethoxysilane, and then control the system to stir and react at 50°C for 120h to obtain secondary aminosilane C;

[0056] (2) Dehydrate and degas 17 parts of polyether polyol (N220, Foshan Shunde Xingzhou Synthetic Materials Co., Ltd.) at 120°C for 3 hours, then cool down to 60°C, and then add 2.25 parts of 1,4-butyl Diol, 12 parts of ethyl acetate, 13 parts of MDI, and 0.6 parts of dibutyltin dilaurate were added to polyether polyol N220, and high-purity nitrogen was introduced as a reaction protection gas, stirred evenly, and then kept at 85°C for 3 hours. , by one-step synthesis of isocyanate-terminated polyurethane prepolymer;

[0057] (3) React the isocyanate-terminated polyurethane prepolymer sy...

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Abstract

The invention discloses a silane terminated polyurethane oligomer and its preparation method. The method comprises the following steps: dehydrating polyether polyol under vacuum condition, degassing, and then cooling to the temperature of 50-100 DEG C; adding a micromolecule chain extender through drying treatment, a solvent through drying treatment, diisocyanate and a catalyst in polyether polyol in order, introducing high purity nitrogen as reaction protection gas, uniformly stirring, insulating at the temperature of 50-90 DEG C, and synthesizing the terminated isocyanate polyurethane prepolymer; reacting the terminated isocyanate polyurethane prepolymer and secondary amine silane, stirring at the temperature of 10-90 DEG C under the protection of high purity nitrogen, completing the reaction until no isocyanic acid is exsited in a system through titration, and removing bubbles under vacuum to obtain the silane terminated polyurethane oligomer. The process for terminating and modifying the polyurethane prepolymer by secondary amine silane is easy to controlled, no gelation phenomenon is generated, and the reappearance is good while the product is prepared.

Description

technical field [0001] The invention relates to modified polyurethane, in particular to a silane-terminated polyurethane oligomer that can be used in the fields of coatings, sealants, adhesives and the like and a preparation method thereof. Background technique [0002] Polyurethane (PU) has good high elasticity, low temperature flexibility, wear resistance and high mechanical strength, and is widely used in construction, automobile, machinery, electronics and other fields. Polyurethane is formed by polyaddition of diisocyanate and polyol as the basic raw materials. Because the ratio of reactants can be adjusted in a wide range, the content of soft and hard segments of the synthesized polyurethane can be adjusted according to the needs of the product. Therefore, polyurethane products have various forms and are used in polyurethane coatings, sealing Glues, adhesives, synthetic fibers, foams and other fields can find their uses. [0003] In recent years, more and more studies...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G18/66C08G18/48C08G18/32C08G18/38C08G18/12
CPCC08G18/12C08G18/6674C08G18/6677C08G2190/00C08G18/3893
Inventor 马文石杨芳邓思荣
Owner SOUTH CHINA UNIV OF TECH
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