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Preparation method for amino-terminated hyperbranched polysiloxane modified waterborne polyurethane

An amino-terminated hyperbranched, water-based polyurethane technology is applied in the field of preparation of amino-terminated hyperbranched polysiloxane-modified water-based polyurethane, and can solve the problems of low emulsion stability, severe phase separation, insufficient mechanical properties and cohesion, etc. , to achieve the effect of increasing interaction, good mechanical properties and bonding properties, and increasing the compatibility of two phases

Active Publication Date: 2019-08-23
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The invention provides a method for preparing amino-terminated hyperbranched polysiloxane-modified waterborne polyurethane to overcome the problems of severe phase separation, low emulsion stability and insufficient mechanical properties and cohesiveness in the prior art

Method used

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  • Preparation method for amino-terminated hyperbranched polysiloxane modified waterborne polyurethane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Step 1: HPSi-NH 2 preparation of

[0018] Add 3.6g of water to 22.14g of kh550, and add 20mL of ethanol to the system, slowly add 10.8g of TMCS dropwise under stirring conditions, and continuously reflux and stir at 50°C for 5h. After the reaction, adjust with sodium ethylate The pH of the system is neutral, and the solid salt generated is removed by high-speed centrifugation, and finally the small molecule ethanol is removed by a rotary evaporator to obtain the amino-terminated hyperbranched polysiloxane HPSi-NH 2 ;

[0019] Step 2: Preparation of HSiPU

[0020] First, add 20g of 1.4-butylene adipate (Mn=2000) and 8.89g of isophorone diisocyanate into a dry three-necked flask after vacuum dehydration, stir evenly, and add 3 drops of catalyst dilauric acid Dibutyltin, react at 75°C for 1.5h; add 1.45g of dimethylolpropionic acid, continue to react for 2.5h, until the -NCO content in the prepolymer remains constant, and obtain a polyurethane prepolymer (PPU);

[0021...

Embodiment 2

[0024] Step 1: HPSi-NH 2 preparation of

[0025] Add 1.8g of water to 22.14g of kh550, and add 20mL of ethanol, slowly add 10.8g of TMCS under stirring conditions, continuously reflux and stir at 50°C for 6h, adjust the pH of the solution to neutral with sodium ethoxide, and centrifuge The salt generated by the reaction was removed by a machine, and the small molecule ethanol was removed by a rotary evaporator to obtain the amino-terminated hyperbranched polysiloxane HPSi-NH 2 ;

[0026] Step 2: Preparation of HSiPU

[0027] First, add 10g of polytetrahydrofuran ether glycol (Mn=1000) and 5.22g of toluene diisocyanate into a dry three-necked flask after vacuum dehydration, stir evenly, add 3 drops of catalyst dibutyltin dilaurate, and react at 75°C 1.5h; add 1.33g dimethylolpropionic acid, continue to react for 2.5h, until the -NCO content in the prepolymer is constant, and obtain the polyurethane prepolymer PPU;

[0028] Then add 0.73g of butylamine to the obtained PPU an...

Embodiment 3

[0030] Step 1: HPSi-NH 2 preparation of

[0031] Add 3.6g of water to 22.14g of kh550, and add 30mL of ethanol, slowly add 15.0g of TMCS under stirring conditions, keep stirring and reflux reaction at 55°C for 5h, adjust the pH of the system to neutral with sodium ethoxide, and centrifuge The generated solid salt was removed by machine, and small molecule ethanol was removed by rotary evaporator to obtain amino-terminated hyperbranched polysiloxane HPSi-NH 2 ;

[0032] Step 2: Preparation of HSiPU

[0033] Add 20g of polyethylene glycol (Mn=2000) and 5.04g of hexamethylene diisocyanate after vacuum dehydration into a dry three-necked flask, stir evenly, add 3 drops of catalyst dibutyltin dilaurate, at 75°C React for 1 hour; add 1.60 g of dimethylolpropionic acid and continue the reaction for 2 hours until the -NCO content in the prepolymer remains constant to obtain PPU;

[0034] Then add 2.40g of pentaerythritol triacrylate to the obtained PPU, react at 80°C for 2h, cool ...

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Abstract

The invention relates to a preparation method for amino-terminated hyperbranched polysiloxane modified waterborne polyurethane. The preparation method comprises the following steps: with 3-aminopropyltriethoxysilane (kh550) and trimethylchlorosilane (TMCS) as raw materials, subjecting 3-aminopropyltriethoxysilane (kh550) and trimethylchlorosilane (TMCS) to hydrolytic condensation so as to prepareamino-terminated hyperbranched polysiloxane (HPSi-NH2); and with the HPSi-NH2 as a cross-linking agent, allowing the HPSi-NH2 to react with a polyurethane prepolymer (PPU), carrying out branching andchain extension so as to prepare the amino-terminated hyperbranched polysiloxane modified waterborne polyurethane (HSiPU), and adding an end-capping agent during synthesis so as to control the degreeof the reaction at the same time. Thus, modified waterborne polyurethane has the performance advantages of traditional organosilicone waterborne polyurethane; meanwhile, phase separation of organosilicone modified waterborne polyurethane is reduced; mechanical properties and bonding performance of the product are increased; and an obtained emulsion has excellent comprehensive performance, and canbe used as a leather adhesive or a water-resistant coating.

Description

technical field [0001] The invention relates to the technical field of organosilicon polymers, in particular to a method for preparing amino-terminated hyperbranched polysiloxane-modified waterborne polyurethane. Background technique [0002] With the promotion of environmental protection, it has become a trend to replace solvent-based polyurethane with water-based polyurethane. The modification of waterborne polyurethane for the deficiencies in water resistance and heat resistance has attracted widespread attention. Silicone has the characteristics of hydrophobicity, heat resistance, and stable chemical properties. The preparation method of traditional silicone-modified waterborne polyurethane is briefly described as follows: linear silicone is used as a mixed soft segment to form silicone block modified waterborne polyurethane; Silicone grafting forms silicone side chain waterborne polyurethane; some people modify waterborne polyurethane with small molecule kh550 through ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G18/61C08G18/28C08G18/48C08G18/73C08G18/66C08G18/76C08G18/75C08G18/42C08G77/04C08G77/06C08G77/388
CPCC08G18/282C08G18/2865C08G18/348C08G18/4238C08G18/4833C08G18/4854C08G18/61C08G18/6659C08G18/672C08G18/73C08G18/755C08G18/7614C08G77/04C08G77/06C08G77/388C08G18/6692C08G18/0823
Inventor 任龙芳牛巧宣
Owner SHAANXI UNIV OF SCI & TECH
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