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A kind of organosilicon modified polyether-polycarbonate waterborne polyurethane and preparation method thereof

A water-based polyurethane and polycarbonate technology, applied in the field of silicone-modified polyether-polycarbonate water-based polyurethane and its preparation, can solve the problems of poor water resistance and heat resistance, insufficient mechanical strength, etc., and achieve the effect of improving water resistance

Active Publication Date: 2021-02-19
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] However, the carbon dioxide-based waterborne polyurethane coating prepared in the above technical scheme has shortcomings such as insufficient mechanical strength and poor water and heat resistance.

Method used

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  • A kind of organosilicon modified polyether-polycarbonate waterborne polyurethane and preparation method thereof
  • A kind of organosilicon modified polyether-polycarbonate waterborne polyurethane and preparation method thereof
  • A kind of organosilicon modified polyether-polycarbonate waterborne polyurethane and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0088] Step 1: Preparation of silicone-modified polyether-polycarbonate polyol

[0089] Before starting the reaction, a 100 mL stainless steel autoclave was cleaned, and vacuum-dried at 80° C. for 2 h to remove water in the autoclave. Add 34.08g (0.587mol) of propylene oxide, 10.4g (0.044mol) of KH560, 10.0g (0.025mol) of PPG-400 and 20mg of zinc-cobalt double metal cyanide complex into the reactor, and fill it with a small amount of CO 2 and warmed up to 100°C, followed by adjustment of CO 2 Pressure to 5MPa reaction 12h. After the reaction, the reactor was cooled in an ice-water bath, and the gas in the reactor was slowly released at normal temperature. The crude product was dissolved in 20 mL of dichloromethane, and then precipitated in 150 mL of n-hexane to obtain a silicone-modified polyether-polycarbonate polyol.

[0090] After testing, the number average molecular weight of the product is 1500g / mol, the PDI is 1.7, the carbonate content is 13.5 mol%, and the organosi...

Embodiment 2

[0095] Step 1: Preparation of silicone-modified polyether-polycarbonate polyol

[0096] The preparation method is the same as step 1 in Example 1, except that the mass of PPG-400 is changed to 8.1g (0.02mol) to obtain a silicone-modified polyether-polycarbonate polyol with a number average molecular weight of 2200g / mol, PDI It is 2.0, the content of carbonate is 17.1 mol%, and the content of organic silicon segment is 4.1 mol%.

[0097] Step 2: Preparation of silicone-modified polyether-polycarbonate waterborne polyurethane

[0098] In a 250mL four-neck flask, add 10g (0.0045mol) of the silicone-modified polyether-polycarbonate polyol prepared in step 1, 0.79g (0.0056mol) of dimethylol propionic acid and 0.001g of dibutyltin dilaurate Catalyst, after heating up to 80°C, slowly add 5g (0.022mol) isophorone diisocyanate dropwise into the flask, react for 2h after the dropwise addition, cool down to 40°C, add 0.60g triethylamine (0.0056mol), react 0.5h, add 12.0g deionized wate...

Embodiment 3

[0101] Step 1: Preparation of silicone-modified polyether-polycarbonate polyol

[0102] The preparation method is the same as step 1 in Example 1, except that the mass of PPG-400 is changed to 5.9g (0.015mol) to obtain a silicone-modified polyether-polycarbonate polyol with a number average molecular weight of 3100g / mol, PDI 2.2, the carbonate content is 21.9 mol%, and the organosilicon segment content is 4.6 mol%.

[0103] Step 2: Preparation of silicone-modified polyether-polycarbonate waterborne polyurethane

[0104] In a 250mL four-necked flask, add 12g (0.0039mol) of the silicone-modified polyether-polycarbonate polyol prepared in step 1, 0.89g (0.0063mol) of dimethylol propionic acid and 0.001g of dibutyltin dilaurate catalyst After the temperature was raised to 80°C, 5g (0.022mol) of isophorone diisocyanate was slowly added dropwise to the flask. After the dropwise addition, it was reacted for 2 hours, and the temperature was lowered to 40°C. 0.67g (0.0063mol) of triet...

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Abstract

The invention discloses a method for preparing silicone-modified polyether-polycarbonate waterborne polyurethane, comprising: (1) mixing epoxy compound, carbon dioxide, initiator, catalyst A and epoxy-containing silane coupling agent , prepared by reaction to obtain silicone-modified polyether-polycarbonate polyol; the initiator is selected from polyhydroxy small molecules or polyhydroxy polymers; (2) the silicone-modified polyether-polyol prepared in step (1) Polycarbonate polyol, diisocyanate, polyhydric hydrophilic chain extender and catalyst B are stirred and reacted to prepare a polyurethane prepolymer with NCO groups at the end, which is then prepared by alkaline neutralizer reaction and chain extension reaction in sequence Obtain silicone-modified polyether-polycarbonate waterborne polyurethane. The silicone-modified polyether-polycarbonate waterborne polyurethane prepared by the method has excellent tensile strength, heat resistance and water resistance.

Description

technical field [0001] The invention belongs to the technical field of water-based polyurethane, and in particular relates to a silicone-modified polyether-polycarbonate water-based polyurethane and a preparation method thereof. Background technique [0002] With the development and progress of society, petroleum resources are being consumed and depleted day by day, and the utilization of petrochemical resources will also cause environmental pollution. Carbon dioxide is an abundant and cheap carbon-resource, and the effective use of carbon dioxide is a breakthrough for the world to get rid of dependence on petroleum resources. [0003] The polyols used in traditional waterborne polyurethanes are mainly polyester polyols and polyether polyols. Polyester polyurethanes have poor hydrolysis resistance, while polyether polyurethanes have poor mechanical properties. Therefore, polyether-polycarbonate obtained by ring-opening copolymerization of carbon dioxide and propylene oxide...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G18/66C08G18/46C08G18/34C08G18/32
CPCC08G18/3228C08G18/348C08G18/4692C08G18/6659
Inventor 范宏马中柱张先伟任杰
Owner ZHEJIANG UNIV
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