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Preparation method for organosilicon-modified crosslinking polyurethane emulsion

A technology of polyurethane emulsion and silicone, which is applied in the field of preparation of silicone-modified cross-linked polyurethane emulsion, which can solve the problems of expensive alkoxy silicone oil, high unit cost of emulsion, and reduced electron cloud density, and achieve excellent low temperature resistance, unit Low cost, good adhesion effect

Inactive Publication Date: 2013-11-06
高明志
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the preparation of silicone-modified polyurethane emulsion mainly adopts two methods, one is to react with polyisocyanate with hydroxyl silicone oil as raw material, because -OH in hydroxyl silicone oil is directly connected with silicon atom, and the existence of empty p orbital of silicon atom, The electron cloud density on the hydroxyl O atom is reduced, the reactivity is reduced, it is difficult to react with -NCO, and the Si-O-C bond formed is easy to hydrolyze, so the emulsion obtained by this method has poor stability and is easy to float oil
Another method is to use alkanol silicone oil as raw material. The modified emulsion prepared by this method has no Si-O-C bonds that are easy to hydrolyze, so the emulsion has good stability, but the alkoxy silicone oil is expensive, so the unit cost of the prepared emulsion is high.

Method used

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  • Preparation method for organosilicon-modified crosslinking polyurethane emulsion
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  • Preparation method for organosilicon-modified crosslinking polyurethane emulsion

Examples

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Embodiment 1

[0024] Embodiment 1: Preparation of organosilicon-modified cross-linked polyurethane emulsion

[0025] In a 250ml there-necked flask with a reflux condenser and a thermometer, add toluene diisocyanate (TDI) 34g, the number average molecular weight after vacuum dehydration is 2000, and the hydroxyl value is equal to polyhexamethylene adipate diol of 55mgKOH / g 100g, react at 90°C constant temperature for 1.5h under mechanical stirring; cool down to 80°C, add dimethylolpropionic acid (DMPA) 5.0g, trimethylolpropane (TMP) 2.0g, acetone 20ml and continue to react for 1h, to obtain Hydrophilic modified PU prepolymer; add 40ml of acetone, wait until the system cools down to about 40°C, add 7.5g of diethylene glycol (DEG), 0.1g of dibutyltin dilaurate, and react to NCO at 60°C The content reaches the theoretical value (determined by the standard di-n-butylamine titration method); cool down to about 30°C, add 3g of aminopropyltriethoxysilane (KH-550) and 6g of hydroxyl silicone oil wit...

Embodiment 2

[0026] Embodiment 2: Preparation of organosilicon-modified cross-linked polyurethane emulsion

[0027] In a 250ml there-necked flask with a reflux condenser and a thermometer, add 39g of toluene diisocyanate (TDI), and the number-average molecular weight after vacuum dehydration is 2000, and the hydroxyl value is equal to polyhexamethylene adipate diol of 55mgKOH / g 100g, 5.6g of dimethylolpropionic acid (DMPA), react at a constant temperature of 80°C for 2h under mechanical stirring; add 40ml of acetone, wait for the system to cool down to about 40°C, add 8.5g of diethylene glycol (DEG), Dibutyltin dilaurate 0.1g, react at 60°C until the NCO content reaches the theoretical value (determined by standard di-n-butylamine titration method); cool down to about 30°C, add aminopropyltriethoxysilane (KH-550 ) 4g, 10g of hydroxyl silicone oil with a number average molecular weight of 1000, reacted at 40°C for 1h, added 4.2g of triethylamine under the action of high shear force at 800 r...

Embodiment 3

[0028] Embodiment 3: Preparation of organosilicon-modified cross-linked polyurethane emulsion

[0029]In a 250ml three-neck flask with a reflux condenser and a thermometer, add 38g of isophorone diisocyanate (IPDI), polytetrahydrofuran diol (PTMG) with a number average molecular weight of 2000 and a hydroxyl value equal to 55mgKOH / g after vacuum dehydration 100g, react at a constant temperature of 90°C for 2.5h under mechanical stirring; cool down to 80°C, add 6.5g of dimethylolpropionic acid (DMPA), 5.2g of trimethylolpropane (TMP), N,N-dimethylolpropane 20ml of formamide continued to react for 1 hour to obtain a hydrophilic modified PU prepolymer; add 60ml of acetone, wait for the system to cool down to about 40°C, add 4.5g of 1,4-butanediol (BDO) and 1.5g of ethylene glycol, 0.1 g each of dibutyltin dilaurate and stannous octoate, and 40 ml of N, N-dimethylformamide were reacted at 60 ° C until the NCO content reached the theoretical value (determined by standard di-n-butyl...

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Abstract

A disclosed preparation method for an organosilicon-modified crosslinking polyurethane emulsion is characterized in that: employing diisocyanate, an oligomer polyol, a hydrophilic chain extender and a chain extender to prepare a polyurethane prepolymer, then using a silane coupling agent for end sealing, then adding hydroxyl silicone oil, after reaction, performing cooling, emulsification and pressure-reducing desolvation to obtain the organosilicon-modified crosslinking polyurethane emulsion. According to the preparation method, the silane coupling agent not only helps to combine organosilicon and polyurethane, but also helps to substantially improve crosslinking degree of the material as a cross-linking agent. The emulsion prepared by the invention is good in stability, green and environment-friendly; and the prepared polyurethane film has the advantages of high mechanical strength, low-temperature resistance, good water proofness and the like, and is widely applicable to the fields of paints, fabric coating glues, leather finishing agents, adhesives and the like.

Description

technical field [0001] The invention relates to the technical field of preparation of polymer materials, in particular to a preparation method of organosilicon-modified cross-linked polyurethane emulsion. Background technique [0002] With the enhancement of people's awareness of environmental protection and the promulgation of various environmental protection regulations, the trend of water-based resins is becoming more and more intense. Water-based polyurethane has the excellent wear resistance, toughness and adhesion of traditional solvent-based polyurethane, but its weather resistance, water resistance and hand feeling are poor. At present, the methods to improve the performance of water-based polyurethane materials mainly include cross-linking modification and composite modification. Crosslinking modification includes methods such as internal crosslinking, external crosslinking, and self-crosslinking. Internal crosslinking is the addition of trifunctional or multifunc...

Claims

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Application Information

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IPC IPC(8): C08G18/65C08G18/61C08G18/38
Inventor 高明志
Owner 高明志
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