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Preparation method of waterborne polyurethane based on glycidyl methacrylate

A technology of glycidyl ester and methacrylic acid, applied in the field of water-based polyurethane preparation, can solve the problems of difficult retention, unstable emulsion, and inability to further solidify, and achieve the effects of small particle size, narrow particle size distribution, and strong processing performance.

Active Publication Date: 2015-10-14
UNIV OF SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The object of the present invention is to provide a kind of water-based polyurethane preparation method based on glycidyl methacrylate, the glycidyl methacrylate containing epoxy group is through free radical polymerization, and the chain segment of introducing polyurethane chain obtains epoxy group Block cationic water-based polyurethane with controllable content to solve the problems of unstable emulsion caused by epoxy groups in water-based polyurethane system, which is difficult to retain and cannot be further cured

Method used

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  • Preparation method of waterborne polyurethane based on glycidyl methacrylate
  • Preparation method of waterborne polyurethane based on glycidyl methacrylate
  • Preparation method of waterborne polyurethane based on glycidyl methacrylate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027]Dehydrate 47.2 grams of PPG (Mn=2000) at 100°C for 1.5 hours, then add 36.8 grams of IPDI, react at 90°C for 2 hours, add 4.8 grams of DEG, react at 70°C for 2 hours, and then add 11.0 grams at 50°C dropwise Add 0.045 g of BHT and 1.1 g of HEA to keep the reaction at 60°C for 1 hour to obtain a polyurethane with a double bond at the end group. Prepolymer; then add 0.05 g of AIBN and 3.0 g of glycidyl methacrylate to the polyurethane prepolymer containing double bonds at the end group, add 100 mL of methyl ethyl ketone, react at 60-75 ° C for 3 hours, cool down to 30 ° C, add After reacting 5.6 grams of acetic acid for 1-5 minutes, 242 mL of water was added under high-speed shearing, and after stirring for 5-30 minutes, the reaction product was desolventized butanone at 45 ° C and 0.01 MPa vacuum to obtain a solid content of 30 wt %. Block cationic water-based polyurethane emulsion Epoxy-CWPU with a glycidyl methacrylate content of 2.9 wt%.

[0028] In order to facilitat...

Embodiment 2

[0031] 50.0 g of PBA (M n =2000) dehydration at 100-120°C for 0.5-1.5 hours, then add 25.0 grams of TDI, add 2.7 grams of BDO after reacting at 80°C for 2 hours, react at 70°C for 2 hours, then at 50°C within 0.5-1 hour Add dropwise a mixed solution of 10.0 g MDEA and 40 mL methyl ethyl ketone, keep at 60 °C for 3 hours, add 0.035 g of HQ and 0.9 g of HEMA, and react at 60 °C for 1 hour to obtain a polyurethane prepolymer with double bonds at the end group; Add 0.03 g of AIBN and 5.1 g of glycidyl methacrylate to the polyurethane prepolymer containing double bonds, add 100 mL of butanone and react at 60-75 °C for 3 hours, then cool down to 30 °C, add 5.06 g of acetic acid for 5 minutes 219mL of water was added under stirring, and after stirring for 5-30 minutes, the reaction product was desolventized butanone under 45°C and 0.01MPa vacuum conditions to obtain a solid content of 30wt% and a glycidyl methacrylate content of 5.4wt%. Block cationic water-based polyurethane emulsi...

Embodiment 3

[0033] Dehydrate 50.0 grams of PTMG (Mn=2000) at 110°C for 0.5-1.5 hours, then add 25.3 grams of HDI, react at 90°C for 2 hours, add 3.3 grams of EG, react at 70°C for 2 hours, and then add 0.5 grams at 50°C Add a mixed solution of 8.0 g MDEA and 40 mL methyl ethyl ketone dropwise within 1 hour, keep the reaction at 65 °C for 3 hours, add 0.07 g BQ and 1.0 g HPA, and react at 60 °C for 1 hour to obtain a polyurethane prepolymer with double bonds in the terminal group; then Add 0.09 g of AIBN and 6.0 g of glycidyl methacrylate to the polyurethane prepolymer with double bonds in the terminal group, add 100 mL of methyl ethyl ketone and react at 70 ° C for 3 hours, then cool down to 30 ° C, add 4.03 g of acetic acid for 5 minutes and react Add 220mL of water under high-speed shearing, stir for 5-30 minutes, and remove the solvent butanone from the reaction product at 45°C and 0.01MPa vacuum to obtain a solid content of 30wt% and a glycidyl methacrylate content of 6.4 wt % block c...

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Abstract

The invention discloses a preparation method of waterborne polyurethane based on glycidyl methacrylate. The preparation method comprises the following steps: firstly carrying out a reaction between diisocyanate and macromolecular dihydric alcohol, micromolecular dihydric alcohol and a hydrophilic chain extender; adding an end-capping reagent to obtain a double bond-terminated polyurethane prepolymer; and carrying out copolymerization by adding glycidyl methacrylate so as to obtain epoxy group-controllable block cationic waterborne polyurethane. According to the method, the epoxy group is bonded to polyurethane through a chemical bond to form a single component system which is convenient to use, can be used along with amines, polyatomic acid or polyisocyanate compounds for cure-crosslinking, modification and the like and has stronger machinable property. The synthesized block cationic waterborne polyurethane has smaller particle size, narrower particle size distribution and higher emulsion storage stability.

Description

1. Technical field [0001] The invention relates to a preparation method of water-based polyurethane based on glycidyl methacrylate, belonging to the technical field of water-based polyurethane materials. 2. Background technology [0002] The epoxy group is a three-membered ring composed of two carbon atoms and one oxygen atom. Due to the high reactivity of the epoxy group, it can react with amino groups and other groups under mild conditions (weak acid or weak base, room temperature). Under certain conditions, it can also react with nucleophilic reagents such as carboxylic acid and halogen, which can realize the functions of material curing, modification, covalent connection between carrier and ligand molecule, etc. Due to the characteristics of safe production, transportation and use, no pollution to the environment, and good comprehensive performance of water-based polyurethane, it has gradually replaced solvent-based polyurethane in recent years. Epoxy-modified waterborn...

Claims

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Application Information

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IPC IPC(8): C08F290/06C08F220/32C08G18/67C08G18/48C08G18/42
Inventor 张兴元李军配杨树张国庆
Owner UNIV OF SCI & TECH OF CHINA
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