Method for preparing block cationic water-borne polyurethane iron (III) chelates

A technology of block cation and polyurethane iron, which is applied in the field of preparation of block cationic waterborne polyurethane iron chelate, can solve the problems of low introduction rate, cumbersome steps, and many side reactions, and achieve adjustable structure and performance, post-treatment The effect of simplicity and mild reaction conditions

Active Publication Date: 2015-09-30
UNIV OF SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The raw materials for polyurethane reaction are generally isocyanate, macromolecular diols, small molecule diols, and diamine compounds. The introduction of functional groups generally uses diols and diamine functional compounds as chain extenders (binary extenders) chain agent), partially or completely replace the small molecule chain extender, but because the 3-hydroxyl in the 3-hydroxy-4-ketopyridine derivatives reacts with isocyanate, the method of modifying it into a dibasic alcohol chain extender is introduced into the There are many side reactions,

Method used

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  • Method for preparing block cationic water-borne polyurethane iron (III) chelates
  • Method for preparing block cationic water-borne polyurethane iron (III) chelates

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] 33.9 grams of PPG (M n=2000) was dehydrated at 110°C for 0.5-1.5 hours, then added 26.4 grams of IPDI, reacted at 90°C for 2 hours, added 3.5 grams of DEG, reacted at 70°C for 2 hours, then added dropwise 7.6 grams of MDEA and 40mL at 50°C The mixed solution of butanone is dropped within 0.5-1 hour. After the drop, keep 65°C for 3 hours, add 0.045 grams of BHT and 1.2 grams of HEA and react at 60°C for 1 hour to obtain a double bond-terminated polyurethane prepolymer; Add 0.05 g of AIBN and 2.1 g of glycidyl methacrylate to the double bond-terminated polyurethane prepolymer, add 100 mL of butanone and react at 75 °C for 2 hours, add 2.8 g of 1-aminoethyl-2-methyl-3- Hydroxy-4-(1H)-pyridone reaction 75°C for 2 hours, then cool down to 30°C, add 3.98 g of acetic acid for 1-5 minutes, then add 181 mL of water under high-speed shear, stir for 5-30 minutes, and the reaction product At 45°C and 0.01MPa vacuum conditions, butanone was removed from the solvent to obtain a soli...

Embodiment 2

[0032] 50.0 g of PBA (M n =2000) was dehydrated at 110°C for 0.5-1.5 hours, then added 24.1 grams of TDI, reacted at 80°C for 2 hours, added 2.8 grams of BDO, reacted at 70°C for 2 hours, then added dropwise 9.0 grams of MDEA and 40 mL at 50°C The mixed solution of butanone is dropped within 0.5-1 hour. After the drop is completed, it is kept at 60°C for 3 hours, and 0.025 grams of HQ and 1.7 grams of HEMA are added to react at 60°C for 1 hour to obtain a double bond-terminated polyurethane prepolymer; Add 0.08 g of AIBN and 2.0 g of glycidyl methacrylate to the double bond-terminated polyurethane prepolymer, add 100 mL of methyl ethyl ketone and react at 65 °C for 2 hours, then add 2.37 g of 1-aminoethyl-2-methyl-3 -Hydroxy-4-(1H)-pyridone reaction at 75°C for 2 hours, then cool down to 30°C, add 4.9 g of acetic acid for 1-5 minutes, then add 215 mL of water under high-speed shear, stir for 5-30 minutes The product was desolventized butanone under 45°C and 0.01MPa vacuum con...

Embodiment 3

[0034] 50.0 grams of PPG (M n =2000) was dehydrated at 110°C for 0.5-1.5 hours, then added 38.87 grams of IPDI, reacted at 90°C for 2 hours, added 2.6 grams of EG, reacted at 70°C for 2 hours, then added dropwise 12.0 grams of MDEA and 40mL at 50°C The mixed solution of butanone is dropped within 0.5-1 hour. After the drop is completed, it is kept at 65°C for 3 hours, and 0.07 grams of BQ and 1.8 grams of HEMA are added to react at 60°C for 1 hour to obtain a double bond-terminated polyurethane prepolymer; Add 0.056 g of AIBN and 5.6 g of glycidyl methacrylate to the double bond-terminated polyurethane prepolymer, add 100 mL of butanone and react at 65 °C for 2 hours, then add 6.6 g of 1-aminoethyl-2-methyl-3 -Hydroxy-4-(1H)-pyridone reacted at 75°C for 2 hours, then cooled to 30°C, added 7.2 g of acetic acid for 1-5 minutes, then added 274 mL of water under high-speed shear, and stirred for 5-30 minutes. The product was desolventized butanone under 45°C and 0.01MPa vacuum co...

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Abstract

The invention discloses a method for preparing block cationic water-borne polyurethane iron (III) chelates. The method comprises reacting diisocyanate with macromolecular dibasic alcohol, micromolecular dibasic alcohol and a hydrophilic chain extender, adding an end-capping reagent to obtain double bond end-capped polyurethane prepolymer, adding glycidyl methacrylate to carry out the copolymerization reaction, adding amino-containing 3-hydroxyl-4-pyridone derivatives to carry out the ring-opening reaction with epoxy groups, and performing covalent linkage to the two ends of polyurethane to obtain the block cationic water-borne polyurethane iron (III) chelates. The method avoids the side reaction between 3 hydroxyl groups and isocyanate, the reaction conditions are mild, the aftertreatment is simple, the obtained micromolecular chelates are located on side chains at the two ends of a chain of polyurethane, the content is adjustable (0.1-15wt%); and the obtained macromolecular chelates can be dissolved in water, acetone, butanone, N,N-dimethylformamide and dimethylsulfoxide.

Description

1. Technical field [0001] The invention relates to a preparation method of a block cationic waterborne polyurethane iron (III) chelate, belonging to the technical field of waterborne polyurethane materials. 2. Background technology [0002] At present, polymer iron chelates are attracting more and more attention, and polymer iron chelates are widely used in water treatment, pollution control, metal ion recovery, active packaging and analytical chemistry and other fields. Because kojic acid, maltol and other pyrone derivatives and 3-hydroxy-4-pyridone derivatives have good iron chelating ability, the raw materials are easy to get, and the price is cheap, so they are often used to synthesize high molecular weight iron chelate thing. [0003] The use of 1-(β-acryloylethyl)-3-hydroxyl-2-methyl- 4-(1H)-pyridone (AHMP), N,N-dimethylacrylamide, N,N'-vinylbisacrylamide yields a polymer containing 3-hydroxy-4-pyridones, which Polymers are insoluble and infusible. Similarly, the u...

Claims

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Application Information

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IPC IPC(8): C08F283/00C08F220/32C08F8/32C08G18/67C08G18/66C08G18/12
Inventor 张兴元李军配杨树张国庆
Owner UNIV OF SCI & TECH OF CHINA
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