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Citric acid chitosan modified waterborne polyurethane and preparation method thereof

A waterborne polyurethane and chitosan modification technology, applied in the field of modified waterborne polyurethane, can solve the problem of high cohesive energy and achieve the effect of improving biodegradability

Active Publication Date: 2020-09-08
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] The molecular structure of polyurethane contains urethane, urea bonds and ionic bonds, which have high cohesive energy and strong adhesion, but there are problems of sustainable development such as green, low carbon and environmental protection.

Method used

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  • Citric acid chitosan modified waterborne polyurethane and preparation method thereof
  • Citric acid chitosan modified waterborne polyurethane and preparation method thereof
  • Citric acid chitosan modified waterborne polyurethane and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Step 1: the preparation of citric acid chitosan:

[0045] Weigh 3.75g of citric acid and 0.63g of sodium hypophosphite in a three-necked flask, add 50g of distilled water to it, shake it up after they are completely dissolved, then weigh 1.5g of chitosan and add it to a three-necked flask, at 105°C React for 3 hours. After the reaction, precipitate with ethanol, wash and filter with suction, place at -55°C for 36 hours in a vacuum freeze-dry, and finally grind and pulverize to obtain powdered citrated chitosan;

[0046] Step 2: Add 30g of dried polytetrahydrofuran ether glycol (PTMG-2000) and 16.7g of isophorone diisocyanate (IPDI) into a three-necked flask, stir evenly, and drop 0.023g of dibutyltin dilaurate (DBTDL) , react at 80°C for 2h; adjust the temperature to 75°C, add 2.3g of dimethylolpropionic acid (DMPA) and 0.93g of 1,4-butanediol (BDO), and continue the reaction for 3h; add absolute ethanol 1.6 g for capping, and react at 70°C for 30 minutes to obtain par...

Embodiment 2

[0050] Step 1: Preparation of Citrated Chitosan

[0051] Weigh 4.5g of citric acid and 0.5g of sodium hypophosphite in a three-necked flask, add 50g of distilled water to it, shake it up after they are completely dissolved, then weigh 1.5g of chitosan and add it to a three-necked flask, at 110°C React for 3 hours. After the reaction, precipitate with ethanol, wash and filter with suction, place at -55°C for 36 hours in a vacuum freeze-dry, and finally grind and pulverize to obtain powdered citrated chitosan;

[0052] Step 2: Add 30g of dried polytetrahydrofuran ether glycol (PTMG-2000) and 20g of isophorone diisocyanate (IPDI) into a three-necked flask, stir evenly, and dropwise add a mass fraction of 0.03g of dibutyltin dilaurate ( DBTDL), reacted at 80°C for 2h; adjusted the temperature to 75°C, added 2.5g dimethylolpropionic acid (DMPA) and 1.0g 1,4-butanediol (BDO), and continued to react for 3h; added anhydrous Block with 2.2g of ethanol and react at 70°C for 30 minutes ...

Embodiment 3

[0056] Step 1: Preparation of Citrated Chitosan

[0057] Weigh 5.3g of citric acid and 0.88g of sodium hypophosphite in a three-necked flask, add 50g of distilled water to it, shake it up after they are completely dissolved, then weigh 1.5g of chitosan and add it to a three-necked flask, at 110°C React for 2.5 hours. After the reaction, precipitate with ethanol, wash and filter with suction, place at -55°C for 36 hours in a vacuum freeze-dry, and finally grind and pulverize to obtain powdered citrated chitosan;

[0058] Step 2: Add 30g of dried polytetrahydrofuran ether glycol (PTMG-2000) and 13.3g of isophorone diisocyanate (IPDI) into a three-necked flask, stir evenly, and drop 0.017g of dibutyltin dilaurate (DBTDL) , react at 80°C for 2h; adjust the temperature to 75°C, add 2.2g dimethylolpropionic acid (DMPA) and 0.86g 1,4-butanediol (BDO), and continue the reaction for 3h; add absolute ethanol 1.0 g for capping, and react at 70°C for 30 minutes to obtain partially blocke...

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Abstract

The invention relates to citrated chitosan modified waterborne polyurethane and a preparation method thereof. Firstly, citrated chitosan is prepared; afterwards, by adopting an internal emulsification method, a partially terminated waterborne polyurethane prepolymer is synthesized according to a stepwise polymerization principle; finally, the partially closed waterborne polyurethane prepolymer is grafted on the citrated chitosan, so that the citrated chitosan modified waterborne polyurethane is obtained. The solid content, the emulsion particle size and the tensile strength of an adhesive film of a waterborne polyurethane emulsion modified by the preparation method are all increased; the modified waterborne polyurethane has favorable biodegradability; the water resistance is also improved; the utilization rate of a biomass resource is improved.

Description

technical field [0001] The invention relates to a modified water-based polyurethane, in particular to a citrated chitosan modified water-based polyurethane and a preparation method thereof. Background technique [0002] The molecular structure of polyurethane contains urethane, urea bonds and ionic bonds, which have high cohesive energy and strong adhesion, but there are problems such as sustainable development of green, low carbon and environmental protection. Since water-based polyurethane uses water as the dispersion medium, the processing process does not require solvents, so it has no pollution to the environment, and the processing process of water-based polyurethane is safe and reliable, the product is safe and environmentally friendly, has no export restrictions, and has good moisture and vapor permeability. [0003] Chitosan is considered as a kind of polymer compound with unique biological activity because of its abundant resources, cheap price and biocompatibility...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G18/75C08G18/66C08G18/48C08G18/64C08G18/32C08G18/34C08G18/12C08J5/18C08L75/08
CPCC08G18/0823C08G18/12C08G18/3206C08G18/348C08G18/4081C08G18/4854C08G18/6484C08G18/6692C08G18/755C08J5/18C08J2375/08C08G18/64
Inventor 任龙芳赵永霞
Owner SHAANXI UNIV OF SCI & TECH