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A kind of high oxygen barrier waterborne polyurethane/montmorillonite nanocomposite emulsion and its preparation method

A water-based polyurethane and nano-composite technology, applied in the direction of polyurea/polyurethane coatings, coatings, fire-retardant coatings, etc., can solve the problems of insignificant increase of MMT interlayer spacing, limited dispersion of modified MMT, etc., and achieve mechanical properties. The effect of improving, enhancing barrier properties and improving compatibility

Active Publication Date: 2021-07-27
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, usually small molecule modifiers have no obvious effect on increasing the interlayer spacing of MMT, and the dispersibility of modified MMT in water is limited.

Method used

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  • A kind of high oxygen barrier waterborne polyurethane/montmorillonite nanocomposite emulsion and its preparation method
  • A kind of high oxygen barrier waterborne polyurethane/montmorillonite nanocomposite emulsion and its preparation method
  • A kind of high oxygen barrier waterborne polyurethane/montmorillonite nanocomposite emulsion and its preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] The preparation of polyethylenimine (Mw=25000) modified montmorillonite dispersion liquid is as follows:

[0053] Weigh 1.0 g of montmorillonite MMT, add 200 mL of distilled water to make 0.5 wt % montmorillonite dispersion, stir at room temperature (stirring speed: 300 rpm) for 24 h, and ultrasonically (power: 300 W) disperse for 30 min. Weigh 2.16g polyethyleneimine, configure 25g aqueous solution in a beaker at normal temperature and stir (stirring speed is 150rpm) for 2h; The dropping time is controlled at 30 minutes, and the reaction is 12 hours. After the reaction is completed, naturally cool to room temperature and centrifuge at 8000-12000rpm at high speed; then wash and centrifuge with deionized water for 2-3 times, and redisperse the centrifuged modified montmorillonite MMT In water and dimethylformamide (DMF) (the ratio of water and DMF is 10:90), the ratio of modified montmorillonite and mixed solvent is 1:100, then adopt cell disruptor to process 1h under ic...

Embodiment 2

[0055] A kind of preparation of aqueous polyurethane nanocomposite emulsion and film, concrete operation is as follows:

[0056] Add 43.5g of 4,4'-dicyclohexylmethane diisocyanate (HMDI) and 46.5g of polytetramethylene glycol (PTMG) into a 250mL four-necked flask equipped with a stirrer, a thermometer and a spherical condenser, and add 0.15g of di Dibutyltin laurate (DBTDL) catalyst and 20g of acetone were reacted at 80°C for 2h, and the temperature was controlled at 85°C; then the temperature was lowered to 60°C, and 6g (2g+2g+2g) of dimethylol propionic acid (DMPA) was added in three times, Add 20g of acetone each time, and react for 1h, 1h, and 4h respectively; finally cool down to 50°C, add 4g of 1,4-butanediol (BDO) and 20g of acetone to react for 2h; measure by toluene-di-n-butylamine back titration Reaction degree until the determined NCO group content reaches the theoretical value to obtain a polyurethane prepolymer; then lower the temperature to 15°C in an ice-water b...

Embodiment 3

[0066] A kind of preparation of aqueous polyurethane / polyethyleneimine modified montmorillonite nanocomposite emulsion and membrane, concrete operation is as follows:

[0067] Get the polyethyleneimine modified montmorillonite dispersion of Example 1 and pour it into a 250mL three-necked flask, and add the neutralized polyurethane prepolymer (polyurethane prepolymer prepared in Example 2) dropwise, wherein the modified The mass ratio of montmorillonite and prepolymer is shown in Table 2. The reaction temperature is 15°C, and it is stirred at a high speed at 1000 rpm; Polyurethane / polyethyleneimine modified montmorillonite nanocomposite emulsion; move the emulsion into a glass mold to dry, and finally prepare a waterborne polyurethane / polyethyleneimine modified montmorillonite nanocomposite film.

[0068] Different (the amount of montmorillonite in montmorillonite solution) modified montmorillonite (PEI-MMT) and (the amount of pure polyurethane in prepolymer) the mass ratio of ...

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Abstract

The invention discloses a high oxygen resistance waterborne polyurethane / montmorillonite nanocomposite emulsion and a preparation method thereof, belonging to the technical field of polymer material modification. The nanoemulsion of the present invention is prepared from the following raw materials by weight: 40-80wt% crystalline polyol, 15-50wt% symmetrical isocyanate, 2-6wt% hydrophilic monomer, 50-80wt% montmorillonite , 0.1-10wt% hyperbranched polyethyleneimine. The nanocomposite emulsion prepared by the present invention has better dispersion stability, and at the same time, the introduction of inorganic nanoparticles can significantly improve the thermal stability and mechanical properties of the waterborne polyurethane coating, and the unique sheet structure of montmorillonite can enhance the barrier performance. It can be widely used in high temperature resistant food, pharmaceutical packaging and other fields.

Description

technical field [0001] The invention relates to a high oxygen resistance water-based polyurethane / montmorillonite nanocomposite emulsion and a preparation method thereof, belonging to the technical field of polymer material modification. Background technique [0002] Water-based polyurethane (WPU) uses water as the dispersion medium, has the advantages of high molecular weight, low viscosity, good comprehensive performance, environmental protection, safety, hygiene, etc., and conforms to the concept of green environmental protection and sustainable development. Has been widely used. However, the mechanical properties, water resistance and other properties of water-based polyurethane are still not comparable to those of traditional solvent-based polyurethane, thus limiting its further wide application. Waterborne polyurethane / inorganic nanocomposite coating The organic combination of polyurethane synthesis technology and inorganic nanomaterials synthesis and dispersion techn...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G18/66C08G18/48C08G18/34C08G18/32C08G18/64C09D175/08C09D7/62C08L75/08C08K9/04C08K3/34C08J5/18
CPCC08G18/3206C08G18/348C08G18/4854C08G18/6423C08G18/6674C08G18/6692C08J5/18C08K3/346C08K9/04C08K9/08C08K2201/011C08L2201/08C08L2201/14C09D5/18C09D175/08C09D7/62C08L75/08
Inventor 张胜文陆俊田大为徐正午东为富
Owner JIANGNAN UNIV