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Ultraviolet curing acrylic ester/modified montmorillonite nano composite material and preparation thereof

A nano-composite material and acrylate technology, applied in the treatment of dyed low molecular organic compounds, fibrous fillers, etc., can solve the problems of high price, low degree of organic modification of montmorillonite, and failure to achieve substantial improvement in material performance. , to achieve the effects of improved mechanical properties and heat resistance, simple and easy modification methods, and broad industrial application prospects

Inactive Publication Date: 2008-09-03
常州华钛化学有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

European "Polymer" magazine (Polymer, 2004, 45: 6175-6187) reported the preparation of UV-curable polyurethane acrylate / montmorillonite nanocomposites with inorganic montmorillonite and quaternary ammonium salt modified montmorillonite, compared Before and after the modification of montmorillonite and the effect of the added content on the properties of nanocomposites, due to the low degree of organic modification of montmorillonite, the interlayer spacing has not been highly expanded, forming an intercalated nanocomposite material, resulting in a failure to achieve a large material performance. Amplitude increase
American Chemical Society "Materials Chemistry" magazine (Chem. Mater, 2005, 17: 3331-3337) introduced the synthesis of a new type of acrylate quaternary ammonium salt surfactant, and used it to intercalate and modify montmorillonite to prepare UV-curable acrylic acid ester / montmorillonite nanocomposites, but their applications are limited by the difficulty and high cost of quaternary ammonium salts with acrylate groups
European "Polymer" magazine (Polymer, 2007, 48: 2231-2240) introduced the preparation of polymer / montmorillonite nanocomposites by ion exchange method and silane grafting method to modify montmorillonite, but due to silane and montmorillonite The low rate and low degree of reaction of hydroxyl groups on the soil surface failed to achieve high-efficiency grafting

Method used

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  • Ultraviolet curing acrylic ester/modified montmorillonite nano composite material and preparation thereof
  • Ultraviolet curing acrylic ester/modified montmorillonite nano composite material and preparation thereof
  • Ultraviolet curing acrylic ester/modified montmorillonite nano composite material and preparation thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Under nitrogen atmosphere and ice-water bath conditions, add 0.20mol diphenylmethylene diisocyanate, 300mL toluene and 0.05wt% dibutyltin laurate into a 500mL three-necked flask, and add 0.20mol methyl 2-Hydroxyethyl acrylate was slowly added dropwise to the three-necked flask at a rate of 10 drops / min. After the dropping, the reaction was continued for 4 hours in an ice-water bath, then the temperature was raised to 60°C, and the amount of double bond of the reactant was added. A few 0.5% p-hydroxyanisole was reacted for 4 hours to obtain a toluene solution of acrylate modifier 1 with a mass concentration of 0.27 g / mL.

[0036] Add 10g of Na-montmorillonite (Na-MMT) and 400mL of distilled water to a 1000mL flask. After stirring for 1 hour at 80°C at 500 rpm, add 1g of cetyltrimethylammonium chloride and continue stirring After 12 hours, filter and wash with distilled water to obtain the product (Na-MMT-1); disperse 10 g of the product (Na-MMT-1) in 200 mL of distilled wate...

Embodiment 2

[0046] Under nitrogen atmosphere and ice-water bath conditions, 0.20 mol of isophorone diisocyanate, 300 mL of tetrahydrofuran, and 0.2wt% of dibutyltin laurate were added to a 500 mL three-necked flask, and 0.20 mol of acrylic acid-2- Hydroxyethyl ester was slowly added dropwise to the three-necked flask. After the dropping, the reaction was continued for 2 hours under ice-water bath conditions, and then the temperature was raised to 50°C. Hydroquinone accounting for 0.5% of the double bond moles of the reactant was added and reacted for 8 hours , A tetrahydrofuran solution of acrylate modifier 2 with a mass concentration of 0.25 g / mL was obtained.

[0047] Add 20 g of K-montmorillonite and 200 mL of distilled water into a 500 mL flask, stir at 60°C at 3000 rpm for 1 hour, add 0.5 g of cetyltrimethylammonium chloride and cetyltrimethyl 0.5g ammonium bromide, continue to stir for 24 hours, filter and wash with distilled water to obtain the product; take 10g product dispersed in 30...

Embodiment 3

[0050] Under nitrogen atmosphere and ice-water bath conditions, 0.20mol of toluene diisocyanate, 200mL of dioxane, 100mL of toluene and 0.1wt% of dibutyl stannous oxide were added to a 500mL three-necked flask, and 0.20mol of acrylic acid- 2-Hydroxypropyl ester was slowly added dropwise to the three-necked flask. After dropping, the reaction was continued for 3 hours under ice-water bath conditions, and then the temperature was raised to 55°C. Phenol accounting for 0.3% of the double bond of the reactant was added and reacted for 6 hours. A toluene / dioxane solution of acrylate modifier 3 with a mass concentration of 0.22 g / L was obtained.

[0051] Add 5g of Na-montmorillonite, 5g of Li-montmorillonite and 200mL of distilled water into a 500mL flask, stir for 1 hour at 70°C at 2000 rpm, then add 0.1g of octadecyltrimethylammonium bromide After stirring for 48 hours, filter and wash with distilled water to obtain the product; disperse 10g of the product in 200mL of distilled water, ...

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Abstract

The invention relates to an ultraviolet light solidified acrylate / modified montmorillonite nanometre composite material and preparation method thereof, comprising montmorillonite being subjected to cation exchange modifying using longchain alkyl quaternary ammonium salts; extending the distance between the montmorillonite layers and improving the chemistry microenvironment; the surface hydroxy group of the montmorillonite being decorated using acrylate modifier with carbimide group and grafted with a large amount of acrylate groups of high response to further extend the interlayer distance; finally mixing the decorated montmorillonite, acrylate monomer, acrylate oligomer and ultraviolet light initiator to produce the ultraviolet light solidified acrylate / modified montmorillonite nanometre composite material. The method is simply and easily operated to realize high delamination and good dispersion pf montmorillonite in polymer substrate. Compared with the pure acrylate material, the material of the invention has greatly improved mechanical property and thermal endurance, with high intension after ultraviolet light solidifying, high hardness, good thermal stability and wide industrial application foreground.

Description

Technical field [0001] The invention belongs to the technical field of ultraviolet light curing acrylate / modified montmorillonite nanocomposite materials, and specifically relates to an ultraviolet light curing acrylate / modified montmorillonite nanocomposite material with organically modified montmorillonite as an additive component and preparation thereof method. Background technique [0002] Since the German Bayer Company successfully developed UV-curable wood coatings in the late 1960s, acrylic resins have been widely used in the field of UV curing. Acrylate has been widely used in adhesives, inks, coatings, composite materials, etc. due to its characteristics of solvent-free volatilization, fast speed, and low energy consumption during light curing. According to the "Prog. Polym. Sci, 2003, 28: 1539-1641) report, one of the keys to the preparation of polymer / nanocomposites by combining acrylate with nano-montmorillonite is lamellar Organically, and organically modified montmo...

Claims

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Application Information

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IPC IPC(8): C08F220/10C08F2/50C08K9/04C08K3/34C09C3/08C09C1/42
Inventor 吕世昌徐俊伟
Owner 常州华钛化学有限公司
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