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

A nanocomposite material and acrylate technology, which is 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 wide industrial application prospects

Inactive Publication Date: 2010-10-06
常州华钛化学有限公司
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  • 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 dibutyl tin laurate accounting for 0.05wt% of the reactant to a 500mL three-necked flask, and 0.20mol methyl Slowly add 2-hydroxyethyl acrylate into the three-necked flask at a rate of 10 drops / minute, continue to react for 4 hours under the condition of ice-water bath after dropping, then raise the temperature to 60°C, add Add 0.5% p-hydroxyanisole and react 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 into a 1000mL flask, stir at 80°C at a speed of 500 rpm for 1 hour, then add 1g of cetyltrimethylammonium chloride, and continue stirring After 12 hours, filter and wash with distilled water to obtain the product (Na-MMT-1); take 10 g of the product (Na-MMT-1) and disperse it in 200 mL of distilled water, add 400 mL of t...

Embodiment 2

[0046] Under nitrogen atmosphere and ice-water bath condition, add 0.20mol isophorone diisocyanate, 300mL tetrahydrofuran and the dibutyl tin laurate ester that accounts for reactant 0.2wt% in the 500mL three-neck flask, 0.20mol acrylate-2- Slowly add hydroxyethyl ester to the three-necked flask, continue to react for 2 hours under the condition of ice-water bath after dropping, then raise the temperature to 50°C, add hydroquinone accounting for 0.5% of the double bond moles of the reactant, and react for 8 hours , to obtain a tetrahydrofuran solution of the acrylate modifier 2 with a mass concentration of 0.25 g / mL.

[0047] Add 20g of K-montmorillonite and 200mL of distilled water into a 500mL flask, stir at 60°C at a speed of 3000 rpm for 1 hour, then add 0.5g of cetyltrimethylammonium chloride and cetyltrimethylammonium Ammonium bromide 0.5g, continue to stir for 24 hours, filter, wash with distilled water to obtain the product; take 10g of the product and disperse it in 3...

Embodiment 3

[0050] Under nitrogen atmosphere and ice-water bath condition, add 0.20mol toluene diisocyanate, 200mL dioxane, 100mL toluene and the dibutyl tin oxide that accounts for reactant 0.1wt% in the 500mL three-necked flask, 0.20mol acrylic acid- 2-Hydroxypropyl ester was slowly added dropwise to the three-necked flask, and after the drop was completed, the reaction was continued for 3 hours under ice-water bath conditions, and then the temperature was raised to 55°C, and 0.3% phenol was added, which accounted for 0.3% of the double bond moles of the reactant, and the reaction was continued 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 at 2000 rpm at 70°C for 1 hour, then add 0.1g of octadecyltrimethylammonium bromide , continue to stir for 48 hours, filter, and wash with distilled water to obtain t...

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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 UV-curable acrylate / modified montmorillonite nanocomposite materials, in particular to UV-curable acrylate / modified montmorillonite nanocomposites with organically modified montmorillonite as added components and their preparation method. Background technique [0002] Acrylic resins have been widely used in the field of UV curing since the late 1960s when German Bayer successfully developed UV-curable wood coatings. Acrylate has been widely used in adhesives, inks, coatings, composite materials, etc. due to its characteristics of no solvent volatilization, fast speed, and low energy consumption during light curing. According to the report of "Progress in Polymer Science" (Prog.Polym.Sci, 2003, 28: 1539-1641), one of the keys to the preparation of polymer / nanocomposite materials by combining acrylate and nano-montmorillonite is the lamellar structure. Organizing, and preparing nanocomposite materials wit...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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