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Sulfhydryl-double bond reaction-based acrylate ester/montmorillonite composite and preparation method

An acrylate and composite material technology, applied in the field of acrylate/montmorillonite nanocomposite materials, can solve the problems of adverse effects on the environment and human health, large sheet steric hindrance effect, unfavorable industrial production, etc., and achieves reactivity and lipophilicity. good effect, less environmental pollution, and broad industrial application prospects

Active Publication Date: 2013-08-14
ZHANGJIAGANG DAWN CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Chinese patent application number 200810020005.5 proposes a kind of grafting of acrylate modifier with isocyanate group on montmorillonite, then adds photoinitiator and acrylate resin, and makes acrylate / In the method of montmorillonite nanocomposite materials, due to the low reactivity of isocyanate and hydroxyl groups on the montmorillonite sheet, and the large steric hindrance effect between the sheets, the dispersion of montmorillonite in the polymer matrix is ​​limited. , the compatibility of the final material is poor; at the same time, the added small molecule photoinitiator will also have adverse effects on the environment and human health
[0005] Chinese patent application number 201210068740.X proposed a modified photoinitiator with quaternary ammonium groups intercalated into the montmorillonite layer, then mixed with acrylate oligomers and monomers, and cured to obtain photoinitiated / Halogen-free flame retardant material method, due to the use of highly toxic acryloyl chloride and methyl iodide in the synthesis process, and the steps are cumbersome, high requirements for equipment; The initiator is used as an intercalation agent, and the waste is large, and the cost of the final product is high, which is not conducive to industrial production

Method used

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  • Sulfhydryl-double bond reaction-based acrylate ester/montmorillonite composite and preparation method
  • Sulfhydryl-double bond reaction-based acrylate ester/montmorillonite composite and preparation method
  • Sulfhydryl-double bond reaction-based acrylate ester/montmorillonite composite and preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] (1) Dissolve 30g of 3-aminopropyltriethoxysilane and 40.17g of trimethylolpropane triacrylate in 50mL of dichloromethane, and dissolve 3-aminopropyltriethoxysilane in a nitrogen atmosphere and ice-water bath. The ethoxysilane solution was added dropwise to the trimethylolpropane triacrylate solution, and the drop was completed in 0.5 hours. Then it was slowly raised to room temperature, and the reaction was continued for 24 hours. After the reaction, the solvent was evaporated to dryness with a rotary evaporator to obtain the product amino polyfunctional acrylate silane coupling agent;

[0043] (2) Mix 117.8g of mercaptoacetic acid, 55g of trimethylolpropane, 5.2g of p-toluenesulfonic acid and 180mL of cyclohexane, add it to a flask with a water separator, and heat to reflux under a nitrogen atmosphere until there is no water produced, after cooling to room temperature, with saturated NaHCO 3 Washed three times with aqueous solution, then washed with anhydrous Na 2 S...

Embodiment 2

[0055] (1) Take 25.0g of 3-aminopropyltriethoxysilane and 52.7g of ditrimethylolpropane tetraacrylate, dissolve them in 50mL of dichloromethane respectively, and dissolve 3-aminopropyl triethoxysilane in nitrogen atmosphere and ice-water bath. The propyltriethoxysilane solution was added dropwise to the ditrimethylolpropane tetraacrylate solution, and the drop was completed in 0.5 hours. Then it was slowly raised to room temperature, and the reaction was continued for 24 hours. After the reaction, the solvent was evaporated to dryness with a rotary evaporator to obtain the product amino polyfunctional acrylate silane coupling agent;

[0056] (2) Mix 101g of 3-mercaptopropionic acid, 30.0g of pentaerythritol, 3.3g of concentrated sulfuric acid and 140g of toluene, add it into a flask with a water separator, heat and reflux under a nitrogen atmosphere until no water is produced, cool to room temperature, and use saturated NaHCO 3 Washed three times with aqueous solution, then ...

Embodiment 3

[0062] (1) Dissolve 20.0g of γ-mercaptopropyltrimethoxysilane, 1.12g of triethylamine and 35.9g of pentaerythritol tetraacrylate in 40mL of anhydrous tetrahydrofuran, and dissolve γ-mercaptopropyltrimethoxysilane in nitrogen atmosphere and ice-water bath. Add the mixed solution of trimethoxysilane and triethylamine dropwise into the pentaerythritol tetraacrylate solution, and drop it in 0.5 hours. Then it was slowly raised to room temperature, and the reaction was continued for 24 hours. After the reaction, the solvent was evaporated to dryness with a rotary evaporator to obtain the product amino polyfunctional acrylate silane coupling agent;

[0063] (2) Mix 135.9g of 6-mercaptohexanoic acid, 30.0g of pentaerythritol, 6.63g of concentrated sulfuric acid with 130g of toluene and 50g of dioxane, add them to a flask with a water separator, and heat to reflux under a nitrogen atmosphere until there is no water produced, after cooling to room temperature, with saturated NaHCO 3 ...

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Abstract

The invention discloses a sulfhydryl-double bond reaction-based acrylate ester / montmorillonite composite and a preparation method. The preparation method is characterized by comprising the steps of: firstly, forming intercalation modification chemical bond grafted acrylic ester functionalized nano-montmorillonite, then mixing the synthesized polyfunctional group sulfur alcohol, acrylate ester oligomer, acrylate monomer and a light initiator, and finally performing ultraviolet light irradiation to obtain the acrylate ester / montmorillonite ultraviolet cured nano composite. A line for synthesizing a polyfunctional group acrylate ester silane coupling agent and the polyfunctional group sulfur alcohol is simple and easy without toxicity; compared with the traditional method in which the initiator takes up 3 to 5% of total mass, the preparation method disclosed by the invention has the advantages that the usage amount of the light initiator is greatly reduced and only takes up 0.1-0.8% of the total mass, the residual light initiator can be effectively reduced, the harm of fragments to the environment and the health of a human body can be reduced, and higher reaction activity and conversion rate can be achieved; and the compatibility between inorganic components and organic components in the composite is good, and the mechanical property and heat-resistant property are obviously improved.

Description

technical field [0001] The invention belongs to the technical field of acrylate / montmorillonite nano-composite materials, in particular to acrylate / montmorillonite composite materials based on mercapto-double bond reactions, which use multifunctional acrylate-modified nano-montmorillonite as an added component and its preparation method. Background technique [0002] The polymer / inorganic nanocomposite material is a composite material in which the polymer is used as the continuous phase and the ultrafine inorganic components with a size of nanometer (1-100nm) are used as the dispersed phase. The role of nanoparticles in polymer composites can not only enhance the mechanical properties, but also endow the matrix materials with other new functions, such as gas barrier properties, weather resistance, antibacterial properties, and specific optical and electromagnetic properties and thermal stability. According to the report in the British journal "Polymer Reviews" (Polymer Revi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F283/00C08F283/10C08F283/01C08F2/48C08K9/04C08K9/06C08K3/34
Inventor 谢寒王春华朱胜武施文芳
Owner ZHANGJIAGANG DAWN CHEM
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