Method for preparing nano composite material of hydroxyl-functional polyester/montmorillonite

A nano-composite material and hydroxyl-functional technology are applied in the preparation of hydroxyl-functional polyester/montmorillonite nano-composite materials, and in the field of in-situ polymerization to prepare hydroxyl-functional polyester/montmorillonite nano-composite materials, which can solve the problem of difficult to achieve Industrialization, insufficient intercalation, difficult molecular chain movement, etc., to achieve the effect of high molecular weight

Inactive Publication Date: 2012-07-18
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, these two methods all have the following disadvantages: the polymer melt intercalation method is relatively difficult due to the molecular chain movement of the polymer, which leads to insufficient intercalation, and finally makes the dispersion of the montmorillonite sheet in the polymer matrix uneven; The solution intercalation method needs to remove a large amount of solvent, which is difficult to achieve industrialization

Method used

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  • Method for preparing nano composite material of hydroxyl-functional polyester/montmorillonite
  • Method for preparing nano composite material of hydroxyl-functional polyester/montmorillonite
  • Method for preparing nano composite material of hydroxyl-functional polyester/montmorillonite

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Experimental program
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Effect test

Embodiment 1

[0032] (1) Weigh 4g of sodium-based montmorillonite and 200ml of deionized water, mix them in a three-necked flask and heat them in a constant temperature water bath at 80°C, and prepare a montmorillonite suspension under stirring; weigh cetyl tri Dissolve 3 g of methyl ammonium bromide (greater than the ion exchange capacity of sodium montmorillonite) in 100 ml of deionized water to prepare a catalyst solution; add the catalyst solution dropwise to a three-neck flask in a constant temperature water bath at 80°C under stirring, and react for 2 hours ; stop heating at constant temperature; stand still, the obtained white precipitate is suction filtered, and washed 3 times with deionized water, the unexchanged catalyst is removed, and dried to obtain organically modified montmorillonite, which is analyzed by XRD. The interlayer spacing of soil increased from 1.24nm before organic modification to 2.11nm after organic modification.

Embodiment 2～5

[0034]Get 18.6g (0.05mol) of bisphenol A epoxy resin, 6.74g (0.033mol) of sebacic acid, 2.44g (0.017mol) of adipic acid and 0.244g (4mol) of benzoic acid are placed in a three-necked flask, prepare the same 5 of the three-necked flasks were added the organically modified montmorillonite prepared in Example 1, and the additions were 1.41g (5wt%), 2.8g (10wt%), 4.2g (15wt%) and 5.6g respectively. g (20 wt%). Put the three-necked flask into silicone oil, at 140°C, N 2 The reaction was stirred mechanically under protection. Sampling every 20 minutes during the reaction, until the hydroxyl functionalized polyester in the sample is insoluble in N, N-dimethylformamide (DMF), stop the reaction; the last DMF-soluble sample is described in the present invention An in situ polymerization of hydroxyl-functionalized polyester / montmorillonite nanocomposites for detection and analysis.

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Abstract

The invention relates to a method for preparing nano composite material of hydroxyl-functional polyester/montmorillonite, belonging to the technical field of polymer material. The method comprises the following steps: firstly intercalating an onium catalyst into sodium-based montmorillonite layers at 60 DEG C to 100 DEG C by adopting a cation exchange method to obtain organic modified montmorillonite; then, mixing the organic modified montmorillonite, dicarboxylic acid, dibasic epoxy compound and monocarboxylic acid for carrying out in-situ polymerization; melting a monomer dibasic epoxy compound and the dicarboxylic acid in a polymerization process for intercalating the organic modified montmorillonite; polymerizing the monomer among the montmorillonite layers and outside the montmorillonite under the action of the onium catalyst so that the montmorillonite sheet layers are pushed off; and finally uniformly distributing the sheet layers in a polyester matrix with a hydroxyl functional group so as to prepare the nano composite material of intercalating or stripping type hydroxyl functional polyester/montmorillonite. The method has the advantages of simplicity and low cost and can be applied to bulk industrial production; and the material can be widely applied to the field of biodegradable materials.

Description

technical field [0001] The present invention relates to a preparation method of hydroxyl-functionalized polyester / montmorillonite nanocomposite material, in particular to a method for preparing hydroxyl-functionalized polyester / montmorillonite nanocomposite material through in-situ polymerization, belonging to high Molecular materials technology field. Background technique [0002] Polyester / montmorillonite nanocomposites are a class of materials that have attracted much attention, but hydroxyl-functionalized polyester / montmorillonite nanocomposites have not been reported. Currently, there are patents disclosing methods for preparing hydroxyl-functionalized polyesters, such as patents US97 / 22276, US5171820, US6346596, US5496910, WO99 / 12991, and CN1269812A. However, the above patents are limited to the preparation of a single-phase hydroxyl-functionalized polyester. By directly adding the catalyst to a dicarboxylic acid and a diepoxide, in the presence of a monocarboxylic ac...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/42C08G63/87C08K9/04C08K3/34
Inventor 张青山李云政徐玲
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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