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Process of preparing polymer/imvite nano composite material by surface controlling polymerization

A nano-composite material, montmorillonite technology, applied in the field of polymer preparation, can solve the problems of lack of good correlation in the polymerization reaction, difficult to insert, and difficult to polymerize.

Inactive Publication Date: 2007-07-18
UNIV OF SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since the chain transfer agent with a high chain transfer constant is not immobilized on the surface of the montmorillonite layer, it is easy to cause the copolymerization reaction between the layers and the polymerization reaction between the montmorillonite particles to be not well correlated, and a completely stripped polymerization reaction is obtained. have certain difficulties
Since it is difficult for general addition-fragmentation chain transfer reagents to be inserted into the interlayer of montmorillonite, it has not been seen so far to immobilize reversible addition-fragmentation chain transfer reagents on the surface of montmorillonite sheets, and then perform reversible addition-fragmentation chain transfer. Reports on Free Radical Polymerization

Method used

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  • Process of preparing polymer/imvite nano composite material by surface controlling polymerization
  • Process of preparing polymer/imvite nano composite material by surface controlling polymerization
  • Process of preparing polymer/imvite nano composite material by surface controlling polymerization

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Embodiment 1. Preparation of polystyrene / montmorillonite nanocomposite

[0023] Synthesis of the reversible addition-fragmentation chain transfer reagent 10-acid-10-dithiobenzyl ester-decyltrimethylammonium bromide:

[0024] Weigh 265 grams (1 mole) of bromoundecanoic acid, dissolve it in 400 grams of tetrahydrofuran, and prepare a solution with a mass concentration of 40%. Take by weighing 540 grams of mass concentration and be that 30% trimethylamine aqueous solution is slowly dripped in 150 grams of sodium hydroxide, and the about 3 moles of trimethylamine gas produced are slowly passed into the above-mentioned bromoundecanoic acid solution, and after reacting for 24 hours, will form Suction filtration of the precipitate. The precipitate was washed and dried in vacuo to obtain 318 g of white powder with a yield of 98%.

[0025] Weigh 324 grams of white powder and 160 grams of liquid bromine (1 mole) prepared by the above method, use 5 grams of phosphorus trichlorid...

Embodiment 2

[0033] Embodiment 2. Preparation of polymethyl acrylate / montmorillonite nanocomposite

[0034] First change the reaction conditions to prepare the reversible addition-fragmentation chain transfer reagent 6-acid-6-dithiobenzyl ester-hexyltrimethylammonium chloride: 164.5 grams (1 mole) of chloro-n-heptanoic acid were dissolved in 1480 grams of acetone In the solution, it is prepared into a solution with a mass concentration of 10%; 900 grams of a mass concentration of 30% trimethylamine aqueous solution is slowly dropped into 200 grams of sodium hydroxide, and about 5 moles of trimethylamine gas produced are slowly passed into the above-mentioned n-heptyl chloride After reacting in acid solution for 24 hours, the resulting precipitate was filtered. The precipitate was washed and vacuum-dried to obtain 221 g of white powder with a yield of 99%.

[0035] Take by weighing 223.5 grams of powder and 240 grams (1.5 moles) of liquid bromine prepared by the above method, 10 grams of p...

Embodiment 3

[0040] Embodiment 3. Preparation of polyacrylic acid / montmorillonite nanocomposite

[0041] Synthesis of reversible addition-fragmentation chain transfer reagent 24-acid-24-dithiobenzyl ester-hexyltrimethylammonium chloride: Weigh 508 grams (1 mole) of iodopentacic acid and dissolve it in 340 grams of ether 180 grams of a mass concentration of 30% trimethylamine aqueous solution is slowly dropped into 50 grams of sodium hydroxide, and about 1 mole of trimethylamine gas is slowly passed into the above-mentioned iodine 20 After reacting in the five-acid solution for 24 hours, the resulting precipitate was filtered; the precipitate was washed and vacuum-dried to obtain 510 g of white powder.

[0042] Take by weighing 567 grams of powder and 208 grams (1.3 moles) of liquid bromine prepared by the above method, use 5 grams of phosphorus trichloride as a catalyst, react at 40 ° C for 18 hours, and remove unreacted bromine in a vacuum to obtain 583 grams of light yellow powder. Yiel...

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Abstract

The surface controllable polymerization process to prepare composite polymer / montmorillonite material includes the following steps: reaction of trimethylamine and halogenated aliphatic acid, the reaction of the product with bromine for 12-48 hr and the reaction of the bromized product with magnesium bromide based dithio benzyl ester for 8-24 hr to obtain omega-acid-omega-dithio benzyl ester-fatty alkyl trimethyl ammonium halide; mixing omega-acid-omega-dithio benzyl ester-fatty alkyl trimethyl ammonium halide and montmorillonite in water through stirring at 40-100 deg.c for 1-48 hr to obtain intercalating montmorillonite; and mixing the intercalating montmorillonite with initiator and monomer in certain weight proportion and reaction at 40-120 deg.c for 4-48 hr to obtain precipitated composite polymer / montmorillonite material. The composite material has high strength, high heat stability, high solvent tolerance and high flame retarding performance.

Description

Technical field: [0001] The invention belongs to a polymer preparation method, in particular to a polymer / montmorillonite nanocomposite material preparation method using a surface polymerization method and a reversible addition-fragmentation chain transfer polymerization method. Background technique: [0002] The U.S. "Material Chemistry" (Chem.Mater., 2001, 13, 2465-2467) and "Langmuir" (Langmuir, 2002, 18, 4511-4518) have reported the use of surface anion initiators to initiate anionic polymerization to prepare polymers / Montmorillonite composite method. However, the anionic polymerization method must remove a small amount of water, and needs to be operated under high vacuum and high temperature, and the reaction conditions are harsh. "Materials Chemistry" (Chem. Mater., 2003, 15, 2693-2695) reported a method for preparing polymer / montmorillonite composite materials by inserting initiators between montmorillonite layers for in-situ atom transfer radical polymerization. ...

Claims

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Application Information

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IPC IPC(8): C08F2/44C08F2/38C08F12/08C08F20/10C08F26/10C08L23/00C08L33/00C08L39/06C08K3/34
Inventor 潘才元张宝庆洪春雁
Owner UNIV OF SCI & TECH OF CHINA
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