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Method of preparing polymer/montmorillonid nano-composite material by montmorillonoid in-situ organization

A nano-composite material and montmorillonite technology, which is applied in the field of montmorillonite in-situ organic preparation of polymer/montmorillonite nano-composite materials, can solve the problems of polymer degradation, discoloration, low thermal decomposition temperature, etc. Saturated vapor pressure, low volatility, improved compatibility

Inactive Publication Date: 2006-03-29
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

"Thermal DegradationChemistry of Alkyl QuatemaryAmmonium Montmorillonite" (Chem. Mater. 2001, 13, 2979-2990) and other literature studies have shown that the thermal decomposition temperature of the existing montmorillonite organic modifier is low, and it can be used in the processing and use of composite materials. Decomposes during the process, leading to degradation and discoloration of the polymer

Method used

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  • Method of preparing polymer/montmorillonid nano-composite material by montmorillonoid in-situ organization
  • Method of preparing polymer/montmorillonid nano-composite material by montmorillonoid in-situ organization
  • Method of preparing polymer/montmorillonid nano-composite material by montmorillonoid in-situ organization

Examples

Experimental program
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Effect test

Embodiment 1

[0049] Take 100 ml of xylene and 0.25 g of 1-methyl-3-tetradecyl imidazole chloride salt, put them into a 250 ml three-necked flask, put in a magnetic stir bar, install a reflux condenser, heat in an oil bath, and control the temperature to 40°C After stirring for 5 hours until the solution is transparent and clear, add 0.5 g of Na-montmorillonite and continue to stir for 24 hours to obtain a slurry of organic montmorillonite. Then, 9.5 g of isotactic polypropylene was added, the temperature was raised to 140±2°C, and the mixture was stirred for 24 hours. Pour the polymer solution in the flask into a large amount of ethanol while it is hot, filter the precipitated flocs, wash with deionized water and ethanol three times, and dry in vacuum to obtain a polypropylene / montmorillonite composite material, XRD and TEM characterization results show that this composite material is polypropylene / montmorillonite nanocomposite, see attached Figure 1a with 1b .

Embodiment 2

[0055] 0.25 g of 1-methyl-3-hexadecyltetrafluoroborate imidazole salt was dried in vacuum at 80°C for 6 hours, 0.5 g of synthetic montmorillonite was dried in vacuum at 100°C for 6 hours, and then added to 250 ml of dry In a three-necked flask, add a dry magnetic stir bar, add 100 ml of dried refluxed toluene with a syringe, install a reflux condenser, under the protection of nitrogen, heat in a water bath, control the temperature at 50±2℃, and stir for 24 hours to obtain Slurry of organic montmorillonite. Take another clean, dry 250ml two-necked flask, put it in a dry magnetic stirrer, seal the mouth of the bottle with a reverse rubber stopper, draw out 50ml of colloidal solution of organic montmorillonite and pour into the flask. Inject propylene gas to a pressure of 770mmHg, add 3ml MAO (1.4mol / l), 2ml Me 2 Si(Ind) 2 ZrCl 2 (1.5μm / l), after polymerization at 40°C for about 30 minutes, acidified ethanol is added to terminate the reaction, the polymerized product is washed with d...

Embodiment 3

[0057] 0.35 g of 1-methyl-3-(4-ethyl-hexadecyl) tetrafluoroborate imidazole salt, dried under vacuum at 80°C for 6 hours, 0.5 g of mixed montmorillonite (Na-montmorillonite and Ca- The mass percentage of montmorillonite is 80 / 20) After vacuum drying at 100°C for 6 hours, add it to a dry 250ml three-necked flask, add a dry magnetic stirrer, and use a syringe to add 100ml of dried refluxed Toluene, install a reflux condenser, under the protection of nitrogen, heat in a water bath, control the temperature at 50±2°C, and stir for 24 hours to obtain a slurry of organic montmorillonite. Take another clean, dry 250ml two-necked flask, put it in a dry magnetic stirrer, seal the mouth of the bottle with a reverse rubber stopper, draw three times, draw 50ml of organic montmorillonite slurry into the flask, Inject ethylene gas to a pressure of 770mmHg, and add 2 millimoles of AlEt 3 , 3 millimoles of MAO (1.4mol / l), 2 milliliters of Et(Ind) 2 ZrCl 2 (1.5 μm / l), after polymerization at 30°C f...

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Abstract

A process for preparing composite polymer / montmorillonite nanoparticles by in-situ organizing of montmorillonite features that the imidazole-type or pyridine-type organic salt is used in non-water solvent to obtain organic modifier for organizing and dispersing the montmorillonite, resulting in the colloidal solution of its nanoparticles. The solvents with different properties and the organic salts with different molecular structures can be chosen for preparing the nanoparticles with relative performance. Its advantages are high thermal stability and high compatibility.

Description

Technical field [0001] The invention belongs to the field of polymer nanomaterials, and particularly relates to a method for preparing polymer / montmorillonite nanocomposites by in-situ organicization of montmorillonite. Background technique [0002] Montmorillonite is the main component of bentonite. It is a kind of high-yield clay mineral in my country. It has been widely used in the fields of chemical industry, medicine, petroleum, foundry, and materials. Polymer materials are the most rapidly developing new materials, and their applications have spread across all areas of people's production and life. It is people's wish to combine polymer materials with clay mineral materials that are abundant in nature to produce new composite materials with better performance, wider application range, and cheaper prices. With the development of nanotechnology, people hope to exfoliate and disperse the montmorillonite with nano-lamellar structure in the polymer matrix to obtain polymer montm...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F2/44C08F10/00C08K13/02C08L23/00
Inventor 董金勇丁运生王志刚
Owner INST OF CHEM CHINESE ACAD OF SCI
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