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

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

Inactive Publication Date: 2007-11-07
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 Quaternary Ammonium 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 is used in the processing and processing of composite materials. Decomposes during use, causing 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
Comparison scheme
Effect test

Embodiment 1

[0049] Take 100 ml of xylene and 0.25 g of 1-methyl-3-tetradecyl imidazolium chloride, add it to a 250 ml three-necked flask, put in a magnetic stirrer, install a reflux condenser, heat in an oil bath, and control the temperature at 40°C , stirred for 5 hours until the solution was transparent and clear, then added 0.5 g of Na-montmorillonite, and continued to stir for 24 hours to obtain a slurry of organic montmorillonite. Then, add 9.5 grams of isotactic polypropylene, heat up to 140±2°C, and stir for 24 hours. The polymer solution in the flask was poured into a large amount of ethanol while it was hot, and the precipitated floc was filtered and washed three times with deionized water and ethanol respectively, and dried in vacuum to obtain a polypropylene / montmorillonite composite material, XRD and The TEM characterization results show that the composite material is a polypropylene / montmorillonite nanocomposite material, as shown in Figures 1a and 1b.

Embodiment 2

[0055] 0.25 g of 1-methyl-3-hexadecyl tetrafluoroborate imidazolium salt was vacuum-dried at 80°C for 6 hours, 0.5 g of synthetic montmorillonite was vacuum-dried at 100°C for 6 hours, and 250 ml of dried In the three-necked flask, add a dry magnetic stirrer, add 100 ml of dry and refluxed toluene with a syringe, install a reflux condenser, and heat in a water bath under nitrogen protection to control the temperature at 50 ± 2 ° C. Stir for 24 hours to obtain Slurry of organomontmorillonite. Get a clean, dry 250 ml two-necked flask in addition, put into a dry magnetic stirrer, seal the bottle mouth with a reverse rubber stopper, after pumping three times, extract 50 ml of organic montmorillonite colloidal solution into the flask, Feed propylene gas to a pressure of 770mmHg, add 3 milliliters of MAO (1.4mol / l), 2 milliliters of Me 2 Si(Ind) 2 ZrCl 2 (1.5 μm / l), after polymerization at 40°C for about 30 minutes, acidified ethanol was added to terminate the reaction, the polym...

Embodiment 3

[0057] 0.35 g of 1-methyl-3-(4-ethyl-hexadecyl) imidazolium tetrafluoroborate was vacuum-dried at 80°C for 6 hours, and 0.5 g of mixed montmorillonite (Na-montmorillonite and Ca- The mass percentage of montmorillonite is 80 / 20) under 100 ℃, after vacuum drying for 6 hours, add in the dry three-necked flask of 250 milliliters, then add and put into dry magnetic stirrer, add 100 milliliters of dry refluxed For toluene, install a reflux condenser, under nitrogen protection, heat in a water bath, control the temperature at 50±2°C, and stir for 24 hours to obtain a slurry of organic montmorillonite. Get a clean, dry 250 ml two-necked flask in addition, put into a dry magnetic stirrer, seal the bottle mouth with a reverse rubber stopper, after pumping three times, extract the slurry liquid of 50 ml of organic montmorillonite and inject it into the flask. Introduce ethylene gas to a pressure of 770mmHg, add 2 mmol of AlEt 3 , 3 mmol of MAO (1.4 mol / l), 2 ml of Et(Ind) 2 ZrCl 2 (1....

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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 nanometer materials, and in particular relates to a method for preparing polymer / montmorillonite nanocomposite materials by organically preparing montmorillonite in situ. Background technique [0002] Montmorillonite is the main component of bentonite and a high-yield clay mineral in my country. It has been widely used in chemical industry, medicine, petroleum, casting, materials and other fields. Polymer materials are the most rapidly developing new materials, and their applications have spread all over the fields of people's production and life. It is people's good wish to combine polymer materials with clay mineral materials that exist in large quantities in nature to produce new composite materials with better performance, wider application range and cheaper price. With the development of nanotechnology, people hope to exfoliate and disperse montmorillonite with nanosheet structure in polymer matrix to...

Claims

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Application Information

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Patent Type & Authority Patents(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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