Zerovalent nano-iron coated polymethyl methacrylate and preparation method thereof

A technology of polymethyl methacrylate and zero-valent nano-iron, which is applied in the field of nanomaterial composites, can solve the problems of poor affinity, weak controllability and complex coating mechanism of inorganic nanoparticles.

Active Publication Date: 2014-03-12
SUZHOU DOUBLE ELEPHANT OPTICAL MATERIALS CO LTD
3 Cites 3 Cited by

AI-Extracted Technical Summary

Problems solved by technology

[0006] However, due to the relatively poor affinity between polymethyl methacrylate and inorganic nanoparticles, and the complex coating mechanism, in the prior art, the controllability in the process of polymethyl methacrylate coating inorganic nanoparticles is relatively poor. We...
View more

Abstract

The invention provides a zerovalent nano-iron coated polymethyl methacrylate and a preparation method thereof. The preparation method comprises the followings: after zerovalent nano-iron, a monomer, a chain transfer agent, a co-stablizer, an emulsifying agent and water are emulsified, a miniemulsion is obtained; under the protection of protective gas, after the miniemulsion obtained in the last step is heated for reaction, the zerovalent nano-iron coated polymethyl methacrylate is obtained; the protective gas is inert gas or nitrogen; the monomer is methyl methacrylate or epoxypropyl methacrylate. In nanocomposite provided by the invention, molecular weight and molecular weight distribution of the polymethyl methacrylate are both controlled, and paramagnetism exists at the same time.

Technology Topic

MiniemulsionMethyl methacrylate +10

Image

  • Zerovalent nano-iron coated polymethyl methacrylate and preparation method thereof
  • Zerovalent nano-iron coated polymethyl methacrylate and preparation method thereof
  • Zerovalent nano-iron coated polymethyl methacrylate and preparation method thereof

Examples

  • Experimental program(4)

Example Embodiment

[0085] Example 1
[0086] Place 4 mL of methyl methacrylate and 0.0077 g of azobisisobutyronitrile in a Schlenk tube and heat to 70°C for reaction. After reacting for 2 hours, add 10 mL of tetrahydrofuran and then add 250 mL of methanol for precipitation. After drying, polymethyl methacrylate is obtained.
[0087] Put 1.15 g of polymethyl methacrylate, 1.20 g of ferrous chloride, and 50 mL of tetrahydrofuran prepared above into a 250 mL three-necked flask, and place it in an ultrasonic cleaner. Under the protection of inert gas and ultrasonic conditions, 22 mL of a mixture of lithium triethylborohydride and 50 mL of tetrahydrofuran was added dropwise to the three-necked flask for 30 minutes. After the addition, the reaction was continued for 1 hour. After the completion of the reaction, 500mL ethanol was added to the three-necked flask for precipitation, and the upper liquid was decanted. The resulting solid mixture was dissolved in 20mL tetrahydrofuran and precipitated with ethanol. Repeated 3 times, finally filtered and dried to obtain polymethacrylic acid. Compound of methyl ester and zero-valent nano-iron.
[0088] Mix 1mL methyl methacrylate, 0.02g polymethyl methacrylate and zero-valent nano-iron complex, 0.0128g chain transfer agent isobutyronitrile dithionaphthoate (CPDN) and 55.2μL hexadecane. The oil phase mixture is obtained, and then under magnetic stirring, the oil phase and 4 mL of Brij98 solution with a mass concentration of 2.3% are stirred and pre-emulsified for 30 minutes, then treated with an ultrasonic cell pulverizer for 6 minutes, and then transferred to an ampoule and frozen- After pumping and thawing 3 times, the inert gas is introduced and the tube is melted and sealed, put in a magnetic stirrer, and reacted at a speed of 1200 rpm and 25°C. After reacting for 150 hours, a polymer coated with zero-valent nano iron is obtained. Methyl methacrylate.
[0089] Scanning electron microscopy of the polymethyl methacrylate coated with zero-valent nano-iron prepared by the above method, the results are as follows figure 1 As shown, figure 1 This is an electron micrograph of the zero-valent nano-iron-coated polymethyl methacrylate prepared in Example 1 of the present invention, and its particle size is about 210 nm.
[0090] The reaction kinetics of the reaction process for the preparation of polymethyl methacrylate coated with zero-valent iron nanoparticles was monitored, and the results were as follows figure 2 As shown, figure 2 This is a reaction kinetics diagram of the polymerization reaction process in Example 1 of the present invention at 25°C.
[0091] The reaction conversion rate, polymer molecular weight and molecular weight distribution of the above-mentioned preparation of polymethyl methacrylate coated with zero-valent nano-iron were monitored, and the results were as follows image 3 As shown, image 3 It is a graph of the relationship between the conversion rate of the polymerization reaction and the molecular weight of the polymer and the molecular weight distribution in Example 1 of the present invention.
[0092] The polymethyl methacrylate coated with zero-valent nano-iron prepared by the above method ( 1 H-NMR) hydrogen nuclear magnetic detection, the results are as follows Image 6 As shown, Image 6 This is the hydrogen nuclear magnetic resonance spectrum of the zero-valent iron-coated polymethyl methacrylate prepared in Example 1 of the present invention.
[0093] MALDI-TOF mass spectrometry was performed on the polymethyl methacrylate coated with zero-valent nano-iron prepared by the above method, and the results are as follows Figure 7 As shown, Figure 7 This is the MALDI-TOF mass spectrum of the polymethyl methacrylate coated with zero-valent nano-iron prepared in Example 1 of the present invention.
[0094] Observation of the polymethyl methacrylate coated with zero-valent nano-iron prepared by the above method, the results are as follows Figure 8 As shown, Figure 8 This is a photograph of the actual photo of the zero-valent nano-iron-coated polymethyl methacrylate prepared in Example 1 of the present invention.
[0095] The appearance of the polymethyl methacrylate coated with zero-valent nano-iron prepared by the above method is compared with the external magnetic field and the magnetic field canceled. The results are as follows Picture 9 As shown, Picture 9 This is a photograph of the comparison of the appearance of the polymethyl methacrylate coated with zero-valent nano-iron prepared in Example 1 of the present invention, with the application of a magnetic field and the magnetic field canceled, and the appearance is compared.

Example Embodiment

[0096] Example 2
[0097] Place 4 mL of methyl methacrylate and 0.0077 g of azobisisobutyronitrile in a Schlenk tube and heat to 70°C for reaction. After reacting for 2 hours, add 10 mL of tetrahydrofuran and then add 250 mL of methanol for precipitation. After drying, polymethyl methacrylate is obtained.
[0098] Put 1.15 g of polymethyl methacrylate, 1.20 g of ferrous chloride, and 50 mL of tetrahydrofuran prepared above into a 250 mL three-necked flask, and place it in an ultrasonic cleaner. Under the protection of inert gas and ultrasonic conditions, 22 mL of a mixture of lithium triethylborohydride and 50 mL of tetrahydrofuran was added dropwise to the three-necked flask for 30 minutes. After the addition, the reaction was continued for 1 hour. After the completion of the reaction, 500mL ethanol was added to the three-necked flask for precipitation, and the upper liquid was decanted. The resulting solid mixture was dissolved in 20mL tetrahydrofuran and precipitated with ethanol. Repeated 3 times, finally filtered and dried to obtain polymethacrylic acid. Compound of methyl ester and zero-valent nano-iron.
[0099] Mix 1mL methyl methacrylate, 0.02g polymethyl methacrylate and zero-valent nano-iron complex, 0.0128g chain transfer agent isobutyronitrile dithionaphthoate (CPDN) and 55.2μL hexadecane. The oil phase mixture is obtained, and then under magnetic stirring, the oil phase and 4 mL of Brij98 solution with a mass concentration of 2.3% are stirred and pre-emulsified for 30 minutes, then treated with an ultrasonic cell pulverizer for 6 minutes, and then transferred to an ampoule and frozen- After pumping and thawing 3 times, the inert gas was introduced and the tube was melted and sealed, put into a magnetic stirrer, and reacted at a speed of 1200 rpm and 60°C. After 45 hours of reaction, a polymer coated with zero-valent nano iron was obtained. Methyl methacrylate.
[0100] The reaction kinetics of the reaction process for the preparation of polymethyl methacrylate coated with zero-valent iron nanoparticles was monitored, and the results were as follows Figure 4 As shown, Figure 4 This is the reaction kinetics diagram of the polymerization reaction process at 60°C in Example 2 of the present invention.
[0101] The reaction conversion rate, polymer molecular weight and molecular weight distribution of the above-mentioned preparation of polymethyl methacrylate coated with zero-valent nano-iron were monitored, and the results were as follows Figure 5 As shown, Figure 5 It is a graph of the relationship between the conversion rate of the polymerization reaction and the molecular weight and molecular weight distribution of the polymer in Example 2 of the present invention.

Example Embodiment

[0102] Example 3
[0103] Place 4 mL of methyl methacrylate and 0.0077 g of azobisisobutyronitrile in a Schlenk tube and heat to 70°C for reaction. After reacting for 2 hours, add 10 mL of tetrahydrofuran and then add 250 mL of methanol for precipitation. After drying, polymethyl methacrylate is obtained.
[0104] Put 2.30 g of polymethyl methacrylate, 1.20 g of ferrous chloride, and 50 mL of tetrahydrofuran prepared above into a 250 mL three-necked flask, and place it in an ultrasonic cleaner. Under the protection of inert gas and ultrasonic conditions, 22 mL of a mixture of lithium triethylborohydride and 50 mL of tetrahydrofuran was added dropwise to the three-necked flask for 30 minutes. After the addition, the reaction was continued for 1 hour. After the completion of the reaction, 500mL ethanol was added to the three-necked flask for precipitation, and the upper liquid was decanted. The resulting solid mixture was dissolved in 20mL tetrahydrofuran and precipitated with ethanol. Repeated 3 times, finally filtered and dried to obtain polymethacrylic acid. Compound of methyl ester and zero-valent nano-iron.
[0105] Mix 1mL methyl methacrylate, 0.0156g polymethyl methacrylate and zero-valent nano-iron complex, 0.0128g chain transfer agent isobutyronitrile dithionaphthoate (CPDN) and 55.2μL hexadecane. The oil phase mixture is obtained, and then under magnetic stirring, the oil phase and 4 mL of Brij98 solution with a mass concentration of 2.3% are stirred and pre-emulsified for 30 minutes, then treated with an ultrasonic cell pulverizer for 6 minutes, and then transferred to an ampoule and frozen- After pumping and thawing 3 times, the inert gas is introduced and the tube is melted and sealed, put in a magnetic stirrer, and reacted at a speed of 1200 rpm and 60°C. After 80 hours of reaction, a polymer coated with zero-valent nano iron is obtained. Methyl methacrylate.

PUM

PropertyMeasurementUnit
Particle size210.0nm

Description & Claims & Application Information

We can also present the details of the Description, Claims and Application information to help users get a comprehensive understanding of the technical details of the patent, such as background art, summary of invention, brief description of drawings, description of embodiments, and other original content. On the other hand, users can also determine the specific scope of protection of the technology through the list of claims; as well as understand the changes in the life cycle of the technology with the presentation of the patent timeline. Login to view more.
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products