[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.
