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Polymer containing pyridine ring and composition magnetic membrane material and preparation method thereof

A technology of magnetic film and pyridine ring, applied in the application of magnetic film to substrate, magnetic layer, organic chemistry, etc., to achieve the effect of low hysteresis loss, easy processing and wide application prospects

Inactive Publication Date: 2010-05-19
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0002] With the continuous progress of social productivity and human civilization, many new industries and innovative technologies continue to develop, and natural magnetic materials can no longer meet people's requirements

Method used

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  • Polymer containing pyridine ring and composition magnetic membrane material and preparation method thereof
  • Polymer containing pyridine ring and composition magnetic membrane material and preparation method thereof
  • Polymer containing pyridine ring and composition magnetic membrane material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Embodiment 1: the preparation method of 4-methacrylamidopyridine monomer (4-MAAP)

[0033] At 0°C, dissolve 2.12g (0.0212mol) of methacryloyl chloride (MAC) in 10ml of anhydrous tetrahydrofuran (THF), and slowly add the above solution dropwise to the solution containing 4-aminopyridine (2g, 0.0212mol) and triethylamine (3ml, 0.0212mol) in 60ml of anhydrous THF solution. After the dropwise addition, put it in an ice bath to react for 24 hours, filter it with suction, and wash it thoroughly with THF. At room temperature, the resulting filtrate and washings were concentrated in vacuo to obtain a light yellow solid, which was then washed with 5% Na 2 CO 3 Wash with aqueous solution and deionized water, and dry in a vacuum oven at room temperature for 24 hours. The dried solid was dissolved in 8 ml of THF, poured into 400 ml of n-hexane, and left to stand overnight to obtain white needle-like crystals which were 4-methacrylamidopyridine monomer (4-MAAP). Yield: 80%, mp 1...

Embodiment 2

[0034] Embodiment 2: the preparation method of 3-methacrylamidopyridine monomer (3-MAAP)

[0035]Place a single-necked flask containing 3-aminopyridine (2g, 0.0212mol), triethylamine (6ml, 0.0424mol), hydroquinone (0.1g) and 40ml of anhydrous THF in an ice-salt bath below 0°C, While stirring, 10 ml of anhydrous THF dissolved with methacryloyl chloride (2.12 g, 0.0212 mol) was slowly added to the flask. After the dropwise addition, continue to react in the ice-salt bath for 8h. The reaction solution was taken out and filtered with suction, and washed thoroughly with THF. The resulting lower layer was concentrated in vacuo at room temperature to give an oil. Use acetone as the eluent to pass through the column, and then recrystallize through ether to obtain milky white needle crystals which are 3-methacrylamidopyridine monomer (3-MAAP). Yield: 85%, mp 85-86°C. FT-IR (KBr, cm -1 ):v 3438(w), 3226-2851(m), 1668(s), 1629(s), 1600(s), 1548(s), 1485(s), 1414(s), 1373(s), 1336(s...

Embodiment 3

[0036] Embodiment 3: the preparation that contains the polymkeric substance (P4MAAP) of p-pyridine ring

[0037] Add 0.5g of 4-methacrylamidopyridine monomer (4-MAAP), 0.005g of azobisisobutyronitrile (AIBN) and 3ml of anhydrous THF into a dry polymerization bottle, freeze, melt and degas three times. React in an oil bath at 65°C for 24h. The reaction solution was precipitated in ether, filtered, and the resulting white solid P4MAAP was washed repeatedly with ether and THF, and dried in vacuum at 60°C for 48h. Yield: 75%, intrinsic viscosity: [η] = 14.0ml / g (DMF, 30°C). FT-IR (KBr, cm -1 ): v 3390-2980(m), 1686(m), 1590(s), 1509(s), 1415(m), 1328(m), 1285(m), 1211(m), 1150(m), 1001(m), 825(m). 1 H NMR (DMSO-d 6 ): δ (ppm) 0.90-1.07 (m, 3H, CH 3 ), 1.73-2.06 (m, 2H, CH 2 ), 7.52 (s, 2H, 2, 6-PyH), 8.31 (s, 2H, 3, 5-PyH), 9.42 (s, 1H, NH).

[0038] The structural formula is

[0039]

[0040] In the formula, Py is para-pyridine, and n is a chain link of a polymer.

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Abstract

The invention relates to a polymer containing pyridine ring and a composition magnetic membrane material and a preparation method thereof. The material is prepared by a layer-by-layer self-assemble method which comprises the following steps of: synthetizing a ligandpolymer containing pyridine ring side-chains and then carrying out the layer-by-layer self-assembly with a transition metal salt of polystyrolsulfon acid on a high density polyethylene membrane matrix by taking coordination mutual action as the driving force. The macromolecule magnetic membrane material is prepared by firstly utilizing the polymer containing pyridine ring side-chains, has novel, simple and easy preparation method, stable magnetic performance, high saturation intensity, low magnetic hysteresis loss, light weight, easy shaping process and is not limited by the shape of the matrix, thereby being an organic soft iron magnetic membrane material with excellent application prospect.

Description

technical field [0001] The invention relates to a polymer containing a pyridine ring and its complex magnetic film material and a preparation method. Background technique [0002] With the continuous progress of social productivity and human civilization, many new industries and innovative technologies continue to develop, and natural magnetic materials can no longer meet people's requirements. In 1985, Miller et al. of DuPont reported for the first time that the electron donor FeCp, which is neither magnetic, * 2 and receptor TCNE (Cp * : pentamethylcyclopentadiene, TCNE: tetracyanoethylene) after coordination, the electron transfer complex obtained by the charge transfer from the donor to the acceptor is the first molecular magnet. Since then, polymers and organic magnetic materials have developed rapidly due to their excellent performance and characteristics, and have attracted more and more attention from domestic and foreign scholars. For decades, countries all over...

Claims

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Application Information

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IPC IPC(8): C08F120/60C07D213/75H01F10/10H01F41/24
Inventor 孙维林林维红阳俊沈之荃
Owner ZHEJIANG UNIV
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