CN105670286A - Alkali-corrosion-resistant organic magnetic material and preparation method thereof - Google Patents

Alkali-corrosion-resistant organic magnetic material and preparation method thereof Download PDF

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CN105670286A
CN105670286A CN201610223404.6A CN201610223404A CN105670286A CN 105670286 A CN105670286 A CN 105670286A CN 201610223404 A CN201610223404 A CN 201610223404A CN 105670286 A CN105670286 A CN 105670286A
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parts
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resin
corrosion resistance
metallic material
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邹黎清
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SUZHOU KEMAO ELECTRONIC MATERIAL TECHNOLOGY Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L79/00Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen or carbon only, not provided for in groups C08L61/00 - C08L77/00
    • C08L79/04Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
    • C08L79/08Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/42Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of organic or organo-metallic materials, e.g. graphene
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/01Magnetic additives
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/014Additives containing two or more different additives of the same subgroup in C08K
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/03Polymer mixtures characterised by other features containing three or more polymers in a blend

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  • Engineering & Computer Science (AREA)
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Abstract

The invention discloses an alkali-corrosion-resistant organic magnetic material.The alkali-corrosion-resistant organic magnetic material is prepared from, by weight, 15-25 parts of acetylferrocene, 3-10 parts of ferrous lactate, 5-10 parts of cupric tartrate trihydrate, 2-6 parts of copper disodium EDTA, 10-13 parts of ABS resin, 2-5 parts of ferric stearate, 9-15 parts of 4-cyclohexyl resin, 12-16 parts of polyimide resin, 10-20 parts of 2, 4-symplectic dialdehyde, 6-10 parts of 2-acetylthiophene ethylene acetal, 5-9 parts of 1-(2-pyridine azo)-2-naphthol, 4-8 parts of dinonyl phthalate and 6-12 parts of ethyl 9-fluorenylideneacetate.The organic magnetic material has good alkali resistance, and operation safety is improved.

Description

A kind of alkali corrosion resistance organo-metallic material and its preparation method
Technical field
The invention belongs to field of magnetic material preparation, it is specifically related to a kind of alkali corrosion resistance organo-metallic material and its preparation method.
Background technology
Magneticsubstance, usually said magneticsubstance refers to ferromagnetic substance, is ancient and purposes functional materials very widely. Modem magnetic materials has been used among our life widely, such as, permanent magnet material is used as motor, the core material being applied in transformer, as the magneto-optic disk that storer uses, and computer magnetic recording floppy disk etc. Saying in big bit information, magneticsubstance is closely related with the every aspect of informationization, automatization, electromechanical integration, national defence, national economy. And it has been generally acknowledged that, magneticsubstance refers to the material that can directly or indirectly produce magnetic by transition element iron, cobalt, nickel and alloy thereof etc. Magneticsubstance can be divided into soft magnetic material and retentive material by the difficulty or ease of degaussing after magnetization. The material easily removing magnetic after magnetization is soft magnetic material, it is not easy to the material of degaussing is retentive material. Soft magnetic material remanent magnetism is less in general, and retentive material remanent magnetism is bigger. For a long time, traditional strong magnetic material is all the inorganic materials such as rare earth metals element, and along with the development of magneticsubstance and magnetics theory, organo-metallic material becomes new research focus gradually; And owing to there is alkaline corrosion risk in some Working environments, the alkali corrosion resistance performance thus how improving organo-metallic material is necessary.
Summary of the invention
For the above technical problem existed in prior art, the present invention provides a kind of alkali corrosion resistance organo-metallic material and its preparation method, and this organo-metallic material possesses good alkaline resistance properties, it is to increase operational safety performance.
Technical scheme: a kind of alkali corrosion resistance organo-metallic material; comprise the composition of following weight part number: ferrocenyl methyl ketone 15-25 part, iron lactate 3-10 part, 2; 3-dihydroxysuccinic acid copper 5-10 part, cupric ethylene diamine tetraacetate sodium 2-6 part, ABS resin 10-13 part, iron stearate 2-5 part, 4-cyclohexyl resin 9-15 part, polyimide resin 12-16 part, 2,4-suberic aldehyde 10-20 part, 2-acetyl thiophene ethylene acetal 6-10 part, 1-(2-pyridylazo)-beta naphthal 5-9 part, dinonyl phthalate 4-8 part, 9-fluorenylidene ethyl acetate 6-12 part.
Preferably; described ferrocenyl methyl ketone 18-22 part, iron lactate 5-8 part, 2; 3-dihydroxysuccinic acid copper 7-9 part, cupric ethylene diamine tetraacetate sodium 3-5 part, ABS resin 11-13 part, iron stearate 3-5 part, 4-cyclohexyl resin 11-14 part, polyimide resin 13-15 part, 2,4-suberic aldehyde 15-18 part, 2-acetyl thiophene ethylene acetal 7-10 part, 1-(2-pyridylazo)-beta naphthal 6-8 part, dinonyl phthalate 5-7 part, 9-fluorenylidene ethyl acetate 8-10 part.
Preferably; described ferrocenyl methyl ketone 20 parts, iron lactate 7 parts, 2; 3-dihydroxysuccinic acid copper 8 parts, 4 parts, cupric ethylene diamine tetraacetate sodium, ABS resin 12 parts, iron stearate 4 parts, 4-cyclohexyl resin 13 parts, polyimide resin 14 parts, 2,4-suberic aldehyde 17 parts, 2-acetyl thiophene ethylene acetal 8 parts, 1-(2-pyridylazo)-beta naphthal 7 parts, dinonyl phthalate 6 parts, 9-fluorenylidene ethyl acetate 9 parts.
A preparation method for alkali corrosion resistance organo-metallic material, comprises the steps:
(1) by ferrocenyl methyl ketone 15-25 part, iron lactate 3-10 part, 2,3-dihydroxysuccinic acid copper 5-10 part, cupric ethylene diamine tetraacetate sodium 2-6 part, ABS resin 10-13 part and iron stearate 2-5 part add in the reactor leading to nitrogen, with speed 2-5 DEG C/min, temperature is risen to 100-120 DEG C, treat that temperature stirs 10-15min fast with speed 200-400r/min after reaching, obtain solution A;
(2) by 4-cyclohexyl resin 9-15 part, polyimide resin 12-16 part, 2,4-suberic aldehyde 10-20 part, 1-(2-pyridylazo)-beta naphthal 5-9 part, dinonyl phthalate 4-8 part and 9-fluorenylidene ethyl acetate 6-12 part add in reactor, rapidly temperature is risen to 130-150 DEG C, reaction 20-30min, obtains solution B;
(3) 2-acetyl thiophene ethylene acetal 6-10 part is added in solution B, solution A, adopt microwave heating method, in power 3000W-5000W, heat 5-8min; Described alkali corrosion resistance organo-metallic material can be obtained subsequently after cooling.
Preferably, the speed heated up in step (1) is 3 DEG C/min, and temperature is 110 DEG C, and the speed of stirring is 300r/min, stirs 13min.
Preferably, in step (2), temperature is 135 DEG C, reaction 25min.
Preferably, in step (3), power is 3500W, heating 7min.
Useful effect:The preparation method of a kind of alkali corrosion resistance organo-metallic material of the present invention, based on iron content organic substance, makes the dispersion of iron content organic substance better by 2-acetyl thiophene ethylene acetal, it is to increase the magnetic of overall magneticsubstance; Simultaneously additional with other chemical materials, it is to increase the corrosion resistance nature of organo-metallic material, especially alkaline resistance properties; After tested, after recycling 1500 times in the alkaline environment of PH=12, Coercive Force decay only has 6%.
Embodiment
Embodiment 1
(1) by ferrocenyl methyl ketone 15 parts, iron lactate 3 parts, 2,3-dihydroxysuccinic acid copper 5 parts, 2 parts, cupric ethylene diamine tetraacetate sodium, ABS resin 10 parts and iron stearate 2 parts add in the reactor leading to nitrogen, with speed 2 DEG C/min, temperature is risen to 100 DEG C, treat that temperature stirs 10min fast with speed 200r/min after reaching, obtain solution A;
(2) by 4-cyclohexyl resin 9 parts, polyimide resin 12 parts, 2,4-suberic aldehyde 10 parts, 1-(2-pyridylazo)-beta naphthal 5 parts, dinonyl phthalate 4 parts and 9-fluorenylidene ethyl acetate 6 parts add in reactor, rapidly temperature is risen to 130 DEG C, reaction 20min, obtains solution B;
(3) 2-acetyl thiophene ethylene acetal 6 parts is added in solution B, solution A, adopt microwave heating method, in power 3000W, heat 5min; Described alkali corrosion resistance organo-metallic material can be obtained subsequently after cooling.
Comparative example 1
(1) ferrocenyl methyl ketone 15 parts, iron lactate 3 parts, ABS resin 10 parts and iron stearate 2 parts are added in the reactor leading to nitrogen, with speed 2 DEG C/min, temperature is risen to 100 DEG C, treat that temperature stirs 10min fast with speed 200r/min after reaching, obtain solution A;
(2) adding in reactor by 4-cyclohexyl resin 9 parts and 2,4-suberic aldehyde 10 parts, rapidly temperature rises to 130 DEG C, reaction 20min, obtains solution B;
(3) solution B and solution A are mixed, adopt microwave heating method, in power 3000W, heat 5min; Magneticsubstance can be obtained subsequently after cooling.
Embodiment 2
(1) by ferrocenyl methyl ketone 25 parts, iron lactate 10 parts, 2,3-dihydroxysuccinic acid copper 10 parts, 6 parts, cupric ethylene diamine tetraacetate sodium, ABS resin 13 parts and iron stearate 5 parts add in the reactor leading to nitrogen, with speed 5 DEG C/min, temperature is risen to 120 DEG C, treat that temperature stirs 15min fast with speed 400r/min after reaching, obtain solution A;
(2) by 4-cyclohexyl resin 15 parts, polyimide resin 16 parts, 2,4-suberic aldehyde 20 parts, 1-(2-pyridylazo)-beta naphthal 9 parts, dinonyl phthalate 8 parts and 9-fluorenylidene ethyl acetate 12 parts add in reactor, rapidly temperature is risen to 150 DEG C, reaction 30min, obtains solution B;
(3) 2-acetyl thiophene ethylene acetal 10 parts is added in solution B, solution A, adopt microwave heating method, in power 5000W, heat 8min; Described alkali corrosion resistance organo-metallic material can be obtained subsequently after cooling.
Comparative example 2
(1) ferrocenyl methyl ketone 25 parts, iron lactate 10 parts, ABS resin 13 parts and iron stearate 5 parts are added in the reactor leading to nitrogen, with speed 5 DEG C/min, temperature is risen to 120 DEG C, treat that temperature stirs 15min fast with speed 400r/min after reaching, obtain solution A;
(2) adding in reactor by 4-cyclohexyl resin 15 parts and 2,4-suberic aldehyde 20 parts, rapidly temperature rises to 150 DEG C, reaction 30min, obtains solution B;
(3) solution B and solution A are mixed, adopt microwave heating method, in power 5000W, heat 8min; Magneticsubstance can be obtained subsequently after cooling.
Embodiment 3
(1) by ferrocenyl methyl ketone 18 parts, iron lactate 5 parts, 2,3-dihydroxysuccinic acid copper 7 parts, 3 parts, cupric ethylene diamine tetraacetate sodium, ABS resin 11 parts and iron stearate 3 parts add in the reactor leading to nitrogen, with speed 2 DEG C/min, temperature is risen to 100 DEG C, treat that temperature stirs 10min fast with speed 200r/min after reaching, obtain solution A;
(2) by 4-cyclohexyl resin 9 parts, polyimide resin 12 parts, 2,4-suberic aldehyde 10 parts, 1-(2-pyridylazo)-beta naphthal 5 parts, dinonyl phthalate 4 parts and 9-fluorenylidene ethyl acetate 6 parts add in reactor, rapidly temperature is risen to 130 DEG C, reaction 20min, obtains solution B;
(3) 2-acetyl thiophene ethylene acetal 7 parts is added in solution B, solution A, adopt microwave heating method, in power 3000W, heat 5min; Described alkali corrosion resistance organo-metallic material can be obtained subsequently after cooling.
Embodiment 4
(1) by ferrocenyl methyl ketone 22 parts, iron lactate 8 parts, 2,3-dihydroxysuccinic acid copper 9 parts, 5 parts, cupric ethylene diamine tetraacetate sodium, ABS resin 13 parts and iron stearate 5 parts add in the reactor leading to nitrogen, with speed 5 DEG C/min, temperature is risen to 120 DEG C, treat that temperature stirs 15min fast with speed 400r/min after reaching, obtain solution A;
(2) by 4-cyclohexyl resin 15 parts, polyimide resin 16 parts, 2,4-suberic aldehyde 20 parts, 1-(2-pyridylazo)-beta naphthal 9 parts, dinonyl phthalate 8 parts and 9-fluorenylidene ethyl acetate 12 parts add in reactor, rapidly temperature is risen to 150 DEG C, reaction 30min, obtains solution B;
(3) 2-acetyl thiophene ethylene acetal 10 parts is added in solution B, solution A, adopt microwave heating method, in power 5000W, heat 8min; Described alkali corrosion resistance organo-metallic material can be obtained subsequently after cooling.
Embodiment 5
(1) by ferrocenyl methyl ketone 20 parts, iron lactate 7 parts, 2,3-dihydroxysuccinic acid copper 8 parts, 4 parts, cupric ethylene diamine tetraacetate sodium, ABS resin 12 parts and iron stearate 4 parts add in the reactor leading to nitrogen, with speed 3 DEG C/min, temperature is risen to 110 DEG C, treat that temperature stirs 13min fast with speed 300r/min after reaching, obtain solution A;
(2) by 4-cyclohexyl resin 13 parts, polyimide resin 14 parts, 2,4-suberic aldehyde 17 parts, 1-(2-pyridylazo)-beta naphthal 7 parts, dinonyl phthalate 6 parts and 9-fluorenylidene ethyl acetate 9 parts add in reactor, rapidly temperature is risen to 135 DEG C, reaction 25min, obtains solution B;
(3) 2-acetyl thiophene ethylene acetal 8 parts is added in solution B, solution A, adopt microwave heating method, in power 3500W, heat 7min; Described alkali corrosion resistance organo-metallic material can be obtained subsequently after cooling.
Detecting in each embodiment above-mentioned and comparative example the performance of the magneticsubstance obtained, result is such as following table:

Claims (7)

1. an alkali corrosion resistance organo-metallic material; it is characterized in that; comprise the composition of following weight part number: ferrocenyl methyl ketone 15-25 part, iron lactate 3-10 part, 2; 3-dihydroxysuccinic acid copper 5-10 part, cupric ethylene diamine tetraacetate sodium 2-6 part, ABS resin 10-13 part, iron stearate 2-5 part, 4-cyclohexyl resin 9-15 part, polyimide resin 12-16 part, 2,4-suberic aldehyde 10-20 part, 2-acetyl thiophene ethylene acetal 6-10 part, 1-(2-pyridylazo)-beta naphthal 5-9 part, dinonyl phthalate 4-8 part, 9-fluorenylidene ethyl acetate 6-12 part.
2. a kind of alkali corrosion resistance organo-metallic material according to claim 1; it is characterized in that; described ferrocenyl methyl ketone 18-22 part, iron lactate 5-8 part, 2; 3-dihydroxysuccinic acid copper 7-9 part, cupric ethylene diamine tetraacetate sodium 3-5 part, ABS resin 11-13 part, iron stearate 3-5 part, 4-cyclohexyl resin 11-14 part, polyimide resin 13-15 part, 2,4-suberic aldehyde 15-18 part, 2-acetyl thiophene ethylene acetal 7-10 part, 1-(2-pyridylazo)-beta naphthal 6-8 part, dinonyl phthalate 5-7 part, 9-fluorenylidene ethyl acetate 8-10 part.
3. a kind of alkali corrosion resistance organo-metallic material according to claim 2; it is characterized in that; described ferrocenyl methyl ketone 20 parts, iron lactate 7 parts, 2; 3-dihydroxysuccinic acid copper 8 parts, 4 parts, cupric ethylene diamine tetraacetate sodium, ABS resin 12 parts, iron stearate 4 parts, 4-cyclohexyl resin 13 parts, polyimide resin 14 parts, 2,4-suberic aldehyde 17 parts, 2-acetyl thiophene ethylene acetal 8 parts, 1-(2-pyridylazo)-beta naphthal 7 parts, dinonyl phthalate 6 parts, 9-fluorenylidene ethyl acetate 9 parts.
4. the preparation method of an alkali corrosion resistance organo-metallic material, it is characterised in that, comprise the steps:
(1) by ferrocenyl methyl ketone 15-25 part, iron lactate 3-10 part, 2,3-dihydroxysuccinic acid copper 5-10 part, cupric ethylene diamine tetraacetate sodium 2-6 part, ABS resin 10-13 part and iron stearate 2-5 part add in the reactor leading to nitrogen, with speed 2-5 DEG C/min, temperature is risen to 100-120 DEG C, treat that temperature stirs 10-15min fast with speed 200-400r/min after reaching, obtain solution A;
(2) by 4-cyclohexyl resin 9-15 part, polyimide resin 12-16 part, 2,4-suberic aldehyde 10-20 part, 1.1-(2-pyridylazo)-beta naphthal 5-9 part, dinonyl phthalate 4-8 part and 9-fluorenylidene ethyl acetate 6-12 part add in reactor, rapidly temperature is risen to 130-150 DEG C, reaction 20-30min, obtains solution B;
(3) 2-acetyl thiophene ethylene acetal 6-10 part is added in solution B, solution A, adopt microwave heating method, in power 3000W-5000W, heat 5-8min; Described alkali corrosion resistance organo-metallic material can be obtained subsequently after cooling.
5. the preparation method of a kind of alkali corrosion resistance organo-metallic material according to claim 4, it is characterised in that, the speed heated up in step (1) is 3 DEG C/min, and temperature is 110 DEG C, and the speed of stirring is 300r/min, stirs 13min.
6. the preparation method of a kind of alkali corrosion resistance organo-metallic material according to claim 4, it is characterised in that, in step (2), temperature is 135 DEG C, reaction 25min.
7. the preparation method of a kind of alkali corrosion resistance organo-metallic material according to claim 4, it is characterised in that, in step (3), power is 3500W, heating 7min.
CN201610223404.6A 2016-04-12 2016-04-12 Alkali-corrosion-resistant organic magnetic material and preparation method thereof Withdrawn CN105670286A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107731440A (en) * 2017-11-22 2018-02-23 苏州科茂电子材料科技有限公司 A kind of corrosion-resistant magnetic material and preparation method thereof
CN108264629A (en) * 2018-02-28 2018-07-10 华南理工大学 A kind of polyurethane associative thickener of double stimuli responsive and preparation method thereof
WO2019134360A1 (en) * 2018-01-05 2019-07-11 华南理工大学 An imide-type compound anionic material having room-temperature ferromagnetism and application thereof
US11084816B2 (en) 2018-01-05 2021-08-10 South China University Of Technology Anionic imide material having ferromagnetism at room temperature and the use thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1267893A (en) * 1999-03-17 2000-09-27 四川师范大学 Magnetic polymer base material and shapes of the material
CN1346135A (en) * 2000-09-26 2002-04-24 四川师范大学 Ultratvide frequency band metal organic compound magnetic material and ultrawide frequency band organic magnetic base material using same as base material

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1267893A (en) * 1999-03-17 2000-09-27 四川师范大学 Magnetic polymer base material and shapes of the material
CN1346135A (en) * 2000-09-26 2002-04-24 四川师范大学 Ultratvide frequency band metal organic compound magnetic material and ultrawide frequency band organic magnetic base material using same as base material

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107731440A (en) * 2017-11-22 2018-02-23 苏州科茂电子材料科技有限公司 A kind of corrosion-resistant magnetic material and preparation method thereof
WO2019134360A1 (en) * 2018-01-05 2019-07-11 华南理工大学 An imide-type compound anionic material having room-temperature ferromagnetism and application thereof
US11084816B2 (en) 2018-01-05 2021-08-10 South China University Of Technology Anionic imide material having ferromagnetism at room temperature and the use thereof
CN108264629A (en) * 2018-02-28 2018-07-10 华南理工大学 A kind of polyurethane associative thickener of double stimuli responsive and preparation method thereof

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Application publication date: 20160615