CN109054364A - A kind of magnetism nylon material and preparation method thereof - Google Patents
A kind of magnetism nylon material and preparation method thereof Download PDFInfo
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- CN109054364A CN109054364A CN201810759906.XA CN201810759906A CN109054364A CN 109054364 A CN109054364 A CN 109054364A CN 201810759906 A CN201810759906 A CN 201810759906A CN 109054364 A CN109054364 A CN 109054364A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
- C08L77/02—Polyamides derived from omega-amino carboxylic acids or from lactams thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/08—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from amino-carboxylic acids
- C08G69/14—Lactams
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2265—Oxides; Hydroxides of metals of iron
- C08K2003/2275—Ferroso-ferric oxide (Fe3O4)
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/01—Magnetic additives
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- Compositions Of Macromolecular Compounds (AREA)
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Abstract
The invention discloses a kind of magnetic nylon materials, it is composed of the following raw materials by weight: caprolactam 120-150, initiator 4-5, four water frerrous chloride 20-30, ferric chloride (FeCl36H2O) 20-30, polyisoprene 1-2, lauryl mercaptan 3-4, tributyl tin trichloride 0.1-0.2, stearic acid 2-5, benzotriazole 0.7-1, dispersing agent 1-2, the present invention is with the modified caprolactam monomer of benzotriazole, with four water frerrous chlorides, ferric chloride (FeCl36H2O) is presoma blending, it polymerize under initiator effect, ammonium hydroxide is added dropwise after polymerization, obtain magnetic polymer, the magnetic polymer solution of alcohol-containing is mixed with stearic acid later, high temperature esterification, further improve dispersion performance of the magnetic particle between polymer, it ensure that the stability and mechanics of magnetic property Stability_intensity.
Description
Technical field
The invention belongs to Material Fields, and in particular to a kind of magnetism nylon material and preparation method thereof.
Background technique
Nylon has very strong vitality, it is modified to essentially consist in it as most important kind maximum in engineering plastics
Realize high performance, the followed by requirement high performance to product of the industries itself such as automobile, electric appliance, communication, electronics, machinery increasingly
Strongly, the rapid development of related industry promotes the process of engineering plastics high performance, and modification of nylon future developing trend is such as
Under: 1. the market demand of high-intensitive high rigidity nylon is increasing, and new reinforcing material such as inorganic crystal whisker enhancing, carbon fiber increase
Strong PA will become important kind, be mainly used for automotive engine component, mechanical part and air equipment component.2. nylon
Alloying will become the mainstream of modified engineered plastic development.Nylon alloy is the realization high performance important channel of nylon, and
Manufacture nylon, nylon PP Pipe Compound, the main means for improving properties of nylons.By blending other high polymers, to improve the suction of nylon
It is aqueous, improve dimensional stability and black brittleness, the heat resistance and wearability of product.To be applicable in what car type difference required
Purposes.3. the manufacturing technology of nano-nylon will be rapidly developed with application.The advantages of nano-nylon, is its hot property, mechanics
Performance, anti-flammability, barrier property are higher than pure nylon, and manufacturing cost is suitable with common nylon.Thus, there is very big competitiveness.
4. for electronics, electrical, the fire-retardant nylon of electric appliance is growing day by day, attention of the greenization fire-retardant nylon increasingly by market.⑤
Antistatic, electroconductive nylon and magnetic nylon will become the preferred material of electronic equipment, mining machinery, textile machine.6. processing
The research and application of auxiliary agent will push the functionalization of modification of nylon, the process of high performance.7. polytechnic application, product
Fining be push its industry development power；
Magnetic nanoparticle is concerned, especially ferroso-ferric oxide (and nanometer di-iron trioxide (nanoparticle, because
For their intensity of magnetization height, toxicity is low, and has practical application at many aspects, be such as used as magnetic resonance imaging reinforcing agent,
Biofluid, can also be removed from office to drug release, cell is separated, prepare it is various for magnetic materials；
The object of the invention is to prepare a kind of nylon material of magnetic coupling, to expand the application range of composite material.
Summary of the invention
In view of the defects and deficiencies of the prior art, the present invention intends to provide a kind of magnetic nylon material and its preparations
Method.
To achieve the above object, the invention adopts the following technical scheme:
A kind of magnetism nylon material, it is composed of the following raw materials by weight:
Caprolactam 120-150, initiator 4-5, four water frerrous chloride 20-30, ferric chloride (FeCl36H2O) 20-30, poly- isoamyl
Diene 1-2, lauryl mercaptan 3-4, tributyl tin trichloride 0.1-0.2, stearic acid 2-5, benzotriazole 0.7-1, dispersion
Agent 1-2.
The dispersing agent is polysorbate, lauric acid amide of ethanol.
The initiator is cumyl peroxide, dibenzoyl peroxide.
A kind of preparation method of magnetism nylon material, comprising the following steps:
(1) initiator is taken, is added in the dehydrated alcohol of 20-30 times of its weight, stirs evenly；
(2) benzotriazole, caprolactam mixing are taken, insulated and stirred 10-40 minutes at 50-55 DEG C, is added to mixing
In the dehydrated alcohol of 6-9 times of weight of material, stirs evenly, obtain modified monomer solution；
(3) four water frerrous chlorides, ferric chloride (FeCl36H2O) mixing are taken, the deionized water of 20-30 times of mixture weight is added to
In, it stirs evenly, mixes, be sent in reaction kettle with above-mentioned modified monomer solution, be passed through nitrogen, adjusting temperature of reaction kettle is
65-70 DEG C, above-mentioned initiator solution is added, insulated and stirred 3-5 hours, the ammonium hydroxide that concentration is 6-8% is added dropwise, adjusting pH is 10-
12, stirring at normal temperature 4-6 hours, discharging cooling obtained magnetic polymer solution；
(4) stearic acid, polyisoprene mixing are taken, insulated and stirred 1-2 hours at 50-55 DEG C, is added to mixture weight
It is 20-30 minutes ultrasonic in the deionized water of 10-17 times of amount, obtain stearic acid dispersion liquid；
(5) above-mentioned magnetic polymer solution, the mixing of stearic acid dispersion liquid are taken, is stirred evenly, increasing temperature is 90-95 DEG C,
Insulated and stirred 2-3 hours, remaining each raw material is added, stirring to room temperature filters, filter cake is washed, dry 1- at 55-60 DEG C of vacuum
It 2 hours, is cooled to room temperature to get the magnetic nylon material.
Advantages of the present invention:
The present invention is forerunner with four water frerrous chlorides, ferric chloride (FeCl36H2O) with the modified caprolactam monomer of benzotriazole
Body is blended, and polymerize under initiator effect, ammonium hydroxide is added dropwise after polymerization, obtains magnetic polymer, later by the magnetic polymeric of alcohol-containing
Object solution is mixed with stearic acid, high temperature esterification, is further improved dispersion performance of the magnetic particle between polymer, be ensure that magnetic
The stability and mechanical stability intensity of performance.
Specific embodiment
Embodiment 1
A kind of magnetism nylon material, it is composed of the following raw materials by weight:
Caprolactam 150, initiator 5, four water frerrous chlorides 30, ferric chloride (FeCl36H2O) 30, polyisoprene 2, dodecane
Base mercaptan 4, tributyl tin trichloride 0.2, stearic acid 5, benzotriazole 1, dispersing agent 2.
The dispersing agent is lauric acid amide of ethanol.
The initiator dibenzoyl peroxide.
A kind of preparation method of magnetism nylon material, comprising the following steps:
(1) initiator is taken, is added in the dehydrated alcohol of 30 times of its weight, stirs evenly；
(2) benzotriazole, caprolactam mixing are taken, insulated and stirred 40 minutes at 55 DEG C are added to mixture weight 9
In dehydrated alcohol again, stirs evenly, obtain modified monomer solution；
(3) four water frerrous chlorides, ferric chloride (FeCl36H2O) mixing are taken, the deionized water of 20-30 times of mixture weight is added to
In, it stirs evenly, mixes, be sent in reaction kettle with above-mentioned modified monomer solution, be passed through nitrogen, adjusting temperature of reaction kettle is 70
DEG C, above-mentioned initiator solution is added, insulated and stirred 5 hours, the ammonium hydroxide that concentration is 8% is added dropwise, adjusting pH is 12, stirring at normal temperature 6
Hour, discharging cooling obtains magnetic polymer solution；
(4) stearic acid, polyisoprene mixing are taken, insulated and stirred 2 hours at 55 DEG C are added to 17 times of mixture weight
Deionized water in, ultrasound 30 minutes, obtain stearic acid dispersion liquid；
(5) above-mentioned magnetic polymer solution, the mixing of stearic acid dispersion liquid are taken, is stirred evenly, increasing temperature is 95 DEG C, heat preservation
Remaining each raw material is added in stirring 3 hours, and stirring to room temperature filters, filter cake is washed, 2 hours dry at 60 DEG C of vacuum, cooling
To room temperature to get the magnetic nylon material.
Embodiment 2
A kind of magnetism nylon material, it is composed of the following raw materials by weight:
Caprolactam 120, initiator 4, four water frerrous chlorides 20, ferric chloride (FeCl36H2O) 20, polyisoprene 1, dodecane
Base mercaptan 3, tributyl tin trichloride 0.1, stearic acid 2, benzotriazole 0.7, dispersing agent 1.
The dispersing agent is polysorbate.
The initiator is cumyl peroxide.
A kind of preparation method of magnetism nylon material, comprising the following steps:
(1) initiator is taken, is added in the dehydrated alcohol of 20 times of its weight, stirs evenly；
(2) benzotriazole, caprolactam mixing are taken, insulated and stirred 10 minutes at 50 DEG C are added to mixture weight 6
In dehydrated alcohol again, stirs evenly, obtain modified monomer solution；
(3) four water frerrous chlorides, ferric chloride (FeCl36H2O) mixing are taken, are added in 20 times of mixture weight of deionized water,
It stirs evenly, mixes, be sent in reaction kettle with above-mentioned modified monomer solution, be passed through nitrogen, adjusting temperature of reaction kettle is 65 DEG C,
Above-mentioned initiator solution is added, insulated and stirred 3 hours, the ammonium hydroxide that concentration is 6% is added dropwise, adjusting pH is 10, and stirring at normal temperature 4 is small
When, discharging cooling obtains magnetic polymer solution；
(4) stearic acid, polyisoprene mixing are taken, insulated and stirred 1 hour at 50 DEG C is added to 10 times of mixture weight
Deionized water in, ultrasound 20 minutes, obtain stearic acid dispersion liquid；
(5) above-mentioned magnetic polymer solution, the mixing of stearic acid dispersion liquid are taken, is stirred evenly, increasing temperature is 90 DEG C, heat preservation
Remaining each raw material is added in stirring 2 hours, and stirring to room temperature filters, filter cake is washed, 1 hour dry at 55 DEG C of vacuum, cooling
To room temperature to get the magnetic nylon material.
Performance test:
The saturation magnetization of the magnetic nylon material of the embodiment of the present invention 1 is 10.1emu/g, tensile strength is
26.3Mpa；
The saturation magnetization of the magnetic nylon material of the embodiment of the present invention 2 is 10.3emu/g, tensile strength is
27.0Mpa。
Claims (4)
1. a kind of magnetism nylon material, which is characterized in that it is composed of the following raw materials by weight:
Caprolactam 120-150, initiator 4-5, four water frerrous chloride 20-30, ferric chloride (FeCl36H2O) 20-30, polyisoprene
1-2, lauryl mercaptan 3-4, tributyl tin trichloride 0.1-0.2, stearic acid 2-5, benzotriazole 0.7-1, dispersing agent 1-
2。
2. a kind of magnetic nylon material according to claim 1, which is characterized in that the dispersing agent be polysorbate,
Lauric acid amide of ethanol.
3. a kind of magnetic nylon material according to claim 1, which is characterized in that the initiator is that peroxidating two is different
Propyl benzene, dibenzoyl peroxide.
4. a kind of preparation method of magnetic nylon material as described in claim 1, which comprises the following steps:
(1) initiator is taken, is added in the dehydrated alcohol of 20-30 times of its weight, stirs evenly；
(2) benzotriazole, caprolactam mixing are taken, insulated and stirred 10-40 minutes at 50-55 DEG C, is added to mixture weight
In the dehydrated alcohol of 6-9 times of amount, stirs evenly, obtain modified monomer solution；
(3) four water frerrous chlorides, ferric chloride (FeCl36H2O) mixing are taken, is added in the deionized water of 20-30 times of mixture weight, stirs
It mixes uniformly, mixes, be sent in reaction kettle with above-mentioned modified monomer solution, be passed through nitrogen, adjusting temperature of reaction kettle is 65-70
DEG C, above-mentioned initiator solution is added, insulated and stirred 3-5 hours, the ammonium hydroxide that concentration is 6-8% is added dropwise, adjusting pH is 10-12, often
Temperature stirring 4-6 hours, discharging cooling, obtains magnetic polymer solution；
(4) stearic acid, polyisoprene mixing are taken, insulated and stirred 1-2 hours at 50-55 DEG C, is added to mixture weight 10-
It is 20-30 minutes ultrasonic in 17 times of deionized water, obtain stearic acid dispersion liquid；
(5) above-mentioned magnetic polymer solution, the mixing of stearic acid dispersion liquid are taken, is stirred evenly, increasing temperature is 90-95 DEG C, heat preservation
Remaining each raw material is added in stirring 2-3 hours, and stirring to room temperature filters, filter cake is washed, and dry 1-2 is small at 55-60 DEG C of vacuum
When, it is cooled to room temperature to get the magnetic nylon material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201810759906.XA CN109054364A (en) | 2018-07-11 | 2018-07-11 | A kind of magnetism nylon material and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810759906.XA CN109054364A (en) | 2018-07-11 | 2018-07-11 | A kind of magnetism nylon material and preparation method thereof |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0971721A (en) * | 1995-09-06 | 1997-03-18 | Unitika Ltd | Magnetic plastic composition |
| CN102477220A (en) * | 2010-11-23 | 2012-05-30 | 合肥杰事杰新材料股份有限公司 | Magnetic nylon microspheres with controllable particle size and preparation method thereof |
| CN105062047A (en) * | 2015-07-29 | 2015-11-18 | 苏州荣昌复合材料有限公司 | Preparation method of magnetic adsorption nylon material |
| CN106893311A (en) * | 2015-12-18 | 2017-06-27 | 上海杰事杰新材料(集团)股份有限公司 | A kind of magnetic Nano polymer composite and preparation method thereof |
-
2018
- 2018-07-11 CN CN201810759906.XA patent/CN109054364A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0971721A (en) * | 1995-09-06 | 1997-03-18 | Unitika Ltd | Magnetic plastic composition |
| CN102477220A (en) * | 2010-11-23 | 2012-05-30 | 合肥杰事杰新材料股份有限公司 | Magnetic nylon microspheres with controllable particle size and preparation method thereof |
| CN105062047A (en) * | 2015-07-29 | 2015-11-18 | 苏州荣昌复合材料有限公司 | Preparation method of magnetic adsorption nylon material |
| CN106893311A (en) * | 2015-12-18 | 2017-06-27 | 上海杰事杰新材料(集团)股份有限公司 | A kind of magnetic Nano polymer composite and preparation method thereof |
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Application publication date: 20181221 |
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