CN108411397A - A kind of magnetic fibre and preparation method thereof - Google Patents
A kind of magnetic fibre and preparation method thereof Download PDFInfo
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- CN108411397A CN108411397A CN201810309003.1A CN201810309003A CN108411397A CN 108411397 A CN108411397 A CN 108411397A CN 201810309003 A CN201810309003 A CN 201810309003A CN 108411397 A CN108411397 A CN 108411397A
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Classifications
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
- D01F6/54—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polymers of unsaturated nitriles
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F120/00—Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride, ester, amide, imide or nitrile thereof
- C08F120/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F120/42—Nitriles
- C08F120/44—Acrylonitrile
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
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- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention discloses a kind of magnetic fibres, it is made of the raw material of following weight parts：2 mercaptobenzimidazoles 0.5 1, filler 24, four water frerrous chlorides 20 30, ferric chloride (FeCl36H2O) 10 15, acrylonitrile 140 200, dibenzoyl peroxide 46, diacetone alcohol 23, glyceryl tristearate 12,10 12% formalin 30 40, ricinoleic acid 35,10 12% ammonium hydroxide 20 25, alkanolamide 67, p-methyl benzenesulfonic acid 0.03 0.1, triethylamine 0.4 0.5, the present invention carries out methylation reaction by catalyst of triethylamine, the mechanical stability of the polyacrylonitrile of finished product magnetic modification is further improved, fiber of the invention has stable magnetism.
Description
Technical field
The invention belongs to fiber arts, and in particular to a kind of magnetic fibre and preparation method thereof.
Background technology
Polyacrylonitrile is obtained through Raolical polymerizable by monomers acrylonitrile.Acrylonitrile unit in macromolecular chain is
Connect what head-tail mode was connected.It is mainly used for polyacrylonitrile fibre processed, the advantages of polyacrylonitrile fibre is weatherability and sun-resistant property
It is good, the 77% of original intensity can also be kept after 18 months in outdoor placement.It goes back chemical-resistant reagent, especially inorganic acid, bleaching
Powder, hydrogen peroxide and general organic reagent；The intensity of polyacrylonitrile fibre is not high, and wearability and fatigue resistance are also poor.It is poly-
The advantages of Dralon is weatherability；Polyacrylonitrile fibre and sun-resistant property are good, can also be kept after 18 months in outdoor placement
The 77% of original intensity.It goes back chemical-resistant reagent, especially inorganic acid, bleaching powder, hydrogen peroxide and general organic reagent.Poly- third
Alkene nitrile is unstable to alkali, meets alkali easy coloring, Sodium Polyacrylate can be hydrolyzed in 80 DEG C or more of concentrated base.In resilience and curling
Property aspect, there are prodigious gaps with wool.With the continuous development of synthetic fibers production technology, composite polypropylene nitrile fiber with
And various modified polyacrylonitriles occur in succession, such as high convergency, anti pilling, hydrophilic, antistatic, fire-retardant, fine denier, profiled-cross-section
Kind all has commodity production；
However, the functionality of polyacrylonitrile fibre is more single at present, to limit its scope of application, therefore, how to assign
The more performances of fiber are the emphasis studied at present.
Invention content
In view of the defects and deficiencies of the prior art, the present invention intends to provide a magnetic fibre kind and its preparation sides
Method.
To achieve the above object, the present invention uses following technical scheme：
A kind of magnetic fibre, it is made of the raw material of following weight parts：
2-mercaptobenzimidazole 0.5-1, filler 2-4, four water frerrous chloride 20-30, ferric chloride (FeCl36H2O) 10-15, acrylonitrile
The formalin 30- of 140-200, dibenzoyl peroxide 4-6, diacetone alcohol 2-3, glyceryl tristearate 1-2,10-12%
40, the ammonium hydroxide 20-25 of ricinoleic acid 3-5,10-12%, alkanolamide 6-7, p-methyl benzenesulfonic acid 0.03-0.1, triethylamine 0.4-
0.5。
The filler is one kind in nano silicon dioxide, bentonite in powder, montmorillonite powder.
A kind of preparation method of magnetic fibre, includes the following steps：
（1）Dibenzoyl peroxide is taken, is added in the absolute ethyl alcohol of 17-20 times of its weight, stirs evenly, it is molten to obtain initiator
Liquid；
（2）2-mercaptobenzimidazole is taken, is added in the dimethylformamide of 40-50 times of its weight, stirs evenly, obtains amide point
Dispersion liquid；
（3）Ricinoleic acid, filler mixing are taken, insulated and stirred 10-20 minutes at 60-65 DEG C, is added to mixture weight 10-16
In deionized water again, alkanolamide is added, it is 3-5 minutes ultrasonic, obtain filler dispersion liquid；
（4）Four water frerrous chlorides, ferric chloride (FeCl36H2O) mixing are taken, is added in the deionized water of 25-30 times of mixture weight, adds
Enter diacetone alcohol, stir evenly, the ammonium hydroxide of 10-12% is added dropwise, is stirred to react 3-4 hours, obtains magnetic dispersion liquid；
（5）Above-mentioned filler dispersion liquid, magnetic dispersion liquid mixing are taken, stirs evenly, p-methyl benzenesulfonic acid is added, increasing temperature is
90-95 DEG C, insulated and stirred 1-2 hours obtains filler modified magnetic solution；
（6）Acrylonitrile is taken, is added in above-mentioned filler modified magnetic solution, is stirred evenly, be sent in reaction kettle, be passed through nitrogen
Gas, it is 65-70 DEG C to adjust temperature of reaction kettle, and initiator solution, insulation reaction 3-4 hours is added, and discharging cooling obtains magnetic polymeric
Object solution；
（7）Glyceryl tristearate is taken, is added in above-mentioned filler modified magnetic solution, stirs evenly, the first of 10-12% is added
Triethylamine is added in aldehyde solution, and insulated and stirred 2-3 hours at 100-110 DEG C, filtering must precipitate；
（8）Above-mentioned precipitation is taken, is added in amide dispersion liquid, stirs evenly, spinning is to get the magnetic fibre.
Advantages of the present invention：
The present invention handles filler using ricinoleic acid, with the alcoholic solution of four water frerrous chlorides, ferric chloride (FeCl36H2O) for forerunner's system
Standby magnetic material, then Catalyzed by P-Toluenesulfonic Acid effect is lower carries out esterification, obtains organically-modified magnetic material, later with
Acrylonitrile is monomer, using filler modified magnetic solution as reaction dissolvent, polymerize under initiator effect, obtains poly- the third of magnetic modification
Alkene nitrile finally carries out methylation reaction by catalyst of triethylamine, further improves the power of the polyacrylonitrile of finished product magnetic modification
Stability is learned, fiber of the invention has stable magnetism, comprehensive performance superior.
Specific implementation mode
Embodiment 1
2-mercaptobenzimidazole 1, filler 4, four water frerrous chlorides 30, ferric chloride (FeCl36H2O) 15, acrylonitrile 200, diphenyl peroxide
Ammonium hydroxide 25, the alkanol of formyl 6, diacetone alcohol 3, the formalin 40 of glyceryl tristearate 2,12%, ricinoleic acid 5,10-12%
Amide 7, p-methyl benzenesulfonic acid 0.1, triethylamine 0.5.
The filler is montmorillonite powder.
A kind of preparation method of magnetic fibre, includes the following steps：
（1）Dibenzoyl peroxide is taken, is added in the absolute ethyl alcohol of 20 times of its weight, is stirred evenly, obtain initiator solution；
（2）2-mercaptobenzimidazole is taken, is added in the dimethylformamide of 50 times of its weight, stirs evenly, obtains amide dispersion
Liquid；
（3）Take ricinoleic acid, filler mixing, insulated and stirred 20 minutes at 65 DEG C, be added to 16 times of mixture weight go from
In sub- water, alkanolamide is added, ultrasound 5 minutes obtains filler dispersion liquid；
（4）Four water frerrous chlorides, ferric chloride (FeCl36H2O) mixing are taken, is added in the deionized water of 30 times of mixture weight, is added
Diacetone alcohol stirs evenly, and 12% ammonium hydroxide is added dropwise, and is stirred to react 4 hours, obtains magnetic dispersion liquid；
（5）Above-mentioned filler dispersion liquid, magnetic dispersion liquid mixing are taken, stirs evenly, p-methyl benzenesulfonic acid is added, it is 95 to increase temperature
DEG C, insulated and stirred 2 hours obtains filler modified magnetic solution；
（6）Acrylonitrile is taken, is added in above-mentioned filler modified magnetic solution, is stirred evenly, be sent in reaction kettle, be passed through nitrogen
Gas, it is 70 DEG C to adjust temperature of reaction kettle, and initiator solution, insulation reaction 4 hours is added, and it is molten to obtain magnetic polymer for discharging cooling
Liquid；
（7）Take glyceryl tristearate, be added in above-mentioned filler modified magnetic solution, stir evenly, be added 12% formaldehyde it is molten
Liquid, is added triethylamine, insulated and stirred 3 hours at 110 DEG C, and filtering must precipitate；
（8）Above-mentioned precipitation is taken, is added in amide dispersion liquid, stirs evenly, spinning is to get the magnetic fibre.
Embodiment 2
2-mercaptobenzimidazole 0.5, filler 2, four water frerrous chlorides 20, ferric chloride (FeCl36H2O) 10, acrylonitrile 140, peroxidating two
Benzoyl 4, diacetone alcohol 2, glyceryl tristearate 1, the formalin 30 of 10-12%, the ammonium hydroxide 20 of ricinoleic acid 3,10%, alkane
Alkylolamides 6, p-methyl benzenesulfonic acid 0.03, triethylamine 0.4.
The filler is nano silicon dioxide.
3, a kind of preparation method of magnetic fibre as described in claim 1, includes the following steps：
（1）Dibenzoyl peroxide is taken, is added in the absolute ethyl alcohol of 17 times of its weight, is stirred evenly, obtain initiator solution；
（2）2-mercaptobenzimidazole is taken, is added in the dimethylformamide of 40 times of its weight, stirs evenly, obtains amide dispersion
Liquid；
（3）Take ricinoleic acid, filler mixing, insulated and stirred 10 minutes at 60 DEG C, be added to 10 times of mixture weight go from
In sub- water, alkanolamide is added, it is 3-5 minutes ultrasonic, obtain filler dispersion liquid；
（4）Four water frerrous chlorides, ferric chloride (FeCl36H2O) mixing are taken, is added in the deionized water of 25 times of mixture weight, is added
Diacetone alcohol stirs evenly, and 10% ammonium hydroxide is added dropwise, and is stirred to react 3 hours, obtains magnetic dispersion liquid；
（5）Above-mentioned filler dispersion liquid, magnetic dispersion liquid mixing are taken, stirs evenly, p-methyl benzenesulfonic acid is added, it is 90 to increase temperature
DEG C, insulated and stirred 1 hour obtains filler modified magnetic solution；
（6）Acrylonitrile is taken, is added in above-mentioned filler modified magnetic solution, is stirred evenly, be sent in reaction kettle, be passed through nitrogen
Gas, it is 65 DEG C to adjust temperature of reaction kettle, and initiator solution, insulation reaction 3 hours is added, and it is molten to obtain magnetic polymer for discharging cooling
Liquid；
（7）Take glyceryl tristearate, be added in above-mentioned filler modified magnetic solution, stir evenly, be added 10% formaldehyde it is molten
Liquid, is added triethylamine, insulated and stirred 2 hours at 100 DEG C, and filtering must precipitate；
（8）Above-mentioned precipitation is taken, is added in amide dispersion liquid, stirs evenly, spinning is to get the magnetic fibre.
Performance test：
The toughness of magnetic fibre of the present invention is 6.7-10MJ/m3；
Saturation magnetization is 63.1-68Am2/kg；
Coercivity is 12.7-14.1kA/m.
Claims (3)
1. a kind of magnetic fibre, which is characterized in that it is made of the raw material of following weight parts：
2-mercaptobenzimidazole 0.5-1, filler 2-4, four water frerrous chloride 20-30, ferric chloride (FeCl36H2O) 10-15, acrylonitrile
The formalin 30- of 140-200, dibenzoyl peroxide 4-6, diacetone alcohol 2-3, glyceryl tristearate 1-2,10-12%
40, the ammonium hydroxide 20-25 of ricinoleic acid 3-5,10-12%, alkanolamide 6-7, p-methyl benzenesulfonic acid 0.03-0.1, triethylamine 0.4-
0.5。
2. a kind of magnetic fibre according to claim 1, which is characterized in that the filler is nano silicon dioxide, swollen
One kind in the native powder of profit, montmorillonite powder.
3. a kind of preparation method of magnetic fibre as described in claim 1, which is characterized in that include the following steps：
（1）Dibenzoyl peroxide is taken, is added in the absolute ethyl alcohol of 17-20 times of its weight, stirs evenly, it is molten to obtain initiator
Liquid；
（2）2-mercaptobenzimidazole is taken, is added in the dimethylformamide of 40-50 times of its weight, stirs evenly, obtains amide point
Dispersion liquid；
（3）Ricinoleic acid, filler mixing are taken, insulated and stirred 10-20 minutes at 60-65 DEG C, is added to mixture weight 10-16
In deionized water again, alkanolamide is added, it is 3-5 minutes ultrasonic, obtain filler dispersion liquid；
（4）Four water frerrous chlorides, ferric chloride (FeCl36H2O) mixing are taken, is added in the deionized water of 25-30 times of mixture weight, adds
Enter diacetone alcohol, stir evenly, the ammonium hydroxide of 10-12% is added dropwise, is stirred to react 3-4 hours, obtains magnetic dispersion liquid；
（5）Above-mentioned filler dispersion liquid, magnetic dispersion liquid mixing are taken, stirs evenly, p-methyl benzenesulfonic acid is added, increasing temperature is
90-95 DEG C, insulated and stirred 1-2 hours obtains filler modified magnetic solution；
（6）Acrylonitrile is taken, is added in above-mentioned filler modified magnetic solution, is stirred evenly, be sent in reaction kettle, be passed through nitrogen
Gas, it is 65-70 DEG C to adjust temperature of reaction kettle, and initiator solution, insulation reaction 3-4 hours is added, and discharging cooling obtains magnetic polymeric
Object solution；
（7）Glyceryl tristearate is taken, is added in above-mentioned filler modified magnetic solution, stirs evenly, the first of 10-12% is added
Triethylamine is added in aldehyde solution, and insulated and stirred 2-3 hours at 100-110 DEG C, filtering must precipitate；
（8）Above-mentioned precipitation is taken, is added in amide dispersion liquid, stirs evenly, spinning is to get the magnetic fibre.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201810309003.1A CN108411397A (en) | 2018-04-09 | 2018-04-09 | A kind of magnetic fibre and preparation method thereof |
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| CN201810309003.1A CN108411397A (en) | 2018-04-09 | 2018-04-09 | A kind of magnetic fibre and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109457315A (en) * | 2018-10-25 | 2019-03-12 | 董荣志 | A kind of anti-oxidant magnetic fibre and preparation method thereof |
| CN109537084A (en) * | 2018-10-25 | 2019-03-29 | 董荣志 | A kind of Resisting fractre magnetic fibre and preparation method thereof |
| CN111926406A (en) * | 2020-06-19 | 2020-11-13 | 浙江工商大学 | Color-developing fiber PAN-MB-PAR and synthetic method and application thereof |
| CN114889271A (en) * | 2022-05-06 | 2022-08-12 | 河南省超亚医药器械有限公司 | Hot-rolled non-woven fabric and preparation method thereof |
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| CN107475784A (en) * | 2016-06-08 | 2017-12-15 | 南京理工大学 | A kind of preparation method of ferriferrous oxide nano fiber |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109457315A (en) * | 2018-10-25 | 2019-03-12 | 董荣志 | A kind of anti-oxidant magnetic fibre and preparation method thereof |
| CN109537084A (en) * | 2018-10-25 | 2019-03-29 | 董荣志 | A kind of Resisting fractre magnetic fibre and preparation method thereof |
| CN111926406A (en) * | 2020-06-19 | 2020-11-13 | 浙江工商大学 | Color-developing fiber PAN-MB-PAR and synthetic method and application thereof |
| CN111926406B (en) * | 2020-06-19 | 2022-08-26 | 浙江工商大学 | Color-developing fiber PAN-MB-PAR and synthetic method and application thereof |
| CN114889271A (en) * | 2022-05-06 | 2022-08-12 | 河南省超亚医药器械有限公司 | Hot-rolled non-woven fabric and preparation method thereof |
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Application publication date: 20180817 |