CN108752662A - A kind of preparation method of magnetosensitive rubber - Google Patents

A kind of preparation method of magnetosensitive rubber Download PDF

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Publication number
CN108752662A
CN108752662A CN201810692840.7A CN201810692840A CN108752662A CN 108752662 A CN108752662 A CN 108752662A CN 201810692840 A CN201810692840 A CN 201810692840A CN 108752662 A CN108752662 A CN 108752662A
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parts
rubber
obtains
quality
mass ratio
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胡次兵
刘侠
宋宇星
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Foshan Gaoming District Claw And New Mstar Technology Ltd
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Foshan Gaoming District Claw And New Mstar Technology Ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L7/00Compositions of natural rubber
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G73/00Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
    • C08G73/02Polyamines
    • C08G73/026Wholly aromatic polyamines
    • C08G73/0266Polyanilines or derivatives thereof
    • 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
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2265Oxides; Hydroxides of metals of iron
    • C08K2003/2275Ferroso-ferric oxide (Fe3O4)
    • 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
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2296Oxides; Hydroxides of metals of zinc
    • 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

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The invention discloses a kind of preparation methods of magnetosensitive rubber, belong to technical field of polymer materials.It counts, weighs successively in parts by weight:50~60 parts of natural rubbers, 30~40 parts of butadiene-styrene rubber, 5~6 parts of zinc oxide, 2~4 parts of accelerating agents, 2~3 parts of stearic acid, 3~4 parts of blended antioxidants, natural rubber and butadiene-styrene rubber are mixed in kneading machine by 2~4 parts of tackifier, 3~6 parts of sulphur and 10~18 parts of additives, and zinc oxide is added into kneading machine, stearic acid, blended antioxidant, accelerating agent, tackifier and additive, after mixed milling, blank is obtained, blank is mixed with sulphur, vulcanize under conditions of being 160~190 DEG C in temperature, obtains magnetosensitive rubber.Magnetosensitive rubber prepared by technical solution of the present invention has the characteristics that excellent tensile strength, has broad prospects in the development of high molecular material industry.

Description

A kind of preparation method of magnetosensitive rubber
Technical field
The invention discloses a kind of preparation methods of magnetosensitive rubber, belong to technical field of polymer materials.
Background technology
Magnetosensitive rubber is one kind of magnetorheological materials, alternatively referred to as magnetic rheology elastic body, is that a kind of rheological property can be by external magnetic field The new function material and intellectual material of control.Since its fast response time, good reversibility (after removing magnetic field, and restore initial State) and can be by adjusting magnetic field size performances consecutive variations such as mechanics, electricity, the magnetics that control material, in aviation The fields such as space flight, automobile, vibration control are with a wide range of applications.Research in terms of magnetic rheology elastic body is later, and grinds Study carefully range and is concentrated mainly on magnetorheological fluid and its application aspect.Magnetosensitive rubber is usually by rubber matrix and ferromagnetic particle and one The additives mixing such as a little vulcanizing agent, accelerating agent, softening agents vulcanizes.It is preferable in order to prepare simple and opposite magnetic rheology effect Magnetosensitive rubber, it is base that many researchers, which have used the single rubber materials such as room temperature vulcanized silicone rubber, natural rubber, nitrile rubber, Body, but the mechanical mechanics property of these magnetosensitive rubber is not fine, and this problem limits the device based on magnetosensitive rubber and exists Application under real-world environment.
Since carrying magnetic, magnetism do not come from a large amount of magnetosensitive rubber itself(For 2-8 times of collagen amount)The filling of magnetic powder, institute With magnetic powder is indispensable to manufacture magnetic rubber.According to ingredient, magnetic additive can be divided into metal magnetic and iron cobalt point, Iron nickel powder and iron barium powder etc., wherein most wide with iron cobalt powder use.Metal magnetic is added due to expensive difficult and is rarely employed. What application was more at present is ferrite powder, they are the compound of iron oxide and certain two valences metals, even if being all a kind of ferrite Class magnetic powder causes final magnetic intensity different because of crystal habit, particle size and uniformity difference.
And traditional magnetosensitive rubber causes to be unable to reach ideal in use there is also the bad problem of tensile property Therefore how effect improves the bad disadvantage of traditional magnetosensitive rubber tensile property, developed with good comprehensive in the hope of exploring The magnetosensitive rubber of energy is problem to be solved.
Invention content
The present invention solves the technical problem of:Have the shortcomings that tensile property is bad for traditional magnetosensitive rubber, provides A kind of preparation method of magnetosensitive rubber.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is:
A kind of preparation method of magnetosensitive rubber, specific preparation process are:
(1)By bentonite and water in mass ratio 1:5~1:10 mixing, obtain bentonite dispersion liquid, by bentonite dispersion liquid and four oxygen Change three-iron in mass ratio 10:1~12:1 mixing, and the silane coupling agent of 0.10~0.12 times of bentonite dispersion liquid quality is added, It after ultrasonic disperse, filters, grinding obtains pretreatment modification bentonite, by pretreatment modification bentonite and cetyl trimethyl bromine Change ammonium in mass ratio 5:1 mixing, and the water of 10~15 times of pretreatment modification bentonite quality is added, it after being stirred, filters, does It is dry, obtain modified alta-mud;
(2)By graphene oxide and absolute ethyl alcohol in mass ratio 1:100~1:110 mix, and after ultrasonic disperse, graphite oxide is added The sodium acetate of 4~6 times of the ferric trichloride and graphene oxide quality that 2~3 times of alkene quality, after being stirred, heating and thermal insulation reaction Afterwards, cooling discharge obtains graphene oxide mixture, and graphene oxide mixture is washed with deionized into cleaning solution without chlorine It is dry after ion, obtain predecessor;
(3)By aniline and hydrochloric acid in mass ratio 1:50~1:60 mixing, and the forerunner of 0.025~0.050 times of aniline quality is added The modified alta-mud of 0.02~0.04 times of object and aniline quality, after being stirred, obtains aniline mixture, by aniline mixture quality 0.2~0.3 times of initiator instills in aniline mixture, and after being stirred to react, filtering, washing to cleaning solution is colourless, and drying obtains Additive;
(4)It counts, weighs successively in parts by weight:50~60 parts of natural rubbers, 30~40 parts of butadiene-styrene rubber, 5~6 parts of zinc oxide, 2 ~4 parts of accelerating agents, 2~3 parts of stearic acid, 3~4 parts of blended antioxidants, 2~4 parts of tackifier, 3~6 parts of sulphur and 10~18 parts add Add agent, natural rubber mixed with butadiene-styrene rubber, and zinc oxide is added, stearic acid, blended antioxidant, accelerating agent, tackifier and Additive after mixed milling, obtains blank, blank is mixed vulcanization with sulphur, obtains magnetosensitive rubber.
Step(3)The initiator is sodium peroxydisulfate, any one in potassium peroxydisulfate or ammonium persulfate.
Step(4)The accelerating agent is accelerator CBS, any one in Vulcanization accelerator TMTD or accelerant CZ.
Step(4)The blended antioxidant is by anti-aging agent RD and antioxidant 4010NA in mass ratio 1:1 mixing, must mix Anti-aging agent.
Step(4)The tackifier are tackifier AHR, any one in terpene resin or rosin.
Step(1)The silane coupling agent is silane resin acceptor kh-550, silane coupling agent KH-560 or silane coupling agent Any one in KH-570.
The beneficial effects of the invention are as follows:
Additive is added when preparing magnetosensitive rubber by the present invention, first, contains organobentonite on the outside of additive, and product is being added In after compatibility between additive and product can be improved, it is magnetic improving product to make additive be uniformly distributed in product While improve product tensile strength, secondly, polyaniline is contained in additive, can be in mixing process after being added in product In with rubber macromolecule generate mechanical snap, to make the cohesive force of product improve, so make product draw high intensity improve, and And since the affinity between polyaniline and rubber macromolecule is preferable, after being added in product, additive can be made to be uniformly distributed in In product, and then make the generation of reduction agglomeration, the tensile strength of product is made to further increase, furthermore, due in additive In preparation process ferroso-ferric oxide predecessor, the group of the ferroso-ferric oxide to be further reduced are fixed using graphene oxide It is poly-, and since the addition of graphene oxide can be such that the tensile strength of product further increases.
Specific implementation mode
By bentonite and water in mass ratio 1:5~1:10 mixing are 45~55 DEG C in temperature, and rotating speed is 300~400r/ Under conditions of min, after being stirred 40~50min, bentonite dispersion liquid is obtained, bentonite dispersion liquid and ferroso-ferric oxide are pressed into matter Measure ratio 10:1~12:1 is mixed in beaker, and the silane idol of 0.10~0.12 times of bentonite dispersion liquid quality is added into beaker Join agent, under conditions of frequency is 45~55kHz, after 1~2h of ultrasonic disperse, filtering obtains filter cake, filter cake is ground, obtains pre- place Modified alta-mud is managed, by pretreatment modification bentonite and cetyl trimethylammonium bromide in mass ratio 5:1 mixing, and locate to pre- It manages and 10~15 times of pretreatment modification bentonite quality is added in the mixture of modified alta-mud and cetyl trimethylammonium bromide Water, in temperature be 70~80 DEG C, rotating speed be 200~280r/min under conditions of be stirred 4~5h after, filtering, obtain modification Bentonite blank obtains modified alta-mud under conditions of being 60~70 DEG C in temperature by modified alta-mud blank after dry 1~3h; By graphene oxide and absolute ethyl alcohol in mass ratio 1:100~1:110 are mixed in flask, in the item that frequency is 45~55kHz Under part, after 1~2h of ultrasonic disperse, the ferric trichloride and graphene oxide matter of 2~3 times of graphene oxide quality are added into flask The sodium acetate of 4~6 times of amount is 50~60 DEG C in temperature, under conditions of rotating speed is 300~400r/min, is stirred 1~2h Afterwards, and by material in flask in temperature be 200 DEG C under conditions of 5~6h of insulation reaction, cooling discharge, obtain graphene oxide mixing Object, after graphene oxide mixture is washed with deionized into cleaning solution without chlorion, under conditions of temperature is 100 DEG C Dry 40~60min, obtains predecessor;The hydrochloric acid in mass ratio 1 for being 7~10% by aniline and mass fraction:50~1:60 are mixed in In three-necked flask, and be added into three-necked flask 0.025~0.05 times of aniline quality predecessor and aniline quality 0.02~ 0.04 times of modified alta-mud is 0~5 DEG C in temperature, under conditions of rotating speed is 500~800r/min, it is stirred 30~ After 50min, aniline mixture is obtained, 0.2~0.3 times of initiator of aniline mixture quality is instilled with the rate of 1~2mL/min In aniline mixture, it is 0~5 DEG C in temperature, under conditions of rotating speed is 200~400r/min, after being stirred to react 1~3h, filters, Additive blank is obtained, it is colourless that additive blank absolute ethyl alcohol and deionized water, which are alternately washed to cleaning solution, and in temperature After being dried in vacuo 40~50h under conditions of being 40~45 DEG C, additive is obtained;It counts, weighs successively in parts by weight:50~60 parts of days T PNR, 30~40 parts of butadiene-styrene rubber, 5~6 parts of zinc oxide, 2~4 parts of accelerating agents, 2~3 parts of stearic acid, 3~4 parts of mixing are anti-old Natural rubber and butadiene-styrene rubber are mixed in kneading machine by agent, 2~4 parts of tackifier, 3~6 parts of sulphur and 10~18 parts of additives In, and zinc oxide is added into kneading machine, stearic acid, blended antioxidant, accelerating agent, tackifier and additive, after mixed milling, Blank is obtained, blank is mixed with sulphur, vulcanizes under conditions of being 160~190 DEG C in temperature, obtains magnetosensitive rubber.The initiator For sodium peroxydisulfate, any one in potassium peroxydisulfate or ammonium persulfate.The accelerating agent is accelerator CBS, Vulcanization accelerator TMTD or rush Into any one in agent CZ.The blended antioxidant is by anti-aging agent RD and antioxidant 4010NA in mass ratio 1:1 mixing, obtains mixed Close anti-aging agent.The tackifier are tackifier AHR, any one in terpene resin or rosin.The silane coupling agent is silane Any one in coupling agent KH-550, silane coupling agent KH-560 or Silane coupling reagent KH-570.
Example 1
By bentonite and water in mass ratio 1:10 mixing are 55 DEG C in temperature, under conditions of rotating speed is 400r/min, are stirred After 50min, bentonite dispersion liquid is obtained, by bentonite dispersion liquid and ferroso-ferric oxide in mass ratio 12:1 is mixed in beaker, and The silane coupling agent of 0.12 times of bentonite dispersion liquid quality is added into beaker, under conditions of frequency is 55kHz, ultrasonic disperse After 2h, filtering obtains filter cake, filter cake is ground, obtain pretreatment modification bentonite, by pretreatment modification bentonite and cetyl three Methyl bromide ammonium in mass ratio 5:1 mixing, and to the mixture of pretreatment modification bentonite and cetyl trimethylammonium bromide The middle water that 15 times of pretreatment modification bentonite quality is added is 80 DEG C in temperature, and rotating speed stirs mixed under conditions of being 280r/min After closing 5h, filtering obtains modified alta-mud blank, under conditions of being 70 DEG C in temperature by modified alta-mud blank after dry 3h, obtains Modified alta-mud;By graphene oxide and absolute ethyl alcohol in mass ratio 1:110 are mixed in flask, in the item that frequency is 55kHz Under part, after ultrasonic disperse 2h, 6 times of the ferric trichloride and graphene oxide quality of 3 times of graphene oxide quality are added into flask Sodium acetate, in temperature be 60 DEG C, rotating speed be 400r/min under conditions of, after being stirred 2h, and by material in flask in temperature Degree is insulation reaction 6h under conditions of 200 DEG C, and cooling discharge obtains graphene oxide mixture, graphene oxide mixture is used After deionized water is washed into cleaning solution without chlorion, dry 60min under conditions of being 100 DEG C in temperature obtains predecessor;By benzene The hydrochloric acid in mass ratio 1 that amine is 10% with mass fraction:60 are mixed in three-necked flask, and aniline matter is added into three-necked flask The modified alta-mud of 0.04 times of the predecessor and aniline quality of 0.05 times of amount is 5 DEG C in temperature, and rotating speed is the condition of 800r/min Under, after being stirred 50min, aniline mixture is obtained, by the initiator of 0.3 times of aniline mixture quality with the rate of 2mL/min It instills in aniline mixture, is 5 DEG C in temperature, under conditions of rotating speed is 400r/min, after being stirred to react 3h, filtering must be added Agent blank, by additive blank absolute ethyl alcohol and deionized water, alternately washing to cleaning solution is colourless, and in temperature be 45 DEG C Under conditions of vacuum drying 50h after, obtain additive;It counts, weighs successively in parts by weight:60 parts of natural rubbers, 40 parts of butylbenzene rubbers Glue, 6 parts of zinc oxide, 4 parts of accelerating agents, 3 parts of stearic acid, 4 parts of blended antioxidants, 4 parts of tackifier, 6 parts of sulphur and 18 parts of additives, Natural rubber and butadiene-styrene rubber are mixed in kneading machine, and zinc oxide is added into kneading machine, stearic acid, blended antioxidant, Accelerating agent, tackifier and additive after mixed milling, obtain blank, blank are mixed with sulphur, the condition for being 190 DEG C in temperature Lower vulcanization, obtains magnetosensitive rubber.The initiator is sodium peroxydisulfate.The accelerating agent is accelerator CBS.The blended antioxidant is By anti-aging agent RD and antioxidant 4010NA in mass ratio 1:1 mixing, obtains blended antioxidant.The tackifier are tackifier AHR.Institute It is silane resin acceptor kh-550 to state silane coupling agent.
Example 2
By graphene oxide and absolute ethyl alcohol in mass ratio 1:110 are mixed in flask, under conditions of frequency is 55kHz, surpass After sound disperses 2h, the acetic acid of 6 times of the ferric trichloride and graphene oxide quality of 3 times of graphene oxide quality is added into flask Sodium, in temperature be 60 DEG C, rotating speed be 400r/min under conditions of, after being stirred 2h, and by material in flask in temperature be 200 Insulation reaction 6h under conditions of DEG C, cooling discharge obtain graphene oxide mixture, by graphene oxide mixture deionized water To after in cleaning solution without chlorion, dry 60min under conditions of being 100 DEG C in temperature obtains predecessor for washing;By aniline and quality The hydrochloric acid in mass ratio 1 that score is 10%:60 are mixed in three-necked flask, and 0.05 times of aniline quality is added into three-necked flask Predecessor, in temperature be 5 DEG C, rotating speed be 800r/min under conditions of, after being stirred 50min, aniline mixture is obtained, by benzene The initiator that 0.3 times of amine blends quality is instilled with the rate of 2mL/min in aniline mixture, is 5 DEG C in temperature, rotating speed is Under conditions of 400r/min, after being stirred to react 3h, filtering, obtain additive blank, by additive blank absolute ethyl alcohol and go from Alternately washing to cleaning solution is colourless for sub- water, and obtains additive after vacuum drying 50h under conditions of being 45 DEG C in temperature;By weight Number meter is measured, is weighed successively:60 parts of natural rubbers, 40 parts of butadiene-styrene rubber, 6 parts of zinc oxide, 4 parts of accelerating agents, 3 parts of stearic acid, 4 parts Natural rubber and butadiene-styrene rubber are mixed in kneading machine by blended antioxidant, 4 parts of tackifier, 6 parts of sulphur and 18 parts of additives, And zinc oxide is added into kneading machine, stearic acid, blended antioxidant, accelerating agent, tackifier and additive after mixed milling, obtain Blank mixes blank with sulphur, vulcanizes under conditions of being 190 DEG C in temperature, obtains magnetosensitive rubber.The initiator is persulfuric acid Sodium.The accelerating agent is accelerator CBS.The blended antioxidant is by anti-aging agent RD and antioxidant 4010NA in mass ratio 1:1 Mixing, obtains blended antioxidant.The tackifier are tackifier AHR.
Example 3
By bentonite and water in mass ratio 1:10 mixing are 55 DEG C in temperature, under conditions of rotating speed is 400r/min, are stirred After 50min, bentonite dispersion liquid is obtained, by bentonite dispersion liquid and ferroso-ferric oxide in mass ratio 12:1 is mixed in beaker, and The silane coupling agent of 0.12 times of bentonite dispersion liquid quality is added into beaker, under conditions of frequency is 55kHz, ultrasonic disperse After 2h, filtering obtains filter cake, filter cake is ground, obtain pretreatment modification bentonite, by pretreatment modification bentonite and cetyl three Methyl bromide ammonium in mass ratio 5:1 mixing, and to the mixture of pretreatment modification bentonite and cetyl trimethylammonium bromide The middle water that 15 times of pretreatment modification bentonite quality is added is 80 DEG C in temperature, and rotating speed stirs mixed under conditions of being 280r/min After closing 5h, filtering obtains modified alta-mud blank, under conditions of being 70 DEG C in temperature by modified alta-mud blank after dry 3h, obtains Modified alta-mud;The hydrochloric acid in mass ratio 1 for being 10% by aniline and mass fraction:60 are mixed in three-necked flask, and are burnt to three mouthfuls The modified alta-mud of 0.04 times of aniline quality is added in bottle, is 5 DEG C in temperature, under conditions of rotating speed is 800r/min, stirring is mixed After closing 50min, aniline mixture is obtained, 0.3 times of initiator of aniline mixture quality is instilled aniline with the rate of 2mL/min to be mixed It closes in object, is 5 DEG C in temperature, under conditions of rotating speed is 400r/min, after being stirred to react 3h, filtering obtains additive blank, will add Adding agent blank absolute ethyl alcohol and deionized water, alternately washing to cleaning solution is colourless, and vacuum under conditions of being 45 DEG C in temperature After dry 50h, additive is obtained;It counts, weighs successively in parts by weight:60 parts of natural rubbers, 40 parts of butadiene-styrene rubber, 6 parts of zinc oxide, 4 parts of accelerating agents, 3 parts of stearic acid, 4 parts of blended antioxidants, 4 parts of tackifier, 6 parts of sulphur and 18 parts of additives, by natural rubber with Butadiene-styrene rubber is mixed in kneading machine, and zinc oxide is added into kneading machine, stearic acid, blended antioxidant, accelerating agent, tackifier And additive, after mixed milling, blank is obtained, blank is mixed with sulphur, vulcanized under conditions of being 190 DEG C in temperature, obtain magnetosensitive Rubber.The initiator is sodium peroxydisulfate.The accelerating agent is accelerator CBS.The blended antioxidant be by anti-aging agent RD with Antioxidant 4010NA in mass ratio 1:1 mixing, obtains blended antioxidant.The tackifier are tackifier AHR.The silane coupling agent For silane resin acceptor kh-550.
Example 4
By bentonite and water in mass ratio 1:10 mixing are 55 DEG C in temperature, under conditions of rotating speed is 400r/min, are stirred After 50min, bentonite dispersion liquid is obtained, by bentonite dispersion liquid and ferroso-ferric oxide in mass ratio 12:1 is mixed in beaker, and The silane coupling agent of 0.12 times of bentonite dispersion liquid quality is added into beaker, under conditions of frequency is 55kHz, ultrasonic disperse After 2h, filtering obtains filter cake, filter cake is ground, obtain pretreatment modification bentonite, by pretreatment modification bentonite and cetyl three Methyl bromide ammonium in mass ratio 5:1 mixing, and to the mixture of pretreatment modification bentonite and cetyl trimethylammonium bromide The middle water that 15 times of pretreatment modification bentonite quality is added is 80 DEG C in temperature, and rotating speed stirs mixed under conditions of being 280r/min After closing 5h, filtering obtains modified alta-mud blank, under conditions of being 70 DEG C in temperature by modified alta-mud blank after dry 3h, obtains Modified alta-mud;By graphene oxide and absolute ethyl alcohol in mass ratio 1:110 are mixed in flask, in the item that frequency is 55kHz Under part, after ultrasonic disperse 2h, 6 times of the ferric trichloride and graphene oxide quality of 3 times of graphene oxide quality are added into flask Sodium acetate, in temperature be 60 DEG C, rotating speed be 400r/min under conditions of, after being stirred 2h, and by material in flask in temperature Degree is insulation reaction 6h under conditions of 200 DEG C, and cooling discharge obtains graphene oxide mixture, graphene oxide mixture is used After deionized water is washed into cleaning solution without chlorion, dry 60min under conditions of being 100 DEG C in temperature obtains predecessor;By weight Number meter is measured, is weighed successively:60 parts of natural rubbers, 40 parts of butadiene-styrene rubber, 6 parts of zinc oxide, 4 parts of accelerating agents, 3 parts of stearic acid, 4 parts Natural rubber and butadiene-styrene rubber are mixed in kneading machine by blended antioxidant, 4 parts of tackifier, 6 parts of sulphur, and into kneading machine It is added zinc oxide, stearic acid, blended antioxidant, accelerating agent, tackifier after mixed milling, obtain blank, blank and sulphur are mixed It closes, vulcanizes under conditions of being 190 DEG C in temperature, obtain magnetosensitive rubber.The initiator is sodium peroxydisulfate.The accelerating agent is to promote Agent CBS.The blended antioxidant is by anti-aging agent RD and antioxidant 4010NA in mass ratio 1:1 mixing, obtains blended antioxidant.Institute It is tackifier AHR to state tackifier.The silane coupling agent is silane resin acceptor kh-550.
Comparative example:The magnetosensitive rubber of Shanghai tech materials production Co., Ltd production.
The magnetosensitive rubber and comparative example product of example 1 to 4 gained of example are subjected to performance detection, specific detection method is such as Under:
Tensile property test is carried out using JPL series multifunctional electronic tensile machines;Hardness survey is carried out with shore LX-A type hardness testers meter Examination.
Specific testing result is as shown in table 1:
1 magnetosensitive rubber performance testing result of table
Detection project Example 1 Example 2 Example 3 Example 4 Comparative example
Shore a hardness 67 62 57 55 43
Tensile strength/MPa 4.2 5.5 7.8 8.4 10.2
By 1 testing result of table it is found that magnetosensitive rubber prepared by technical solution of the present invention has the characteristics that excellent tensile strength, It has broad prospects in the development of high molecular material industry.

Claims (6)

1. a kind of preparation method of magnetosensitive rubber, which is characterized in that specifically preparation process is:
(1)By bentonite and water in mass ratio 1:5~1:10 mixing, obtain bentonite dispersion liquid, by bentonite dispersion liquid and four oxygen Change three-iron in mass ratio 10:1~12:1 mixing, and the silane coupling agent of 0.10~0.12 times of bentonite dispersion liquid quality is added, It after ultrasonic disperse, filters, grinding obtains pretreatment modification bentonite, by pretreatment modification bentonite and cetyl trimethyl bromine Change ammonium in mass ratio 5:1 mixing, and the water of 10~15 times of pretreatment modification bentonite quality is added, it after being stirred, filters, does It is dry, obtain modified alta-mud;
(2)By graphene oxide and absolute ethyl alcohol in mass ratio 1:100~1:110 mix, and after ultrasonic disperse, graphite oxide is added The sodium acetate of 4~6 times of the ferric trichloride and graphene oxide quality that 2~3 times of alkene quality, after being stirred, heating and thermal insulation reaction Afterwards, cooling discharge obtains graphene oxide mixture, and graphene oxide mixture is washed with deionized into cleaning solution without chlorine It is dry after ion, obtain predecessor;
(3)By aniline and hydrochloric acid in mass ratio 1:50~1:60 mixing, and the forerunner of 0.025~0.050 times of aniline quality is added The modified alta-mud of 0.02~0.04 times of object and aniline quality, after being stirred, obtains aniline mixture, by aniline mixture quality 0.2~0.3 times of initiator instills in aniline mixture, and after being stirred to react, filtering, washing to cleaning solution is colourless, and drying obtains Additive;
(4)It counts, weighs successively in parts by weight:50~60 parts of natural rubbers, 30~40 parts of butadiene-styrene rubber, 5~6 parts of zinc oxide, 2 ~4 parts of accelerating agents, 2~3 parts of stearic acid, 3~4 parts of blended antioxidants, 2~4 parts of tackifier, 3~6 parts of sulphur and 10~18 parts add Add agent, natural rubber mixed with butadiene-styrene rubber, and zinc oxide is added, stearic acid, blended antioxidant, accelerating agent, tackifier and Additive after mixed milling, obtains blank, blank is mixed vulcanization with sulphur, obtains magnetosensitive rubber.
2. a kind of preparation method of magnetosensitive rubber according to claim 1, it is characterised in that:Step(3)The initiator For sodium peroxydisulfate, any one in potassium peroxydisulfate or ammonium persulfate.
3. a kind of preparation method of magnetosensitive rubber according to claim 1, it is characterised in that:Step(4)The accelerating agent For accelerator CBS, any one in Vulcanization accelerator TMTD or accelerant CZ.
4. a kind of preparation method of magnetosensitive rubber according to claim 1, it is characterised in that:Step(4)The mixing is anti- Old agent is by anti-aging agent RD and antioxidant 4010NA in mass ratio 1:1 mixing, obtains blended antioxidant.
5. a kind of preparation method of magnetosensitive rubber according to claim 1, it is characterised in that:Step(4)The tackifier For tackifier AHR, any one in terpene resin or rosin.
6. a kind of preparation method of magnetosensitive rubber according to claim 1, it is characterised in that:Step(1)The silane is even Connection agent is silane resin acceptor kh-550, any one in silane coupling agent KH-560 or Silane coupling reagent KH-570.
CN201810692840.7A 2018-06-29 2018-06-29 A kind of preparation method of magnetosensitive rubber Pending CN108752662A (en)

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CN110425253A (en) * 2019-08-12 2019-11-08 青岛科技大学 A kind of operation is disconnected with the V band automatically controlled

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Application publication date: 20181106