CN106519340A - Anti-cracking seal rubber material and preparation method thereof - Google Patents
Anti-cracking seal rubber material and preparation method thereof Download PDFInfo
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- CN106519340A CN106519340A CN201611096037.4A CN201611096037A CN106519340A CN 106519340 A CN106519340 A CN 106519340A CN 201611096037 A CN201611096037 A CN 201611096037A CN 106519340 A CN106519340 A CN 106519340A
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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
- C08L9/00—Compositions of homopolymers or copolymers of conjugated diene hydrocarbons
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/10—Materials in mouldable or extrudable form for sealing or packing joints or covers
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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
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/10—Materials in mouldable or extrudable form for sealing or packing joints or covers
- C09K2003/1034—Materials or components characterised by specific properties
- C09K2003/1078—Fire-resistant, heat-resistant materials
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Abstract
The invention discloses an anti-cracking seal rubber material which is prepared from the following raw materials in parts by weight: 2-4 parts of magnesium sulfate, 1-3 parts of barium metaborate, 0.3-1 part of bisphenol a diglycidyl ether, 2-4 parts of alkyl ketene dimer, 3-4 parts of anti-aging agent TNP, 26-30 parts of butyl methacrylate, 10-14 parts of graphene oxide, 1-2 parts of sodium borohydride, 3-4 parts of sulfanilic acid, 14-20 parts of 0.8-1 mol/L hydrochloric acid, 0.3-0.5 part of potassium persulfate, 0.5-1 part of hydrazine hydrate, 210-300 parts of cis-1,4-polybutadiene rubber, 1.7-2 parts of vulcanizing agent PM, 1-2 parts of tin monosulfide, 3-4 parts of glyceryl carboxylate, 2-3 parts of polyamide wax micropowder, 0.7-1 part of 4-dimethylaminopyridine, 10-14 parts of wollastonite powder and 0.7-1 part of silane coupling agent kh560. The rubber material has the advantages of favorable sealing property, high surface strength, favorable addition property, high cracking resistance and high impact resistance.
Description
Technical field
The present invention relates to technical field of rubber material, more particularly to a kind of cracking resistance caulking gum material and its preparation side
Method.
Background technology
Graphene-based polymer nanocomposites are considered as the most promising field of Graphene application.Main cause
On the one hand it is that more and more important role act as due to the product of macromolecular material in people's life, has surmounted inorganic non-
Metal material and metal material, become the maximum material of consumption in people's life;On the other hand, Graphene and its derivative oxidation
The black alkene of stone each possesses the two-dimensional structure and excellent properties of uniqueness, is preferable filler.At present, prepare Graphene/polymer multiple
Condensation material mainly has 3 kinds of preparation methods：Flame melts blending, solution blending and in-situ polymerization.These three methods respectively have quality:Dissolve altogether
It is mixed can in relatively low, the simple to operate but resulting composite of large-scale operation, cost Graphene it is often dispersed poor, because
And few is improved to the performance of polymeric matrix material;The amount of Graphene required for solution blended process is less and dispersed preferable,
But organic solvent will be used substantially, and different solvents is needed to dissolve different polymer, not enough economical and environmentally friendly;It is former
Graphene is first blended by position polymerization with monomer or performed polymer, then under the initiation of initiator, carries out polymerisation.It is in situ poly-
It is legal prepare graphite refining/polymer composite on the one hand ensure that the hook dispersion in the polymer of graphite refining filler and its
With the strong interaction of matrix, on the other hand, many changes can be also brought on the molecular weight and monodispersity of polymer.It is former
The example of position polymerization has polyethylene, polymethyl methacrylate, polystyrene etc.；
However, it is noteworthy that Graphene and graphene oxide in the performance for improving polymeric matrix material often with its
Dispersiveness in polymeric matrix has direct relation, due to there is stronger Van der Waals between Graphene and graphene oxide layer
Power interacts so that its piece interlayer is easy to be occurred to reunite.Therefore, graphene/graphene oxide is being added to into macromolecule
Before matrix material, often functional modification will be carried out to Graphene and graphene oxide；
At present, it is solution blending or training with graphene oxide as presoma to prepare graphene-based composite most common method
Melt the methods such as blending, after graphene oxide is mixed with other materials, then through reduction, finally give target composite wood
Material.For Graphene, the substantial amounts of oxy radical contained by graphene oxide weakens graphene sheet layer to a certain extent
Between Van der Waals force, but these hydrophilic oxy radicals, or be difficult to be thoroughly dispersed in organic solvent or polymeric matrix
In, which greatly limits the application of graphene oxide；With Graphene functional modification in terms of achieve it is very big
Progress, covalent bond and non-covalent bond modified graphite olefinic base material are to improve its interaction such as with various solvents and polymer
Modified molecules are covered in graphene film layer surface by a kind of very effective method, so as to hinder the model between graphene sheet layer
The power effect of moral China, and then the reunion and accumulation of graphene film interlayer are prevented, improve its phase in the material such as solvent and polymer
Capacitive, expands the range of application of Graphene.But at present, graphene functionalized method is not very ripe, await it is further perfect,
Realize that its industrialization also needs to further investigation, specifically how will be with special using the modified method of covalent bond and non-covalent bond
The function chemoattractant molecule of different structure and performance is combined with Graphene, gives full play to both advantages, is the emphasis of current research；
It is found that being that graphene oxide is easy to send out subject matter present in graphene oxide/polymer complex process is prepared
It is raw to reunite, and dispersiveness inequality is hooked in the polymer, graphene oxide is in poor shape with the combination interface of polymer, ultimately results in
The combination property of graphene oxide/polymer composites is not high, so as to limit its further commercial Application.Therefore people
Generally using the method for functional modification being carried out to which, improve the processing characteristics of graphene oxide；Research shows, to Graphene
It is a kind of very effective method for solving Graphene agglomeration traits to carry out functional modification, and which can not only improve Graphene and exist
Dispersiveness in solution and polymeric matrix, but also effectively can strengthen mutual between Graphene and polymer matrix body interface
Effect.
The content of the invention
The object of the invention is exactly for the defect for making up prior art, there is provided a kind of cracking resistance caulking gum material and its system
Preparation Method.
The present invention is achieved by the following technical solutions：
A kind of cracking resistance caulking gum material, it is made up of the raw material of following weight parts：
Magnesium sulfate 2-4, barium metaborate 1-3, bis-phenol a diglycidyl ether 0.3-1, alkyl ketene dimer 2-4, age resistor
TNP3-4, butyl methacrylate 26-30, graphene oxide 10-14, sodium borohydride 1-2, p-aminobenzene sulfonic acid 3-4,0.8-
1mol/l hydrochloric acid 14-20, natrium nitrosum 1-2, styrene 43-50, potassium peroxydisulfate 0.3-0.5, hydrazine hydrate 0.5-1, butadiene rubber
210-300, vulcanizing agent PM1.7-2, stannous sulfide 1-2, short and long-chain acyl triglyceride molecules 3-4, polyamide wax micropowder 2-3,4- dimethylamino pyrrole
Pyridine 0.7-1, wollastonite in powder 10-14, silane coupler kh5600.7-1.
A kind of preparation method of described cracking resistance caulking gum material, comprises the following steps：
（1）Above-mentioned wollastonite in powder is calcined into 1-2 hours at 700-800 DEG C, normal temperature is cooled to, is added to its weight 20-30 times
Deionized water in, add above-mentioned barium metaborate, it is 60-70 DEG C to rise high-temperature, and the hydrochloric acid of 10-15mol/l is added dropwise, and adjusts pH and is
2-3, insulated and stirred 20-30 minute, filters, and precipitation is mixed with above-mentioned graphene oxide, 1-2 is dried little at vacuum 50-60 DEG C
When, obtain composite graphite alkene；
（2）Composite graphite alkene is added in the deionized water of its weight 900-1000 times, ultrasonic 27-30 minutes, Graphene is obtained
Suspension；
（3）Above-mentioned sodium borohydride is added in its weight 15-20 times water, is stirred, sodium carbonate of the concentration for 4-6% is added dropwise
The aqueous solution, regulation pH are 9-10, are mixed with above-mentioned graphene suspension, the insulated and stirred 60-70 minute at 80-86 DEG C, are cooled down
To room temperature, ultrasonic 10-20 minutes, prereduction Graphene is obtained；
（4）Natrium nitrosum is added in its weight 170-200 times water, 2-3 DEG C is cooled to, with p-aminobenzene sulfonic acid, 0.8-
1mol/l mixed in hydrochloric acid, sends in ice-water bath, stirring reaction 30-40 minute, and discharging is added drop-wise in above-mentioned prereduction Graphene,
Stir 100-120 minutes under room temperature, obtain sulfonated graphene；
（5）Above-mentioned sulfonated graphene, styrene are mixed, ultrasonic 10-20 minutes, add potassium peroxydisulfate, stir, be passed through nitrogen
Gas, the insulated and stirred 6-7 hour at 70-76 DEG C add above-mentioned hydrazine hydrate, and it is 80-85 DEG C to rise high-temperature, insulation reaction 20-25
Hour, room temperature is cooled to, abovementioned alkyl ketene dimer, bis-phenol a diglycidyl ethers is added, is stirred, filtered, will precipitation
Send in air dry oven, be dried complete, discharging, obtain polystyrene graphene composite material；
（6）Above-mentioned polyamide wax micropowder is added in the absolute ethyl alcohol of its weight 10-13 times, it is 90-96 DEG C to rise high-temperature, is protected
Temperature stirring 20-30 minutes, above-mentioned stannous sulfide is added, is stirred to 60-65 DEG C, add above-mentioned polystyrene Graphene composite wood
Material, silane coupler kh560, insulated and stirred 30-40 minute, obtain silane-modified alcohol liquid；
（7）By above-mentioned silane-modified alcohol liquid, butadiene rubber, age resistor TNP, butyl methacrylate, magnesium sulfate mixing, in 46-
Plasticate at 50 DEG C 2-3 minutes, add remaining each raw material, knead 4-6 minutes, the elastomeric compound for obtaining is placed in two roller mills,
Supplement mixing 6-10 minutes at 30-40 DEG C, sizing material is parked 20-25 hours at room temperature for discharging, sends into vulcanizing press
In, vulcanized at 150-155 DEG C, obtained final product.
It is an advantage of the invention that：The present invention stannic oxide/graphene nano piece surface contain substantial amounts of C-0-C ,-OH and-
The oxygen-containing functional groups such as COOH, when using sodium borohydride reduction, the various oxygen-containing functional groups in sodium borohydride and graphene oxide are first
Generation coordination, forms boron oxygen complex intermediate, and then the hydroxyl in graphene oxide and carbonyl are with boron-oxygen
Together slough, remove most of oxygen-containing functional group on stannic oxide/graphene nano piece surface, then which is carried out with sulfonic acid aryldiazonium salt
Covalent bond graft modification, has prepared sulfonated graphene, further enhances the water solubility of graphene oxide sheet, to improve its work
For the emulsifying capacity of solids emulsifying agent, the sulfonated graphene can should as a kind of effective solid particle surfaces activating agent
Prepare for cinnamic emulsion, and by emulsion polymerization, finally given sulfonated graphene/pipe/polyhenylethylene nano multiple
Compound, the Graphene of the functionalization can be in that the state highly peeled off is evenly dispersed in polystyrene microsphere；Effectively limit
The free movement of polymer chain is made；Further, since Graphene possesses huge specific surface area, therefore can be with thermal histories
Polymer and thermal source are separated, thus the addition of Graphene is finally effectively improved the heat endurance and mechanical property of polymer
Energy；The elastomeric material of the present invention has good sealing property, and surface strength is high, plus individual character is good, and cracking resistance, impact resistance are strong.
Specific embodiment
A kind of cracking resistance caulking gum material, it is made up of the raw material of following weight parts：
Magnesium sulfate 2, barium metaborate 1, bis-phenol a diglycidyl ethers 0.3, alkyl ketene dimer 2, age resistor TNP3, methyl-prop
Olefin(e) acid butyl ester 26, graphene oxide 10, sodium borohydride 1, p-aminobenzene sulfonic acid 3,0.8mol/l hydrochloric acid 14, natrium nitrosum 1, benzene second
Alkene 43, potassium peroxydisulfate 0.3, hydrazine hydrate 0.5, butadiene rubber 210, vulcanizing agent PM1.7, stannous sulfide 1, short and long-chain acyl triglyceride molecules 3, polyamides
Amine wax micro mist 2,4 dimethylamino naphthyridines 0.7, wollastonite in powder 10, silane coupler kh5600.7.
A kind of preparation method of described cracking resistance caulking gum material, comprises the following steps：
（1）Above-mentioned wollastonite in powder is calcined 1 hour at 700 DEG C, normal temperature is cooled to, the deionized water of 20 times of its weight is added to
In, above-mentioned barium metaborate is added, it is 60 DEG C to rise high-temperature, and the hydrochloric acid of 10mol/l is added dropwise, and it is 2 to adjust pH, 20 points of insulated and stirred
Clock, filters, and precipitation is mixed with above-mentioned graphene oxide, is dried 1 hour, obtains composite graphite alkene at 50 DEG C of vacuum；
（2）Composite graphite alkene is added in the deionized water of 900 times of its weight, ultrasound 27 minutes obtains graphene suspension；
（3）Above-mentioned sodium borohydride is added in 15 times of water of its weight, is stirred, the sodium carbonate that concentration is 4% is added dropwise water-soluble
Liquid, it is 9 to adjust pH, is mixed with above-mentioned graphene suspension, insulated and stirred 60 minutes at 80 DEG C, is cooled to room temperature, ultrasound 10
Minute, obtain prereduction Graphene；
（4）Natrium nitrosum is added in 170 times of water of its weight, 2 DEG C are cooled to, with p-aminobenzene sulfonic acid, 0.8mol/l hydrochloric acid
Mixing, sends in ice-water bath, stirring reaction 30 minutes, and discharging is added drop-wise in above-mentioned prereduction Graphene, stirs 100 under room temperature
Minute, obtain sulfonated graphene；
（5）Above-mentioned sulfonated graphene, styrene are mixed, ultrasound 10 minutes adds potassium peroxydisulfate, stirs, be passed through nitrogen,
Insulated and stirred 6 hours at 70 DEG C, add above-mentioned hydrazine hydrate, and it is 80 DEG C to rise high-temperature, and insulation reaction 20 hours is cooled to room
Temperature, adds abovementioned alkyl ketene dimer, bis-phenol a diglycidyl ethers, stirs, and filters, and precipitation is sent into forced air drying
In case, complete, discharging is dried, polystyrene graphene composite material is obtained；
（6）Above-mentioned polyamide wax micropowder is added in the absolute ethyl alcohol of 10 times of its weight, it is 90 DEG C to rise high-temperature, insulated and stirred
20 minutes, above-mentioned stannous sulfide is added, is stirred to 60 DEG C, add above-mentioned polystyrene graphene composite material, silane coupler
Kh560, insulated and stirred 30 minutes obtain silane-modified alcohol liquid；
（7）By above-mentioned silane-modified alcohol liquid, butadiene rubber, age resistor TNP, butyl methacrylate, magnesium sulfate mixing, at 46 DEG C
Under plasticate 2 minutes, add remaining each raw material, knead 4 minutes, the elastomeric compound for obtaining is placed in two roller mills, at 30 DEG C
Mixing 6 minutes is supplemented, sizing material is parked 20 hours, sends in vulcanizing press, sulphur is carried out at 150 DEG C by discharging at room temperature
Change, obtain final product.
Stretch breaking strength（MPa）：18.1；
Surely stretch modulus 100%（MPa）：2.6；
Mooney viscosity：63；
70 DEG C × 70h air oven aging tests：
Breaking strength reduced rate：4.7%th, elongation at break reduced rate：8.2%.
Claims (2)
1. a kind of cracking resistance caulking gum material, it is characterised in that it is made up of the raw material of following weight parts：
Magnesium sulfate 2-4, barium metaborate 1-3, bis-phenol a diglycidyl ether 0.3-1, alkyl ketene dimer 2-4, age resistor
TNP3-4, butyl methacrylate 26-30, graphene oxide 10-14, sodium borohydride 1-2, p-aminobenzene sulfonic acid 3-4,0.8-
1mol/l hydrochloric acid 14-20, natrium nitrosum 1-2, styrene 43-50, potassium peroxydisulfate 0.3-0.5, hydrazine hydrate 0.5-1, butadiene rubber
210-300, vulcanizing agent PM1.7-2, stannous sulfide 1-2, short and long-chain acyl triglyceride molecules 3-4, polyamide wax micropowder 2-3,4- dimethylamino pyrrole
Pyridine 0.7-1, wollastonite in powder 10-14, silane coupler kh5600.7-1.
2. a kind of preparation method of cracking resistance caulking gum material as claimed in claim 1, it is characterised in that including following step
Suddenly：
（1）Above-mentioned wollastonite in powder is calcined into 1-2 hours at 700-800 DEG C, normal temperature is cooled to, is added to its weight 20-30 times
Deionized water in, add above-mentioned barium metaborate, it is 60-70 DEG C to rise high-temperature, and the hydrochloric acid of 10-15mol/l is added dropwise, and adjusts pH and is
2-3, insulated and stirred 20-30 minute, filters, and precipitation is mixed with above-mentioned graphene oxide, 1-2 is dried little at vacuum 50-60 DEG C
When, obtain composite graphite alkene；
（2）Composite graphite alkene is added in the deionized water of its weight 900-1000 times, ultrasonic 27-30 minutes, Graphene is obtained
Suspension；
（3）Above-mentioned sodium borohydride is added in its weight 15-20 times water, is stirred, sodium carbonate of the concentration for 4-6% is added dropwise
The aqueous solution, regulation pH are 9-10, are mixed with above-mentioned graphene suspension, the insulated and stirred 60-70 minute at 80-86 DEG C, are cooled down
To room temperature, ultrasonic 10-20 minutes, prereduction Graphene is obtained；
（4）Natrium nitrosum is added in its weight 170-200 times water, 2-3 DEG C is cooled to, with p-aminobenzene sulfonic acid, 0.8-
1mol/l mixed in hydrochloric acid, sends in ice-water bath, stirring reaction 30-40 minute, and discharging is added drop-wise in above-mentioned prereduction Graphene,
Stir 100-120 minutes under room temperature, obtain sulfonated graphene；
（5）Above-mentioned sulfonated graphene, styrene are mixed, ultrasonic 10-20 minutes, add potassium peroxydisulfate, stir, be passed through nitrogen
Gas, the insulated and stirred 6-7 hour at 70-76 DEG C add above-mentioned hydrazine hydrate, and it is 80-85 DEG C to rise high-temperature, insulation reaction 20-25
Hour, room temperature is cooled to, abovementioned alkyl ketene dimer, bis-phenol a diglycidyl ethers is added, is stirred, filtered, will precipitation
Send in air dry oven, be dried complete, discharging, obtain polystyrene graphene composite material；
（6）Above-mentioned polyamide wax micropowder is added in the absolute ethyl alcohol of its weight 10-13 times, it is 90-96 DEG C to rise high-temperature, is protected
Temperature stirring 20-30 minutes, above-mentioned stannous sulfide is added, is stirred to 60-65 DEG C, add above-mentioned polystyrene Graphene composite wood
Material, silane coupler kh560, insulated and stirred 30-40 minute, obtain silane-modified alcohol liquid；
（7）By above-mentioned silane-modified alcohol liquid, butadiene rubber, age resistor TNP, butyl methacrylate, magnesium sulfate mixing, in 46-
Plasticate at 50 DEG C 2-3 minutes, add remaining each raw material, knead 4-6 minutes, the elastomeric compound for obtaining is placed in two roller mills,
Supplement mixing 6-10 minutes at 30-40 DEG C, sizing material is parked 20-25 hours at room temperature for discharging, sends into vulcanizing press
In, vulcanized at 150-155 DEG C, obtained final product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201611096037.4A CN106519340A (en) | 2016-12-02 | 2016-12-02 | Anti-cracking seal rubber material and preparation method thereof |
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| CN201611096037.4A CN106519340A (en) | 2016-12-02 | 2016-12-02 | Anti-cracking seal rubber material and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116285130A (en) * | 2023-02-21 | 2023-06-23 | 山东永誉橡胶有限公司 | Tire curing bladder with long service life and preparation method thereof |
-
2016
- 2016-12-02 CN CN201611096037.4A patent/CN106519340A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116285130A (en) * | 2023-02-21 | 2023-06-23 | 山东永誉橡胶有限公司 | Tire curing bladder with long service life and preparation method thereof |
| CN116285130B (en) * | 2023-02-21 | 2023-09-08 | 山东永誉橡胶有限公司 | Tire curing bladder with long service life and preparation method thereof |
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Application publication date: 20170322 |