CN106554525A - A kind of fire protection flame retarding elastomeric material and preparation method thereof - Google Patents
A kind of fire protection flame retarding elastomeric material and preparation method thereof Download PDFInfo
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- CN106554525A CN106554525A CN201611096594.6A CN201611096594A CN106554525A CN 106554525 A CN106554525 A CN 106554525A CN 201611096594 A CN201611096594 A CN 201611096594A CN 106554525 A CN106554525 A CN 106554525A
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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
- C08F112/00—Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
- C08F112/02—Monomers containing only one unsaturated aliphatic radical
- C08F112/04—Monomers containing only one unsaturated aliphatic radical containing one ring
- C08F112/06—Hydrocarbons
- C08F112/08—Styrene
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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
- C08F2/00—Processes of polymerisation
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/22—Emulsion polymerisation
- C08F2/24—Emulsion polymerisation with the aid of emulsifying agents
- C08F2/26—Emulsion polymerisation with the aid of emulsifying agents anionic
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- 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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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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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
- C08L2201/02—Flame or fire retardant/resistant
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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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Abstract
The invention discloses a kind of fire protection flame retarding elastomeric material, it is made up of the raw material of following weight parts：Antimony oxide 34, Ethylene glycol dimethacrylate 24 30, age resistor CEA3 5, graphene oxide 10 14, sodium borohydride 12, p-aminobenzene sulfonic acid 34, 0.8 1mol/l hydrochloric acid 14 20, sodium nitrite 12, styrene 43 50, potassium peroxydisulfate 0.3 0.5, hydrazine hydrate 0.5 1, butadiene rubber 210 300, sulfur 1.7 2, 10 oleate 23 of polyglycereol, hexafluoroacetylacetone 12, 2 mercaptobenzimidazoles 23, Pulvis Talci 10 12, hydration zinc borate 34, pyromellitic acid dianhydride 0.6 1, molybdenum bisuphide 34.The antimony oxide for adding of the invention, Pulvis Talci, hydration zinc borate etc., all effectively raise the fire retardant performance of finished product.
Description
Technical field
The present invention relates to technical field of rubber material, more particularly to a kind of fire protection flame retarding elastomeric material and preparation method thereof.
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 derivant 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 methoies：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 often dispersibility is 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 dispersibility preferably,
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 polyreaction.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
Dispersibility 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, graphene oxide is mixed with other materials after equal Uniform, 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 dispersibility 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
Dispersibility 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 fire protection flame retarding elastomeric material and its preparation
Method.
The present invention is achieved by the following technical solutions：
A kind of fire protection flame retarding elastomeric material, it is made up of the raw material of following weight parts：
Antimony oxide 3-4, Ethylene glycol dimethacrylate 24-30, age resistor CEA3-5, graphene oxide 10-14, boron hydrogen
Change sodium 1-2, p-aminobenzene sulfonic acid 3-4,0.8-1mol/l hydrochloric acid 14-20, sodium nitrite 1-2, styrene 43-50, potassium peroxydisulfate
0.3-0.5, hydrazine hydrate 0.5-1, butadiene rubber 210-300, sulfur 1.7-2, Natrulon H-10 oleate 2-3, hexafluoroacetylacetone
1-2,2-mercaptobenzimidazole 2-3, Pulvis Talci 10-12, hydration zinc borate 3-4, pyromellitic acid dianhydride 0.6-1, molybdenum bisuphide 3-
4。
A kind of preparation method of described fire protection flame retarding elastomeric material, comprises the following steps：
（1）Add graphene oxide in the deionized water of its weight 900-1000 times, ultrasonic 27-30 minutes, obtain Graphene
Suspension；
（2）By above-mentioned antimony oxide, molybdenum bisuphide, hydration zinc borate mixing, be added to compound weight 30-40 times go from
In sub- water, it is 60-70 DEG C to rise high-temperature, adds above-mentioned Natrulon H-10 oleate, insulated and stirred 10-17 minute, with above-mentioned graphite
Alkene suspension mixes, and 100-200 rev/min of stirring 3-4 minute, obtains composite graphite alkene suspension；
（3）Above-mentioned sodium borohydride is added in its weight 15-20 times water, is stirred, sodium carbonate of the Deca concentration for 4-6%
Aqueous solution, regulation pH are 9-10, are mixed with above-mentioned composite graphite alkene suspension, and it is 80-86 DEG C to rise high-temperature, insulated and stirred 60-
70 minutes, room temperature is cooled to, ultrasonic 10-20 minutes, prereduction Graphene is obtained；
（4）Sodium nitrite 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 2-mercaptobenzimidazole is added in the dehydrated alcohol of its weight 7-10 times, it is 50-60 DEG C to rise high-temperature,
Insulated and stirred 3-4 minute, above-mentioned hexafluoroacetylacetone is added, is stirred to room temperature, is mixed with above-mentioned sulfonated graphene, ultrasonic 2-3
Minute, obtain sulfonated graphite enol liquid；
（6）Above-mentioned sulfonated graphite enol liquid, styrene are mixed, ultrasonic 10-20 minutes, add potassium peroxydisulfate, stir, led to
Enter nitrogen, the insulated and stirred 6-7 hour at 70-76 DEG C adds above-mentioned hydrazine hydrate, it is 80-85 DEG C to rise high-temperature, insulation reaction
20-25 hours, are cooled to room temperature, filter, and precipitation is sent in air dry oven, are dried complete, discharging, obtain polystyrene graphite
Alkene composite；
（7）By above-mentioned polystyrene graphene composite material, Ethylene glycol dimethacrylate, Pulvis Talci, butadiene rubber, anti-old
Agent CEA mixes, and plasticates 2-3 minutes at 46-50 DEG C, adds remaining each raw material, kneads 4-6 minutes, the elastomeric compound for obtaining is put
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,
Send in vulcanizing press, 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 solublity 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 stability and mechanical property of polymer
Energy；The antimony oxide for adding of the invention, Pulvis Talci, hydration zinc borate etc., all effectively raise the fire protection flame retarding of finished product
Energy.
Specific embodiment
A kind of fire protection flame retarding elastomeric material, it is made up of the raw material of following weight parts：
Antimony oxide 3, Ethylene glycol dimethacrylate 24, age resistor CEA3, graphene oxide 10, sodium borohydride 1, to ammonia
Base benzenesulfonic acid 3,0.8mol/l hydrochloric acid 14, sodium nitrite 1, styrene 43, potassium peroxydisulfate 0.3, hydrazine hydrate 0.5, butadiene rubber
210th, sulfur 1.7, polyglycerol acrylate 2, hexafluoroacetylacetone 1,2 mercaptobenzimidazoles 2, Pulvis Talci 10, hydration zinc borate 3,
Pyromellitic acid dianhydride 0.6, molybdenum bisuphide 3.
A kind of preparation method of described fire protection flame retarding elastomeric material, comprises the following steps：
（1）Add graphene oxide in the deionized water of 900 times of its weight, ultrasound 27 minutes obtains graphene suspension；
（2）By above-mentioned antimony oxide, molybdenum bisuphide, hydration zinc borate mixing, the deionization of 30 times of compound weight is added to
In water, it is 60 DEG C to rise high-temperature, adds above-mentioned polyglycerol acrylate, and insulated and stirred 10 minutes is mixed with above-mentioned graphene suspension
Close, 100 revs/min are stirred 3 minutes, obtain composite graphite alkene suspension；
（3）Above-mentioned sodium borohydride is added in 15 times of water of its weight, is stirred, Deca concentration be 4% sodium carbonate it is water-soluble
Liquid, it is 9 to adjust pH, is mixed with above-mentioned composite graphite alkene suspension, and it is 80 DEG C to rise high-temperature, and insulated and stirred 60 minutes is cooled to
Room temperature, ultrasound 10 minutes, obtains prereduction Graphene；
（4）Sodium nitrite 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 2 mercaptobenzimidazole is added in the dehydrated alcohol of 7 times of its weight, it is 50 DEG C to rise high-temperature, insulated and stirred
3 minutes, above-mentioned hexafluoroacetylacetone is added, is stirred to room temperature, is mixed with above-mentioned sulfonated graphene, ultrasound 2 minutes obtains sulfonation stone
Black enol liquid；
（6）Above-mentioned sulfonated graphite enol liquid, 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, insulation reaction 20 hours, cooling
To room temperature, filter, precipitation is sent in air dry oven, be dried complete, discharging, obtain polystyrene graphene composite material；
（7）By above-mentioned polystyrene graphene composite material, Ethylene glycol dimethacrylate, Pulvis Talci, butadiene rubber, anti-old
Agent CEA mixes, and plasticates 2 minutes at 46 DEG C, adds remaining each raw material, kneads 4 minutes, the elastomeric compound for obtaining is placed in two rollers and is opened
In mill, mixing 6 minutes is supplemented at 30 DEG C, sizing material is parked 20 hours by discharging at room temperature, is sent in vulcanizing press,
Vulcanized at 150 DEG C, obtained final product.
Stretch breaking strength（MPa）：18.2；
Surely stretch modulus 100%（MPa）：2.7；
Mooney viscosity：62；
70 DEG C × 70h air oven aging tests：
Breaking strength reduction rate：4.7%th, elongation at break reduction rate：8.2%.
Claims (2)
1. a kind of fire protection flame retarding elastomeric material, it is characterised in that it is made up of the raw material of following weight parts：
Antimony oxide 3-4, Ethylene glycol dimethacrylate 24-30, age resistor CEA3-5, graphene oxide 10-14, boron hydrogen
Change sodium 1-2, p-aminobenzene sulfonic acid 3-4,0.8-1mol/l hydrochloric acid 14-20, sodium nitrite 1-2, styrene 43-50, potassium peroxydisulfate
0.3-0.5, hydrazine hydrate 0.5-1, butadiene rubber 210-300, sulfur 1.7-2, Natrulon H-10 oleate 2-3, hexafluoroacetylacetone
1-2,2-mercaptobenzimidazole 2-3, Pulvis Talci 10-12, hydration zinc borate 3-4, pyromellitic acid dianhydride 0.6-1, molybdenum bisuphide 3-
4。
2. a kind of preparation method of fire protection flame retarding elastomeric material as claimed in claim 1, it is characterised in that including following step
Suddenly：
（1）Add graphene oxide in the deionized water of its weight 900-1000 times, ultrasonic 27-30 minutes, obtain Graphene
Suspension；
（2）By above-mentioned antimony oxide, molybdenum bisuphide, hydration zinc borate mixing, be added to compound weight 30-40 times go from
In sub- water, it is 60-70 DEG C to rise high-temperature, adds above-mentioned Natrulon H-10 oleate, insulated and stirred 10-17 minute, with above-mentioned graphite
Alkene suspension mixes, and 100-200 rev/min of stirring 3-4 minute, obtains composite graphite alkene suspension；
（3）Above-mentioned sodium borohydride is added in its weight 15-20 times water, is stirred, sodium carbonate of the Deca concentration for 4-6%
Aqueous solution, regulation pH are 9-10, are mixed with above-mentioned composite graphite alkene suspension, and it is 80-86 DEG C to rise high-temperature, insulated and stirred 60-
70 minutes, room temperature is cooled to, ultrasonic 10-20 minutes, prereduction Graphene is obtained；
（4）Sodium nitrite 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 2-mercaptobenzimidazole is added in the dehydrated alcohol of its weight 7-10 times, it is 50-60 DEG C to rise high-temperature,
Insulated and stirred 3-4 minute, above-mentioned hexafluoroacetylacetone is added, is stirred to room temperature, is mixed with above-mentioned sulfonated graphene, ultrasonic 2-3
Minute, obtain sulfonated graphite enol liquid；
（6）Above-mentioned sulfonated graphite enol liquid, styrene are mixed, ultrasonic 10-20 minutes, add potassium peroxydisulfate, stir, led to
Enter nitrogen, the insulated and stirred 6-7 hour at 70-76 DEG C adds above-mentioned hydrazine hydrate, it is 80-85 DEG C to rise high-temperature, insulation reaction
20-25 hours, are cooled to room temperature, filter, and precipitation is sent in air dry oven, are dried complete, discharging, obtain polystyrene graphite
Alkene composite；
（7）By above-mentioned polystyrene graphene composite material, Ethylene glycol dimethacrylate, Pulvis Talci, butadiene rubber, anti-old
Agent CEA mixes, and plasticates 2-3 minutes at 46-50 DEG C, adds remaining each raw material, kneads 4-6 minutes, the elastomeric compound for obtaining is put
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,
Send in vulcanizing press, vulcanized at 150-155 DEG C, obtained final product.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113345637A (en) * | 2021-06-04 | 2021-09-03 | 广东金华电缆股份有限公司 | Multi-core low-smoke halogen-free flame-retardant cable and preparation method thereof |
-
2016
- 2016-12-02 CN CN201611096594.6A patent/CN106554525A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113345637A (en) * | 2021-06-04 | 2021-09-03 | 广东金华电缆股份有限公司 | Multi-core low-smoke halogen-free flame-retardant cable and preparation method thereof |
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Application publication date: 20170405 |