CN108586810A - A kind of graphene-based non-halogen flame-proof smoke-restraining agent preparation method and applications - Google Patents
A kind of graphene-based non-halogen flame-proof smoke-restraining agent preparation method and applications Download PDFInfo
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
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- C08K3/00—Use of inorganic substances as compounding ingredients
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- C08K3/32—Phosphorus-containing compounds
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
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- C08K5/34—Heterocyclic compounds having nitrogen in the ring
- C08K5/3467—Heterocyclic compounds having nitrogen in the ring having more than two nitrogen atoms in the ring
- C08K5/3477—Six-membered rings
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- C08K5/34922—Melamine; Derivatives thereof
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- C08K5/00—Use of organic ingredients
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- C08K5/34—Heterocyclic compounds having nitrogen in the ring
- C08K5/3467—Heterocyclic compounds having nitrogen in the ring having more than two nitrogen atoms in the ring
- C08K5/3477—Six-membered rings
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- C08K5/00—Use of organic ingredients
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
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- C08K3/32—Phosphorus-containing compounds
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Abstract
The present invention designs a kind of graphene-based non-halogen flame-proof smoke-restraining agent preparation method and applications.Specific embodiment is that the graphene oxide prepared by Hummers methods is template, then it is combined by chemical mode with fire retardant phosphorous derivant, nitrogen containing derivative, smoke suppressant ferrocene derivatives, it is restored finally by green reducing agent, a kind of graphene-based non-halogen flame-proof smoke-restraining agent is prepared.Graphene-based non-halogen flame-proof smoke-restraining agent prepared by the present invention has preparation process easy, collects acid source, air source and smoke suppressant one, and hygroscopicity is relatively low, preferable with polyolefins matrix compatibility, has good flame-retardant smoke inhibition effect to cable material of polyolefin.
Description
Technical field
The invention belongs to fire retardant technology of preparing and field of high polymer material modification, and in particular to a kind of graphene-based
Non-halogen flame-proof smoke-restraining agent and preparation method thereof and its application in polyvinyl chloride cable.
Background technology
Polyolefin is widely applied in industry-by-industries such as electronics, electric appliance, building, transport, furniture and mine cables.
But polyolefin needs that a large amount of plasticizer is added in process, with improve resin can processing type, may result in tree in this way
The anti-flammability of fat is greatly reduced, and becomes combustible material, and the life smoke of polyolefin is larger, in addition to this, a large amount of increase is added
Modeling agent can substantially reduce strength for polyvinyl chloride, its application is made to be restricted.
Common polyolefine fire retardant includes phosphorous, nitrogenous or inorganic filler smoke suppressant, and often physics is added to base-material
In, complex procedures are added, and anti-flaming smoke-inhibiting agent is easy the moisture absorption, in addition to this also results in base often with matrix poor compatibility
Body intensity is greatly reduced.
Graphene was found as a kind of emerging carbon nanomaterial in 2004 for the first time, be one kind by single layer of carbon atom
The cellular two-dimentional conjugated structure constituted, the specific surface area of super large, unique chemical constitution and impayable electricity, power
The performances such as, calorifics make it be caused widely in new energy field, photocatalysis field, biological field and environmental area etc.
Using.Especially graphene oxide has the functional groups such as abundant hydroxyl, epoxy group, carboxyl on graphene oxide, can be very big
Improve the dispersibility of graphene, and functional group thereon provides reaction site for later stage modification.
Invention content
The present invention is directed to overcome the deficiencies of the prior art and provide a kind of graphene-based non-halogen flame-proof smoke-restraining agent and its preparation side
Method.
A kind of graphene-based non-halogen flame-proof smoke-restraining agent, the preparation method that the present invention takes are：
1）Graphene oxide is scattered in organic solvent, carries out ultrasonic disperse 4-8 hours, obtains graphene oxide dispersion,
The organic solvent is dimethylformamide or dimethyl sulfoxide (DMSO), and the graphene oxide content is 0.1-1 mg/ml.
2）Into the graphene oxide solution obtained by step (1), the phosphoric acid derivatives of different proportion, nitrogenous derivative is added
After object, ferrocene derivatives, after stirring and dissolving, catalyst is added, raising reaction temperature is to 90-130 DEG C, after reacting 2-6 hours,
Green reducing agent is added to be filtered, washed, dried with nylon membrane after the reaction was continued 4-8 hours, grinds, a kind of graphite is prepared
Alkenyl non-halogen flame-proof smoke-restraining agent.
In the present invention, the graphene oxide is prepared using well known Hummers.
In the present invention, the graphene oxide and phosphoric acid derivatives, nitrogen containing derivative, ferrocene derivatives：Reducing agent
Weight ratio be：0.1：（1-10）：（1-10）：（1-10）：（1-5）.
In the present invention, the phosphoric acid derivatives are selected from phosphoric acid, triethyl phosphate, diethyl phosphate, triphenyl phosphate, Asia
Phosphate, N, at least one of bis- (2- ethoxys) the aminomethy-lenephosphonic acids diethylesters of N-..
In the present invention, the nitrogen containing derivative is selected from melamine, trimethylol melamine, three（2- ethoxys）It is different
At least one of cyanurate.
In the present invention, the ferrocene derivatives are selected from Aminoferrocene, diamino ferrocene, carboxyl ferrocene, two
At least one of carboxyl ferrocene, ferrocene methanol.
In the present invention, the reducing agent be green reducing agent, selected from vitamin C, ascorbic acid, citric acid, maltose,
At least one of glucose.
In the present invention, the catalyst is selected from p-methyl benzenesulfonic acid.
Graphene-based non-halogen flame-proof smoke-restraining agent concrete application mode is used in the present invention can hand over to prepare a kind of halogen-free flameproof
Join cable material of polyolefin, is made of the raw material of following parts by weight：100 parts of polyolefin base material, plasticizer phthalic acid ester 10-40
Part, 10-30 parts of graphene-based non-halogen flame-proof smoke-restraining agent, 40-60 parts of magnesium hydroxide, 0.1-5 parts of vinyl silicane coupling agent, processing
0.5-2 parts of compositions of auxiliary agent.
The invention further relates to the preparation methods of such CABLE MATERIALS
（1）Filler is added separately in star lapping machine, is added in ethanol/water (50/50 mass parts), vinyl is then added
Silane coupling agent is ground 5-10 hours, and grinding temperature is no more than 40 DEG C, and fineness of grind reaches<20um, then by grinding slurry
It dried, crush the filler for preparing and being modified；
（2）Polyolefin base material, step (1) modified inorganic filler, graphene-based non-halogen flame-proof smoke-restraining material, plasticizer, processing are helped
Agent is added in high-speed mixer and is uniformly mixed, and then mixed material is added in screw extruder again, and extrusion temperature control exists
140-160 DEG C, is divided to be granulated through melting extrusion in screw speed 20-200 rpm/.
It by graphene is template set that the technical solution adopted by the present invention, which is by acid source, air source, carbon forming agent and smoke suppressant,
Close one, it is on the one hand heated when catching fire, phosphoric acid class acid source can charing black lead alkene or matrix, form carbon-coating, and air source by
Heat releases gas, carbon-coating can be made to expand, and forms porous carbon layer, fire-retardant heat transfer, while smoke suppressant can reduce smog
It generates, on the other hand, the addition of a large amount of anti-flaming smoke-inhibiting agents often leads to the intensity decline of matrix, and the addition of graphene can be shown
Write the intensity for improving matrix, while additions of graphene can avoid commonly using the water absorption issue that brings of carbon source pentaerythrite, acid source,
Carbon source and smoke suppressant are by reactive grafting to graphene, avoiding what each component was separately added to bring for a long time in matrix from moving
Shifting problem.
Compared with prior art, the present invention has following usefulness：
The present invention utilizes graphene oxide large specific surface area, and reaction site is more, and fire-retardant acid source, air source and smoke suppressant are led to
It crosses in chemical reaction set to graphene oxide, the graphene-based non-halogen flame-proof smoke-restraining agent prepared has fire-retardant, smoke suppressing effect
Good, preparation process is easy, feature easy to use, and good with the compatibility of matrix, and can significantly improve improves the fire-retardant of material
Smoke suppressing, while the good mechanical performance of graphene, can also improve the intensity of cable material of polyolefin, utilize the graphene of preparation
The agent of base non-halogen flame-proof smoke-restraining can prepare the cable material of polyolefin of excellent combination property, have good application prospect.
Specific implementation mode
For a further understanding of the present invention, the present invention is illustrated with reference to specific implementation case.
Embodiment 1
A kind of graphene-based non-halogen flame-proof smoke-restraining agent, specific solution are：
1）1g graphene oxides are scattered in organic solvent, carry out ultrasonic disperse 4-8 hours, obtain graphene oxide dispersion
Liquid, the organic solvent are dimethylformamide or dimethyl sulfoxide (DMSO), and the graphene oxide content is 0.2 mg/ml.
2）Into the graphene oxide solution obtained by step (1), 10g phosphoric acid, 10g melamines, two cyclopentadienyl of 10g carboxyls is added
After iron, after stirring and dissolving, 0.5g p-methyl benzenesulfonic acids are added, increases reaction temperature to 90-130 DEG C, after reacting 2-6 hours, adds
Enter 10g vitamin Cs, after the reaction was continued 4-8 hours, be filtered, washed, dried with nylon membrane, grinds, a kind of graphene is prepared
Base non-halogen flame-proof smoke-restraining agent, product are brown-black powder product.
Embodiment 2
A kind of graphene-based non-halogen flame-proof smoke-restraining agent, specific solution are：
1）1g graphene oxides are scattered in organic solvent, carry out ultrasonic disperse 4-8 hours, obtain graphene oxide dispersion
Liquid, the organic solvent are dimethylformamide or dimethyl sulfoxide (DMSO), and the graphene oxide content is 0.2 mg/ml.
2）Into the graphene oxide solution obtained by step (1), 10g triethyl phosphates, 20g trihydroxy methyl melamines is added
After amine, 30g carboxyl ferrocene, after stirring and dissolving, 0.5g p-methyl benzenesulfonic acids are added, increase reaction temperature to 90-130 DEG C, instead
After answering 2-6 hours, 10g vitamin Cs are added and is filtered, washed, dried with nylon membrane after the reaction was continued 4-8 hours, grind, prepare
A kind of graphene-based non-halogen flame-proof smoke-restraining agent is obtained, product is brown-black powder product.
Embodiment 3
A kind of graphene-based non-halogen flame-proof smoke-restraining agent, specific solution are：
1）1g graphene oxides are scattered in organic solvent, carry out ultrasonic disperse 4-8 hours, obtain graphene oxide dispersion
Liquid, the organic solvent are dimethylformamide or dimethyl sulfoxide (DMSO), and the graphene oxide content is 0.2 mg/ml.
2）Into the graphene oxide solution obtained by step (1), 50g diethyl phosphites, 90g tri- is added（2- ethoxys）
After isocyanuric acid ester, 60g carboxyl ferrocene, after stirring and dissolving, 0.5g p-methyl benzenesulfonic acids are added, increase reaction temperature to 90-
130 DEG C, after reacting 2-6 hours, 30g citric acids is added and is filtered, washed, dried with nylon membrane, ground after the reaction was continued 4-8 hours
Mill, is prepared a kind of graphene-based non-halogen flame-proof smoke-restraining agent, and product is brown-black powder product.
In order to further verify the effect of graphene-based non-halogen flame-proof smoke-restraining agent prepared by the present invention, with the graphite of embodiment preparation
Alkenyl non-halogen flame-proof smoke-restraining agent prepares CABLE MATERIALS, and tests the performance of CABLE MATERIALS, and correlated performance is shown in Table lattice 1；
100 parts of polyolefin base material, 10-40 parts of plasticizer phthalic acid ester, 10-30 parts of graphene-based non-halogen flame-proof smoke-restraining agent,
0.5-2 parts of 40-60 parts of magnesium hydroxide, 0.1-5 parts of vinyl silicane coupling agent, processing aid compositions.
A kind of preparation method of cable material of polyolefin is：
（1）Filler is added separately in star lapping machine, is added in ethanol/water (50/50 mass parts), vinyl is then added
Silane coupling agent is ground 5-10 hours, and grinding temperature is no more than 40 DEG C, and fineness of grind reaches<20um, then by grinding slurry
It dried, crush the filler for preparing and being modified；
（2）Polyolefin base material, step (1) modified inorganic filler, graphene-based non-halogen flame-proof smoke-restraining material, plasticizer, processing are helped
Agent is added in high-speed mixer and is uniformly mixed, and then mixed material is added in screw extruder again, and extrusion temperature control exists
140-160 DEG C, is divided to be granulated through melting extrusion in screw speed 20-200 rpm/.
Table 1
| Project | Embodiment 4 | Embodiment 5 | Embodiment 6 | Embodiment 7 | Embodiment 8 | Comparative example 1 |
| Polyolefin base material | 100 | 100 | 100 | 100 | 100 | 100 |
| Phthalic acid ester | 20 | 20 | 20 | 20 | 20 | 20 |
| 1 graphene-based non-halogen flame-proof smoke-restraining agent of embodiment | 10 | 20 | 30 | |||
| 2 graphene-based non-halogen flame-proof smoke-restraining agent of embodiment | 20 | 20 | ||||
| 3 graphene-based non-halogen flame-proof smoke-restraining agent of embodiment | 20 | |||||
| Magnesium hydroxide | 50 | 50 | 50 | 50 | 50 | 50 |
| Vinyl silicane coupling agent | 1 | 1 | 1 | 1 | 1 | 1 |
| Processing aid | 1 | 1 | 1 | 1 | 1 | 1 |
| Tensile strength (MPa) | 19.3 | 18.7 | 17.5 | 18.9 | 19.2 | 23.5 |
| Elongation at break（%） | 250 | 230 | 190 | 210 | 220 | 270 |
| Smoke density（There is cigarette） | 23 | 19 | 17 | 21 | 20 | 34 |
| Oxygen index (OI) | 31 | 37 | 39 | 38 | 36 | 23 |
From the point of view of 1 result of embodiment 5-8 and comparative example, by the polyolefin cable for adding graphene-based non-halogen flame-proof smoke-restraining agent
Material has good smoke suppressing effect and preferable flame retardant property, and adding procedure is convenient, preferable with the compatibility of matrix, does not allow
Easily it is precipitated from matrix.
Claims (9)
1. a kind of preparation method of graphene-based non-halogen flame-proof smoke-restraining agent, which is characterized in that including following preparation process：
1）Graphene oxide is scattered in organic solvent, carries out ultrasonic disperse 4-8 hours, obtains graphene oxide dispersion,
The organic solvent is dimethylformamide or dimethyl sulfoxide (DMSO), and the graphene oxide content is 0.1-1 mg/ml;
2）Into the graphene oxide solution obtained by step (1), the phosphoric acid derivatives of different proportion, nitrogen containing derivative, two are added
After luxuriant iron derivative, after stirring and dissolving, catalyst is added, increases reaction temperature to 90-130 DEG C, after reacting 2-6 hours, is added
Green reducing agent is filtered, washed with nylon membrane, is dried after the reaction was continued 4-8 hours, grinding, is prepared a kind of graphene-based
Non-halogen flame-proof smoke-restraining agent.
2. a kind of preparation method of graphene-based non-halogen flame-proof smoke-restraining agent according to claim 1, which is characterized in that described
Graphene oxide using well known Hummers prepare.
3. a kind of preparation method of graphene-based non-halogen flame-proof smoke-restraining agent according to claim 1, which is characterized in that described
The weight ratio of graphene oxide and phosphoric acid derivatives, nitrogen containing derivative, ferrocene derivatives, reducing agent be：0.1：（1-10）：
（1-10）：（1-10）：（1-5）.
4. a kind of preparation method of graphene-based non-halogen flame-proof smoke-restraining agent according to claim 1, which is characterized in that described
Phosphoric acid derivatives be selected from phosphoric acid, triethyl phosphate, diethyl phosphate, triphenyl phosphate, phosphite ester, N, bis- (the 2- hydroxyl second of N-
Base) aminomethy-lenephosphonic acids diethylester at least one.
5. a kind of preparation method of graphene-based non-halogen flame-proof smoke-restraining agent according to claim 1, which is characterized in that described
Nitrogen containing derivative be selected from melamine, trimethylol melamine, three（2- ethoxys）At least one of isocyanuric acid ester.
6. a kind of preparation method of graphene-based non-halogen flame-proof smoke-restraining agent according to claim 1, which is characterized in that described
Ferrocene derivatives be selected from Aminoferrocene, diamino ferrocene, carboxyl ferrocene, dicarboxyl ferrocene, ferrocene methanol
At least one.
7. a kind of preparation method of graphene-based non-halogen flame-proof smoke-restraining agent according to claim 1, which is characterized in that described
Reducing agent be green reducing agent, selected from vitamin C, ascorbic acid, citric acid, maltose, at least one of glucose.
8. a kind of preparation method of graphene-based non-halogen flame-proof smoke-restraining agent according to claim 1, which is characterized in that described
Catalyst be selected from p-methyl benzenesulfonic acid.
9. a kind of preparation method of graphene-based non-halogen flame-proof smoke-restraining agent according to claim 1-8, which is characterized in that institute
A kind of halogen-free flameproof crosslinkable polyolefin CABLE MATERIALS stated, is made of the raw material of following parts by weight：100 parts of polyolefin base material increases
Mould 10-40 parts of agent phthalic acid ester, 10-30 parts of graphene-based non-halogen flame-proof smoke-restraining agent, 40-60 parts of magnesium hydroxide, vinyl
0.5-2 parts of 0.1-5 parts of silane coupling agent, processing aid compositions.
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| CN110643070B (en) * | 2019-10-17 | 2021-07-13 | 西北师范大学 | Attapulgite/graphene oxide composite material, preparation method thereof and application of attapulgite/graphene oxide composite material as high polymer material auxiliary agent |
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Application publication date: 20180928 |