CN107987451A - A kind of graphene oxide polypropylene plastics and preparation method - Google Patents
A kind of graphene oxide polypropylene plastics and preparation method Download PDFInfo
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- CN107987451A CN107987451A CN201711414989.0A CN201711414989A CN107987451A CN 107987451 A CN107987451 A CN 107987451A CN 201711414989 A CN201711414989 A CN 201711414989A CN 107987451 A CN107987451 A CN 107987451A
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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
- C08L51/00—Compositions of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers
- C08L51/06—Compositions of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers grafted on to homopolymers or copolymers of aliphatic hydrocarbons containing only one carbon-to-carbon double bond
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F255/00—Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00
- C08F255/02—Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00 on to polymers of olefins having two or three carbon atoms
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/2224—Magnesium hydroxide
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
- C08K2003/387—Borates
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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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- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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Abstract
The invention discloses a kind of graphene oxide polypropylene plastics and preparation method thereof, by the way that by polypropylene, fire retardant, modified addition lubricant, antioxidant are blended to obtain graphene oxide polypropylene plastics respectively.The preparation method breaches technological deficiency of the conventional mechanical with highstrenghtpiston's poor toughness, by adding graphene oxide, improve dispersing technology, graphene oxide is preferably combined with polypropylene, so that the heat resistance and intensity of graphene oxide polypropylene plastics prepared by the present invention are improved, increase polypropylene and the intermiscibility of other functional materials, and the preparation method is simple, raw material is easy to get, the polypropylene plastics products safety and environmental protection of preparation, has preferable application value.
Description
Technical field
The present invention relates to plastics preparation field, particularly a kind of graphene oxide polypropylene plastics and preparation method thereof.
Background technology
The electrical enclosure material that China uses at present is still based on polyvinyl chloride, however, halogen cable is meltable when heated
Melt, toxic gas caused by fire is occurring with the health of serious threat to fire victim, while also give rescue work band
To hinder.The electrical enclosure prepared at the same time using polyvinyl chloride, is generated heat under electric long-term work state, is also also easy to produce harmful gas
Taste endangers health of people.
Polypropylene is the highly crystalline polymer of nontoxic, odorless, tasteless milky, is product most light in current all plastics
One of kind, its is heat-resist, and continuous use temperature can reach 110~120 DEG C；Chemical property is good, hardly absorbs water, with absolutely mostly
Number chemicals does not react, and quality is pure, non-toxic；Not only it can be used as rubber, but also can be used as thermoplastic elastomer (TPE), also act as modeling
The anti-impact modifier and toughener of material, low-temperature flexibility is good, cost-effective, and EP rubbers, quilt are just gradually substituted in many occasions
It is widely used in modifying plastics.Since polypropylene quality is light, its mechanical strength is relatively weak, is not temporarily widely used in electricity at present
Device shell.
The content of the invention
It is an object of the invention to provide a kind of graphene oxide polypropylene plastics and preparation method thereof, to meet increasingly to increase
The demand of long halogen-free cable material.
The present invention is achieved by the following technical solutions：The preparation method of graphene oxide polypropylene plastics includes as follows
Step：
S1. polypropylene modification：Dispersant, maleic anhydride, high density poly propylene, initiator are added graphene oxide into, is led to
Cross double screw extruder melt blending and obtain modified polypropene；
S2. fire retardant is modified：Will metal compound fire retardant, borosilicate fire retardant drying after add silane coupling agent, dispersant,
Absolute ethyl alcohol question response is complete, is ultrasonically treated, and treats that ethanol volatilization is complete, is drying to obtain modified flame-retardant agent；
S3. stock up：Modified polypropene, modified flame-retardant agent, lubricant, antioxidant are put into high-speed mixer and are blended,
3 days are stood, it is stand-by to obtain mixture；S4. prepare：Mixture in step S3 is obtained by three-screw extruder melt blending
Graphene oxide polypropylene plastics.
Preferably, each component number is 40~60 parts of high density poly propylene, graphene oxide 16 in the modified polypropene
~26 parts, 1~5 part of maleic anhydride, 20~30 parts of dispersant, 0.1~3 part of initiator.
Preferably, each component number is 10~20 parts of metal compound fire retardant, borosilicate fire retardant 5 in the modified flame-retardant agent
~15 parts, 6~9 parts of silane coupling agent, 1~3 part of dispersant, 5~10 parts of absolute ethyl alcohol.
Preferably, the lubricant is the one or more in silicone oil, esters of silicon acis, phosphate, fluorocarbon oil, Tissuemat E.
Preferably, the antioxidant is one kind in double Lauryl Alcohol esters, bi-myristoleyl, double octadecanol esters.
Preferably, the dispersant is one kind in ethanol, methanol, acetone.
Preferably, borosilicate fire retardant is zinc borate and two kinds in silicones, Polyborosiloxane；Metal compound fire retardant is
Magnesium hydroxide presses 1 with aluminium hydroxide:1 ratio mixes.
Preferably, the initiator is polyvinylpyrrolidone, neopelex, sodium lignin sulfonate, poly- second
One or more in enol, polyethylene glycol oxide, polyacrylic acid, polymethylacrylic acid, polyacrylamide.
Preferably, the silane coupling agent is γ-(methacryloxypropyl) propyl trimethoxy silicane (KH570).
Compared with prior art, the invention has the advantages that：
Graphene oxide is added in graphene oxide polypropylene plastics prepared by the present invention, graphene oxide has in water
Superior dispersiveness, still, graphene oxide be of virtually it is amphipathic, from graphene platelet edge to center present it is hydrophilic to
Hydrophobic property distribution.Therefore, graphene oxide can generally there are interface such as interfacial agent, and reduce the energy between interface
Amount, the functional group enriched with higher specific surface area and surface, efficiently solves the intermiscibility of polypropylene and other materials, makes
Polypropylene while can accelerate raw material reaction rate, greatly reduce the reaction time with multiple compounds graft reaction, extend
Polyacrylic application range.
After oxidation processes, graphite oxide still keeps the layer structure of graphite, therefore and maleic anhydride inoculated polypropylene
Effective solution enhances polyacrylic heat resistance and ageing resistance after mixing.
The present invention utilizes the non-polar polymer that polypropylene is Halogen, can be compatible with multiple material after graft modification, with oxygen
There is the excellent of good mechanical and physical performance, electric property and splendid mixing and expressing technique performance after graphite alkene is compatible
Point, by special modified technique, using advanced Tri-screw Extrusion melt blending technique, obtains high temperature resistant, wear-resisting, fire-retardant etc.
Level is high, graphene oxide polypropylene plastics, and the igelite of mainstream can be effectively accounted for instead of first market, is provided simultaneously with pacifying
The features such as loopful is protected, performance is stable, service life is long.
Embodiment
The present invention is further described with reference to specific embodiment.Unless stated otherwise, the embodiment of the present invention uses
Various raw materials can by it is conventional it is purchased in market obtain, or be prepared according to the conventional method of this area, device therefor is real
Test commonly used equipment.Unless otherwise defined or described herein, all professional and scientific terms and art technology used herein are ripe
It is identical to practice meaning known to personnel.The present invention is described further by the following examples.
Embodiment 1
A kind of preparation method of graphene oxide polypropylene plastics includes the following steps：
S1. polypropylene modification：16 parts of graphene oxides are added into 20 parts of ethanol, 1 part of maleic anhydride, 40 parts of high density poly- third
Alkene, 0.1 part of polyvinylpyrrolidone, are blended 12min by 1900r/min high-speed mixers, are melted by double screw extruder
Blending obtains polymer-modified, and 192 DEG C, head pressure 3MPa, screw speed 98r/min of head temperature of control obtains modified poly- third
Alkene；
S2. fire retardant is modified：10 parts of metal compound fire retardants, 5 parts of borosilicate fire retardants are done in 105 DEG C of constant temperature oven
When 6 parts of silane coupling agents of addition, 1 part of acetone, 3 parts of absolute ethyl alcohols supersound process 3 are small after dry 24h, question response is complete, ethanol volatilization
Completely, dry 36h is placed in 105 DEG C of constant temperature oven up to modified flame-retardant agent；
S3. stock up：Modified polypropene, modified flame-retardant agent, 5 parts of lubricant, 8 parts of antioxidant are put into 1900r/min high
Blending in fast mixer, stands 3 days, it is stand-by to obtain mixture；
S4. prepare：By the mixture in step S3 by three-screw extruder melt blending, 190 DEG C of head temperature is controlled,
Head pressure 10MPa, 80~100r/min of screw speed, obtains graphene oxide polypropylene plastics.
Embodiment 2
A kind of preparation method of graphene oxide polypropylene plastics includes the following steps：
S1. polypropylene modification：18 parts of graphene oxides are added into 22 parts of ethanol, 2 parts of maleic anhydrides, 44 parts of high density poly- third
Alkene, 1 part of neopelex, are blended 12min by 1900r/min high-speed mixers, are melted by double screw extruder
Blending obtains polymer-modified, and 192 DEG C, head pressure 3MPa, screw speed 98r/min of head temperature of control obtains modified poly- third
Alkene；
S2. basic fire retardant is modified：By the constant temperature oven of 12 parts of metal compound fire retardants, 8 parts of borosilicate fire retardants at 105 DEG C
When 7 parts of silane coupling agents of addition, 2 parts of acetone, 4 parts of absolute ethyl alcohols supersound process 3 are small after middle dry 24h, question response is complete, ethanol
Volatilization is complete, is placed in 105 DEG C of constant temperature oven dry 36h up to modified basic fire retardant；
S3. stock up：Modified polypropene, modified flame-retardant agent, 5 parts of lubricant, 8 parts of antioxidant are put into 1900r/min high
Blending in fast mixer, stands 3 days, it is stand-by to obtain mixture；
S4. prepare：By the mixture in step S3 by three-screw extruder melt blending, 190 DEG C of head temperature is controlled,
Head pressure 10MPa, 80~100r/min of screw speed, obtains graphene oxide polypropylene plastics.
Embodiment 3
A kind of preparation method of graphene oxide polypropylene plastics includes the following steps：
S1. polypropylene modification：20 parts of graphene oxides are added into 25 parts of methanol, 3 parts of maleic anhydrides, 50 parts of high density poly- third
Alkene, 2 parts of neopelexes, are blended 12min by 1900r/min high-speed mixers, are melted by double screw extruder
Blending obtains polymer-modified, and 192 DEG C, head pressure 3MPa, screw speed 98r/min of head temperature of control obtains modified poly- third
Alkene；
S2. basic fire retardant is modified：15 parts of metal compound fire retardants, 10 parts of borosilicate fire retardants are dried in 105 DEG C of constant temperature
When 8 parts of silane coupling agents of addition, 2 parts of acetone, 6 parts of absolute ethyl alcohols supersound process 3 are small after dry 24h in case, question response is complete, second
Alcohol volatilization is complete, is placed in 105 DEG C of constant temperature oven dry 36h up to modified basic fire retardant；
S3. stock up：Modified polypropene, modified flame-retardant agent, 5 parts of lubricant, 8 parts of antioxidant are put into 1900r/min high
Blending in fast mixer, stands 3 days, it is stand-by to obtain mixture；
S4. prepare：By the mixture in step S3 by three-screw extruder melt blending, 190 DEG C of head temperature is controlled,
Head pressure 10MPa, 80~100r/min of screw speed, obtains graphene oxide polypropylene plastics.
Embodiment 4
A kind of preparation method of graphene oxide polypropylene plastics includes the following steps：
S1. polypropylene modification：26 parts of graphene oxides are added into 30 parts of acetone, 5 parts of maleic anhydrides, 60 parts of high density poly- third
Alkene, 3 parts of neopelexes, are blended 12min by 1900r/min high-speed mixers, are melted by double screw extruder
Blending obtains polymer-modified, and 192 DEG C, head pressure 3MPa, screw speed 98r/min of head temperature of control obtains modified poly- third
Alkene；
S2. basic fire retardant is modified：20 parts of metal compound fire retardants, 10 parts of borosilicate fire retardants are dried in 105 DEG C of constant temperature
When 9 parts of silane coupling agents of addition, 3 parts of acetone, 8 parts of absolute ethyl alcohols supersound process 3 are small after dry 24h in case, question response is complete, second
Alcohol volatilization is complete, is placed in 105 DEG C of constant temperature oven dry 36h up to modified basic fire retardant；
S3. stock up：Modified polypropene, modified flame-retardant agent, 5 parts of lubricant, 8 parts of antioxidant are put into 1900r/min high
Blending in fast mixer, stands 3 days, it is stand-by to obtain mixture；
S4. prepare：By the mixture in step S3 by three-screw extruder melt blending, 190 DEG C of head temperature is controlled,
Head pressure 10MPa, 80~100r/min of screw speed, obtains graphene oxide polypropylene plastics.
Comparative example 1
A kind of preparation method of graphene oxide polypropylene plastics includes the following steps：
S1. polypropylene modification：5 parts of maleic anhydrides, 60 parts of high density poly propylenes, 3 parts of neopelexes are added
In 30 parts of THF, 12min is blended by 1900r/min high-speed mixers, is obtained by double screw extruder melt blending modified poly-
Compound, controls 192 DEG C of head temperature, head pressure 3MPa, screw speed 98r/min obtains modified polypropene；
S2. basic fire retardant is modified：20 parts of metal compound fire retardants, 10 parts of borosilicate fire retardants are dried in 105 DEG C of constant temperature
When 3 parts of silane coupling agents of addition, 3 parts of THF, 8 parts of absolute ethyl alcohols supersound process 3 are small after dry 24h in case, question response is complete, second
Alcohol volatilization is complete, is placed in 105 DEG C of constant temperature oven dry 36h up to modified basic fire retardant；
S3. stock up：Modified polypropene, modified flame-retardant agent, 5 parts of lubricant, 8 parts of antioxidant are put into 1900r/min high
Blending in fast mixer, stands 3 days, it is stand-by to obtain mixture；
S4. prepare：By the mixture in step S3 by three-screw extruder melt blending, 190 DEG C of head temperature is controlled,
Head pressure 10MPa, 80~100r/min of screw speed, obtains graphene oxide polypropylene plastics.
Comparative example 2
S1. polypropylene modification：18 parts of graphene oxides are added into 30 parts of ethanol, 60 parts of high density poly propylenes, 3 parts of dodecanes
Base benzene sulfonic acid sodium salt, is blended 12min by 1900r/min high-speed mixers, is modified by double screw extruder melt blending
Polymer, controls 192 DEG C of head temperature, head pressure 3MPa, screw speed 98r/min obtains modified polypropene；
S2. prepared by fire retardant：By 20 parts of metal compound fire retardants, 3 parts of silane coupling agents, 3 parts of THF, borosilicate fire retardant, 3
When 8 parts of part silane coupling agent, 3 parts of dispersants, absolute ethyl alcohol supersound process 3 are small, question response is complete, ethanol volatilization is complete, is placed in
Dry 36h is up to fire retardant in 105 DEG C of constant temperature oven.
S3. stock up：It is mixed at a high speed that modified polypropene, fire retardant, 5 parts of lubricant, 8 parts of antioxidant are put into 1900r/min
Blending in conjunction machine, stands 3 days, it is stand-by to obtain mixture；
S4. prepare：By the mixture in step S3 by three-screw extruder melt blending, 190 DEG C of head temperature is controlled,
Head pressure 10MPa, 80~100r/min of screw speed, obtains graphene oxide polypropylene plastics.Detect example 1
To obtained graphene oxide polypropylene plastics in embodiment 1~4 and comparative example 1~2 according to GB/T1040.3-
2006 detection tensile strength and elongation at break, detect impact flexibility with GB/T1043.1-2008, the results are shown in Table 1.
Table 1
The preferred embodiment of the present invention described in detail above, still, during present invention is not limited to the embodiments described above
Detail, in the range of the technology design of the present invention, a variety of simple variants can be carried out to technical scheme, this
A little simple variants belong to protection scope of the present invention.
The measure of Martin Heat Resistant Temperature carries out in Martin heat resistance baking oven
It is further to note that each particular technique feature described in above-mentioned embodiment, in not lance
In the case of shield, can be combined by any suitable means, in order to avoid unnecessary repetition, the present invention to it is various can
The combination of energy no longer separately illustrates.
In addition, various embodiments of the present invention can be combined randomly, as long as it is without prejudice to originally
The thought of invention, it should equally be considered as content disclosed in this invention.
Claims (7)
- A kind of 1. preparation method of graphene oxide polypropylene plastics, it is characterised in that：Its preparation includes the following steps：S1. polypropylene modification：Dispersant, maleic anhydride, high density poly propylene, initiator are added graphene oxide into, by double Screw extruder melt blending obtains modified polypropene；S2. fire retardant is modified：Silane coupling agent, dispersant, anhydrous will be added after metal compound fire retardant, the drying of borosilicate fire retardant Ethanol question response is complete, is ultrasonically treated, and treats that ethanol volatilization is complete, is drying to obtain modified flame-retardant agent；S3. stock up：Modified polypropene, modified flame-retardant agent, lubricant, antioxidant are put into high-speed mixer and is blended, stands 3 My god, it is stand-by to obtain mixture；S4. prepare：Mixture in step S3 is obtained into graphene oxide polypropylene plastics by three-screw extruder melt blending Material.
- 2. graphene oxide polypropylene plastics according to claim 1, it is characterised in that：Each group in the modified polypropene Portioning number is 40 ~ 60 parts of high density poly propylene, 16 ~ 26 parts of graphene oxide, 1 ~ 5 part of maleic anhydride, 20 ~ 30 parts of dispersant, is drawn Send out 0.1 ~ 3 part of agent.
- 3. graphene oxide polypropylene plastics according to claim 1, it is characterised in that：Each group in the modified flame-retardant agent Portioning number is 10 ~ 20 parts of metal compound fire retardant, 5 ~ 15 parts of borosilicate fire retardant, 6 ~ 9 parts of silane coupling agent, 1 ~ 3 part of dispersant, nothing 5 ~ 10 parts of water-ethanol.
- 4. graphene oxide polypropylene plastics according to claim 1, it is characterised in that：The lubricant is silicone oil, silicon One or more in acid esters, phosphate, fluorocarbon oil, Tissuemat E.
- 5. graphene oxide polypropylene plastics according to claim 1, it is characterised in that：The antioxidant is double 12 carbon One kind in alcohol ester, bi-myristoleyl, double octadecanol esters.
- 6. graphene oxide polypropylene plastics according to claim 1, it is characterised in that：The dispersant is ethanol, first One kind in alcohol, acetone；Borosilicate fire retardant is zinc borate and two kinds in silicones, Polyborosiloxane；Metal compound fire retardant 1 is pressed for magnesium hydroxide and aluminium hydroxide:1 ratio mixes.
- 7. graphene oxide polypropylene plastics according to claim 1, it is characterised in that：The initiator is polyethylene pyrrole Pyrrolidone, neopelex, sodium lignin sulfonate, polyvinyl alcohol, polyethylene glycol oxide, polyacrylic acid, polymethyl One or more in acid, polyacrylamide.
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| CN109939611A (en) * | 2019-03-21 | 2019-06-28 | 山东华冠智能卡有限公司 | Graphene-based electrocondution slurry dispersing agent and preparation method thereof |
| CN111534108A (en) * | 2020-04-27 | 2020-08-14 | 浙江邦德管业有限公司 | Polypropylene pipe for buried high-voltage power cable and preparation method thereof |
| CN114213759A (en) * | 2022-01-04 | 2022-03-22 | 深圳中塑化工高性能材料有限公司 | Preparation method and application of polyphosphate grafted graphene flame-retardant modified polypropylene |
| CN117510730A (en) * | 2023-10-24 | 2024-02-06 | 上海泽明塑胶有限公司 | Preparation method of polyolefin for nylon production |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109939611A (en) * | 2019-03-21 | 2019-06-28 | 山东华冠智能卡有限公司 | Graphene-based electrocondution slurry dispersing agent and preparation method thereof |
| CN111534108A (en) * | 2020-04-27 | 2020-08-14 | 浙江邦德管业有限公司 | Polypropylene pipe for buried high-voltage power cable and preparation method thereof |
| CN114213759A (en) * | 2022-01-04 | 2022-03-22 | 深圳中塑化工高性能材料有限公司 | Preparation method and application of polyphosphate grafted graphene flame-retardant modified polypropylene |
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| CN117510730A (en) * | 2023-10-24 | 2024-02-06 | 上海泽明塑胶有限公司 | Preparation method of polyolefin for nylon production |
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