CN112574489A - Antistatic flame-retardant polyethylene material, preparation method thereof and mining polyethylene composite pipe - Google Patents
Antistatic flame-retardant polyethylene material, preparation method thereof and mining polyethylene composite pipe Download PDFInfo
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- CN112574489A CN112574489A CN201910945705.3A CN201910945705A CN112574489A CN 112574489 A CN112574489 A CN 112574489A CN 201910945705 A CN201910945705 A CN 201910945705A CN 112574489 A CN112574489 A CN 112574489A
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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
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/04—Homopolymers or copolymers of ethene
- C08L23/06—Polyethene
-
- C—CHEMISTRY; METALLURGY
- 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
- C08K3/32—Phosphorus-containing compounds
- C08K2003/321—Phosphates
- C08K2003/322—Ammonium phosphate
-
- C—CHEMISTRY; METALLURGY
- 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
- C08K2201/00—Specific properties of additives
- C08K2201/001—Conductive additives
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- C—CHEMISTRY; METALLURGY
- 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
- 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
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/016—Additives defined by their aspect ratio
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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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/04—Antistatic
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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
- C08L2203/00—Applications
- C08L2203/18—Applications used for pipes
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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
- C08L2207/00—Properties characterising the ingredient of the composition
- C08L2207/06—Properties of polyethylene
- C08L2207/062—HDPE
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Abstract
The invention provides an antistatic flame-retardant polyethylene material, a preparation method thereof and a mining polyethylene composite pipe, and relates to the field of high polymer materials. The antistatic flame-retardant polyethylene material solves the problems of mechanical property deterioration, poor processability and local non-uniform conductivity of the high-density polyethylene material caused by adding conductive carbon black as an antistatic agent into the high-density polyethylene. The antistatic flame-retardant polyethylene material comprises a flame retardant, a conductive agent, a surface treatment agent, an antioxidant and high-density polyethylene, wherein the conductive agent is a mixture of graphene and carbon nano tubes. The invention is used for preparing the mining polyethylene composite pipe.
Description
Technical Field
The invention relates to the field of high polymer materials, in particular to an antistatic flame-retardant polyethylene material, a preparation method thereof and a mining polyethylene composite pipe.
Background
The polyethylene pipe has the advantages of good corrosion resistance, long service life, light weight, convenient construction and the like, and is widely applied to various fields, in particular to the coal mining industry. When the polyethylene pipe is applied to the coal mine industry, the polyethylene pipe not only has the physical and mechanical properties of common polyethylene pipes, but also meets the special requirements of coal mines, such as antistatic property and flame retardance. However, since Polyethylene is an organic polymer material, which has a very High volume resistivity, generates static electricity by friction and is accumulated on the surface of plastic, which may cause fire and gas explosion, it is necessary to perform antistatic modification on High Density Polyethylene (High Density Polyethylene) for producing mining pipes.
Since the conductive carbon black has a large specific surface area and a good surface chemical property, and can obtain a good antistatic effect, in the prior art, the conductive carbon black is usually added to high-density polyethylene as an antistatic agent to achieve an antistatic effect. In order to obtain excellent antistatic property, a large amount of carbon black is often required to be added into the high-density polyethylene, and the problems of deterioration of mechanical property, poor processability and the like of the high-density polyethylene material are caused; in addition, the problem of nonuniform local conductivity of the high-density polyethylene material is easily caused due to insufficient stability of the carbon black type conductive material, so that the high-density polyethylene material cannot meet the requirement of the mining pipe.
Disclosure of Invention
In view of the above, embodiments of the present invention provide an antistatic flame-retardant polyethylene material, a preparation method thereof, and a mining polyethylene composite pipe, to solve the problems of mechanical property degradation, poor processability, and local non-uniform conductivity of a high-density polyethylene material caused by adding conductive carbon black as an antistatic agent to high-density polyethylene, and compared with the prior art, the antistatic flame-retardant polyethylene material provided by embodiments of the present invention has more excellent antistatic property, flame retardancy, and mechanical property.
In order to achieve the above purpose, the embodiment of the invention adopts the following technical scheme:
in a first aspect, an embodiment of the present invention provides an antistatic flame-retardant polyethylene material, including a flame retardant, a conductive agent, a surface treatment agent, an antioxidant, and high-density polyethylene, where the conductive agent is a mixture of graphene and carbon nanotubes.
Optionally, the flame retardant, the conductive agent, the surface treatment agent, the antioxidant and the high-density polyethylene are respectively 3-15 parts, 2-10 parts, 6-15 parts, 0.1-2 parts and 58-88.9 parts by mass; and/or in the conductive agent, the mass parts of the graphene and the carbon nano tube are 1-5 parts.
Optionally, the graphene has 2-10 layers of sheets, the maximum radial dimension of 2-20 μm, and the conductivity of 104s/m～105s/m; and/or the length-diameter ratio of the carbon nano tube is 10-25, and the conductivity is more than or equal to 6500 s/m.
Optionally, the weight average molecular weight of the high-density polyethylene is 5000-1000000; and/or, the surface treatment agent comprises polyethylene wax; and/or the flame retardant comprises at least one of a phosphorus flame retardant, a metal hydroxide, a nitrogen flame retardant and an intumescent flame retardant.
In a second aspect, an embodiment of the present invention provides a method for preparing an antistatic flame-retardant polyethylene material, for preparing the antistatic flame-retardant polyethylene material according to the first aspect, comprising: s1, melting and blending the flame retardant, the conductive agent, the surface treatment agent and the antioxidant to obtain the antistatic flame retardant; s2, melting and blending the high-density polyethylene, the antistatic flame retardant and the dispersing agent to obtain a high-density polyethylene/antistatic flame retardant mixture; and step S3, granulating the high-density polyethylene/antistatic flame retardant mixture to obtain the antistatic flame-retardant polyethylene material.
Optionally, when the antistatic flame retardant is prepared in step S1, the melt blending time is 30S to 300S, and the melt blending temperature is 50 to 180 ℃.
Optionally, the step S2 of melt blending the high-density polyethylene, the antistatic flame retardant, and the dispersant includes: step S21, melt blending the high-density polyethylene and the antistatic flame retardant; step S22, adding the dispersing agent into the mixture obtained in the step S21, and continuing melt blending; wherein the mixing rate of the step S22 is greater than the mixing rate of the step S21.
Optionally, in step S21, when the high-density polyethylene and the antistatic flame retardant are melt-blended, the melt-blending time is 30S to 300S, and the melt-blending temperature is 50 to 180 ℃; and/or, in step S22, adding the dispersing agent into the mixture obtained in step S21, and when the melt blending is continued, the melt blending time is 30-300S, and the melt blending temperature is 50-180 ℃.
Optionally, the addition amount of the dispersing agent is 1-5% of the total mass of the flame retardant, the conductive agent, the surface treatment agent, the antioxidant and the high-density polyethylene.
The third aspect and the embodiment of the invention also provide a mining polyethylene composite pipe, wherein the mining polyethylene composite pipe is made of the antistatic flame-retardant polyethylene material in the first aspect; and/or the mining polyethylene composite pipe is made of the antistatic flame-retardant polyethylene material prepared by the preparation method of the antistatic flame-retardant polyethylene material in the second aspect.
Based on this, the antistatic flame-retardant polyethylene material provided by the embodiment of the invention comprises the conductive agent which is a mixture of graphene and carbon nanotubes, and the graphene and the carbon nanotubes form a conductive network with a surface and line structure, so that a relatively perfect conductive path is formed, static charges on the surface of the HDPE material can be rapidly dispersed more easily, and a better antistatic effect is obtained. The molecular chain of the HDPE is wound and interpenetrated on a line and surface structure formed by the graphene and the carbon nano tube to form a high-molecular network structure, so that the winding degree of the molecular chain of the HDPE is improved, and the mechanical property of the HDPE material can be enhanced; in addition, the line and plane structure formed by the graphene and the carbon nano tube is beneficial to transmitting stress of a certain point to the whole high-molecular network by the HDPE molecular chain, so that the phenomenon that the HDPE material is broken due to stress concentration of the certain point in the material can not occur, and the mechanical property of the HDPE material is enhanced. The line and surface structure formed by the graphene and the carbon nano tube can promote the dispersion of the graphene and the carbon nano tube and the dispersion of the flame retardant, so that the flame retardant property of the HDPE material is greatly enhanced; in addition, the graphene and the carbon nano tube can be used as a synergist to play a synergistic effect with a flame retardant, so that a compact carbon layer is formed more easily in combustion for barrier protection, and the flame retardant effect is better. Therefore, compared with the prior art, the antistatic flame-retardant polyethylene material provided by the embodiment of the invention has more excellent antistatic property, flame retardance and mechanical property.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic flow chart of a method for preparing an antistatic flame-retardant polyethylene material according to an embodiment of the present invention;
fig. 2 is a schematic flow chart of a preparation method of another antistatic flame-retardant polyethylene material provided by an embodiment of the invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the prior art, conductive carbon black is usually added to high density polyethylene as an antistatic agent to achieve an antistatic effect. In order to obtain excellent antistatic property, a large amount of carbon black is often required to be added into the high-density polyethylene, and the problems of deterioration of mechanical property, poor processability and the like of the high-density polyethylene material are caused; in addition, the problem of nonuniform local conductivity of the high-density polyethylene material is easily caused due to insufficient stability of the carbon black type conductive material, so that the high-density polyethylene material cannot meet the requirement of the mining pipe.
In view of the above problems, in a first aspect, an embodiment of the present invention provides an antistatic flame-retardant polyethylene material, including a flame retardant, a conductive agent, a surface treatment agent, an antioxidant, and high-density polyethylene, where the conductive agent is a mixture of graphene and carbon nanotubes.
To illustrate the antistatic flame-retardant polyethylene material provided by the embodiments of the present invention more clearly, it should be noted that, firstly, the conductive agent has a large specific surface area and inherent van der waals force exists between molecules, so that the conductive agent is very easy to agglomerate, and the surface treatment agent is a functional assistant capable of forming a thin film having affinity with the high-density polyethylene material on the surface of the conductive agent, so that the thin film can effectively prevent the agglomeration of the conductive agent and improve the dispersibility of the conductive agent in polyethylene.
Second, high density Polyethylene (hdpe), also called low pressure Polyethylene, is a kind of Polyethylene (PE) plastic. The properties of polyethylene depend on its mode of polymerization. Ziegler-Natta polymerizations conducted under moderate pressure (15-30 atmospheres) organic compound catalyzed conditions are High Density Polyethylene (HDPE). The polyethylene molecules polymerized under such conditions are linear and have long molecular chains, up to several hundred thousand.
And thirdly, the graphene is a two-dimensional honeycomb lattice structure formed by tightly stacking single-layer carbon atoms, has a large pi bond conjugated system, unique physical structural characteristics and excellent properties, and can remarkably improve the electrical, mechanical and thermal properties of the composite material by only adding a small amount of graphene in the high-density polyethylene-based composite material due to the excellent properties.
The carbon nanotube is a one-dimensional quantum material with a special structure (the radial dimension is nanometer magnitude, the axial dimension is micrometer magnitude, and two ends of the tube are basically sealed), mainly comprises carbon atoms arranged in a hexagon to form a coaxial circular tube with a plurality of layers to dozens of layers, and the layers keep a fixed distance of about 0.34nm and the diameter is generally 2-20 nm. The carbon nano tube is used as a one-dimensional nano material, has light weight, perfect connection of a hexagonal structure and a plurality of abnormal mechanical, electrical and chemical properties.
Graphene and carbon nanotubes have similar properties in the aspects of electricity, mechanics and the like, but have many differences due to different structures, and carbon nanotubes and graphene are excellent one-dimensional and two-dimensional carbon materials respectively, and exhibit one-dimensional and two-dimensional anisotropy, such as electrical conductivity, mechanical properties, thermal conductivity and the like.
The antistatic flame-retardant polyethylene material provided by the embodiment of the invention combines the advantages of the antistatic flame-retardant polyethylene material and the carbon nanotube, and the graphene and the carbon nanotube are compounded and used for the composite material. Graphene and carbon nanotubes are compounded to form a linear and planar network structure, and the graphene and carbon nanotubes have more excellent performances than any single material, such as better isotropic conductivity, three-dimensional microporous network and the like, through a synergistic effect between the graphene and the carbon nanotubes.
Based on this, the antistatic flame-retardant polyethylene material provided by the embodiment of the invention comprises the conductive agent which is a mixture of graphene and carbon nanotubes, and the graphene and the carbon nanotubes form a conductive network with a surface and line structure, so that a relatively perfect conductive path is formed, static charges on the surface of the HDPE material can be rapidly dispersed more easily, and a better antistatic effect is obtained. The molecular chain of the HDPE is wound and interpenetrated on a line and surface structure formed by the graphene and the carbon nano tube to form a high-molecular network structure, so that the winding degree of the molecular chain of the HDPE is improved, and the mechanical property of the HDPE material can be enhanced; in addition, the line and plane structure formed by the graphene and the carbon nano tube is beneficial to transmitting stress of a certain point to the whole high-molecular network by the HDPE molecular chain, so that the phenomenon that the HDPE material is broken due to stress concentration of the certain point in the material can not occur, and the mechanical property of the HDPE material is enhanced. The line and surface structure formed by the graphene and the carbon nano tube can promote the dispersion of the graphene and the carbon nano tube and the dispersion of the flame retardant, so that the flame retardant property of the HDPE material is greatly enhanced; in addition, the graphene and the carbon nano tube can be used as a synergist to play a synergistic effect with a flame retardant, so that a compact carbon layer is formed more easily in combustion for barrier protection, and the flame retardant effect is better.
The performance test of the flame-retardant antistatic polyethylene provided by the embodiment of the invention can obtain that: surface resistance of 102-106Omega, the flame retardance is V0 grade, the tensile strength is 16-23MPa, the elongation at break is 450% -670%, and the impact strength is 22-28KJ/m2And the oxidation induction time (210 ℃) is more than or equal to 25 min.
Therefore, compared with the prior art, the antistatic flame-retardant polyethylene material provided by the embodiment of the invention has more excellent antistatic property, flame retardance and mechanical property. Solves the problems of the mechanical property deterioration, poor processability, high carbon deposition rate and non-uniform local conductivity of the high-density polyethylene material caused by adding the conductive carbon black as an antistatic agent into the high-density polyethylene.
In addition, the antistatic flame-retardant polyethylene materials (such as special materials for mineral pipes) on the market at present adopt imported carbon black, the addition amount is more than 8 wt%, the market influence is international, the selling price of the imported carbon black can reach 4-6 ten thousand per ton, and the carbon black accounts for large cost and specific gravity. The antistatic flame-retardant polyethylene material provided by the embodiment of the invention adopts the compound of graphene and carbon nano tubes as the antistatic agent, and the compound of graphene and carbon nano tubes has excellent conductivity, and the compound addition amount of graphene and carbon nano tubes is less than 4 wt%, so that the antistatic effect can be achieved, and the cost of the antistatic agent is reduced.
Illustratively, the flame retardant, the conductive agent, the surface treatment agent, the antioxidant and the high-density polyethylene are respectively 3-15 parts, 2-10 parts, 6-15 parts, 0.1-2 parts and 58-88.9 parts by mass. When the mass ratio of the flame retardant, the conductive agent, the surface treatment agent, the antioxidant and the high-density polyethylene is in the range, the antistatic property, the flame retardance and the mechanical property of the antistatic flame-retardant polyethylene material can be effectively improved under the condition of ensuring that the amount of the conductive agent is less.
In the conductive agent, the mass parts of the graphene and the carbon nano tube are 1-5 parts. When the mass ratio of the graphene to the carbon nano tube in the conductive agent is within the range, the forming surface and the line structure of the graphene and the carbon nano tube can be more stable and perfect, and the antistatic property, the flame retardance and the mechanical property of the antistatic flame-retardant polyethylene material provided by the embodiment of the invention are further improved.
Optionally, the graphene has 2-10 layers of sheets, the maximum radial dimension of 2-20 μm, and the conductivity of 104s/m～105s/m。
It is understood that graphene is a sheet-like structure material composed of a single layer of carbon atoms, which constitute a hexagonal honeycomb lattice structure with sp2 hybridized orbitals. The fewer graphene sheets are, the smaller the maximum radial dimension is, the larger the specific surface area is, the better the conductivity is, a more complete conductive path is easy to form, the better the conductivity of the obtained HDPE composite material is, and further the antistatic effect of the HDPE composite material is better.
Optionally, the length-diameter ratio of the carbon nanotube is 10-25, and the conductivity is greater than or equal to 6500 s/m.
It can be understood that, in order to form a line-plane network structure (three-dimensional) by matching with graphene, an ideal carbon nanotube here should be a rigid needle-shaped body with a larger long diameter, and the length-diameter ratio of the carbon nanotube should be as large as possible, but research shows that as the length-diameter ratio of the carbon nanotube increases, the number of carbon atom hole defects increases, which seriously affects the intrinsic comprehensive properties of force, electricity, heat, and the like; however, excessively reducing the length-diameter ratio of the carbon nanotube can cause the reduction of the toughening efficiency of the carbon nanotube to the HDPE composite material from the aspect of mechanical properties. Therefore, carbon nanotubes having an aspect ratio of 10 to 25 and a conductivity of 6500s/m or more are preferable.
Specifically, the antioxidant includes antioxidant 168 (tris [ 2.4-di-tert-butylphenyl ] phosphite).
Specifically, the weight average molecular weight of the high-density polyethylene is 5000-1000000.
Optionally, the surface treatment agent comprises one or more of polyethylene wax, silane coupling agent, titanate coupling agent, octadecylamine and isocyanic acid.
For the flame retardant, the flame retardant technology and the market are limited, the low-price halogen flame retardant is often selected for the high-density polyethylene used for producing the mining pipe, but strong acid gas and dense smoke are released in the combustion process of the halogen flame retardant, so that the environment is polluted. In recent years, it has been gradually replaced by halogen-free flame retardants. The existing halogen-free flame retardant comprises metal hydroxide, nitrogen flame retardant, phosphorus flame retardant and intumescent flame retardant.
Research shows that when the hydroxide is used as a flame retardant, the hydroxide can be decomposed into water in the combustion process to cause the damage of a flame-retardant system, so that the aim of flame retardance is fulfilled.
The nitrogen flame retardant is easy to release CO in case of fire2、N2、NH3、NO2And H2And the non-combustible gas such as O dilutes the concentration of oxygen in the air and the combustible gas generated when the HDPE is heated and decomposed, and simultaneously takes away a part of heat. The nitrogen can capture free radicals and inhibit the chain reaction of HDPE, thereby achieving the purpose of flame retardance.
The intumescent flame retardant is a flame retardant system which takes ammonium polyphosphate, ammonium phosphate, polyphosphate, sulfuric acid and other substances as acid elements, takes pentaerythritol, dipentaerythritol, ethylene glycol, expandable graphite and other substances as carbon sources, and takes melamine, urea, dicyandiamide and other substances as nitrogen sources. The composite has the advantages of high flame retardancy, no dripping behavior, excellent resistance to long-term or repeated exposure to flame, environmental protection and the like.
Phosphorus-based flame retardant systems are widely used industrially because of their advantages such as good flame retardancy and low toxicity. The red phosphorus forms phosphoric acid derivatives during combustion, and has the function of absorbing heat to prevent the formation of combustion products. The generated PO & free radical captures-H and-OH free radicals in the flame and plays a role in flame retardance. It is reported that the addition of 8% red phosphorus can achieve the flame retardancy of HDPE grade UL94V 0.
Based on this, optionally, the flame retardant of the antistatic flame-retardant polyethylene material provided by the embodiment of the present invention includes at least one of a phosphorus flame retardant, a metal hydroxide, a nitrogen flame retardant, and an intumescent flame retardant. Wherein the phosphorus flame retardant specifically comprises at least one of ammonium polyphosphate, ammonium phosphate, phosphite ester, organic phosphate and phosphine heterocyclic compound.
In a second aspect, as shown in fig. 1, an embodiment of the present invention further provides a method for preparing an antistatic flame-retardant polyethylene material, for preparing the antistatic flame-retardant polyethylene material according to the first aspect, including steps S1 to S3:
s1, melting and blending the flame retardant, the conductive agent, the surface treatment agent and the antioxidant to obtain the antistatic flame retardant; wherein the conductive agent is a mixture of graphene and carbon nanotubes.
S2, melting and blending the high-density polyethylene, the antistatic flame retardant and the dispersing agent to obtain a high-density polyethylene/antistatic flame retardant mixture;
and S3, granulating the high-density polyethylene/modified antistatic flame retardant mixture to obtain the antistatic flame-retardant polyethylene material.
It is understood that, first, the conductive agent is a mixture of graphene and carbon nanotubes, and is very easily agglomerated due to a large specific surface area of the mixture and inherent van der waals force between molecules. When the antistatic flame retardant is prepared in the step 1, namely the flame retardant, the conductive agent, the surface treatment agent and the antioxidant are melted and blended, the surface treatment agent can form a layer of film with affinity with the high-density polyethylene on the surface of the conductive agent, so that when the high-density polyethylene/antistatic flame retardant mixture is prepared in the step 2, namely the high-density polyethylene, the antistatic flame retardant obtained in the step 1 and the dispersing agent are melted and blended, the agglomeration of the conductive agent can be effectively prevented, and the dispersing ability of the conductive agent in the high-density polyethylene is improved.
Second, the dispersing agent is removed during the pelletization process of the high density polyethylene/modified antistatic flame retardant mixture in step S3, and thus the antistatic flame retardant polyethylene material of the first aspect, which is prepared by the above method, does not contain the above dispersing agent.
Compared with the prior art, the preparation method of the antistatic flame-retardant polyethylene material provided by the embodiment of the invention has the same beneficial effects as the antistatic flame-retardant polyethylene material provided by the embodiment, and the details are not repeated herein.
Specifically, the dispersant may be white oil.
Wherein, when the antistatic flame retardant is prepared in the step S1, the material mixing time is 30-300S, and the material mixing temperature is 50-180 ℃.
Specifically, as shown in fig. 2, step S2, melt-blending the high-density polyethylene, the antistatic flame retardant, and the dispersant, includes:
step S21, melting and blending the high-density polyethylene and the antistatic flame retardant;
step S22, adding a dispersing agent into the mixture obtained in the step S21, and continuing to melt and blend; wherein the blending rate of step S22 is greater than the blending rate of step S21.
Specifically, in the step S21, when the high-density polyethylene and the antistatic flame retardant are melt-blended, the mixing time is 30-300S, and the mixing temperature is 50-180 ℃;
and/or in step S22, adding a dispersing agent into the mixture obtained in step S21, and continuously mixing the materials for 30-300S and at the temperature of 50-180 ℃ when the melt blending is continued.
The addition amount of the dispersant is 1-5% of the total mass of the flame retardant, the conductive agent, the surface treatment agent, the antioxidant and the high-density polyethylene.
Specifically, in both the step S1 and the step S2, a high-speed mixer or an internal mixer can be used as a processing tool; step S3 may employ a twin-screw extruder or a single-screw extruder as a processing tool.
The embodiment of the invention also provides an antistatic flame-retardant mining polyethylene composite pipe, which is made of the antistatic flame-retardant polyethylene material in the first aspect; and/or the antistatic flame-retardant polyethylene material prepared by the preparation method of the antistatic flame-retardant polyethylene material of the second aspect.
Compared with the prior art, the antistatic flame-retardant mining polyethylene composite pipe provided by the embodiment of the invention has the same beneficial effect as the antistatic flame-retardant polyethylene material provided by the embodiment, and the details are not repeated herein.
Several examples of antistatic flame retardant polyethylene materials are given below and analyzed for material properties.
Example 1
1. Firstly, 3 parts of ammonium phosphate, 1 part of graphene, 1 part of carbon nano tube, 6 parts of polyethylene wax and 0.1 part of antioxidant 168 are put into a high-speed mixer, mixed and heated to 50 ℃ for 30 s.
2. Adding 88.9 parts of HDPE, continuously mixing for 60s, adding white oil with the total amount of 2%, continuously high-mixing for 30s, and taking out the material.
3. And (3) placing the mixed material in an extruder to extrude and granulate, thus obtaining the flame-retardant antistatic polyethylene.
The performance of the flame-retardant antistatic polyethylene in the example was tested, and the surface resistance was 106 Ω, the flame retardancy was V0 grade, the tensile strength was 22.6MPa, the elongation at break was 670%, and the impact strength was 22KJ/m2The oxidative induction time (210 ℃ C.) was 25 min.
Example 2
1. Firstly, putting 10 parts of ammonium polyphosphate, 5 parts of polyphosphate ester, 5 parts of graphene, 5 parts of carbon nano tube, 15 parts of polyethylene wax and 2 parts of antioxidant 168 into a high-speed mixer, mixing while heating to 50 ℃, and mixing for 60 s.
2. Adding 58 parts of HDPE, continuously mixing for 120s, adding white oil with the total amount of 4%, continuously high-mixing for 30s, and taking out the material.
3. And (3) placing the mixed material in an extruder to extrude and granulate, thus obtaining the flame-retardant antistatic polyethylene.
The performance of the flame-retardant antistatic polyethylene in the example was tested, and the surface resistance was 102 Ω, the flame retardancy was V0 grade, the tensile strength was 16MPa, the elongation at break was 470%, and the impact strength was 27KJ/m2The oxidation induction time (210 ℃ C.) was 26.5 min.
Example 3
1. Firstly, putting 8 parts of phosphine heterocyclic compound, 2 parts of ammonium phosphate, 2 parts of graphene, 3 parts of carbon nano tube, 6 parts of ethylene wax and 0.5 part of antioxidant 168 into a high-speed mixer, mixing while heating to 110 ℃, and mixing for 30 s.
2. Adding 78.5 parts of HDPE, continuously mixing for 90s, adding white oil with the total amount of 3%, continuously high-mixing for 30s, and taking out the material.
3. And (3) placing the mixed material in an extruder to extrude and granulate, thus obtaining the flame-retardant antistatic polyethylene.
The performance of the flame-retardant and antistatic polyethylene in the embodiment was measured, and the surface resistance was 2.1 × 103Omega, flame retardancy of V0 grade, tensile strength of 22MPa, elongation at break of 580%, and impact strength of 25KJ/m2The oxidation induction time (210 ℃) was 27 min.
Example 4
1. Firstly, 3 parts of phosphate, 2 parts of ammonium phosphate, 3 parts of polyphosphate, 3 parts of graphene, 2 parts of carbon nano tube, 4 parts of ethylene wax and 1 part of antioxidant 168 are put into a high-speed mixer, mixed and heated to 130 ℃ for 30 s.
2. Adding 82 parts of HDPE, continuously mixing for 120s, adding white oil with the total amount of 5%, continuously high-mixing for 30s, and taking out the material.
3. And (3) placing the mixed material in an extruder to extrude and granulate, thus obtaining the flame-retardant antistatic polyethylene.
Performance of the flame-retardant antistatic polyethylene in this exampleDetection shows that the surface resistance is 5.6 multiplied by 103Omega, flame retardancy of V0 grade, tensile strength of 21MPa, elongation at break of 650% and impact strength of 23KJ/m2The oxidation induction time (210 ℃ C.) was 25.5 min.
Comparative example 1
1. Firstly, 8 parts of phosphite ester, 2 parts of ammonium phosphate, 5 parts of cabot VXC72 carbon black, 6 parts of ethylene wax and 0.5 part of antioxidant 168 are put into a high-speed mixer and are mixed while the temperature is raised to 110 ℃ for 30 s.
2. Adding 78.5 parts of HDPE, continuously mixing for 90s, adding white oil with the total amount of 3%, continuously high-mixing for 30s, and taking out the material.
3. And (3) placing the mixed material in an extruder to extrude and granulate, thus obtaining the flame-retardant antistatic polyethylene.
The performance of the flame-retardant antistatic polyethylene in the comparative example is detected, and the surface resistance is 6 multiplied by 107Omega, flame retardancy of V1 grade, tensile strength of 13MPa, elongation at break of 400%, and impact strength of 17KJ/m2The oxidation induction time (210 ℃) was 20 min.
Comparative example 2
1. Firstly, 8 parts of organic phosphate, 2 parts of ammonium phosphate, 9 parts of cabot VXC72 carbon black, 6 parts of ethylene wax and 0.5 part of antioxidant 168 are put into a high-speed mixer and are mixed while the temperature is raised to 110 ℃ and the mixture is mixed for 30 s.
2. Adding 74.5 parts of HDPE, continuously mixing for 90s, adding white oil with the total amount of 3%, continuously high-mixing for 30s, and taking out the material.
3. And (3) placing the mixed material in an extruder to extrude and granulate, thus obtaining the flame-retardant antistatic polyethylene.
The performance of the flame-retardant antistatic polyethylene in the comparative example is detected, and the surface resistance is 3.3 multiplied by 105Omega, flame retardancy of V0 grade, tensile strength of 12.7MPa, elongation at break of 350 percent and impact strength of 18.1KJ/m2The oxidation induction time (210 ℃ C.) was 21.3 min.
Comparing examples 1 to 4 with comparative examples 1 to 2, it can be seen that:
in the above examples 1 to 4, the conductive agent (the composite of graphene and carbon nanotube) was used as the antistatic agent, and in the comparative examples 1 and 2, carbon black was used as the antistatic agent, so that the surface resistance, the flame retardancy, and the mechanical properties of the materials obtained in examples 1 to 4 were superior to those of the materials obtained in comparative examples 1 to 2.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention, and all the changes or substitutions should be covered within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.
Claims (10)
1. The antistatic flame-retardant polyethylene material is characterized by comprising a flame retardant, a conductive agent, a surface treatment agent, an antioxidant and high-density polyethylene, wherein the conductive agent is a mixture of graphene and carbon nano tubes.
2. The antistatic flame-retardant polyethylene material as claimed in claim 1, wherein the flame retardant, the conductive agent, the surface treatment agent, the antioxidant and the high-density polyethylene are respectively 3-15 parts, 2-10 parts, 6-15 parts, 0.1-2 parts and 58-88.9 parts by mass;
and/or in the conductive agent, the mass parts of the graphene and the carbon nano tube are 1-5 parts.
3. The antistatic flame-retardant polyethylene material according to claim 1,
the graphene has 2-10 layers of sheets, the maximum radial dimension of 2-20 mu m and the conductivity of 104s/m～105s/m；
And/or the length-diameter ratio of the carbon nano tube is 10-25, and the conductivity is more than or equal to 6500 s/m.
4. The antistatic flame retardant polyethylene material according to claim 1, wherein the high density polyethylene has a weight average molecular weight of 5000 to 1000000;
and/or, the surface treatment agent comprises polyethylene wax;
and/or the flame retardant comprises at least one of a phosphorus flame retardant, a metal hydroxide, a nitrogen flame retardant and an intumescent flame retardant.
5. A preparation method of the antistatic flame-retardant polyethylene material, which is used for preparing the antistatic flame-retardant polyethylene material as claimed in any one of claims 1 to 4, and is characterized by comprising the following steps:
s1, melting and blending the flame retardant, the conductive agent, the surface treatment agent and the antioxidant to obtain the antistatic flame retardant;
s2, melting and blending the high-density polyethylene, the antistatic flame retardant and the dispersing agent to obtain a high-density polyethylene/antistatic flame retardant mixture;
and step S3, granulating the high-density polyethylene/antistatic flame retardant mixture to obtain the antistatic flame-retardant polyethylene material.
6. The method for preparing an antistatic flame-retardant polyethylene material according to claim 5, wherein the melt blending time is 30S-300S and the melt blending temperature is 50-180 ℃ when the antistatic flame retardant is prepared in step S1.
7. The method for preparing the antistatic flame-retardant polyethylene material according to claim 5, wherein the step S2 of melt blending the high-density polyethylene, the antistatic flame retardant and the dispersing agent comprises:
step S21, melt blending the high-density polyethylene and the antistatic flame retardant;
step S22, adding the dispersing agent into the mixture obtained in the step S21, and continuing melt blending;
wherein the mixing rate of the step S22 is greater than the mixing rate of the step S21.
8. The method for preparing an antistatic flame-retardant polyethylene material according to claim 7,
in step S21, when the high-density polyethylene and the antistatic flame retardant are melt-blended, the melt-blending time is 30-300S, and the melt-blending temperature is 50-180 ℃;
and/or, in step S22, adding the dispersing agent into the mixture obtained in step S21, and when the melt blending is continued, the melt blending time is 30-300S, and the melt blending temperature is 50-180 ℃.
9. The method for preparing an antistatic flame-retardant polyethylene material according to claim 5, wherein the amount of the dispersant added is 1-5% of the total mass of the flame retardant, the conductive agent, the surface treatment agent, the antioxidant and the high-density polyethylene.
10. A mining polyethylene composite pipe is characterized in that the mining polyethylene composite pipe is made of the antistatic flame-retardant polyethylene material according to any one of claims 1-4;
and/or the presence of a gas in the gas,
the mining polyethylene composite pipe is made of the antistatic flame-retardant polyethylene material prepared by the preparation method of the antistatic flame-retardant polyethylene material according to any one of claims 5 to 9.
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