CN109608732A - A kind of anti-electrostatic fire retardant type polyethylene composition, particle, tubing and its preparation method and the purposes as coal mine tubing - Google Patents
A kind of anti-electrostatic fire retardant type polyethylene composition, particle, tubing and its preparation method and the purposes as coal mine tubing Download PDFInfo
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- 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
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Abstract
The present invention discloses a kind of anti-electrostatic fire retardant type polyethylene composition, particle, tubing and preparation method thereof and the purposes as coal mine tubing.The composition includes high density polyethylene (HDPE), graphene, fire retardant, dispersion liquid, nucleating agent and antioxidant, it solves the problems, such as that existing anti-electrostatic fire retardant type polythene material fire retardant, antistatic agent, conductive filler additive amount are excessive, overcomes the additive amount of existing graphene greatly and dispersed poor defect.The present invention activeness and quietness characteristic excellent using graphene, so that system is without adding toughener, graphene/polythene material the mechanical property being prepared simultaneously reaches the requirement (tensile strength >=9MPa, elongation at break >=300%) of GB/T8804-2003 in colliery industry standard MT558.1-2005 " measurement of thermoplastic plastic pipe tensile property ", product of the present invention tensile strength is up to 28MPa, and elongation at break is up to 340%.
Description
Technical field
The present invention relates to anti-electrostatic fire retardant type polythene material field, in particular to a kind of anti-electrostatic fire retardant type polyethylene
Composition, particle, tubing and its preparation method and purposes as coal mine tubing.
Background technique
Polyethylene (PE) tubing has many advantages, such as good corrosion resistance, long service life, light weight, easy for construction, extensive
Use applied to every field, especially in coal mining.But the PE tubing of underground mine use is in antistatic and flame retardant property
The requirement of aspect is extremely harsh, and needs to have good mechanical mechanics property.
Since PE itself belongs to flammable and insulation material, in underground coal mine use, there are very big hidden danger.Usual way
It is that fire retardant and the antistatic agent of certain content are added into system to meet fire-retardant, antistatic property the requirement of tubing.
CN1221604C discloses anti-electrostatic flame-retardant polyvinyl composite pipe and preparation process, using bromide fire retardant and contains
Antimonial cooperative flame retardant, and conductive black is modified, mixing extruding pelletization, it prepares a kind of with fire retardant, antistatic
Polyvinyl piping materials.Synergistic fire retardant additive amount is larger in the preparation method (25wt% for accounting for about system), to the mechanics of tubing
Performance is affected, and the noxious material environmental pollution for generation of burning is serious, not with current halogen-free flame retardants usage trend
Symbol.
CN103172920A discloses environmental-protection flame-retardant electrostatic resistant polythene mining tube, passes through the high concentration of 30~50wt%
Dilution is blended with HDPE matrix and is prepared antistatic polyethylene pipe material for black masterbatch, and preparation high concentration master batch needs very strong spiral shell
Bar shearing force, it is at high cost, production efficiency is low.CN106633344A disclose a kind of antistatic functional masterbatch and its production technology,
Polyvinyl piping materials production technology, using superconductive carbon black: 15-30%, lubricant: 0.1-10%, coupling agent: 0.5-5%, dispersion
Agent: 3-11%, linear low density polyethylene (LLDPE): 30-80% obtains antistatic functional masterbatch, due to normal process temperature
At 180~240 DEG C or so, the charcoal clandestine meeting of high additive amount promotes system viscosity excessively high, in order to reduce the viscosity of system, needs to add
Work temperature is improved to 260~300 DEG C, however processing temperature higher in this way can destroy the high temperature degradation of substrate molecule chain, is destroyed
The structure of filler.CN104277279A discloses a kind of fire retardant, antistatic polyethylene pipe material and preparation method thereof, by 20~
The conductive black of 40wt% is added in high density polyethylene (HDPE) matrix, under coupling agent and adjuvant effect, reaches antistatic work
With, but high additive amount carbon black leads to mechanical properties of tubular goods degradation, while multiple material melt viscosity is got higher, tube extrusion process
In torque occur excessive, squeeze out phenomena such as unstable, can also make tubing matter double wall thick, rough surface.
CN106867076A discloses a kind of mining graphene enhancing dual anti-tubing preparation method of ultra-high molecular weight polyethylene,
The invention is using ultra-high molecular weight polyethylene as tubing matrix, by many auxiliary agents by reinforcing filler nano-graphene in ethyl alcohol
After being modified in system, dispersion is prepared in the base, however graphite of the graphene after ethyl alcohol infiltration washing, after drying
Alkene specific surface area can obviously become smaller, and electric conductivity is deteriorated.Meanwhile ultra-high molecular weight polyethylene due to molecular weight it is larger (350~
1000 ten thousand), and melt viscosity is high, cause its processing difficulties, complex process, and graphene additive amount larger (3~5wt%), cost
It is higher.Corresponding graphene tubing tensile strength has dropped 20~30% for comparing pure ultra-high molecular mass polyethylene, not
Highlight conduction and reinforcing effect of the graphene in High molecular weight polyethylene system.
CN104262740A discloses a kind of hdpe pipe, prepares graphene powder using screw extruder
Modified hdpe pipe, but the graphene powder specific surface area of high-quality is larger, lamella is few, apparent activation energy ratio
It is higher, easily reunite, density is small, and for the additive amount for the graphene that this application uses for 5~6wt%, additive amount is relatively high, and should
Graphene powder is blended using direct Screw Extrusion in application, but graphene powder is also difficult to directly squeeze by twin-screw at this stage
Out, it will cause graphene powder all to float on spout upper layer, be not easy to be added in plastics system, cause to disperse poor, final production
Tubing sheet resistance 1.0 × 106Ω or more does not meet pipe material for coal mine standard.In addition, the fire retardant that this application uses
For deca-BDE and antimony oxide, wherein deca-BDE is 6-14wt%, antimony oxide 7-15wt%, fire retardant
Additive amount is larger.
In summary the analysis of the prior art is it is found that largely the addition of fire retardant, antistatic agent is to polyvinyl piping materials sheet
The mechanical property of body such as tensile strength, toughness is affected, and polyvinyl piping materials mechanical property can be made to cause the decline of certain amplitude,
Tubing system viscosity can be made excessively high simultaneously, and then need higher processing temperature and longer process time, tubing base can be destroyed
The structure of body and filler, tube extrusion occur phenomena such as torque is excessive, and extrusion is unstable in the process, can also make tubing matter double wall thick,
Rough surface is not able to satisfy the demand of mine underground tubing.
In addition, in the prior art using graphene modified polythene tube, graphene additive amount is larger, polyethylene is caused
Mechanical properties of tubular goods such as tensile strength reduces, while graphene dispersibility in plastics system is poor.
In short, fire retardant, antistatic agent and conductive filler in the anti-electrostatic fire retardant type polythene material of the prior art
(such as carbon black, expanded graphite) additive amount is excessive, and the additive amount of graphene is big and dispersibility is poor, so that the poly- second of anti-electrostatic fire retardant type
Alkene tube wall thickness, matter weight, mechanical property are poor, so that anti-electrostatic fire retardant type polyvinyl piping materials obtained do not meet coal mine use
Pipe standard.
The content of background technology part is only the technology that inventor is known, not the existing skill of natural representative this field
Art.
Summary of the invention
It is excessive in order to solve existing anti-electrostatic fire retardant type polythene material fire retardant, antistatic agent, conductive filler additive amount
The problem of, overcome the defect that the additive amount of existing graphene is big and dispersibility is poor, the present invention provides a kind of anti-electrostatic fire retardants
Type polyethylene composition, while providing anti-electrostatic fire retardant type polyethylene particles, anti-electrostatic fire retardant type polyvinyl piping materials and its system
Preparation Method and purposes.
Since graphene is most light, most thin two-dimensional material, with excellent conductive, fire-retardant, physical and chemical stability and
Activeness and quietness performance, the graphene sheet layer of bigger serface is under the modifying function of dispersing agent, the active force of graphene film interlayer
It reduces, while increasing the binding force between graphene and matrix, graphene film is dispersed in plastics system,
Antistatic property is excellent, guarantee flame retardant effect while instead of part fire retardant addition, effectively make up functional stuffing height
Performance caused by additive amount is insufficient.Therefore, to achieve the goals above, graphene is added to anti-electrostatic fire retardant type and gathered by the present invention
It in vinyl composition, while being evenly spread in system under dispersion liquid effect, obtains a kind of the antistatic of excellent in mechanical performance
Flame retardant type polyethylene composition, the scheme specifically used are as follows.
The present invention provides a kind of anti-electrostatic fire retardant type polyethylene composition, including following parts by weight of component:
100 parts of high density polyethylene (HDPE)；
0.5~4 part of graphene；
0.5~12 part of fire retardant；
1~5 part of dispersion liquid；
0.5~4 part of nucleating agent；
0.5~4 part of antioxidant.
According to an aspect of the present invention, above-mentioned anti-electrostatic fire retardant type polyethylene composition, including following parts by weight group
Point:
100 parts of high density polyethylene (HDPE)；
2~3 parts of graphene；
1~8 part of fire retardant；
1.5~4 parts of dispersion liquid；
1~3 part of nucleating agent；
1~3 part of antioxidant.
According to an aspect of the present invention, above-mentioned anti-electrostatic fire retardant type polyethylene composition, including following parts by weight group
Point:
100 parts of high density polyethylene (HDPE)；
2.5 parts of graphene；
6 parts of fire retardant；
2 parts of dispersion liquid；
1.5 parts of nucleating agent；
2 parts of antioxidant.
According to an aspect of the present invention, 0.92~0.98g/cm of density of the high density polyethylene (HDPE)3, preferably 0.94
~0.97g/cm3。
According to an aspect of the present invention, specific surface area >=430m of the graphene2/ g, preferably >=505m2/g；Partial size
D50≤27 μm, preferably 5 μm≤D50≤15 μm, most preferably 8 μm；Mass fraction≤3% of oxygen, preferably≤1%；Graphite
The number of plies≤10 layer of alkene, preferably≤8 layer.
Wherein the mass fraction of the oxygen of the graphene refers to the mass fraction of oxygen atom in graphene.
According to an aspect of the present invention, the fire retardant is selected from red phosphorus, magnesium hydroxide, aluminium hydroxide, hexabromo ring 12
At least one of alkane, antimony oxide.
According to an aspect of the present invention, the decentralized medium of the dispersion liquid is selected from PE wax, EBS (the double stearic acid acyls of ethylene
Amine), at least one of hyper-dispersant A8021 or R1618.
According to an aspect of the present invention, the mass percentage that decentralized medium accounts for dispersion liquid in the dispersion liquid is 8-
12wt%, preferably 10wt%.
According to an aspect of the present invention, the dispersed phase of the dispersion liquid uses white oil.
The preparation method of the dispersion liquid include: using white oil as dispersed phase, with PE wax, EBS (ethylene bis stearic acid amide),
The group of one or more of hyper-dispersant A8021 or hyper-dispersant R1618 is combined into decentralized medium, is configured to dispersion liquid.
According to an aspect of the present invention, the nucleating agent is in calcium stearate, barium sulfate, silicate, titanium dioxide
At least one.
According to an aspect of the present invention, the antioxidant is selected from antioxidant B215, antioxidant 1010, antioxidant 264
Or at least one of antioxidant B225 etc..
Antioxidant B215 is four (β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid) pentaerythritol esters (abbreviation: antioxidant
1010) with three [2,4- di-tert-butyl-phenyl] phosphite esters (referred to as: irgasfos 168) with compound obtained by the mass ratio of 1:2
Referred to as；
Antioxidant 1010 is the abbreviation of four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol esters；
Antioxidant 264 is the abbreviation of 2,6 di tert butyl 4 methyl phenol；
Antioxidant B225 is four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol esters (abbreviation: antioxidant
1010) with three (2,4- di-tert-butyl-phenyl) phosphite esters (referred to as: irgasfos 168) with compound obtained by the mass ratio of 1:1
Referred to as.
The present invention also provides a kind of anti-electrostatic fire retardant type polyethylene particles, using above-mentioned anti-electrostatic fire retardant type polyethylene group
Object is closed to be prepared.
The present invention also provides a kind of preparation methods of anti-electrostatic fire retardant type polyethylene particles, according to above-mentioned anti-electrostatic fire retardant
It is prepared by each component and proportion relation in type polyethylene composition, comprising:
It prepares flame retardant type polyethylene particles: high density polyethylene (HDPE), antioxidant, fire retardant is subjected to mixing, extruding pelletization, system
Obtain flame retardant type polyethylene particles；
Mixing: flame retardant type polyethylene particles obtained above are mixed with dispersion liquid, graphene, nucleating agent, are mixed
Object；With
Resulting mixture mixing, extruding pelletization to get.
According to an aspect of the present invention, in described the step of preparing flame retardant type polyethylene particles, the mixing is using close
Mill carries out mixing, and equal mixing is in a molten state to material.
Preferably, the revolving speed of the mixer is 10~40r/min, preferably 15~40r/min；
Preferably, the temperature of the mixing is controlled at 180~280 DEG C, and preferably 185~240 DEG C；
Preferably, the mixing time is 10~30min, preferably 12~25min.
According to an aspect of the present invention, in described the step of preparing flame retardant type polyethylene particles, the extruding pelletization is adopted
Extruding pelletization is carried out with double wrist pelletizers.
Preferably, the extrusion revolving speed of the pelletizer is 5~35r/min, and preferably revolving speed is 15~30r/min；
Preferably, the extrusion temperature is 180~260 DEG C, preferably 200~240 DEG C.
According to an aspect of the present invention, it in the mixing step, is mixed using high-speed mixer.
Preferably, the revolving speed of the high-speed mixer is 300~800r/min, and preferably revolving speed is 350~650r/min.
According to an aspect of the present invention, in the mixing step, when the mixed temperature is 10 DEG C~70 DEG C, mixes
Between be 5~60min.Preferably, the mixing temperature is 25 DEG C~40 DEG C, incorporation time preferably 10~30min.
According to an aspect of the present invention, in the step of mixture mixing, mixing, equal mixing are carried out using mixer
It is in a molten state to material.
Preferably, the revolving speed of the mixer is 10~40r/min, preferably 15~40r/min；
Preferably, the temperature of the mixing is controlled at 180~280 DEG C, and preferably 185~240 DEG C；
Preferably, the mixing time is 10~30min, preferably 12~25min.
According to an aspect of the present invention, extruding pelletization squeeze out using double wrist pelletizers and is made after the mixture mixing
Grain.
Preferably, the extrusion revolving speed of the pelletizer is 5~35r/min, and preferably revolving speed is 15~30r/min；
Preferably, the extrusion temperature is 180~260 DEG C, preferably 200~240 DEG C.
The present invention also provides a kind of anti-electrostatic fire retardant type polyethylene prepared by above-mentioned anti-electrostatic fire retardant type polyethylene particles
Tubing.
The present invention also provides a kind of preparation methods of anti-electrostatic fire retardant type polyvinyl piping materials, comprising: by above-mentioned antistatic resistance
Combustion type polyethylene particles are squeezed out with pipe extruder.
The present invention also provides the purposes that a kind of anti-electrostatic fire retardant type polyvinyl piping materials are used as coal mine tubing.
The invention has the following beneficial effects:
(1) present invention enables to graphene sheet layer to be uniformly dispersed in system under dispersing agent effect, so that graphene/
Polyvinyl piping materials have both excellent antistatic, fire-retardant and mechanical property, effectively compensate for due to the high additive amount of functional stuffing and
The performance of caused tubing is insufficient, meets the standard of pipe material for coal mine.
(2) present invention utilizes graphene high flame retardant and its architectural characteristic, and the graphene/polyethylene being prepared answers material
Oxygen index (OI) reach 22~26%, improve 15%~40% compared to pure polyethylene, it is therefore, more nonflammable, preparation it is poly-
Ethylene tubing anti-flammability meets MT181-88 " the plastic pipe for coal mine safety in colliery industry standard MT558.1-2005
Can inspection specification " require, while when reaching the flame retardant effect of same levels as filler compared to carbon black, it is of the invention in fire retardant
Additive amount declines 30wt% or so, reduces its pollution to environment, and reduce the influence to mechanical properties of tubular goods.
(3) can be made in the case that the present invention discloses the additive amount (2~3 parts) of component using graphene high conductivity characteristic
The sheet resistance of polyvinyl piping materials reaches 106Ω hereinafter, and tubing surface is smooth, light, easy for construction, antistatic property more
Persistently.
(4) present invention activeness and quietness characteristic excellent using graphene, so that system is prepared simultaneously without adding toughener
Obtained by graphene/polythene material mechanical property reach GB/T8804-2003 in colliery industry standard MT558.1-2005
The requirement (tensile strength >=9MPa, elongation at break >=300%) of " measurement of thermoplastic plastic pipe tensile property ", the present invention produce
Product tensile strength is up to 28MPa, and elongation at break is up to 340%.
(5) graphene/polyvinyl piping materials of the invention have the mechanical properties such as excellent tensile strength and elongation at break,
So that extruding pipe material wall thickness corresponding under same nominal pressure and outer diameter reduces 10~20%, tubing unit is reduced
The dosage of length, therefore, graphene/polyvinyl piping materials of the invention can reach pressure resistance scale in the lower situation of wall thickness
Standard improves the transfer efficiency of tubing.
Specific embodiment
Hereinafter, certain illustrative embodiments are simply just described.As one skilled in the art will recognize that
As, without departing from the spirit or scope of the present invention, the various not Tongfangs such as increase, deletion, modification can be passed through
Formula modifies described embodiment.Therefore, description is considered essentially illustrative rather than restrictive.
In the description of the present invention, term " effect is more preferable " cannot simply be understood to group according to specific embodiment
Part, formula, technological parameter etc. it is obtained the result is that preferably, for those of ordinary skills, in concrete condition
Under, term " effect is more preferable " should also comprehensively consider the factors such as economy, environment, time.
In the specific embodiment of the present invention, a kind of anti-electrostatic fire retardant type polyethylene composition is provided, including following
Parts by weight of component:
100 parts of high density polyethylene (HDPE)；
0.5~4 part of graphene；
0.5~12 part of fire retardant；
1~5 part of dispersion liquid；
0.5~4 part of nucleating agent；
0.5~4 part of antioxidant.
Such as: 100 parts of high density polyethylene (HDPE), 12 parts of fire retardant, 1 part of dispersion liquid, 4 parts of nucleating agent, resists 0.5 part of graphene
0.5 part of oxygen agent；100 parts of high density polyethylene (HDPE), 4 parts of graphene, 0.5 part of fire retardant, 5 parts of dispersion liquid, 0.5 part of nucleating agent, antioxygen
4 parts of agent；100 parts of high density polyethylene (HDPE), 2 parts of graphene, 6 parts of fire retardant, 3 parts of dispersion liquid, 2 parts of nucleating agent, 3 parts of antioxidant, etc.
Deng.
As the preferred embodiment of present embodiment, above-mentioned anti-electrostatic fire retardant type polyethylene composition, including following weight
Part component:
100 parts of high density polyethylene (HDPE)；
2~3 parts of graphene；
1~8 part of fire retardant；
1.5~4 parts of dispersion liquid；
1~3 part of nucleating agent；
1~3 part of antioxidant.
Such as: 100 parts of high density polyethylene (HDPE), 2 parts of graphene, 8 parts of fire retardant, 1.5 parts of dispersion liquid, 3 parts of nucleating agent, antioxygen
1 part of agent；100 parts of high density polyethylene (HDPE), 3 parts of graphene, 1 part of fire retardant, 4 parts of dispersion liquid, 1 part of nucleating agent, 3 parts of antioxidant；It is high
100 parts of density polyethylene, 2.5 parts of graphene, 5 parts of fire retardant, 2 parts of dispersion liquid, 2 parts of nucleating agent, 2.5 parts of antioxidant, etc..
As the more preferable scheme of present embodiment, above-mentioned anti-electrostatic fire retardant type polyethylene composition, including it is following heavy
Measure part component:
100 parts of high density polyethylene (HDPE)；
2.5 parts of graphene；
6 parts of fire retardant；
2 parts of dispersion liquid；
1.5 parts of nucleating agent；
2 parts of antioxidant.
According to a preferred embodiment of the present invention, 0.92~0.98g/cm of density of the high density polyethylene (HDPE)3, work as height
The density of density polyethylene is 0.94~0.97g/cm3Shi Xiaoguo is more preferable.
According to a preferred embodiment of the present invention, specific surface area >=430m of the graphene2/ g, when specific surface area >=
505m2Effect is more preferable when/g；Partial size D50≤27 μm of graphene, effect is more preferable when for 5 μm≤D50≤15 μm, most preferably 8 μ
m；Mass fraction≤3% of the oxygen of graphene, effect is more preferable when for≤1%；The number of plies≤10 layer of graphene, when being≤8 layers
Shi Xiaoguo is more preferable.
Wherein the mass fraction of the oxygen of the graphene refers to the mass fraction of oxygen atom in graphene.
According to a preferred embodiment of the present invention, the fire retardant is selected from red phosphorus, magnesium hydroxide, aluminium hydroxide, hexabromo
At least one of cyclododecane, antimony oxide.
According to a preferred embodiment of the present invention, the decentralized medium of the dispersion liquid is selected from PE wax, (ethylene is double hard by EBS
Resin acid amide), at least one of hyper-dispersant A8021 or R1618.
According to a preferred embodiment of the present invention, decentralized medium accounts for the mass percentage of dispersion liquid in the dispersion liquid
For 8-12wt%, such as: 8wt%, 9wt%, 10wt%, 11wt%, 12wt% etc., as 10wt%, effect is more preferable.
According to a preferred embodiment of the present invention, the dispersed phase of the dispersion liquid uses white oil.
According to a preferred embodiment of the present invention, the preparation method of the dispersion liquid include: using white oil as dispersed phase, with
The group of one or more of PE wax, EBS (ethylene bis stearic acid amide), hyper-dispersant A8021 or hyper-dispersant R1618
It is combined into decentralized medium, is configured to dispersion liquid.
According to a preferred embodiment of the present invention, the nucleating agent is selected from calcium stearate, barium sulfate, silicate, dioxy
Change at least one of titanium.
According to a preferred embodiment of the present invention, the antioxidant is selected from antioxidant B215, antioxidant 1010, antioxygen
At least one of agent 264 or antioxidant B225 etc..
In yet another embodiment of the present invention, a kind of anti-electrostatic fire retardant type polyethylene particles are provided, using above-mentioned
Anti-electrostatic fire retardant type polyethylene composition is prepared.
In yet another embodiment of the present invention, a kind of preparation method of anti-electrostatic fire retardant type polyethylene particles is provided,
According in above-mentioned anti-electrostatic fire retardant type polyethylene composition each component and proportion relation prepared, comprising:
It prepares flame retardant type polyethylene particles: high density polyethylene (HDPE), antioxidant, fire retardant is subjected to mixing, extruding pelletization, system
Obtain flame retardant type polyethylene particles；
Mixing: flame retardant type polyethylene particles obtained above are mixed with dispersion liquid, graphene, nucleating agent, are mixed
Object；With
Resulting mixture mixing, extruding pelletization to get.
According to a preferred embodiment of the present invention, in described the step of preparing flame retardant type polyethylene particles, the mixing
Mixing is carried out using mixer, equal mixing is in a molten state to material.
According to a preferred embodiment of the present invention, the revolving speed of the mixer is 10~40r/min, such as: 10r/
Min, 20r/min, 30r/min, 40r/min etc., when the revolving speed of the mixer is 15~40r/min, effect is more preferable, such as:
15r/min, 20r/min, 25r/min, 30r/min, 35r/min, 40r/min etc.；And/or the temperature control of the mixing exists
180~280 DEG C, such as: 180 DEG C, 200 DEG C, 220 DEG C, 240 DEG C, 260 DEG C, 280 DEG C etc., select 185~240 DEG C when effect more
It is good, such as: 185 DEG C, 195 DEG C, 205 DEG C, 215 DEG C, 225 DEG C, 235 DEG C, 240 DEG C etc.；And/or the mixing time be 10~
30min, such as 10min, 15min, 20min, 25min, 30min, mixing time select 12~25min when effect it is more preferable, such as
12min, 15min, 17min, 20min, 22min, 25min etc..
According to a preferred embodiment of the present invention, in described the step of preparing flame retardant type polyethylene particles, the extrusion
It is granulated and carries out extruding pelletization using double wrist pelletizers.
According to a preferred embodiment of the present invention, the extrusion revolving speed of the pelletizer is 5~35r/min, such as: 5r/
Min, 10r/min, 15r/min, 20r/min, 25r/min, 30r/min, 35r/min etc., when revolving speed is 15~30r/min timeliness
Fruit is more preferable, such as: 15r/min, 20r/min, 25r/min, 30r/min etc.；Extrusion temperature is 180~260 DEG C, such as: 180
DEG C, 200 DEG C, 220 DEG C, 240 DEG C, 260 DEG C etc., when extrusion temperature is 200~240 DEG C, effect is more preferable, such as: 200 DEG C, 210
DEG C, 220 DEG C, 230 DEG C, 240 DEG C etc..
According to a preferred embodiment of the present invention, it in the mixing step, is mixed using high-speed mixer.
According to a preferred embodiment of the present invention, the revolving speed of the high-speed mixer is 300~800r/min, such as:
300r/min、350r/min、400r/min、450r/min、500r/min、550r/min、600r/min、650r/min、700r/
Min, 750r/min, 800r/min etc., effect is more preferable when 350~650r/min of selection of speed, such as: 350r/min, 400r/
Min, 450r/min, 500r/min, 550r/min, 600r/min, 650r/min etc..
According to a preferred embodiment of the present invention, in the mixing step, the mixed temperature is 10 DEG C~70 DEG C,
Such as: 10 DEG C, 15 DEG C, 20 DEG C, 25 DEG C, 30 DEG C, 35 DEG C, 40 DEG C, 45 DEG C, 50 DEG C, 55 DEG C, 60 DEG C, 65 DEG C, 70 DEG C etc.；Mixing
Time be 5~60min, such as: 5min, 10min, 15min, 20min, 25min, 30min, 35min, 40min, 45min,
50min, 55min, 60min etc.；The mixing temperature is 25 DEG C~40 DEG C, and effect is more preferable when incorporation time is 10~30min, example
Such as mixing temperature: 25 DEG C, 30 DEG C, 35 DEG C, 40 DEG C；Incorporation time: 10min, 15min, 20min, 25min, 30min etc..
According to a preferred embodiment of the present invention, in the step of mixture mixing, mixing is carried out using mixer,
Equal mixing is in a molten state to material.
According to a preferred embodiment of the present invention, the revolving speed of the mixer is 10~40r/min, such as: 10r/
min、15r/min、18r/min、20r/min、23r/min、25r/min、30r/min、33r/min、35r/min、37r/min、
40r/min, etc.；Effect is more preferable when the revolving speed of mixer selects 15~40r/min, such as: 15r/min, 18r/min, 20r/
Min, 23r/min, 25r/min, 28r/min, 30r/min, 33r/min, 35r/min, 39r/min, 40r/min, etc.；And/or
The temperature of the mixing is controlled at 180~280 DEG C, such as: 180 DEG C, 200 DEG C, 220 DEG C, 240 DEG C, 260 DEG C, 280 DEG C etc., choosing
Effect is more preferable when selecting 185~240 DEG C, such as: 185 DEG C, 195 DEG C, 205 DEG C, 215 DEG C, 225 DEG C, 235 DEG C, 240 DEG C etc.；And/or
The mixing time is 10~30min, such as 10min, 15min, 20min, 25min, 30min, mixing time selection 12~
Effect is more preferable when 25min, such as 12min, 15min, 17min, 20min, 22min, 25min etc..
According to a preferred embodiment of the present invention, extruding pelletization is carried out using double wrist pelletizers after the mixture mixing
Extruding pelletization.
According to a preferred embodiment of the present invention, the extrusion revolving speed of the pelletizer is 5~35r/min, such as: 5r/
Min, 10r/min, 15r/min, 20r/min, 25r/min, 30r/min, 35r/min etc., when revolving speed is 15~30r/min timeliness
Fruit is more preferable, such as: 15r/min, 20r/min, 25r/min, 30r/min etc.；Extrusion temperature is 180~260 DEG C, such as: 180
DEG C, 200 DEG C, 220 DEG C, 240 DEG C, 260 DEG C etc., when extrusion temperature is 200~240 DEG C, effect is more preferable, such as: 200 DEG C, 210
DEG C, 220 DEG C, 230 DEG C, 240 DEG C etc..
In another embodiment of the invention, one kind is provided by above-mentioned anti-electrostatic fire retardant type polyethylene particles system
Standby anti-electrostatic fire retardant type polyvinyl piping materials.
In another embodiment of the invention, a kind of preparation side of anti-electrostatic fire retardant type polyvinyl piping materials is provided
Method, comprising: squeeze out above-mentioned anti-electrostatic fire retardant type polyethylene particles with pipe extruder.
In another embodiment of the invention, a kind of anti-electrostatic fire retardant type polyvinyl piping materials are provided and are used as coal mine
The purposes of well casing material.
Below to a preferred embodiment of the present invention will be described in detail.It should be understood that preferred reality described herein
Apply example only for the purpose of illustrating and explaining the present invention and is not intended to limit the present invention.
The graphene that following embodiment uses is the highly conductive type graphene product of the hexa-atomic element production in Changzhou.
Embodiment 1
This example demonstrates that the preparation method of anti-electrostatic fire retardant type polyvinyl piping materials of the invention, comprising:
It (1) is 0.5 parts by weight, 1 weight of fire retardant magnesium hydroxide by 100 parts by weight of high density polyethylene (HDPE), antioxidant B225
It part is added sequentially to carry out melt blending in mixer, the revolving speed of mixer is 40r/min, and temperature control is at 200 DEG C, total mixing
Time is 20min；By double wrist pelletizer extruding pelletizations, the extrusion revolving speed of the pelletizer is 30r/min, extrusion temperature control
At 200 DEG C, flame retardant type polyethylene particles are prepared；
(2) using white oil 88g as dispersed phase, using PE wax 12g as decentralized medium, it is configured to the PE wax white oil dispersion of 12wt%
Liquid；
(3) by above-mentioned flame retardant type polyethylene particles, 1 parts by weight of PE wax white oil dispersion liquid, graphene (BET=487m2/ g,
D50=27 μm, O%≤1.0%) 2 parts by weight, 1 parts by weight of calcium stearate are added sequentially to mix in high-speed mixer, wherein
Mixing temperature is 40 DEG C, revolving speed 650r/m；Incorporation time is 30min；
(4) step (3) resulting mixture is added in mixer and carries out abundant melt blending, the revolving speed of mixer is
40r/min, at 200 DEG C, total mixing time is 20min for temperature control；Gained mixing material passes through double wrist pelletizer extruding pelletizations, institute
The extrusion revolving speed for stating pelletizer is 30r/min, and extrusion temperature is controlled at 200 DEG C, and gained particle is squeezed out through pipe extruder, is made
Anti-electrostatic fire retardant type polyvinyl piping materials.
Embodiment 2
This example demonstrates that the preparation method of anti-electrostatic fire retardant type polyvinyl piping materials of the invention, step include:
(1) by 100 parts by weight of high density polyethylene (HDPE), antioxidant B225 be 2 parts by weight, 6 parts by weight of fire retardant red phosphorus successively
It is added in mixer and carries out melt blending, the revolving speed of mixer is 30r/min, and temperature control is in 230 DEG C, total mixing time
25min；By double wrist pelletizer extruding pelletizations, the extrusion revolving speed of the pelletizer is 25r/min, and extrusion temperature is controlled 220
DEG C, prepare flame retardant type polyethylene particles；
(2) using white oil 90g as dispersed phase, using A8021 10g as decentralized medium, it is configured to the A8021 white oil point of 10wt%
Dispersion liquid；
It (3) is 2 parts by weight, graphene (BET=550m by above-mentioned flame retardant type polyethylene particles, A8021 white oil dispersion liquid2/
G, D50=8 μm, O%≤1.0%) 2.5 parts by weight, 1.5 parts by weight of calcium stearate are added sequentially to mix in high-speed mixer,
Wherein, mixing temperature is 40 DEG C, revolving speed 600r/min；Incorporation time is 30min；
(4) step (3) resulting mixture is added in mixer and carries out abundant melt blending, the revolving speed of mixer is
30r/min, at 230 DEG C, total mixing time is 25min for temperature control；Gained mixing material passes through double wrist pelletizer extruding pelletizations, institute
The extrusion revolving speed for stating pelletizer is 25r/min, and extrusion temperature is controlled at 220 DEG C, and gained particle is squeezed out through pipe extruder, is made
Anti-electrostatic fire retardant type polyvinyl piping materials.
Embodiment 3
This example demonstrates that the preparation method of anti-electrostatic fire retardant type polyvinyl piping materials of the invention, step include:
It (1) is 1.5 parts by weight, 8 weight of fire retardant aluminium hydroxide by 100 parts by weight of high density polyethylene (HDPE), antioxidant B215
It part is added sequentially to carry out melt blending in mixer, the revolving speed of mixer is 10r/min, and temperature control is at 180 DEG C, total mixing
Time is 10min；By double wrist pelletizer extruding pelletizations, the extrusion revolving speed of the pelletizer is 35r/min, extrusion temperature control
At 240 DEG C, flame retardant type polyethylene particles are prepared；
(2) using white oil 92g as dispersed phase, using EBS 8g as decentralized medium, it is configured to the EBS white oil dispersion liquid of 8wt%；
(3) by above-mentioned flame retardant type polyethylene particles, 5 parts by weight of EBS white oil dispersion liquid, graphene (BET=520m2/ g,
D50=24 μm, O%≤3.0%) 3 parts by weight, 4 parts by weight of barium sulfate are added sequentially to mix in high-speed mixer, wherein it is mixed
Closing temperature is 70 DEG C, revolving speed 300r/min；Incorporation time is 60min；
(4) step (3) resulting mixture is added in mixer and carries out abundant melt blending, the revolving speed of mixer is
10r/min, at 180 DEG C, total mixing time is 10min for temperature control；Gained mixing material passes through double wrist pelletizer extruding pelletizations, institute
The extrusion revolving speed for stating pelletizer is 35r/min, and extrusion temperature is controlled at 240 DEG C, and gained particle is squeezed out through pipe extruder, is made
Anti-electrostatic fire retardant type polyvinyl piping materials.
Embodiment 4
This example demonstrates that the preparation method of anti-electrostatic fire retardant type polyvinyl piping materials of the invention, step include:
It (1) is 1 parts by weight, 12 parts by weight of fire retardant aluminium hydroxide by 100 parts by weight of high density polyethylene (HDPE), antioxidant B215
It is added sequentially to carry out melt blending in mixer, the revolving speed of mixer is 15r/min, and temperature is controlled at 280 DEG C, total mixing
Between be 12min；By double wrist pelletizer extruding pelletizations, the extrusion revolving speed of the pelletizer is 15r/min, and extrusion temperature control exists
260 DEG C, prepare flame retardant type polyethylene particles；
(2) using white oil 90g as dispersed phase, using EBS10g as decentralized medium, it is configured to the EBS white oil dispersion liquid of 10wt%；
(3) by above-mentioned flame retardant type polyethylene particles, 1.5 parts by weight of EBS white oil dispersion liquid, graphene (BET=505m2/ g,
D50=8 μm, O%≤1.0%) 0.5 parts by weight, 3 parts by weight of barium sulfate are added sequentially to mix in high-speed mixer, wherein it is mixed
Closing temperature is 10 DEG C, revolving speed 800r/min；Incorporation time is 10min；
(4) step (3) resulting mixture is added in mixer and carries out abundant melt blending, the revolving speed of mixer is
30r/min, at 230 DEG C, total mixing time is 25min for temperature control；Gained mixing material passes through double wrist pelletizer extruding pelletizations, institute
The extrusion revolving speed for stating pelletizer is 25r/min, and extrusion temperature is controlled at 220 DEG C, and gained particle is squeezed out through pipe extruder, is made
Anti-electrostatic fire retardant type polyvinyl piping materials.
Embodiment 5
This example demonstrates that the preparation method of anti-electrostatic fire retardant type polyvinyl piping materials of the invention, step include:
(1) by 100 parts by weight of high density polyethylene (HDPE), antioxidant B225 be 4 parts by weight, 0.5 parts by weight of fire retardant red phosphorus according to
Secondary be added in mixer carries out melt blending, and the revolving speed of mixer is 30r/min, and temperature control is at 185 DEG C, total mixing time
For 30min；By double wrist pelletizer extruding pelletizations, the extrusion revolving speed of the pelletizer is 5r/min, and extrusion temperature is controlled 180
DEG C, prepare flame retardant type polyethylene particles；
(2) using white oil 90g as dispersed phase, using A8021 10g as decentralized medium, it is configured to the A8021 white oil point of 10wt%
Dispersion liquid；
It (3) is 4 parts by weight, graphene (BET=430m by above-mentioned flame retardant type polyethylene particles, A8021 white oil dispersion liquid2/
G, D50=15 μm, O%≤1.0%) 4 parts by weight, 0.5 parts by weight of calcium stearate are added sequentially to mix in high-speed mixer,
In, mixing temperature is 25 DEG C, revolving speed 350r/min；Incorporation time is 5min；
(4) step (3) resulting mixture is added in mixer and carries out abundant melt blending, the revolving speed of mixer is
30r/min, at 240 DEG C, total mixing time is 25min for temperature control；Gained mixing material passes through double wrist pelletizer extruding pelletizations, institute
The extrusion revolving speed for stating pelletizer is 25r/min, and extrusion temperature is controlled at 220 DEG C, and gained particle is squeezed out through pipe extruder, is made
Anti-electrostatic fire retardant type polyvinyl piping materials.
Anti-electrostatic fire retardant type polyvinyl piping materials made from embodiment are tested for the property, and are not added with graphene with existing
Carbon black polyvinyl piping materials (D1 in following table) and a kind of hdpe pipe according to disclosed in CN104262740A (in following table
D2 performance) is compared, and as a result participates in following table:
It can be seen that anti-electrostatic fire retardant type polyvinyl piping materials provided by the invention from the data of above-described embodiment and table to have both
Have excellent antistatic, fire-retardant and mechanical property, compared with D1, the tubing of all embodiments its smooth in appearance, it is smooth, without gas
Bubble, uniform color；The tensile strength of anti-electrostatic fire retardant type polyvinyl piping materials provided by the invention is big, is 23-28MPa, is above
The tensile strength 11MPa of D1, and it is higher than the tensile strength 22Mpa of D2；Anti-electrostatic fire retardant type polyvinyl piping materials provided by the invention
Elongation at break it is high, be 312%-340%, the elongation at break 310% higher than D1, the significantly larger than elongation at break of D2
150%；The sheet resistance of anti-electrostatic fire retardant type polyvinyl piping materials provided by the invention is low, is 6.4 × 104Ω-9.2×105Ω,
Sheet resistance 8.9 × 10 lower than D15The sheet resistance 4 × 10 of Ω and D26Ω。
Finally, it should be noted that the foregoing is only a preferred embodiment of the present invention, it is not intended to restrict the invention,
Although the present invention is described in detail referring to the foregoing embodiments, for those skilled in the art, still may be used
To modify the technical solutions described in the foregoing embodiments or equivalent replacement of some of the technical features.
All within the spirits and principles of the present invention, any modification, equivalent replacement, improvement and so on should be included in of the invention
Within protection scope.
Claims (12)
1. a kind of anti-electrostatic fire retardant type polyethylene composition, including following parts by weight of component:
100 parts of high density polyethylene (HDPE)；
0.5~4 part of graphene；
0.5~12 part of fire retardant；
1~5 part of dispersion liquid；
0.5~4 part of nucleating agent；
0.5~4 part of antioxidant.
2. anti-electrostatic fire retardant type polyethylene composition according to claim 1, including following parts by weight of component:
100 parts of high density polyethylene (HDPE)；
2~3 parts of graphene；
1~8 part of fire retardant；
1.5~4 parts of dispersion liquid；
1~3 part of nucleating agent；
1~3 part of antioxidant.
3. anti-electrostatic fire retardant type polyethylene composition according to claim 1, including following parts by weight of component:
100 parts of high density polyethylene (HDPE)；
2.5 parts of graphene；
6 parts of fire retardant；
2 parts of dispersion liquid；
1.5 parts of nucleating agent；
2 parts of antioxidant.
4. anti-electrostatic fire retardant type polyethylene composition according to any one of claim 1-3, it is characterised in that: the height
0.92~0.98g/cm of density of density polyethylene3, preferably 0.94~0.97g/cm3；
And/or specific surface area >=430m of the graphene2/ g, preferably >=505m2/g；
And/or partial size D50≤27 μm of the graphene, preferably 5 μm≤D50≤15 μm, most preferably 8 μm；
And/or mass fraction≤3% of the oxygen of the graphene, preferably≤1%；
And/or the number of plies≤10 layer of the graphene of the graphene, preferably≤8 layer；
And/or the fire retardant in red phosphorus, magnesium hydroxide, aluminium hydroxide, hexabromocyclododecane, antimony oxide extremely
Few one kind；
And/or the decentralized medium of the dispersion liquid be selected from PE wax, EBS (ethylene bis stearic acid amide), hyper-dispersant A8021 or
At least one of R1618；Preferably, the mass percentage that decentralized medium accounts for dispersion liquid in the dispersion liquid is 8-
12wt%, preferably 10wt%；
And/or the dispersed phase of the dispersion liquid uses white oil；
And/or the nucleating agent is selected from least one of calcium stearate, barium sulfate, silicate, titanium dioxide；
And/or the antioxidant is selected from the antioxidant and was selected from for four (β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid) seasons penta
Four alcohol esters and three [2,4- di-tert-butyl-phenyl] phosphite esters are with compound, four [β-(the tertiary fourths of 3,5- bis- obtained by the mass ratio of 1:2
Base -4- hydroxy phenyl) propionic acid] pentaerythritol ester, 2,6 di tert butyl 4 methyl phenol or four [β-(3,5- di-t-butyl -4-
Hydroxy phenyl) propionic acid] pentaerythritol ester and three (2,4- di-tert-butyl-phenyl) phosphite esters are with compound obtained by the mass ratio of 1:1
At least one of.
5. a kind of anti-electrostatic fire retardant type polyethylene particles, poly- using anti-electrostatic fire retardant type of any of claims 1-4
Vinyl composition is prepared.
6. a kind of preparation method of anti-electrostatic fire retardant type polyethylene particles, it is characterised in that: according to any one of claim 1-4 institute
It is prepared by each component in anti-electrostatic fire retardant type polyethylene composition and proportion relation stated, comprising:
It prepares flame retardant type polyethylene particles: high density polyethylene (HDPE), antioxidant, fire retardant being subjected to mixing, resistance is made in extruding pelletization
Combustion type polyethylene particles；
Mixing: flame retardant type polyethylene particles obtained above are mixed with dispersion liquid, graphene, nucleating agent, obtain mixture；With
Resulting mixture mixing, extruding pelletization to get.
7. preparation method according to claim 6, it is characterised in that: described the step of preparing flame retardant type polyethylene particles
In, the mixing carries out mixing using mixer, and equal mixing is in a molten state to material；Preferably, turn of the mixer
Speed is 10~40r/min, and the temperature of preferably 15~40r/min and/or the mixing is controlled at 180~280 DEG C, preferably
185~240 DEG C and/or the mixing time are 10~30min, preferably 12~25min；
And/or in described the step of preparing flame retardant type polyethylene particles, the extruding pelletization is squeezed out using double wrist pelletizers
It is granulated；Preferably, the extrusion revolving speed of the pelletizer is 5~35r/min, and preferably revolving speed is 15~30r/min；Extrusion temperature is
180~260 DEG C, preferably 200~240 DEG C.
8. preparation method according to claim 6, it is characterised in that: in the mixing step, using high-speed mixer into
Row mixing, it is preferable that the revolving speed of the high-speed mixer is 300~800r/min, and preferably revolving speed is 350~650r/min；
And/or in the mixing step, the mixed temperature is 10 DEG C~70 DEG C, incorporation time is 5~60min, preferably
Ground, the mixing temperature are 25 DEG C~40 DEG C, incorporation time preferably 10~30min.
9. preparation method according to claim 6, it is characterised in that: in the step of the mixture mixing, using mixing
Machine carries out mixing, and equal mixing is in a molten state to material；Preferably, the revolving speed of the mixer is 10~40r/min, preferably
It is 15~40r/min and/or the control of the temperature of the mixing is at 180~280 DEG C, preferably 185~240 DEG C and/or described close
The refining time is 10~30min, preferably 12~25min；
And/or extruding pelletization uses double wrist pelletizers to carry out extruding pelletizations after the mixture mixing, it is preferable that the granulation
The extrusion revolving speed of machine is 5~35r/min, and preferably revolving speed is 15~30r/min；Extrusion temperature be 180~260 DEG C, preferably 200
~240 DEG C.
10. the anti-electrostatic fire retardant type polyvinyl piping materials of anti-electrostatic fire retardant type polyethylene particles preparation according to claim 5.
11. the preparation method of anti-electrostatic fire retardant type polyvinyl piping materials according to claim 10, it is characterised in that: will be described
Anti-electrostatic fire retardant type polyethylene particles are squeezed out with pipe extruder.
12. the purposes that anti-electrostatic fire retardant type polyvinyl piping materials described in any one of claim 10 are used as coal mine tubing.
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| CN201711135352 | 2017-11-16 | ||
| CN2017111353528 | 2017-11-16 |
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Application publication date: 20190412 |
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