CN110229402A - A kind of Cross-linked Polyethylene Composites and preparation method thereof of high dc breakdown field strength - Google Patents
A kind of Cross-linked Polyethylene Composites and preparation method thereof of high dc breakdown field strength Download PDFInfo
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Abstract
The invention discloses a kind of Cross-linked Polyethylene Composites and preparation method thereof of high dc breakdown field strength, Cross-linked Polyethylene Composites of the present invention include: the low density polyethylene (LDPE) of (a) 100 parts by weight；(b) 2 parts by weight of crosslinking agent；(c) 0.005~0.04 parts by weight silane coupling agent；(d) 0.5~4 parts by weight compound nanoparticle, and the compounding nanoparticle is boron nitride nanosheet and alumina nano fiber；The amount ratio of the silane coupling agent and the nanoparticle is fixed as 1:100.The Cross-linked Polyethylene Composites of high dc breakdown field strength of the present invention are to effectively improve Cross-linked Polyethylene Composites electrical breakdown withstand capability using boron nitride nanosheet and alumina nano fiber as additive；When the additive amount for compounding nanoparticle is 2.0 phr, breakdown strength is maximum, has reached 502.5 kV/mm, 369.7 kV/mm with pure cross-linking polyethylene materials, compared to improving 35.9%.
Description
Technical field
The invention belongs to technical field of material chemistry, are related to a kind of electrical insulating material, and specially a kind of resistance to ultra-high voltage cross-linking is poly-
Ethylene composite material and preparation method.
Background technique
Compared with High Level AC Voltage (HVAC) power transmission, high voltage direct current (HVDC) power transmission becomes increasingly have competition
Power is transmitted especially for the large-capacity power of long range, and high voltage direct current cable shows very big excellent in terms of power transmission
Gesture, such as: compared with high-voltage alternating cable, high voltage direct current cable can ensure that longer power transmission distance and transmission capacity；It is high
Press direct current cables that there is lower capital cost and lower transmission energy loss；High voltage direct current cable has preferable electric power
Transmission stability, and the short circuit current in high voltage AC transmission system can be limited；The length of high voltage direct current cable is not filled
The limitation of electric current, high-voltage alternating electric output power has certain limit, and direct current output electric output power is unrestricted；High pressure
The connector of direct current cables wants much simpler, and facilitates the connection between different power grids.Crosslinked polyethylene has excellent insulation
Performance, mechanical performance, heat resistance and it is light-weight the advantages that and be widely used in D.C. high voltage transmission, but in the work of high voltage electric field
With easily forming space charge in crosslinked polyethylene and lead to the breakdown of insulating materials, so that its use value decreases.It is logical
Many-sided performance of crosslinked polyethylene can more be effectively improved by crossing composite material prepared by the mode of incorporation inorganic nano-particle.
In recent years, numerous studies scholar has found that nanometer dielectric plays an important role the raising of electrostrictive polymer performance.
Si-Jiao Wang et al. (Preparation, microstructure and properties of polyethylene/
alumina nanocomposites for HVDC insulation[J].IEEE Transactions on
Dielectrics&Electrical Insulation, 2016,22 (6): 3350-3356) in pass through in LDPE add be modified
Al2O3With unmodified Al2O3Nano particle, the results showed that modified nanoparticle can effectively improve the breakdown strength of composite material.
Patent CN108129725A shows that different-shape magnesia is added in crosslinked polyethylene can effectively improve crosslinked polyethylene material
The dc breakdown field strength of material, and fibrous magnesia the breakdown strength of composite material is improved it is more obvious.Patent
CN108610535A shows that fibrous magnesia-magnesium aluminate is added in crosslinked polyethylene effectively improves cross-linking polyethylene materials
The breakdown capability of resistance to superhigh voltage DC.Patent CN106633303A shows that nano silicon nitride boron particles are added in crosslinked polyethylene to be had
Effect improves the dc breakdown field strength of cross-linking polyethylene materials.Qi Li is in Solution-processed ferroelectric
terpolymernanocomposites with high breakdown strength and energy density
Utilizing boron nitride nanosheets, Energy&Environmental Science, 2015,8 (3):
Boron nitride nanosheet addition is reported in 922-931 can effectively improve composite material breakdown field in P (VDF-TrFE-CFE)
By force, compared with the breakdown strength of original P (VDF-TrFE-CFE), composite material highest disruptive field intensity improves 70%.Boron nitride
Nanometer sheet and aluminium oxide can effectively improve the disruptive field intensity of composite material, but there is not yet boron nitride nanosheet and aluminium oxide are fine
The report of dimension and crosslinked polyethylene dc breakdown field strength of material after compound.
Summary of the invention
In view of the deficiencies of the prior art, it is multiple that the object of the present invention is to provide a kind of crosslinked polyethylenes of high dc breakdown field strength
Condensation material and preparation method thereof obtains relatively thin boron nitride nanosheet by the present invention in that being removed with liquid nitrogen to boron nitride,
Boron nitride nanosheet is compound with crosslinked polyethylene, to effectively improve the dc breakdown field strength of crosslinked polyethylene.
The present invention is achieved by the following technical solutions:
A kind of Cross-linked Polyethylene Composites of high dc breakdown field strength comprising: (a) low-density of 100 parts by weight is poly-
Ethylene；(b) 2 parts by weight of crosslinking agent；(c) 0.005~0.04 parts by weight silane coupling agent；(d) 0.5~4 parts by weight compound nanometer
Particle, the compounding nanoparticle are boron nitride nanosheet and/or alumina nano fiber；The silane coupling agent is received with described
The amount ratio of rice corpuscles is fixed as 1:100；When the additive amount for compounding nanoparticle is 2.0phr, breakdown strength is maximum, reaches
502.5kV/mm is arrived, the 369.7kV/mm with pure cross-linking polyethylene materials, compared to promotion 35.9%.
Further, the boron nitride nanosheet is to be removed using the boron nitride with a thickness of 300~400nm using liquid nitrogen
Method be made, the boron nitride nanosheet diameter is between 10~20nm.
Further, the alumina nano fiber is using aluminium isopropoxide as raw material, using electrostatic spinning technique and high temperature
Means of calcination is made, and the diameter of the material is between 200~400nm.
Preferably, the boron nitride nanosheet and alumina nano fiber are compounded with the weight ratio of 2:3.
Further, the density of the low density polyethylene (LDPE) is less than 0.940g/cm3, melt flow index be 2.1g~
2.2g/10min, fusing point is at 122~124 DEG C.
Further, the crosslinking agent is cumyl peroxide, diethylenetriamines, di-tert-butyl peroxide, mistake
One of hydrogen oxide diisopropylbenzene (DIPB), preferably cumyl peroxide.
Further, the silane coupling agent is 3- aminopropyl triethoxysilane, 3- aminopropyl trimethoxysilane, N-
(β-aminoethyl)-gamma-aminopropyl-triethoxy-silane, one of γ-aminopropyltriethoxy diethoxy silane, preferably 3-
Aminopropyl triethoxysilane.
A kind of preparation method of the Cross-linked Polyethylene Composites of high dc breakdown field strength, passes through boron nitride nanosheet and oxygen
Change preparation, the silane coupling agent processing magnesia, the obtained insulating materials of solution blending of aluminium nanofiber.
Preferably, the preparation method specifically includes the following steps:
Step 1 removes blocky boron nitride: boron nitride being heated to 300 DEG C first and keeps the temperature 1h, under high temperature action, nitrogen
The Van der Waals force and interaction force of the middle layer and interlayer of changing boron molecule will weaken, the interfloor distance of such boron nitride molecule
Can all it expand with volume；Then boron nitride is immersed in -196 DEG C of low temperature liquid nitrogens immediately, the variation of local temperature does not only result in piece
The curling and layering of shape boron nitride, but also cause liquid nitrogen to be acutely expanded into gaseous state and remove boron nitride；N2Molecule can be from nitrogen
The crimped edge for changing boron enters, and gradually penetrates into crack in middle layer, so that boron nitride is removed；Above-mentioned steps repeat more
It is secondary to prepare ultrathin boron nitride nanosheet；
Step 2 prepares alumina nano fiber: aluminium isopropoxide being placed in dehydrated alcohol, after ultrasonic treatment, is persistently being stirred
Addition glacial acetic acid and concentrated hydrochloric acid during mixing are stirred continuously until aluminium isopropoxide sufficiently dissolves and obtains transparent clear solution；Institute
It obtains in solution and polyvinylpyrrolidone is added, be stirred continuously to obtain thick solution；Thick solution is taken to be spun with syringe
Silk operation, obtained spinning fibre obtain alumina nano fiber through high-temperature calcination；
Step 3 handles nanoparticle with silane coupling agent: by boron nitride nanosheet obtained and alumina nano fiber point
It is not dispersed in isopropanol, is ultrasonically treated, silane coupling agent is taken to dilute stir process in deionized water, it will be even added with silane
Join the aqueous isopropanol of agent respectively with the aqueous isopropanol containing boron nitride nanosheet and contain the isopropyl of alumina nano fiber
Alcoholic solution mixing, gained mixed solution high-speed stirred under heating condition；The suspension of acquisition is repeatedly washed with isopropanol, most
It is dry in vacuum oven afterwards；
Step 4 dissolves low density polyethylene (LDPE): low density polyethylene (LDPE) being cleaned postposition with ethyl alcohol and is dried in a vacuum drying oven
It is dry, then be dissolved in xylene solvent, until low density polyethylene (LDPE) is completely dissolved；And crosslinking agent is dissolved in above-mentioned solution
In；
Step 5, composite material is made using solution casting method: the boron nitride nanosheet and aluminium oxide handled through step 3 is received
Rice fiber is compounded, and compounding nanoparticle is placed in dimethylbenzene, ultrasonic disperse then heats and it is made to dissolve in step 4 system
In standby solution, mixed solution is then transferred to the glass mold in 115 DEG C of airtight vacuum drying boxes, solvent is evaporated,
Obtained film shifts to be handled in 180 DEG C of vacuum ovens, is then made its cooled to room temperature, is taken film off；The film is
For the Cross-linked Polyethylene Composites of the high dc breakdown field strength.
Beneficial effects of the present invention are as follows:
(1) a kind of Cross-linked Polyethylene Composites of high dc breakdown field strength of the present invention are with boron nitride nanosheet and oxygen
Change aluminium nanofiber is additive, can effectively improve insulating materials dc breakdown field strength；
(2) boron nitride nanosheet and alumina nano fiber compounding nanoparticle content are in insulating materials of the present invention
Performance is best when 2phr (1phr indicates a compounding nanoparticle of addition in cross-linking polyethylene materials per hundred parts), with pure crosslinking
Polythene material is compared, and breakdown voltage is promoted by 369.7kV/mm to 502.5kV/mm, improves 35.9%.
Detailed description of the invention
Fig. 1 be pure crosslinked polyethylene and be added to different content compounding nanoparticle Cross-linked Polyethylene Composites it is resistance to
The Weibull probability distribution graph of high voltage direct current breakdown；
In Fig. 1: the high pressure resistant dc breakdown ability of the pure crosslinked polyethylene of × expression；Expression is added to 0.5phr compounding and receives
The high pressure resistant dc breakdown ability of the crosslinked polyethylene of rice corpuscles；▲ indicate the poly- second of crosslinking for being added to 1phr compounding nanoparticle
The high pressure resistant dc breakdown ability of alkene；● indicate that the high pressure resistant direct current for being added to the crosslinked polyethylene of 2phr compounding nanoparticle is hit
Wear ability；Indicate the high pressure resistant dc breakdown ability for being added to the crosslinked polyethylene of 3phr compounding nanoparticle；Indicate addition
The high pressure resistant dc breakdown ability of the crosslinked polyethylene of 4phr compounding nanoparticle；
Fig. 2 is the scanning electron microscope (SEM) photograph for the boron nitride nanosheet being stripped；
Fig. 3 is the scanning electron microscope (SEM) photograph of fibrous alumina.
Specific embodiment
Following embodiment further illustrates the contents of the present invention, but should not be construed as limiting the invention.Without departing substantially from
In the case where spirit of that invention and essence, to modification made by the method for the present invention, step or condition and replaces, belong to the present invention
Range.Unless otherwise specified, the conventional means that technological means used in embodiment is well known to those skilled in the art.
Embodiment 1
A kind of Cross-linked Polyethylene Composites of high dc breakdown field strength, by weight, the material are every 100 parts
Low density polyethylene (LDPE) cooperates 2 parts of crosslinking agents, 0.005~0.04 (0.005,0.01,0.02,0.03,0.04) part silane coupling agent
Nanoparticle is compounded with 0.5~4 (0.5,1,2,3,4) part.Wherein silane coupling agent and the amount ratio for compounding nanoparticle
It is fixed as 1:100.
The boron nitride nanosheet is using the boron nitride with a thickness of 300~400nm, using the method system of liquid nitrogen removing
, the boron nitride nanosheet diameter is between 10~20nm.
The alumina nano fiber is using aluminium isopropoxide as raw material, using electrostatic spinning technique and high-temperature calcination means system
, the diameter of the material is between 200~400nm.
The boron nitride nanosheet and alumina nano fiber are to be compounded with mass ratio for the ratio of 3:2.
The density of the low density polyethylene (LDPE) is less than 0.940g/cm3, melt flow index is 2.1~2.2g/10min, is melted
O'clock at 122~124 DEG C.
The crosslinking agent is cumyl peroxide.
The silane coupling agent is 3- aminopropyl triethoxysilane.
The preparation method of the Cross-linked Polyethylene Composites of the high dc breakdown field strength, removing and oxygen including boron nitride
The preparation and silane coupling agent for changing aluminium nanofiber handle boron nitride nanosheet and alumina nano fiber, solution casting method
Insulating materials is made.It is specific as follows:
Step 1: blocky boron nitride is removed
Boron nitride is heated to 300 DEG C first and keeps the temperature one hour, boron nitride is then immersed into -196 DEG C of Low Temperature Liquids immediately
In nitrogen, the variation of local temperature does not only result in the curling and layering of platelet boron nitride, but also liquid nitrogen is caused acutely to be expanded into gas
State simultaneously removes boron nitride.It repeats the step 5 time and obtains ultrathin boron nitride nanosheet.
Step 2: alumina nano fiber is prepared
(1) 10mL dehydrated alcohol is placed in 25mL round-bottomed flask, 1.9g aluminium isopropoxide ultrasound is added into round-bottomed flask
After handling half an hour, continue that 0.5mL glacial acetic acid and 0.8mL concentrated hydrochloric acid is slowly added dropwise in whipping process, under room temperature sealing condition
Stirring 6h makes aluminium isopropoxide obtain the clear solution of homogeneous transparent after completely dissolution.0.2g polyethylene pyrrole is added in acquired solution
Pyrrolidone, and continue to stir 12h under room temperature sealing condition, obtain thick solution；
(2) take the above-mentioned solution of 10mL for spinning operation with syringe；Setting solidification distance is 14cm, and feed rate is
0.3mL/h, electrostatic spinning voltage are 19kV, and spinning temperature is 30 DEG C, using masking foil as spinning receiver.Obtained spinning fibre
Through 12h dry in 60 DEG C of thermostatic drying chambers, it is subsequently placed in the calcining of Muffle furnace high temperature.Primary calcining: from starting to warm up at room temperature,
It is risen to after 600 DEG C with 1 DEG C/min heating rate and keeps the temperature 2h, then rise to 800 DEG C with 5 DEG C/min heating rate, continue to keep the temperature 2h；Two
Secondary calcining: the product once calcined is directly added into 1300 DEG C of Muffle furnace high temperature calcinings, so that the product once calcined is quick
It is converted into a-Al2O3。
Step 3: nanoparticle is handled with silane coupling agent
(1) alumina nano fiber prepared by boron nitride nanosheet made from step 1 and step 2 is respectively placed in 100
Dry 12h in DEG C vacuum oven；
(2) 1g boron nitride nanosheet and alumina nano fiber are weighed to be dispersed in respectively in 20mL isopropanol, is ultrasonically treated
1h；
(3) the 20mL isopropanol and step (2) by two parts added with 0.01g 3- aminopropyl triethoxysilane obtain
Two kinds of mixed solutions are mixed respectively, in 70 DEG C of heating water bath 12h under gained mixed solution high-speed stirred；
(4) two kinds of suspension isopropanols centrifugation that step (3) obtain washed, filter and washes repeatedly to remove extra coupling
Agent, finally in a vacuum drying oven 60 DEG C, dry 12h.
Step 4: dissolution low density polyethylene (LDPE)
Low density polyethylene (LDPE) is cleaned postposition with ethyl alcohol to dry in a vacuum drying oven, then to be dissolved in 90 DEG C of dimethylbenzene molten
In agent, until low density polyethylene (LDPE) is completely dissolved；And in the above solution by crosslinking agent dissolution.
Step 5: composite material is made using solution casting method
Silane coupling agent of learning from else's experience respectively processing 0.5 part of compounding nanoparticle, 1 part, 2 parts, 3 parts, 4 parts be placed in dimethylbenzene
In, ultrasonic disperse 1h is then heated to 90 DEG C, and dissolves in low density polyethylene (LDPE) and cumyl peroxide, will be mixed molten
Liquid is transferred to the glass mold being placed in 115 DEG C of airtight vacuum drying boxes, and after solvent is evaporated, obtained film moves to 180 DEG C of vacuum
10min is handled in drying box, then makes its cooled to room temperature, takes film off, which is the high dc breakdown field
Strong Cross-linked Polyethylene Composites.It should be noted that the film is only a kind of form of expression of the composite material, this hair
The Cross-linked Polyethylene Composites of the bright high dc breakdown field strength include but is not limited to the form of expression of film.
Reference examples 1
This reference examples is the pure cross-linking polyethylene materials for being not added with any packing material.The insulating materials is by by weight
Part is 100 parts of low density polyethylene (LDPE)s, and 2 parts of cumyl peroxides are dissolved in 90 DEG C of dimethylbenzene, are then transferred to solution and are placed in 115
Glass mold in DEG C airtight vacuum drying box, solvent is evaporated, obtained film is moved in 180 DEG C of vacuum ovens and handled
10min then makes its cooled to room temperature, takes film off.
Test case 1
Under the rate of rise of 0.5kV/s, under measurement DC voltage prepared by embodiment 1 and reference examples 1 respectively two kinds are multiple
Close the breakdown voltage of film.
As shown in Figure 1, compounding the cross-linking polyethylene materials of nanoparticle and right for addition different content described in embodiment 1
The 1 pure crosslinked polyethylene insulation material prepared as usual, in the Weibull probability distribution of high pressure resistant dc breakdown.Its
In, the high pressure resistant dc breakdown ability of the pure crosslinked polyethylene of × expression；
Indicate the high pressure resistant dc breakdown ability for being added to the crosslinked polyethylene of 0.5phr compounding nanoparticle；
▲ indicate the high pressure resistant dc breakdown ability for being added to the crosslinked polyethylene of 1phr compounding nanoparticle；
● indicate the high pressure resistant dc breakdown ability for being added to the crosslinked polyethylene of 2phr compounding nanoparticle；
Indicate the high pressure resistant dc breakdown ability for being added to the crosslinked polyethylene of 3phr compounding nanoparticle；
Indicate the high pressure resistant dc breakdown ability for being added to the crosslinked polyethylene of 4phr compounding nanoparticle.
In conjunction with the embodiments 1, analyze breakdown voltage result such as table 1:
1 threadiness Al of table2O3The Weibull distribution parameter table of/BNNS/XLPE composite material
α indicates dc breakdown intensity corresponding when the accumulative breakdown probability of laminated film is 0.632 in table 1, can see
The dc breakdown intensity when the content for compounding nanoparticle is 2phr reaches maximum out, reaches 502.5kV/mm, with pure friendship
The 369.7kV/mm of connection polythene material is compared, and improves 35.9%.β indicates that the point institute of breakdown laminated film when test is right
The form parameter for answering dc breakdown voltage Weibull to be distributed, characterizes the dispersion degree of point, β is bigger, and dispersion degree is smaller.
Embodiment 2
A kind of Cross-linked Polyethylene Composites of high dc breakdown field strength, by weight, the material are every 100 parts
Low density polyethylene (LDPE) cooperates 2 parts of crosslinking agents, 0.005~0.04 part of silane coupling agent and 0.5~4 part of compounding nanoparticle.Wherein
Silane coupling agent is fixed as 1:100 with the amount ratio for compounding nanoparticle.
The boron nitride nanosheet is using the boron nitride with a thickness of 300~400nm, using the method system of liquid nitrogen removing
, the boron nitride nanosheet diameter is between 10~20nm.
The alumina nano fiber is using aluminium isopropoxide as raw material, using electrostatic spinning technique and high-temperature calcination means system
, the diameter of the material is between 200~400nm.
The boron nitride nanosheet and alumina nano fiber are to be compounded with mass ratio for the ratio of 2:2.
The density of the low density polyethylene (LDPE) is less than 0.940g/cm3, melt flow index is 2.1~2.2g/10min, is melted
O'clock at 122~124 DEG C.
The crosslinking agent is diethylenetriamine.
The silane coupling agent is 3- aminopropyl triethoxysilane.
The preparation method of the Cross-linked Polyethylene Composites of the high dc breakdown field strength, removing and oxygen including boron nitride
The preparation and silane coupling agent for changing aluminium nanofiber handle boron nitride nanosheet and alumina nano fiber, solution casting method
Insulating materials is made.It is specific as follows:
Step 1: blocky boron nitride is removed
Boron nitride is heated to 300 DEG C first and keeps the temperature one hour, boron nitride is then immersed into -196 DEG C of Low Temperature Liquids immediately
In nitrogen, the variation of local temperature does not only result in the curling and layering of platelet boron nitride, but also liquid nitrogen is caused acutely to be expanded into gas
State simultaneously removes boron nitride.It repeats the step 5 time and obtains ultrathin boron nitride nanosheet.
Step 2: alumina nano fiber is prepared
(1) 10mL dehydrated alcohol is placed in 25mL round-bottomed flask, 1.9g aluminium isopropoxide ultrasound is added into round-bottomed flask
After handling half an hour, continue that 0.5mL glacial acetic acid and 0.8mL concentrated hydrochloric acid is slowly added dropwise in whipping process, under room temperature sealing condition
Stirring 6h makes aluminium isopropoxide obtain the clear solution of homogeneous transparent after completely dissolution.0.2g polyethylene pyrrole is added in acquired solution
Pyrrolidone, and continue to stir 12h under room temperature sealing condition, obtain thick solution；
(2) take the above-mentioned solution of 10mL for spinning operation with syringe；Setting solidification distance is 14cm, and feed rate is
0.3mL/h, electrostatic spinning voltage are 19kV, and spinning temperature is 30 DEG C, using masking foil as spinning receiver.Obtained spinning fibre
Through 12h dry in 60 DEG C of thermostatic drying chambers, it is subsequently placed in the calcining of Muffle furnace high temperature.Primary calcining: from starting to warm up at room temperature,
It is risen to after 600 DEG C with 1 DEG C/min heating rate and keeps the temperature 2h, then rise to 800 DEG C with 5 DEG C/min heating rate, continue to keep the temperature 2h；Two
Secondary calcining: the product once calcined is directly added into 1300 DEG C of Muffle furnace high temperature calcinings, so that the product once calcined is quick
It is converted into a-Al2O3。
Step 3: nanoparticle is handled with silane coupling agent
(1) alumina nano fiber prepared by boron nitride nanosheet made from step 1 and step 2 is respectively placed in 100
Dry 12h in DEG C vacuum oven；
(2) 1g boron nitride nanosheet and alumina nano fiber are weighed to be dispersed in respectively in 20mL isopropanol, is ultrasonically treated
1h；
(3) the 20mL isopropanol and step (2) by two parts added with 0.01g 3- aminopropyl triethoxysilane obtain
Two kinds of mixed solutions are mixed respectively, in 70 DEG C of heating water bath 12h under gained mixed solution high-speed stirred；
(4) two kinds of suspension isopropanols centrifugation that step (3) obtain washed, filter and washes repeatedly to remove extra coupling
Agent, finally in a vacuum drying oven 60 DEG C, dry 12h.
Step 4: dissolution low density polyethylene (LDPE)
Low density polyethylene (LDPE) is cleaned postposition with ethyl alcohol to dry in a vacuum drying oven, then to be dissolved in 90 DEG C of dimethylbenzene molten
In agent, until low density polyethylene (LDPE) is completely dissolved；And in the above solution by crosslinking agent dissolution.
Step 5: composite material is made using solution casting method
Silane coupling agent of learning from else's experience respectively processing 0.5 part of compounding nanoparticle, 1 part, 2 parts, 3 parts, 4 parts be placed in dimethylbenzene
In, ultrasonic disperse 1h is then heated to 90 DEG C, and dissolves in low density polyethylene (LDPE) and cumyl peroxide, will be mixed molten
Liquid is transferred to the glass mold being placed in 115 DEG C of airtight vacuum drying boxes, and after solvent is evaporated, obtained film moves to 180 DEG C of vacuum
10min is handled in drying box, then makes its cooled to room temperature, takes film off, which is the high dc breakdown field
Strong Cross-linked Polyethylene Composites.It should be noted that the film is only a kind of form of expression of the composite material, this hair
The Cross-linked Polyethylene Composites of the bright high dc breakdown field strength include but is not limited to the form of expression of film.
Embodiment 3
A kind of Cross-linked Polyethylene Composites of high dc breakdown field strength, by weight, the material are every 100 parts
Low density polyethylene (LDPE) cooperates 2 parts of crosslinking agents, 0.005~0.04 part of silane coupling agent and 0.5~4 part of compounding nanoparticle.Wherein
Silane coupling agent is fixed as 1:100 with the amount ratio for compounding nanoparticle.
The boron nitride nanosheet is using the boron nitride with a thickness of 300~400nm, using the method system of liquid nitrogen removing
, the boron nitride nanosheet diameter is between 10~20nm.
The alumina nano fiber is using aluminium isopropoxide as raw material, using electrostatic spinning technique and high-temperature calcination means system
, the diameter of the material is between 200~400nm.
The boron nitride nanosheet and alumina nano fiber are to be compounded with mass ratio for the ratio of 3:2.
The density of the low density polyethylene (LDPE) is less than 0.940g/cm3, melt flow index is 2.1~2.2g/10min, is melted
O'clock at 122~124 DEG C.
The crosslinking agent is cumyl peroxide.
The silane coupling agent is 3- aminopropyl trimethoxysilane.
The preparation method of the Cross-linked Polyethylene Composites of the high dc breakdown field strength, removing and oxygen including boron nitride
The preparation and silane coupling agent for changing aluminium nanofiber handle boron nitride nanosheet and alumina nano fiber, solution casting method
Insulating materials is made.It is specific as follows:
Step 1: blocky boron nitride is removed
Boron nitride is heated to 300 DEG C first and keeps the temperature one hour, boron nitride is then immersed into -196 DEG C of Low Temperature Liquids immediately
In nitrogen, the variation of local temperature does not only result in the curling and layering of platelet boron nitride, but also liquid nitrogen is caused acutely to be expanded into gas
State simultaneously removes boron nitride.It repeats the step 5 time and obtains ultrathin boron nitride nanosheet.
Step 2: alumina nano fiber is prepared
(1) 10mL dehydrated alcohol is placed in 25mL round-bottomed flask, 1.9g aluminium isopropoxide ultrasound is added into round-bottomed flask
After handling half an hour, continue that 0.5mL glacial acetic acid and 0.8mL concentrated hydrochloric acid is slowly added dropwise in whipping process, under room temperature sealing condition
Stirring 6h makes aluminium isopropoxide obtain the clear solution of homogeneous transparent after completely dissolution.0.2g polyethylene pyrrole is added in acquired solution
Pyrrolidone, and continue to stir 12h under room temperature sealing condition, obtain thick solution；
(2) take the above-mentioned solution of 10mL for spinning operation with syringe；Setting solidification distance is 14cm, and feed rate is
0.3mL/h, electrostatic spinning voltage are 19kV, and spinning temperature is 30 DEG C, using masking foil as spinning receiver.Obtained spinning fibre
Through 12h dry in 60 DEG C of thermostatic drying chambers, it is subsequently placed in the calcining of Muffle furnace high temperature.Primary calcining: from starting to warm up at room temperature,
It is risen to after 600 DEG C with 1 DEG C/min heating rate and keeps the temperature 2h, then rise to 800 DEG C with 5 DEG C/min heating rate, continue to keep the temperature 2h；Two
Secondary calcining: the product once calcined is directly added into 1300 DEG C of Muffle furnace high temperature calcinings, so that the product once calcined is quick
It is converted into a-Al2O3。
Step 3: nanoparticle is handled with silane coupling agent
(1) alumina nano fiber prepared by boron nitride nanosheet made from step 1 and step 2 is respectively placed in 100
Dry 12h in DEG C vacuum oven；
(2) 1g boron nitride nanosheet and alumina nano fiber are weighed to be dispersed in respectively in 20mL isopropanol, is ultrasonically treated
1h；
(3) the 20mL isopropanol and step (2) by two parts added with 0.01g 3- aminopropyl triethoxysilane obtain
Two kinds of mixed solutions are mixed respectively, in 70 DEG C of heating water bath 12h under gained mixed solution high-speed stirred；
(4) two kinds of suspension isopropanols centrifugation that step (3) obtain washed, filter and washes repeatedly to remove extra coupling
Agent, finally in a vacuum drying oven 60 DEG C, dry 12h.
Step 4: dissolution low density polyethylene (LDPE)
Low density polyethylene (LDPE) is cleaned postposition with ethyl alcohol to dry in a vacuum drying oven, then to be dissolved in 90 DEG C of dimethylbenzene molten
In agent, until low density polyethylene (LDPE) is completely dissolved；And in the above solution by crosslinking agent dissolution.
Step 5: composite material is made using solution casting method
Silane coupling agent of learning from else's experience respectively processing 0.5 part of compounding nanoparticle, 1 part, 2 parts, 3 parts, 4 parts be placed in dimethylbenzene
In, ultrasonic disperse 1h is then heated to 90 DEG C, and dissolves in low density polyethylene (LDPE) and cumyl peroxide, will be mixed molten
Liquid is transferred to the glass mold being placed in 115 DEG C of airtight vacuum drying boxes, and after solvent is evaporated, obtained film moves to 180 DEG C of vacuum
10min is handled in drying box, then makes its cooled to room temperature, takes film off, which is the high dc breakdown field
Strong Cross-linked Polyethylene Composites.It should be noted that the film is only a kind of form of expression of the composite material, this hair
The Cross-linked Polyethylene Composites of the bright high dc breakdown field strength include but is not limited to the form of expression of film.
Embodiment 4
A kind of Cross-linked Polyethylene Composites of high dc breakdown field strength, by weight, the material are every 100 parts
Low density polyethylene (LDPE) cooperates 2 parts of crosslinking agents, 0.005~0.04 (0.005,0.01,0.02,0.03,0.04) part silane coupling agent
With 0.5~4 (0.5,1,2,3,4) part boron nitride nanosheet.The wherein amount ratio of silane coupling agent and the boron nitride nanosheet
It is fixed as 1:100.
The boron nitride nanosheet is using the boron nitride with a thickness of 300~400nm, using the method system of liquid nitrogen removing
, the boron nitride nanosheet diameter is between 10~20nm.
The density of the low density polyethylene (LDPE) is less than 0.940g/cm3, melt flow index is 2.1~2.2g/10min, is melted
O'clock at 122~124 DEG C.
The crosslinking agent is cumyl peroxide.
The silane coupling agent is 3- aminopropyl triethoxysilane.
The preparation method of the Cross-linked Polyethylene Composites of the high dc breakdown field strength, the removing including boron nitride, with
And insulating materials is made in silane coupling agent processing boron nitride nanosheet, solution casting method.It is specific as follows:
Step 1: blocky boron nitride is removed
Boron nitride is heated to 300 DEG C first and keeps the temperature one hour, boron nitride is then immersed into -196 DEG C of Low Temperature Liquids immediately
In nitrogen, the variation of local temperature does not only result in the curling and layering of platelet boron nitride, but also liquid nitrogen is caused acutely to be expanded into gas
State simultaneously removes boron nitride.It repeats the step 5 time and obtains ultrathin boron nitride nanosheet.
Step 2: boron nitride nanosheet is handled with silane coupling agent
(1) boron nitride nanosheet made from step 1 is placed in 100 DEG C of vacuum ovens dry 12h；
(2) it weighs 1g boron nitride nanosheet to be dispersed in 20mL isopropanol, is ultrasonically treated 1h；
(3) by the mixing of 20mL isopropanol and step (2) acquisition added with 0.01g 3- aminopropyl triethoxysilane
Solution is mixed, in 70 DEG C of heating water bath 12h under gained mixed solution high-speed stirred；
(4) the suspension isopropanol centrifugation that step (3) obtain washed, filter and washes repeatedly to remove extra coupling agent,
It is 60 DEG C in a vacuum drying oven last, dry 12h.
Step 3: dissolution low density polyethylene (LDPE)
Low density polyethylene (LDPE) is cleaned postposition with ethyl alcohol to dry in a vacuum drying oven, then to be dissolved in 90 DEG C of dimethylbenzene molten
In agent, until low density polyethylene (LDPE) is completely dissolved；And in the above solution by crosslinking agent dissolution.
Step 4: composite material is made using solution casting method
Silane coupling agent of learning from else's experience processing 0.5 part of boron nitride nanosheet, 1 part, 2 parts, 3 parts, 4 parts be placed in dimethylbenzene, surpass
Sound disperses 1h, is then heated to 90 DEG C, and dissolve in low density polyethylene (LDPE) and cumyl peroxide, mixed solution is transferred to
The glass mold being placed in 115 DEG C of airtight vacuum drying boxes, after solvent is evaporated, obtained film moves to 180 DEG C of vacuum ovens
Middle processing 10min, then makes its cooled to room temperature, takes film off, which is the friendship of the high dc breakdown field strength
Join composite polyethylene material.It should be noted that the film is only a kind of form of expression of the composite material, it is of the present invention
High dc breakdown field strength Cross-linked Polyethylene Composites include but is not limited to film the form of expression.
Embodiment 5
A kind of Cross-linked Polyethylene Composites of high dc breakdown field strength, by weight, the material are every 100 parts
Low density polyethylene (LDPE) cooperates 2 parts of crosslinking agents, 0.005~0.04 (0.005,0.01,0.02,0.03,0.04) part silane coupling agent
With 0.5~4 (0.5,1,2,3,4) part alumina nano fiber.The wherein use of silane coupling agent and the alumina nano fiber
Amount ratio is fixed as 1:100.
The alumina nano fiber is using aluminium isopropoxide as raw material, using electrostatic spinning technique and high-temperature calcination means system
, the diameter of the material is between 200~400nm.
The density of the low density polyethylene (LDPE) is less than 0.940g/cm3, melt flow index is 2.1~2.2g/10min, is melted
O'clock at 122~124 DEG C.
The crosslinking agent is cumyl peroxide.
The silane coupling agent is 3- aminopropyl triethoxysilane.
The preparation method of the Cross-linked Polyethylene Composites of the high dc breakdown field strength, including alumina nano fiber
Insulating materials is made in preparation and silane coupling agent processing alumina nano fiber, solution casting method.It is specific as follows:
Step 1: alumina nano fiber is prepared
(1) 10mL dehydrated alcohol is placed in 25mL round-bottomed flask, 1.9g aluminium isopropoxide ultrasound is added into round-bottomed flask
After handling half an hour, continue that 0.5mL glacial acetic acid and 0.8mL concentrated hydrochloric acid is slowly added dropwise in whipping process, under room temperature sealing condition
Stirring 6h makes aluminium isopropoxide obtain the clear solution of homogeneous transparent after completely dissolution.0.2g polyethylene pyrrole is added in acquired solution
Pyrrolidone, and continue to stir 12h under room temperature sealing condition, obtain thick solution；
(2) take the above-mentioned solution of 10mL for spinning operation with syringe；Setting solidification distance is 14cm, and feed rate is
0.3mL/h, electrostatic spinning voltage are 19kV, and spinning temperature is 30 DEG C, using masking foil as spinning receiver.Obtained spinning fibre
Through 12h dry in 60 DEG C of thermostatic drying chambers, it is subsequently placed in the calcining of Muffle furnace high temperature.Primary calcining: from starting to warm up at room temperature,
It is risen to after 600 DEG C with 1 DEG C/min heating rate and keeps the temperature 2h, then rise to 800 DEG C with 5 DEG C/min heating rate, continue to keep the temperature 2h；Two
Secondary calcining: the product once calcined is directly added into 1300 DEG C of Muffle furnace high temperature calcinings, so that the product once calcined is quick
It is converted into a-Al2O3。
Step 2: nanoparticle is handled with silane coupling agent
(1) alumina nano fiber made from step 1 is placed in 100 DEG C of vacuum ovens dry 12h；
(2) it weighs 1g alumina nano fiber to be dispersed in 20mL isopropanol, is ultrasonically treated 1h；
(3) by the mixing of 20mL isopropanol and step (2) acquisition added with 0.01g 3- aminopropyl triethoxysilane
Solution is mixed, in 70 DEG C of heating water bath 12h under gained mixed solution high-speed stirred；
(4) the suspension isopropanol centrifugation that step (3) obtain washed, filter and washes repeatedly to remove extra coupling agent,
It is 60 DEG C in a vacuum drying oven last, dry 12h.
Step 3: dissolution low density polyethylene (LDPE)
Low density polyethylene (LDPE) is cleaned postposition with ethyl alcohol to dry in a vacuum drying oven, then to be dissolved in 90 DEG C of dimethylbenzene molten
In agent, until low density polyethylene (LDPE) is completely dissolved；And in the above solution by crosslinking agent dissolution.
Step 4: composite material is made using solution casting method
Silane coupling agent of learning from else's experience processing 0.5 part of alumina nano fiber, 1 part, 2 parts, 3 parts, 4 parts be placed in dimethylbenzene,
Ultrasonic disperse 1h is then heated to 90 DEG C, and dissolves in low density polyethylene (LDPE) and cumyl peroxide, and mixed solution is turned
Enter the glass mold being placed in 115 DEG C of airtight vacuum drying boxes, after solvent is evaporated, obtained film moves to 180 DEG C of vacuum drying
10min is handled in case, then makes its cooled to room temperature, takes film off, which is the high dc breakdown field strength
Cross-linked Polyethylene Composites.It should be noted that the film is only a kind of form of expression of the composite material, institute of the present invention
The Cross-linked Polyethylene Composites for the high dc breakdown field strength stated include but is not limited to the form of expression of film.
Protection content of the invention is not limited to above embodiments.Without departing from the spirit and scope of the invention, originally
Field technical staff it is conceivable that variation and advantage be all included in the present invention, and with the attached claims be protection
Range.
Claims (9)
1. a kind of Cross-linked Polyethylene Composites of high dc breakdown field strength comprising :(a) the low density polyethylene of 100 parts by weight
Alkene；(b) 2 parts by weight of crosslinking agent；(c) 0.005~0.04 parts by weight silane coupling agent；(d) 0.5~4 parts by weight compound nanoparticle
Son, the compounding nanoparticle are boron nitride nanosheet and alumina nano fiber；The silane coupling agent and the nanoparticle
The amount ratio of sub- boron nitride nanosheet and alumina nano fiber is fixed as 1:100.
2. a kind of Cross-linked Polyethylene Composites of high dc breakdown field strength according to claim 1, which is characterized in that institute
Stating boron nitride nanosheet is made using the method for liquid nitrogen removing, the boron nitride using the boron nitride with a thickness of 300 ~ 400 nm
Nanometer sheet diameter is between 10 ~ 20 nm.
3. a kind of Cross-linked Polyethylene Composites of high dc breakdown field strength according to claim 1, which is characterized in that institute
Stating alumina nano fiber is made using electrostatic spinning technique and high-temperature calcination means, the material using aluminium isopropoxide as raw material
Diameter between 200 ~ 400 nm.
4. a kind of Cross-linked Polyethylene Composites of high dc breakdown field strength according to claim 1, which is characterized in that institute
Boron nitride nanosheet and alumina nano fiber is stated to be compounded with the weight ratio of 2:3.
5. a kind of Cross-linked Polyethylene Composites of high dc breakdown field strength according to claim 1, which is characterized in that institute
The density of low density polyethylene (LDPE) is stated less than 0.940 g/cm3, melt flow index in 2.1 ~ 2.2g/10min, fusing point 122~
124 ℃。
6. a kind of Cross-linked Polyethylene Composites of high dc breakdown field strength according to claim 1, which is characterized in that institute
Stating crosslinking agent is cumyl peroxide, diethylenetriamines, di-tert-butyl peroxide, one in di-isopropylbenzene hydroperoxide
Kind.
7. a kind of Cross-linked Polyethylene Composites of high dc breakdown field strength according to claim 1, which is characterized in that institute
Stating silane coupling agent is 3- aminopropyl triethoxysilane, 3- aminopropyl trimethoxysilane, N- (β-aminoethyl)-γ-ammonia third
Ethyl triethoxy silicane alkane, one of γ-aminopropyltriethoxy diethoxy silane.
8. a kind of described in any item preparation sides of the Cross-linked Polyethylene Composites of high dc breakdown field strength of claim 1~7
Method, which is characterized in that magnesia, molten is handled by the preparation of boron nitride nanosheet and alumina nano fiber, silane coupling agent
Liquid, which is blended, is made insulating materials.
9. a kind of preparation method of the Cross-linked Polyethylene Composites of high dc breakdown field strength according to claim 8,
It is characterized in that, specifically comprises the following steps:
Step 1 removes blocky boron nitride: boron nitride being heated to 300 DEG C first and keeps the temperature 1 h；Then boron nitride is soaked immediately
Enter in -196 DEG C of low temperature liquid nitrogens, so that boron nitride is removed；Above-mentioned steps, which are repeated as many times, prepares ultrathin boron nitride nanosheet；
Step 2 prepares alumina nano fiber: aluminium isopropoxide being placed in dehydrated alcohol, after ultrasonic treatment, persistently stirred
Glacial acetic acid and concentrated hydrochloric acid are added in journey, are stirred continuously until aluminium isopropoxide sufficiently dissolves and obtains transparent clear solution；It is molten in gained
Polyvinylpyrrolidone is added in liquid, is stirred continuously to obtain thick solution；Thick solution is taken to carry out spinning behaviour with syringe
Make, obtained spinning fibre obtains alumina nano fiber through high-temperature calcination；
Step 3 handles nanoparticle with silane coupling agent: will aoxidize made from boron nitride nanosheet made from step 1 and step 2
Aluminium nanofiber is dispersed in isopropanol respectively, and ultrasonic treatment takes silane coupling agent to dilute stir process in isopropanol, will add
Added with silane coupling agent aqueous isopropanol respectively with the aqueous isopropanol containing boron nitride nanosheet and contain aluminium oxide nano
The aqueous isopropanol of fiber mixes, gained mixed solution high-speed stirred under heating condition；By the suspension isopropanol of acquisition
Repeatedly washing, it is finally dry in vacuum oven；
Step 4 dissolves low density polyethylene (LDPE): low density polyethylene (LDPE) being cleaned postposition with ethyl alcohol and is dried in a vacuum drying oven, then
It is dissolved in xylene solvent, until low density polyethylene (LDPE) is completely dissolved；And in the above solution by crosslinking agent dissolution；
Composite material is made using solution casting method in step 5: the boron nitride nanosheet and aluminium oxide nano handled through step 3 is fine
Dimension is compounded, and compounding nanoparticle is placed in dimethylbenzene, ultrasonic disperse, then heats and it is made to dissolve in step 4 preparation
In solution, mixed solution is then transferred to the glass mold in 115 DEG C of airtight vacuum drying boxes, solvent is evaporated, is obtained
Film be transferred in 180 DEG C of vacuum ovens and handle, then make its cooled to room temperature, take film off；The film is
The Cross-linked Polyethylene Composites of the high dc breakdown field strength.
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