CN107778765A - A kind of cable insulation material preparation method - Google Patents

A kind of cable insulation material preparation method Download PDF

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CN107778765A
CN107778765A CN201711048477.7A CN201711048477A CN107778765A CN 107778765 A CN107778765 A CN 107778765A CN 201711048477 A CN201711048477 A CN 201711048477A CN 107778765 A CN107778765 A CN 107778765A
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parts
mud
modified alta
density polyethylene
low density
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王尧尧
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L61/00—Compositions of condensation polymers of aldehydes or ketones; Compositions of derivatives of such polymers
    • C08L61/04—Condensation polymers of aldehydes or ketones with phenols only
    • C08L61/06—Condensation polymers of aldehydes or ketones with phenols only of aldehydes with phenols
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
    • H01B3/18—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances
    • H01B3/30—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes
    • H01B3/36—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes condensation products of phenols with aldehydes or ketones
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2217—Oxides; Hydroxides of metals of magnesium
    • C08K2003/222—Magnesia, i.e. magnesium oxide
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/002—Physical properties
    • C08K2201/003—Additives being defined by their diameter
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/011—Nanostructured additives
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/08—Stabilised against heat, light or radiation or oxydation
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00—Applications
    • C08L2203/20—Applications use in electrical or conductive gadgets
    • C08L2203/202—Applications use in electrical or conductive gadgets use in electrical wires or wirecoating
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2207/00—Properties characterising the ingredient of the composition
    • C08L2207/06—Properties of polyethylene
    • C08L2207/066—LDPE (radical process)

Abstract

The present invention relates to a kind of high pressure, the preparation method of extra-high-tension cable insulating materials, the cable insulation material includes 10 20 parts of low density polyethylene (LDPE)/modified alta-mud, 5 10 parts of nano magnesia, 80 100 parts of phenolic resin, 10 20 parts of carbonitride, 20 30 parts of polystyrene, 30 40 parts of epoxy resin, 58 parts of antioxidant, 5 10 parts of plasticizer, 10 15 parts of glass fibre, 20 30 parts of 20 30 parts of neoprene and polyvinyl chloride, the heat resistance and intensity of insulating materials can be improved, reduce the ageing time of insulating materials, HTHP effect can be kept lower non-degradable for a long time.

Description

A kind of cable insulation material preparation method
Technical field
The present invention relates to a kind of preparation method of cable insulation material, the cable insulation material include nano magnesia, Low density polyethylene (LDPE)/modified alta-mud, the heat resistance and intensity of insulating materials can be improved, when reducing the aging of insulating materials Between, it can keep non-degradable for a long time under high temperature action.
Background technology
Cable is mainly made up of following 4 part：1. conducting wire center, it is made of high conductivity material (copper or aluminium).2. insulate Layer, the insulating materials as cable should have a high insulaion resistance, high breakdown field strength, low dielectric loss and low Dielectric constant.The insulating materials commonly used in cable has oil-paper, polyvinyl chloride, polyethylene, crosslinked polyethylene, rubber etc..It is 3. close Closure set, protect protection insulated wire heart from the damage of machinery, moisture, moisture, chemical substance, light etc..Insulation for moisture-sensitive, one As use lead or aluminium extrusion sealing sheath.4. coating is protected, to protect sealing sheath from mechanical damage.It is general to use plating Zinc steel band, steel wire or copper strips, copper wire etc. surround outside sheath (title armored cable) as armor, and armor plays electric field shielding simultaneously With the effect for preventing external electromagnetic wave interference.
At present, it is high polymer material that the insulating barrier of cable is most commonly used, and on electrotechnics, specific insulation is more than 109The material that Ω cm material is formed is referred to as insulating materials, that is, for making device electrically to prevent electric current The material passed through.Crosslinked polyethylene has excellent dielectric properties and mechanical performance, and oneself is widely used in high pressure and super-pressure In plastic insulating power cable.With the development of super-pressure, extra-high voltage direct-current power transmission and transformation system, the insulation ag(e)ing in running Problem is increasingly severe, and oneself turns into the major obstacle that insulated cable develops to super-pressure.When the applied electric field of insulating polymer is strong When degree reaches 1/10th of breakdown field strength, poplar bundles can be caused in the Electric Power Equipment Insulation to work long hours, reduce electricity Cable service life.The high voltage power cable insulating materials being made up of low density polyethylene (LDPE), by various in During Process of Long-term Operation The gradual aging of influence of aging action, causes the decline of the dielectric properties and mechanical performance of material.According to the classification of aging action Voltage ageing, heat ageing, mechanical aging and Electrochemical Ageing can be divided into.Wherein heat ageing is the main of PE cable insulation infringement Inducement, different thermal aging times and condition can cause the difference of polyethylene inner molecular structure, and then influence its space charge spy Property.
Research shows, under DC electric field effect, space charge is easily formed in polymer insulation, and space charge can make Electric Field Distribution is distorted, and aggravates polymer insulation aging, and the aging of material result in the decline of material electric property.Polymer Space-charge is mainly by the same polarity space charge and insulator that enter sunken carrier or transportable current-carrying of electrode injection Organic or inorganic impurity ionized under electric field action caused by heteropolarity electricity.In order to suppress the formation of space charge, it is necessary to poly- It is ethylene modified so as to change trap energy therein and distribution, change distribution of space charge, lower distortion probability, improve polymer Dielectric properties, polymer insulation aging is reduced, and do not influence the processing characteristics of polymer simultaneously.
Bentonite is also known as palygorskite（Palygorskite）Or Palygorskite, it is a kind of magnesium containing Shuifu County for having chain layer structure Aluminosilicate clays mineral.Its structure belongs to 2：1 type clay mineral.Each 2：In 1 unit structure layer, tetrahedron chip angle top every Certain distance direction overturns, forming layer chain.Bentonite stone clay refers to bentonite stone（attapulgite）For key component A kind of clay mineral.Bentonite stone is that a kind of crystalloid is hydrated alumina magnesia silicate, has unique layer chain structure feature, Crystal lattice in its structure be present, contain variable amount of Na in crystal+、Ca2+、Fe3+、Al3+, crystal is in needle-like, threadiness or Fiber collection shape.There is bentonite stone the good colloidal natures such as unique scattered, high temperature resistant, salt resistance alkali and higher absorption to take off Color ability, and there is certain plasticity and cohesive force, its preferable chemical molecular formula is：Mg5Si8O20(OH)2(OH2)4· 4H2O.With between chain structure and layer structureItBetween intermediate structure.Due to the unique crystal structure of bentonite stone, it is allowed to With many special materializations and processing performance.Main physical and chemical performance and processing performance have：Cation interchangeability, water imbibition, Adsorption bleaching, big specific surface area（9.6~36m2/g）And colloid index and expansion capacity.The current bentonite stone ore production money in China Source reserves are entirely capable of meeting industrial demand, and have obvious performance compared with the Resource Properties of other various countries of the world Advantage.Bentonite stone has preferable draw ratio and abundant inner duct, is both that preferable reinforcing material has fire retardation again, Lose constitution water at high temperature and produce vapor, can with blocking oxygen, and can produce better heat stability with magnesia, Al2O3Based on oxide-isolation layer.
Poletene/lamina material has certain advantage, and mainly lighter than Conventional filler compound, density is relatively low, tool There are higher heat resistance, high intensity, high-modulus, high gas-obstructing character and the relatively low coefficient of expansion, electricity can be widely used in Son, household electrical appliances, power industry.
The content of the invention
Dielectric Properties at present on polyethylene/bentonite clay material are less, although bentonite has, cheap, performance is good The features such as, but its surface has certain hydrophily, it is not easy to merged with polymer surfaces, therefore, present invention research passes through It is bentonite modified, using its space layer chain structure, stable space layer chain is then formed with polyethylene and is combined, is reduced bentonitic Surface free energy, the dissipation rate of charge migration speed and space charge is improved, to refuse electric field tight so as to suppress media interior Distort again, suppress space charge accumulation, reduce space charge amount, improve distribution of space charge, improve charge transport, can be notable Reduce the aging phenomenon of insulating materials.And because bentonite clay material has good heat resistance in itself, by it is modified can Heat transfer inside polyvinyl alcohol material is want with the extraneous heat of barrier, the thermal diffusion of high temperature degradation is prevented, insulation can be improved The resistance to elevated temperatures of material.
First, in order to improve bentonitic surface acidity, increase polar group, be modified using acid, increase bentonitic ratio Surface area, gap structure distribution is improved, optimization layer chain space structure, increases lamella and chain length, is advantageous to be combined with polyethylene, So as to avoid only internal intercalation, Dispersion on surface can also be formed and polymerize, be advantageous to combining closely for the two；The present invention uses Weak acid include acetic acid, citric acid, malic acid, concentration 0.1-2mol/l, the acidic functionality that above-mentioned organic acid includes is more, i.e., Destruction of the strong acid to bentonitic layer chain is avoided, it is gentle stable, but also certain three-dimensional effect can be formed, beneficial to CO-, NH- isopolarity small molecule groups occupy active room, with bentonitic surface and interior layer link be configured to combine closely, with It, with dispersion space electric charge, can be advantageous to prevent the aggregation of space charge after low density polyethylene (LDPE) mixing, it is anti-aging so as to be advantageous to.
Polyimides is one of optimal high-molecular organic material of combination property, and high temperature resistant makes for a long time up to more than 400 DEG C With temperature range -200~300 DEG C, no sharp melting point, high insulating property, 103 Dielectric constant 4.0 under HZ, dielectric loss is only 0.004~0.007, category F to H class F insulating material Fs.And with the characteristic such as low friction, wear-resistant, it is commonly used for protection materials.
Polyimides is to contain imide ring on main chain（-CO-NH-CO-）A kind of polymer, while there is CO-, NH- Polar micromolecules group, bentonite is carried out to polyimide modified, the increase polar micromolecules degree of polymerization, further increase lamella sky Between, and due to small polarity CO-, NH- presence adds the degree of polymerization of interior volume and surface polyethylene, and process is overcritical After extraction, the expansion of piece sheaf space, density of material is reduced with polymer combination latter aspect, forms more light material, separately On the one hand bentonitic surface free energy is reduced, improves the dissipation rate of electric charge, prevent space charge to gather, reduce insulation The aging of material.Polyimides has good resistance to elevated temperatures in itself, and on the one hand bentonite is modified, and on the one hand may be used also With play it is resistant to elevated temperatures a little, improve insulating materials system resistance to elevated temperatures, further optimize insulating materials.
The impact of low density polyethylene (LDPE)/modified alta-mud nano composite material is measured using izodtest method Intensity, this method principle are that the sample that will be perpendicular to cantilever beam support is destroyed with pendulum one-shot, measurement sample fracture when institute The ratio between the impact energy of absorption, the cross-sectional area that impact energy is hit with sample is impact strength.Result of the test shows, low The impact strength of density polyethylene/modified alta-mud nano-composite insulating material is 31.8kJ/m2;And common low density polyethylene (LDPE) Impact strength be only 20kJ/m2。
Using CONCEPT80 broadband dielectric spectrum measurement systems, it can be seen that nano magnesia-low density polyethylene (LDPE)/changes Property bentonite active component real part and the imaginary part of complex dielectric permittivity be all higher than common low-density polyethylene material, Ke Yi 103-106Reach in the range of Hz in the range of 2.9-3.2, significantly larger than the 2.0-2.1 scopes of common polythene, due to composite Complex dielectric permittivity increase, hole and electron injection difficulty increase, cause aggregation space charge reduce, so as to reduce aging.
Electrostrictive polymer ageing process and electric charge enter to fall into and detrapping process is relevant, enter and fall into the releasing along with energy with detrapping Put and shift.Ultraviolet radioactive caused by electronics and hole-recombination is cause depolymerization main in electrostrictive polymer ageing process Factor.Degraded according to light, voltage ageing similitude and polymer light theoretical, a small amount of inorganic nano oxygen is introduced toward polyethylene base-material is interior Compound particle, as nano magnesia, nano zine oxide are respectively provided with good light scattering ability and larger specific surface area, favorably In the Charge Transport Proper ty for improving polyethylene, aging is reduced, improves service life.
The present invention relates to a kind of high pressure, extra-high-tension cable insulating materials, the cable insulation material include nano magnesia/ Low density polyethylene (LDPE)/modified alta-mud 10-20 parts, phenolic resin 80-100 parts, carbonitride 10-20 parts, polystyrene 20-30 Part, epoxy resin 30-40 parts, antioxidant 5-8 parts, plasticizer 5-10 parts, glass fibre 10-15 parts, neoprene 20-30 parts and Polyvinyl chloride 20-30 parts, wherein modified alta-mud refer to bentonite by after low-kappa number by polyimide grafted modification.
The plasticizer is acetyl tributyl citrate.The particle diameter of the nano magnesia is 30-100nm, preferably 30-70nm.The antioxidant master can effectively prevent the autoxidation of polymer, mainly using antioxidant 1024, antioxidant 565th, antioxidant 1010 etc., and it is not limited to antioxidant material commonly used in the art.
Wherein, the mass ratio of low density polyethylene (LDPE)/modified alta-mud is 10-20：2-10.
The insulating materials is to be prepared in accordance with the following steps：
（1）Prepare modified alta-mud：Bentonite original ore soil is added in 150mL distilled water, mistake after 10~30min of ultrasonic disperse The large particulate matter except beaker bottom is filtered off, is centrifuged, is dried, is ground, roasting；It is 0.1- that baked bentonite is placed in into concentration React 1~2h in 2mol/L acetum after ultrasonic disperse at 80 DEG C~90 DEG C, finally filter, wash until neutrality, dries It is dry.The bentonite of acidifying is added in toluene 15~20min of ultrasonic disperse under nitrogen protection, temperature is then risen to 110 It is added to after~120 DEG C in the aqueous solution of polyethyleneimine, 5~6h is reacted at 80~100 DEG C after ultrasonic 20-30min is scattered, Then filter, washed with distilled water and absolute ethyl alcohol, being dried in vacuo 10~12h at 60~80 DEG C, obtaining modified alta-mud, it is modified Bentonite particle diameter is 0.5-1mm, preferably 0.5-0.8mm.
（2）Prepare low density polyethylene (LDPE)/modified alta-mud nano composite material：Using high shear type double screw extruder, Modified bentonite is dropped under agitation to be well mixed with low density polyethylene (LDPE), with twin-screw extrusion mixed material, is granulated, into Type.The mass ratio of wherein nano magnesia and low density polyethylene (LDPE)/modified alta-mud is 0.5-2：10.
（3）Low density polyethylene (LDPE)/modified alta-mud nano composite material and nano magnesia are mixed：Take low density polyethylene Alkene/modified alta-mud nano composite material is dissolved in toluene solution, and then nano oxidized magnesium particle is added in above-mentioned solution, Temperature is kept for 80-120 DEG C, stirs 2h, ultrasonic disperse 2h.The mixed liquor of preparation is then placed in desolventizing in baking oven, so as to make Obtain nano inorganic-organic composite material of nano oxidized magnesium particle/low density polyethylene (LDPE)/modified alta-mud；
（4）Phenolic resin 80-100 parts, carbonitride 10-20 parts, polystyrene 20-30 parts, epoxy resin（Weight average molecular weight 9000）30-40 parts, antioxidant 5-8 parts, plasticizer 5-10 parts, glass fibre 10-15 parts, neoprene 20-30 parts and polychlorostyrene second Alkene 20-30 parts and step（3）Composite 10-20 parts pour into homogenizer, at room temperature first use 800-1000 revs/min Speed stir 30 minutes, 30min, the batch mixing that will be stirred then are stirred with 3000-4000 revs/min of speed at 60 DEG C Discharge, then melts, injection molding, obtains the cable insulation material.The melting temperature is 200-280 DEG C, the injection Forming temperature is 120-150 DEG C, preferably 130-150 DEG C.
Composite cable insulating materials can be substantially reduced in the application in high pressure and super-pressure plastic insulating power cable Aging, improve the high temperature resistant and intensity of cable insulation material.
Embodiment
With reference to embodiment, the present invention is further detailed explanation.
Embodiment 1
（1）Bentonite original ore soil is added in 150mL distilled water, filtered off after ultrasonic disperse 10min big except beaker bottom Particulate matter, centrifuge, dry, grind, roasting；Baked bentonite is placed in the acetum that concentration is 0.5mol/L and surpassed 1h is reacted at 80 DEG C after sound is scattered, finally filters, wash until neutral, drying.The bentonite of acidifying is added in toluene Ultrasonic disperse 20min under nitrogen protection, it is added in the aqueous solution of polyethyleneimine, surpasses after temperature then is risen into 120 DEG C 5h is reacted at 80 DEG C after sound 20min is scattered, then filters, washed with distilled water and absolute ethyl alcohol, in 80 DEG C of vacuum drying 12h, obtain modified alta-mud.
（2）Using high shear type double screw extruder, under agitation by modified bentonite and low density polyethylene (LDPE) It is well mixed, with twin-screw extrusion mixed material, it is granulated, shaping.
（3）Take step（2）The low density polyethylene (LDPE) of preparation/modified alta-mud nano composite material is dissolved in toluene solution, Then the nano oxidized magnesium particle that particle diameter is 30nm is added in above-mentioned solution, temperature is kept for 100 DEG C, stirs 2h, ultrasound point Dissipate 2h.The mixed liquor of preparation is then placed in desolventizing in baking oven, so that obtained nano oxidized magnesium particle/low density polyethylene (LDPE)/ Modified alta-mud nano composite material；Wherein nano magnesia accounts for low density polyethylene (LDPE)/modified alta-mud nano composite material matter It is 0.5% to measure percentage.
（4）80 parts of phenolic resin, 10 parts of carbonitride, 20 parts of polystyrene, epoxy resin（Weight average molecular weight 9000）30 parts, 5 parts of antioxidant, 5 parts of plasticizer, 10 parts of glass fibre, 20 parts of neoprene and 20 parts of polyvinyl chloride and step（3）Composite wood 20 parts of material pours into homogenizer, is first stirred 30 minutes using 1000 revs/min of speed at room temperature, then at 60 DEG C with 3000 Rev/min speed stirring 30min, by the batch mixing to stir discharge, then 200 DEG C melting, 150 DEG C of injection moldings, obtain The cable insulation material.
Embodiment 2
（1）Prepare modified alta-mud：Bentonite original ore soil is added in 150mL distilled water, filtered off after ultrasonic disperse 30min Except the large particulate matter of beaker bottom, centrifuge, dry, grind, roasting；It is 1mol/L's that baked bentonite is placed in into concentration React 1h in acetum after ultrasonic disperse at 80 DEG C DEG C, finally filter, wash until neutral, drying.By the swelling of acidifying Soil is added in toluene ultrasonic disperse 15min under nitrogen protection, and polyethyleneimine is added to after temperature then is risen into 110 DEG C The aqueous solution in, 6h is reacted at 100 DEG C after ultrasonic 20min is scattered, then filtering, washed with distilled water and absolute ethyl alcohol, 80 DEG C of vacuum drying 12h, obtain modified alta-mud.
（2）Using high shear type double screw extruder, modified bentonite and low density polyethylene (LDPE) drop under agitation It is well mixed, with twin-screw extrusion mixed material, it is granulated, shaping.
（3）Take step（2）Low density polyethylene (LDPE)/modified alta-mud nano composite material is dissolved in toluene solution, then will 50nm nano oxidized magnesium particle is added in above-mentioned solution, and temperature is kept for 80 DEG C, stirs 2h, ultrasonic disperse 2h.Then will system Standby mixed liquor is placed in desolventizing in baking oven, so as to which receiving for nano oxidized magnesium particle/low density polyethylene (LDPE)/modified alta-mud be made Rice inorganic-organic composite material；Wherein nano magnesia accounts for low density polyethylene (LDPE)/modified alta-mud nano composite material quality hundred Divide than being 1.0%.
（4）100 parts of phenolic resin, 20 parts of carbonitride, 30 parts of polystyrene, epoxy resin（Weight average molecular weight 9000）40 Part, 8 parts of antioxidant, 10 parts of plasticizer, 15 parts of glass fibre, 30 parts of neoprene and 30 parts of polyvinyl chloride and step（3）Answer 20 parts of condensation material pours into homogenizer, at room temperature first using 1000 revs/min speed stir 30 minutes, then 60 DEG C with 3000 revs/min of speed stirring 30min, the batch mixing to stir is discharged, then 200 DEG C of meltings, then 130 DEG C are molded into Type, obtain the cable insulation material.
Embodiment 3
（1）Bentonite original ore soil is added in 150mL distilled water, filtered off after ultrasonic disperse 30min big except beaker bottom Particulate matter, centrifuge, dry, grind, roasting；Baked bentonite is placed in ultrasound in the acetum that concentration is 2mol/L 2h is reacted at 90 DEG C after scattered, finally filters, wash until neutral, drying.The bentonite of acidifying is added in toluene The lower ultrasonic disperse 20min of nitrogen protection, then temperature is risen to after 120 DEG C be added in the aqueous solution of polyethyleneimine, ultrasound 5h is reacted at 80 DEG C after 30min is scattered, then filters, washed with distilled water and absolute ethyl alcohol, being dried in vacuo 10h at 60 DEG C, Obtain modified alta-mud.
（2）Prepare low density polyethylene (LDPE)/modified alta-mud nano composite material：Using high shear type double screw extruder, Modified bentonite is dropped under agitation to be well mixed with low density polyethylene (LDPE), with twin-screw extrusion mixed material, is granulated, into Type.
（3）Low density polyethylene (LDPE)/modified alta-mud nano composite material and nano magnesia are mixed：Take low density polyethylene Alkene/modified alta-mud nano composite material is dissolved in toluene solution, is then added to nanometer 70nm magnesia particle above-mentioned In solution, temperature is kept for 100 DEG C, stirs 2h, ultrasonic disperse 2h.The mixed liquor of preparation is then placed in desolventizing in baking oven, from And nano oxidized magnesium particle/low density polyethylene (LDPE)/modified alta-mud nano composite material is made；Wherein nano magnesia accounts for low close It is 2% to spend polyethylene/modified alta-mud nano composite material mass percent.
（4）100 parts of phenolic resin, 10 parts of carbonitride, 20 parts of polystyrene, epoxy resin（Weight average molecular weight 9000）40 Part, 8 parts of antioxidant, 5 parts of plasticizer, 10 parts of glass fibre, 20 parts of neoprene and 30 parts of polyvinyl chloride and step（3）It is compound 20 parts of material pours into homogenizer, at room temperature first using 1000 revs/min speed stir 30 minutes, then 60 DEG C with 3000 revs/min of speed stirring 30min, the batch mixing to stir is discharged, then 220 DEG C of meltings, 150 DEG C of injection moldings, Obtain the cable insulation material.
Comparative example 1
Only with common bentonite, without modifying process, other experiment parameters are the same as embodiment 1.
Comparative example 2
Nano magnesia is added without, other experiment parameters are the same as embodiment 1.
Specific detection
Detect the tensile strength (σ t/MPa) of above-mentioned anti-aging cable insulation material, elongation at break (δ/ %), density, hardness, Then above-mentioned anti-aging cable insulation material was subjected to hot air aging all over the world by 200 DEG C × 30 days, 250 DEG C × 20, then Detect stretching strength retentivity (E1/ %) and elongation at break conservation rate (E2/ %), concrete outcome is shown in Table 1.
The each index of the Electric insulation material of table 1
Embodiment 1 Embodiment 2 Embodiment 3 Comparative example 1 Comparative example 2
Density, g/cm3 1.01 1.071 1.12 1.25 1.347
Hardness, ShoreA 91 90 87 77 78
Tensile strength, MPa 55 58 59 40 38
Elongation at break % 580 570 590 380 350
200 DEG C × 30 days, E1/ % 98.8 99.7 97.1 78.5 77.4
200 DEG C × 30 days, E2/ % 92.1 93.2 94.7 87.4 77.6
250 DEG C × 20 days, E1/ % 94.1 95.2 91.4 70.4 70.9
250 DEG C × 20 days, E2/ % 90.4 89.4 91.4 68.7 65.9
There are the above results to can be seen that after modified alta-mud cross-link low-density polyethylene, add a small amount of inorganic nano oxidation Magnesium forms active component, then further advantageously reduces the density of insulating materials with other components mixed-forming, improves insulation The heat resistance and intensity of material, the ageing time of insulating materials is reduced, can kept under high temperature action for a long time（200℃×30 My god, 250 DEG C × 20 days）It is non-degradable.
The foregoing is only a specific embodiment of the invention, but protection scope of the present invention is not limited thereto, any Those skilled in the art disclosed herein technical scope in, can without the change that creative work is expected or Replace, should all be included within the scope of the present invention.Therefore, protection scope of the present invention should be limited with claims Fixed protection domain is defined.

Claims (6)

1. a kind of preparation method of cable insulation material, it is characterised in that the cable insulation material includes nano magnesia/low Density polyethylene/modified alta-mud about 10-20 parts, phenolic resin 80-100 parts, carbonitride 10-20 parts, polystyrene 20-30 Part, epoxy resin 30-40 parts, antioxidant 5-8 parts, plasticizer 5-10 parts, glass fibre 10-15 parts, neoprene 20-30 parts and Polyvinyl chloride 20-30 parts；Insulating materials is specifically prepared in accordance with the following steps, and the weight average molecular weight of its epoxy resin is 9000：
（1）Modified alta-mud：By after low-kappa number by polyimide grafted modification；
（2）Prepare low density polyethylene (LDPE)/modified alta-mud nano composite material：Using high shear type double screw extruder, stirring Modified bentonite is well mixed with low density polyethylene (LDPE) under the conditions of mixing, with twin-screw extrusion mixed material, is granulated, shaping；
（3）Low density polyethylene (LDPE)/modified alta-mud nano composite material and nano magnesia are mixed, it is nano oxidized so as to be made Magnesium particle/low density polyethylene (LDPE)/modified alta-mud nano composite material；
（4）The each component of above-mentioned insulating materials is mixed, homogenizer is poured into and stirs, be then discharged out, melts, is molded into Type, obtain the cable insulation material；
The step of modified alta-mud is that bentonite original ore soil is added in 150mL distilled water, 10~30min of ultrasonic disperse The large particulate matter except beaker bottom is filtered off afterwards, is centrifuged, is dried, and is ground, roasting；Baked bentonite is placed in into concentration is React 1~2h in 1~5mol/L acetum after ultrasonic disperse at 80 DEG C~90 DEG C, finally filter, wash up to neutral, Drying, is added in toluene ultrasonic disperse about 15~20min under nitrogen protection by the bentonite of acidifying, then rises to temperature Be added to after 110~120 DEG C in the aqueous solution of polyethyleneimine, after ultrasonic 20-30min is scattered at 80~100 DEG C reaction 5~ 6h, then filter, washed with distilled water and absolute ethyl alcohol, being dried in vacuo 10~12h at 60~80 DEG C, obtaining modified alta-mud, Wherein modified alta-mud particle diameter is 0.5-0.8mm；
Step（3）It is that low density polyethylene (LDPE)/modified alta-mud nano composite material is dissolved in toluene solution, then by nano oxygen Change magnesium particle to be added in above-mentioned solution, temperature is kept for 80-120 DEG C, 2h, ultrasonic disperse 2h is stirred, then by the mixing of preparation Liquid is placed in desolventizing in baking oven；Wherein nano magnesia accounts for low density polyethylene (LDPE)/modified alta-mud nano composite material quality hundred It is 0.5-2% to divide ratio.
2. preparation method as claimed in claim 1, it is characterised in that the plasticizer is acetyl tributyl citrate.
3. preparation method as claimed in claim 1 or 2, it is characterised in that the particle diameter of the nano magnesia is 30-100nm.
4. preparation method as claimed in claim 1 or 2, it is characterised in that the mass ratio of low density polyethylene (LDPE)/modified alta-mud For 10-20：2-10.
5. preparation method as claimed in claim 1, it is characterised in that the step（4）In stir, be at room temperature first Stirred 30 minutes using 1000 revs/min of speed, then stir 30min segmentation with 3000 revs/min of speed at 60 DEG C Whipping process.
6. preparation method as claimed in claim 1, it is characterised in that the melting temperature is 200-280 DEG C, described to be molded into Type temperature is 120-150 DEG C.
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