CN107286455A - A kind of preparation method of middle-high voltage power cable shield semiconductors layer sizing - Google Patents

A kind of preparation method of middle-high voltage power cable shield semiconductors layer sizing Download PDF

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CN107286455A
CN107286455A CN201710590576.1A CN201710590576A CN107286455A CN 107286455 A CN107286455 A CN 107286455A CN 201710590576 A CN201710590576 A CN 201710590576A CN 107286455 A CN107286455 A CN 107286455A
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attapulgite
added
high voltage
voltage power
power cable
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魏善恒
何立群
肖本国
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Anhui Guodian Cable Group Co Ltd
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Anhui Guodian Cable Group Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
    • C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L23/04—Homopolymers or copolymers of ethene
    • C08L23/08—Copolymers of ethene
    • C08L23/0846—Copolymers of ethene with unsaturated hydrocarbons containing other atoms than carbon or hydrogen atoms
    • C08L23/0853—Vinylacetate
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00—Mixing; Kneading
    • B29B7/002—Methods
    • B29B7/005—Methods for mixing in batches
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00—Mixing; Kneading
    • B29B7/002—Methods
    • B29B7/007—Methods for continuous mixing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C43/00—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor
    • B29C43/32—Component parts, details or accessories; Auxiliary operations
    • B29C43/58—Measuring, controlling or regulating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C43/00—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor
    • B29C43/32—Component parts, details or accessories; Auxiliary operations
    • B29C43/58—Measuring, controlling or regulating
    • B29C2043/5808—Measuring, controlling or regulating pressure or compressing force
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C43/00—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor
    • B29C43/32—Component parts, details or accessories; Auxiliary operations
    • B29C43/58—Measuring, controlling or regulating
    • B29C2043/5816—Measuring, controlling or regulating temperature
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/001—Conductive additives
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B9/00—Power cables
    • H01B9/02—Power cables with screens or conductive layers, e.g. for avoiding large potential gradients
    • H01B9/021—Features relating to screening tape per se
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B9/00—Power cables
    • H01B9/02—Power cables with screens or conductive layers, e.g. for avoiding large potential gradients
    • H01B9/027—Power cables with screens or conductive layers, e.g. for avoiding large potential gradients composed of semi-conducting layers

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
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  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Thermistors And Varistors (AREA)

Abstract

The invention discloses a kind of preparation method of middle-high voltage power cable with shield semiconductors layer sizing, base-material of the present invention is to replace EVA using part CSM rubber, halogen is introduced in semi-conductive screen sizing material, so as to improve the electric conductivity of semi-conductive screen sizing material, the present invention uses doped carbon nanometer pipe and tin indium oxide composite conducting attapulgite as the conductive filler of alternative carbon black, on the one hand its high conductivity can reduce the specific insulation of EVA/CSM semi-conductive screen composites, on the other hand its special conductive network formed in macromolecule matrix is more difficult destroyed in thermal expansion process, this conductive network more stablized causes stability enhancing of the specific insulation of EVA/CSM semi-conductive screen composites under alternating temperature, it substantially prolongs the service life of middle-high voltage power cable.

Description

A kind of preparation method of middle-high voltage power cable shield semiconductors layer sizing
Technical field
The present invention relates to a kind of preparation method of middle-high voltage power cable with shield semiconductors layer sizing, belong to macromolecule material Expect technical field.
Background technology
General power cable is made up of copper or the stranded conductor wire core of aluminium single line, insulating barrier and restrictive coating.For 6KV And for above middle-high voltage power cable, because outside applies, voltage is higher, and the electric field stress that insulating barrier is born is big, along insulating barrier The Electric Field Distribution of inwall is uneven, is also easy to produce corona discharge, causes insulating barrier to puncture.In order to avoid cable internal electric field stress concentration With protection insulating barrier, it is desirable to conductor wire core and insulating barrier and between insulating barrier and restrictive coating respectively plus one layer of semi-conductive screen Layer, its main function insulating surface electric field stress is evenly distributed, and improves cable internal electric field radial distribution, prevents shelf depreciation, Electric-field intensity is reduced, so as to improve the electrical strength of cable, conductor wire core and the air gap on insulating barrier interface is reduced, improves electricity Cable originates corona voltage and the resistance to free discharge performance of cable, and reduction insulating barrier heating to a certain extent, protection insulation Layer, extends the service life of cable.
Semiconductive shielding layer is the important component of middle-high voltage power cable structure, can make the electric field point inside cable Cloth is more uniform, reduces the destruction that stress concentration is caused for cable insulation.The quality of semi-conductive screen layer sizing is to cable Use safety and service life play vital effect.The electric conductivity and volume of composite used in semiconductive shielding layer Resistivity must keep preferable stability at different temperatures and during being used for a long time.But current semiconductive shielding layer glue Material is more using carbon black as the polymer composites of conductive filler, and when temperature is reached near fusing point, carbon black particle can be in polymer Rearrangement occurs in matrix causes conductive network to change, so as to cause composite volume resistivity to become big, locally puts The decline of electricity and dielectric properties directly influences service life during power cable operation.
The content of the invention
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to provide a kind of middle-high voltage power cable semi-conductive shield glue The preparation method of material, semi-conductive screen sizing material produced by the present invention has the advantages that specific insulation is low and excellent in stability.
To achieve the above object, the present invention is adopted the following technical scheme that：
A kind of middle-high voltage power cable preparation method of shield semiconductors layer sizing, comprises the following steps：
（1）According to mass ratio 8-10:6-9:2-4:1-2:0.5-1:0.3-0.6 weigh base-material, conductive attapulgite, plasticizer, Vulcanizing agent, lubricant and processing aid；
（2）Base-material is added in banbury, 30-50s is kneaded at 70-80 DEG C, conductive attapulgite total amount is sequentially added 1/3-1/2, lubricant and processing aid, 60-120s is kneaded at 80-90 DEG C, sequentially adds remaining conductive attapulgite and increasing Agent is moulded, 40-60s is kneaded at 90-100 DEG C, is eventually adding vulcanizing agent, 20-40s is kneaded at 75-85 DEG C, treat that temperature is down to Dumping at 40-50 DEG C；
（3）Mill roll spacing is adjusted to 1-2mm, input sizing material is thin logical, beats triangle bag, thin logical 3-5 times, and roll spacing is adjusted to 3- 4mm, puts into sizing material bag roller, treats the smooth bubble-free in surface, bottom sheet；
（4）By step（3）Be made elastomeric compound first temperature be 160-190 DEG C, pressure be hot pressing 10- under conditions of 10-15MPa 15min, then temperature be 10-15 DEG C, pressure be to be cold-pressed 5-10min under conditions of 20-25MPa, that is, mesohigh electric power electricity is made Cable shield semiconductors layer sizing.
The base-material is by Bayer Bitterfeld GmbH EVA 456 and repaiies remote chemical industry CSM3550 according to mass ratio 7-9:1-3 mixing compositions.
The preparation method of the conductive attapulgite is as follows：
（1）Attapulgite is calcined into 2-3h at 380-440 DEG C, is cooled to after room temperature according to solid-to-liquid ratio 1:15-20 is added to matter Fraction is measured in 15% hydrochloric acid solution, heating water bath soaks 1-2h to 50-60 DEG C, and filtering is washed with distilled water to neutrality, dried 1-2h is calcined at 450-500 DEG C after dry, room temperature is cooled to；
（2）According to solid-to-liquid ratio 1:20-30 is by step（1）The attapulgite of processing is added in distilled water, is added equivalent to bumps Rod soil property amount 2-4% PVP K-30, stirs 30-40min, the ultrasonic disperse 20- under 200-250W power 30min, obtains attapulgite suspension；
（3）By indium metal and metallic tin In in mass ratio2O3:SnO2=9:1 mixing, then according to solid-to-liquid ratio 1:6-8 will mix gold Category is added in the hydrochloric acid solution that mass fraction is 40%, and heating water bath stirs 20-30min, obtain indium pink salt molten to 60-70 DEG C Liquid；
（4）By step（3）Obtained solution is added to step（2）In obtained attapulgite suspension, 20-30min is stirred, so Add the sodium hydroxide solution that mass fraction is 25% under agitation afterwards, when system pH=7-8, stop addition sodium hydroxide molten Liquid, filtering, is washed with distilled water to no Cl-, after drying under an argon atmosphere in oil bath heat, temperature be 280-320 DEG C, Pressure is temperature-resistant under conditions of 1.5-2MPa, to heat 2-4h, pressure then being down into 0.8-1.2MPa, continues to heat 0.5-1.5h, naturally cools to room temperature, produces attapulgite/indium tin oxide composite；
（5）According to mass ratio 1:3-6 weighs CNT and attapulgite/indium tin oxide composite, described CNT It is less than 6nm for multi-walled carbon nanotube and caliber；
（6）According to solid-to-liquid ratio 1:CNT is added to by mass fraction the concentrated nitric acid and mass fraction that are 70% by 30-40 75% concentrated sulfuric acid is according to volume ratio 1:In the mixed acid solution that 2-4 is mixed, heating water bath stirs 4-6h to 60-70 DEG C, Take out according still further to solid-to-liquid ratio 1:The CNT of carboxylated is added in thionyl chloride by 20-30, heating water bath to 80-90 DEG C, 3-5h is stirred, the CNT of chloride is obtained；
（7）According to solid-to-liquid ratio 1:Attapulgite/indium tin oxide composite is added to 3- (2- aminoethylaminos) third by 8-10 In ylmethyl dimethoxysilane, heating water bath stirs 8-10h, obtains attapulgite/oxygen of Aminosilylation to 90-100 DEG C Change indium tin composite material；
（8）According to solid-to-liquid ratio 1:The CNT of chloride is added in tetrahydrofuran by 20-25, is stirred, then is added Enter attapulgite/indium tin oxide composite of Aminosilylation, the water after ultrasonic disperse 0.5-1h under 100-150W power Bath is heated to 70-80 DEG C, stirs 4-6h, and filtering, with water washing is distilled 2-3 times, is dried, obtains doped carbon nanometer pipe and indium oxide Tin composite conducting attapulgite, is required conductive attapulgite.
The plasticizer is dioctyl phthalate, diisobutyl phthalate, phthalic acid two（2- ethyl hexyls Base）One or more groups in ester, acetyl ricinoleic acid methoxyethyl ester, tetrahydrofurfuryl oleate, trichloroethyl phosphate Compound.
The vulcanizing agent is according to mass ratio 2.5-3.5 by peroxide and assistant crosslinking agent:1 mixes；The peroxide Compound is cumyl peroxide, dual-tert-butyl peroxy isopropyl base benzene, benzoyl peroxide, 2,5- dimethyl -2,5- two（Tertiary fourth Base peroxidating）Hexane, 4,4- bis-（Tert-butyl hydroperoxide）One kind in n-butyl pentanoate；The assistant crosslinking agent is that triallyl is different Cyanurate, TAC, trimethyol propane triacrylate, trihydroxy methyl propane trimethyl acrylate, Penylene BMI, dizinc acrylate resin, diformazan between ethylene glycol diacrylate, GDMA, N, N'- One kind in base zinc acrylate resin.
The lubricant is that chlorinated paraffin, microcrystalline wax, n-butyl stearate, 12- hydroxy lithium stearates, three stearic acid are sweet One or more compositions in grease, di-2-ethylhexylphosphine oxide stearamide, N- hydroxymethylstear amides, pentaerythritol monooleate.
The processing aid is according to mass ratio 1-2 by accelerator and age resistor:1 mixes；The accelerator is two Tetraethylthiuram sulfide, tetra-sulfurized pair pentamethylene thiuram, 4,4'- dithio morpholines, N, N'- di-o-tolyls thiocarbamide, 2- （4- morpholinodithios）One or more compositions in benzothiazole, N tert butyl benzothiazole 2 sulfenamide；It is described Age resistor is N, N'- bis-（Betanaphthyl）P-phenylenediamine, 3 methy 6 tert butyl phenol, N- cyclohexyl p-ethoxyaniline, three One or more compositions in nonylphenylphosphite, styrenated phenol.
Beneficial effects of the present invention：
（1）The present invention will be mixed by the indium tin-salt solution of raw material of indium metal and metallic tin with attapulgite suspension, with hydrogen-oxygen Change sodium is precipitating reagent, and tin indium oxide is coated on attapulgite by hydrothermal co-precipitation method；Finally CNT is entered respectively Row chloride is handled, and Aminosilylation processing is carried out to attapulgite/indium tin oxide composite；The work being bonded by amido link It is coated on by CNT in attapulgite/indium tin oxide composite, makes obtained attapulgite that there is two layers of clad, One layer is tin indium oxide internal coating, and another layer is nano-sized carbon external coating, and modified attapulgite not only has excellent Electric conductivity, also has the advantages that high mechanical strength, heat endurance be good, chemical stability is good；
（2）Base-material of the present invention is to replace EVA using part CSM rubber, and halogen is introduced in semi-conductive screen sizing material, so that The electric conductivity of semi-conductive screen sizing material is improved, the present invention is made using doped carbon nanometer pipe and tin indium oxide composite conducting attapulgite For the conductive filler of alternative carbon black, its high conductivity of one side can reduce the volume of EVA/CSM semi-conductive screen composites Resistivity, on the other hand its special conductive network for being formed in macromolecule matrix is more difficult in thermal expansion process is broken Bad, this conductive network more stablized causes the specific insulation of EVA/CSM semi-conductive screen composites under alternating temperature Stability strengthens, and substantially prolongs the service life of middle-high voltage power cable.
Embodiment
Embodiment 1
A kind of middle-high voltage power cable preparation method of shield semiconductors layer sizing, comprises the following steps：
（1）According to mass ratio 8:6:2:1:0.5:0.3 weigh base-material, conductive attapulgite, plasticizer, vulcanizing agent, lubricant and Processing aid；
（2）Base-material is added in banbury, 50s is kneaded at 70 DEG C, the 1/3 of conductive attapulgite total amount is sequentially added, moistens Lubrication prescription and processing aid, 120s is kneaded at 80 DEG C, is sequentially added remaining conductive attapulgite and plasticizer, is kneaded at 90 DEG C 60s, is eventually adding vulcanizing agent, and 40s is kneaded at 75 DEG C, dumping when temperature is down to 40 DEG C；
（3）Mill roll spacing is adjusted to 1mm, input sizing material is thin logical, beat triangle bag, it is thin logical 3 times, roll spacing is adjusted to 3mm, thrown Enter sizing material bag roller, treat the smooth bubble-free in surface, bottom sheet；
（4）By step（3）Be made elastomeric compound first temperature be 160 DEG C, pressure be hot pressing 15min under conditions of 10MPa, then in temperature Degree is 10 DEG C, pressure is to be cold-pressed 5min under conditions of 20MPa, that is, middle-high voltage power cable shield semiconductors layer sizing is made.
The base-material is by Bayer Bitterfeld GmbH EVA 456 and repaiies remote chemical industry CSM3550 according to mass ratio 7:3 mixing compositions.
The preparation method of the conductive attapulgite is as follows：
（1）Attapulgite is calcined into 3h at 380 DEG C, is cooled to after room temperature according to solid-to-liquid ratio 1:15, which are added to mass fraction, is In 15% hydrochloric acid solution, heating water bath soaks 2h to 50 DEG C, and filtering is washed with distilled water to neutrality, after drying at 450 DEG C 2h is calcined, room temperature is cooled to；
（2）According to solid-to-liquid ratio 1:20 by step（1）The attapulgite of processing is added in distilled water, is added equivalent to attapulgite The PVP K-30 of quality 2%, stirs 30min, the ultrasonic disperse 30min under 200W power, obtains attapulgite and hangs Supernatant liquid；
（3）By indium metal and metallic tin In in mass ratio2O3:SnO2=9:1 mixing, then according to solid-to-liquid ratio 1:6 by hybrid metal It is added in the hydrochloric acid solution that mass fraction is 40%, heating water bath stirs 30min, obtain indium tin-salt solution to 60 DEG C；
（4）By step（3）Obtained solution is added to step（2）In obtained attapulgite suspension, 20min is stirred, then The sodium hydroxide solution that mass fraction is 25% is added under agitation, when system pH=7, stops adding sodium hydroxide solution, mistake Filter, is washed with distilled water to no Cl-, heated under an argon atmosphere in oil bath after drying, temperature be 280 DEG C, pressure be Under conditions of 1.5MPa, 4h is heated, pressure is then down to 0.8MPa, it is temperature-resistant, continue to heat 1.5h, naturally cool to room Temperature, produces attapulgite/indium tin oxide composite；
（5）According to mass ratio 1:3 weigh CNT and attapulgite/indium tin oxide composite, and described CNT is Multi-walled carbon nanotube and caliber are less than 6nm；
（6）According to solid-to-liquid ratio 1:30 CNT is added to by mass fraction into the concentrated nitric acid and mass fraction that are 70% is 75% The concentrated sulfuric acid is according to volume ratio 1:In 2 mixed acid solutions mixed, heating water bath stirs 6h to 60 DEG C, takes out according still further to solid Liquor ratio 1:20 are added to the CNT of carboxylated in thionyl chloride, and heating water bath stirs 5h, obtain chloride to 80 DEG C CNT；
（7）According to solid-to-liquid ratio 1:Attapulgite/indium tin oxide composite is added to 3- (2- aminoethylaminos) propyl group first by 8 In base dimethoxysilane, heating water bath stirs 10h to 90 DEG C, and the attapulgite/tin indium oxide for obtaining Aminosilylation is combined Material；
（8）According to solid-to-liquid ratio 1:20 are added to the CNT of chloride in tetrahydrofuran, stir, add ammonia Attapulgite/indium tin oxide composite of base silane, under 100W power after ultrasonic disperse 1h heating water bath to 70 DEG C, 6h is stirred, filtering, with water washing is distilled 2 times, is dried, obtains doped carbon nanometer pipe and tin indium oxide composite conducting attapulgite, As required conductive attapulgite.
The plasticizer is phthalic acid two（2- ethylhexyls）Ester.
The vulcanizing agent is according to mass ratio 2.5 by peroxide and assistant crosslinking agent:1 mixes；The peroxide For dual-tert-butyl peroxy isopropyl base benzene；The assistant crosslinking agent is trihydroxy methyl propane trimethyl acrylate.
The lubricant is chlorinated paraffin, two kinds of compositions of N- hydroxymethylstear amides, and chlorinated paraffin, N- methylols are hard The mass ratio of acyl amine between the two is 2:1.
The processing aid is according to mass ratio 1 by accelerator and age resistor:1 mixes；The accelerator is four sulphur Change double pentamethylene thiurams, N, two kinds of compositions of N'- di-o-tolyl thiocarbamides, tetra-sulfurized pair pentamethylene thiuram, N, the adjacent first of N'- bis- The mass ratio of phenylthiourea between the two is 3:1；The age resistor is N, N'- bis-（Betanaphthyl）P-phenylenediamine, 3- methyl -6- Two kinds of compositions of tert-butyl phenol, N, N'- bis-（Betanaphthyl）P-phenylenediamine, 3 methy 6 tert butyl phenol are between the two Mass ratio is 1:1.
Embodiment 2
A kind of middle-high voltage power cable preparation method of shield semiconductors layer sizing, comprises the following steps：
（1）According to mass ratio 9:7:3:1.5:0.8:0.4 weighs base-material, conductive attapulgite, plasticizer, vulcanizing agent, lubricant And processing aid；
（2）Base-material is added in banbury, 40s is kneaded at 75 DEG C, the 1/3 of conductive attapulgite total amount is sequentially added, moistens Lubrication prescription and processing aid, 90s is kneaded at 85 DEG C, is sequentially added remaining conductive attapulgite and plasticizer, is kneaded at 950 DEG C 50s, is eventually adding vulcanizing agent, and 30s is kneaded at 80 DEG C, dumping when temperature is down to 45 DEG C；
（3）Mill roll spacing is adjusted to 1.5mm, input sizing material is thin logical, beats triangle bag, it is thin to lead to 4 times, by roll spacing adjust to 3.5mm, puts into sizing material bag roller, treats the smooth bubble-free in surface, bottom sheet；
（4）By step（3）Be made elastomeric compound first temperature be 175 DEG C, pressure be hot pressing 12min under conditions of 12MPa, then in temperature Degree is 12 DEG C, pressure is to be cold-pressed 8min under conditions of 22MPa, that is, middle-high voltage power cable shield semiconductors layer sizing is made.
The base-material is by Bayer Bitterfeld GmbH EVA 456 and repaiies remote chemical industry CSM3550 according to mass ratio 8:2 mixing compositions.
The preparation method of the conductive attapulgite is as follows：
（1）Attapulgite is calcined into 2.5h at 410 DEG C, is cooled to after room temperature according to solid-to-liquid ratio 1:18, which are added to mass fraction, is In 15% hydrochloric acid solution, heating water bath soaks 1.5h to 55 DEG C, and filtering is washed with distilled water to neutrality, at 480 DEG C after drying Lower calcining 1.5h, is cooled to room temperature；
（2）According to solid-to-liquid ratio 1:25 by step（1）The attapulgite of processing is added in distilled water, is added equivalent to attapulgite The PVP K-30 of quality 3%, stirs 35min, the ultrasonic disperse 25min under 220W power, obtains attapulgite and hangs Supernatant liquid；
（3）By indium metal and metallic tin In in mass ratio2O3:SnO2=9:1 mixing, then according to solid-to-liquid ratio 1:7 by hybrid metal It is added in the hydrochloric acid solution that mass fraction is 40%, heating water bath stirs 25min, obtain indium tin-salt solution to 65 DEG C；
（4）By step（3）Obtained solution is added to step（2）In obtained attapulgite suspension, 25min is stirred, then The sodium hydroxide solution that mass fraction is 25% is added under agitation, when system pH=7.5, stops adding sodium hydroxide solution, Filtering, is washed with distilled water to no Cl-, heated under an argon atmosphere in oil bath after drying, temperature be 300 DEG C, pressure be Under conditions of 1.8MPa, 3h is heated, pressure is then down to 1MPa, it is temperature-resistant, continue to heat 1h, naturally cool to room temperature, Produce attapulgite/indium tin oxide composite；
（5）According to mass ratio 1:4 weigh CNT and attapulgite/indium tin oxide composite, and described CNT is Multi-walled carbon nanotube and caliber are less than 6nm；
（6）According to solid-to-liquid ratio 1:35 CNT is added to by mass fraction into the concentrated nitric acid and mass fraction that are 70% is 75% The concentrated sulfuric acid is according to volume ratio 1:In 3 mixed acid solutions mixed, heating water bath stirs 5h to 65 DEG C, takes out according still further to solid Liquor ratio 1:25 are added to the CNT of carboxylated in thionyl chloride, and heating water bath stirs 4h, obtain chloride to 85 DEG C CNT；
（7）According to solid-to-liquid ratio 1:Attapulgite/indium tin oxide composite is added to 3- (2- aminoethylaminos) propyl group first by 9 In base dimethoxysilane, heating water bath stirs 9h to 95 DEG C, and the attapulgite/tin indium oxide for obtaining Aminosilylation is combined Material；
（8）According to solid-to-liquid ratio 1:22 are added to the CNT of chloride in tetrahydrofuran, stir, add ammonia Attapulgite/indium tin oxide composite of base silane, under 120W power after ultrasonic disperse 1h heating water bath to 75 DEG C, 5h is stirred, filtering, with water washing is distilled 2 times, is dried, obtains doped carbon nanometer pipe and tin indium oxide composite conducting attapulgite, As required conductive attapulgite.
The plasticizer is dioctyl phthalate, two kinds of compositions of acetyl ricinoleic acid methoxyethyl ester, adjacent benzene The mass ratio of diformazan dioctyl phthalate, acetyl ricinoleic acid methoxyethyl ester between the two is 4:1.
The vulcanizing agent is according to mass ratio 3 by peroxide and assistant crosslinking agent:1 mixes；The peroxide is 2,5- dimethyl -2,5- two（Tert-butyl hydroperoxide）Hexane；The assistant crosslinking agent is penylene BMI between N, N'-.
The lubricant is microcrystalline wax, two kinds of compositions of pentaerythritol monooleate, microcrystalline wax, pentaerythrite list The mass ratio of oleate between the two is 2:1.
The processing aid is according to mass ratio 1.5 by accelerator and age resistor:1 mixes；The accelerator is 4, 4'- dithio morpholines, 2-（4- morpholinodithios）Three kinds of benzothiazole, N tert butyl benzothiazole 2 sulfenamide Composition, 4,4'- dithio morpholines, 2-（4- morpholinodithios）Benzothiazole, the N- tert-butyl groups -2-[4-morpholinodithio time sulphonyl Mass ratio between amine three is 3:2:1；The age resistor is N, N'- bis-（Betanaphthyl）P-phenylenediamine, three nonyl phenyl phosphorous Two kinds of compositions of acid esters, N, N'- bis-（Betanaphthyl）The mass ratio of p-phenylenediamine, trisnonylphenyl phosphite between the two For 3:1.
Embodiment 3
A kind of middle-high voltage power cable preparation method of shield semiconductors layer sizing, comprises the following steps：
（1）According to mass ratio 10:9:4:2:1:0.6 weighs base-material, conductive attapulgite, plasticizer, vulcanizing agent, lubricant and adds Work auxiliary agent；
（2）Base-material is added in banbury, 30s is kneaded at 80 DEG C, the 1/2 of conductive attapulgite total amount is sequentially added, moistens Lubrication prescription and processing aid, 60s is kneaded at 90 DEG C, is sequentially added remaining conductive attapulgite and plasticizer, is kneaded at 100 DEG C 40s, is eventually adding vulcanizing agent, and 20s is kneaded at 85 DEG C, dumping when temperature is down to 50 DEG C；
（3）Mill roll spacing is adjusted to 2mm, input sizing material is thin logical, beat triangle bag, it is thin logical 5 times, roll spacing is adjusted to 4mm, thrown Enter sizing material bag roller, treat the smooth bubble-free in surface, bottom sheet；
（4）By step（3）Be made elastomeric compound first temperature be 190 DEG C, pressure be hot pressing 10min under conditions of 15MPa, then in temperature Degree is 15 DEG C, pressure is to be cold-pressed 5min under conditions of 25MPa, that is, middle-high voltage power cable shield semiconductors layer sizing is made.
The base-material is by Bayer Bitterfeld GmbH EVA 456 and repaiies remote chemical industry CSM3550 according to mass ratio 9:1 mixing composition.
The preparation method of the conductive attapulgite is as follows：
（1）Attapulgite is calcined into 2h at 440 DEG C, is cooled to after room temperature according to solid-to-liquid ratio 1:20, which are added to mass fraction, is In 15% hydrochloric acid solution, heating water bath soaks 1h to 60 DEG C, and filtering is washed with distilled water to neutrality, after drying at 500 DEG C 1h is calcined, room temperature is cooled to；
（2）According to solid-to-liquid ratio 1:30 by step（1）The attapulgite of processing is added in distilled water, is added equivalent to attapulgite The PVP K-30 of quality 4%, stirs 40min, the ultrasonic disperse 20min under 250W power, obtains attapulgite and hangs Supernatant liquid；
（3）By indium metal and metallic tin In in mass ratio2O3:SnO2=9:1 mixing, then according to solid-to-liquid ratio 1:8 by hybrid metal It is added in the hydrochloric acid solution that mass fraction is 40%, heating water bath stirs 30min, obtain indium tin-salt solution to 70 DEG C；
（4）By step（3）Obtained solution is added to step（2）In obtained attapulgite suspension, 30min is stirred, then The sodium hydroxide solution that mass fraction is 25% is added under agitation, when system pH=8, stops adding sodium hydroxide solution, mistake Filter, is washed with distilled water to no Cl-, heated under an argon atmosphere in oil bath after drying, temperature be 320 DEG C, pressure be Under conditions of 2MPa, 2h is heated, pressure is then down to 1.2MPa, it is temperature-resistant, continue to heat 0.5h, naturally cool to room Temperature, produces attapulgite/indium tin oxide composite；
（5）According to mass ratio 1:6 weigh CNT and attapulgite/indium tin oxide composite, and described CNT is Multi-walled carbon nanotube and caliber are less than 6nm；
（6）According to solid-to-liquid ratio 1:40 CNT is added to by mass fraction into the concentrated nitric acid and mass fraction that are 70% is 75% The concentrated sulfuric acid is according to volume ratio 1:In 4 mixed acid solutions mixed, heating water bath stirs 4h to 70 DEG C, takes out according still further to solid Liquor ratio 1:30 are added to the CNT of carboxylated in thionyl chloride, and heating water bath stirs 3h, obtain chloride to 90 DEG C CNT；
（7）According to solid-to-liquid ratio 1:Attapulgite/indium tin oxide composite is added to 3- (2- aminoethylaminos) propyl group by 10 In methyl dimethoxysilane, heating water bath stirs 8h to 100 DEG C, and the attapulgite/tin indium oxide for obtaining Aminosilylation is multiple Condensation material；
（8）According to solid-to-liquid ratio 1:25 are added to the CNT of chloride in tetrahydrofuran, stir, add ammonia Attapulgite/indium tin oxide composite of base silane, under 150W power after ultrasonic disperse 0.5h heating water bath to 80 DEG C, 4h is stirred, filtering, with water washing is distilled 3 times, is dried, obtains doped carbon nanometer pipe and tin indium oxide composite conducting concave convex rod Soil, is required conductive attapulgite.
The plasticizer is phthalic acid two（2- ethylhexyls）Ester, tetrahydrofurfuryl oleate, trichloroethyl phosphoric acid Three kinds of compositions of ester, phthalic acid two（2- ethylhexyls）Ester, tetrahydrofurfuryl oleate, the three of trichloroethyl phosphate It is 5 to plant the mass ratio between composition three:3:1.
The vulcanizing agent is according to mass ratio 3.5 by peroxide and assistant crosslinking agent:1 mixes；The peroxide For 4,4- bis-（Tert-butyl hydroperoxide）In n-butyl pentanoate；The assistant crosslinking agent is zinc dimethacrylate.
The lubricant is glyceryl tristearate, two kinds of compositions of di-2-ethylhexylphosphine oxide stearamide, three glycerol stearates Ester, the mass ratio of di-2-ethylhexylphosphine oxide stearamide between the two are 4:1.
The processing aid is according to mass ratio 2 by accelerator and age resistor:1 mixes；The accelerator is two sulphur Change Thiuram, two kinds of compositions of N tert butyl benzothiazole 2 sulfenamide, tetraethylthiuram disulfide, N- The tert-butyl group-the mass ratio of 2-[4-morpholinodithio sulfenamide between the two is 1:1；The age resistor is N, N'- bis-（Betanaphthyl）It is right Three kinds of compositions in phenylenediamine, N- cyclohexyl p-ethoxyaniline, styrenated phenol, N, N'- bis-（Betanaphthyl）To benzene two Mass ratio between amine, N- cyclohexyl p-ethoxyaniline, styrenated phenol three is 4:2:1.

Claims (7)

1. a kind of middle-high voltage power cable preparation method of shield semiconductors layer sizing, it is characterised in that comprise the following steps：
According to mass ratio 8-10:6-9:2-4:1-2:0.5-1:0.3-0.6 weighs base-material, conductive attapulgite, plasticizer, vulcanization Agent, lubricant and processing aid；
Base-material is added in banbury, 30-50s is kneaded at 70-80 DEG C, the 1/3- of conductive attapulgite total amount is sequentially added 1/2nd, lubricant and processing aid, 60-120s is kneaded at 80-90 DEG C, sequentially adds remaining conductive attapulgite and plasticizer, 40-60s is kneaded at 90-100 DEG C, vulcanizing agent is eventually adding, 20-40s is kneaded at 75-85 DEG C, treats that temperature is down to 40-50 DEG C When dumping；
（3）Mill roll spacing is adjusted to 1-2mm, input sizing material is thin logical, beats triangle bag, thin logical 3-5 times, and roll spacing is adjusted to 3- 4mm, puts into sizing material bag roller, treats the smooth bubble-free in surface, bottom sheet；
（4）By step（3）Be made elastomeric compound first temperature be 160-190 DEG C, pressure be hot pressing 10- under conditions of 10-15MPa 15min, then temperature be 10-15 DEG C, pressure be to be cold-pressed 5-10min under conditions of 20-25MPa, that is, mesohigh electric power electricity is made Cable shield semiconductors layer sizing.
2. a kind of preparation method of middle-high voltage power cable shield semiconductors layer sizing according to claim 1, it is special Levy and be, the base-material is by Bayer Bitterfeld GmbH EVA 456 and repaiies remote chemical industry CSM3550 according to mass ratio 7-9:1-3 mixing compositions.
3. a kind of preparation method of middle-high voltage power cable shield semiconductors layer sizing according to claim 1, it is special Levy and be, the preparation method of the conductive attapulgite is as follows：
（1）Attapulgite is calcined into 2-3h at 380-440 DEG C, is cooled to after room temperature according to solid-to-liquid ratio 1:15-20 is added to matter Fraction is measured in 15% hydrochloric acid solution, heating water bath soaks 1-2h to 50-60 DEG C, and filtering is washed with distilled water to neutrality, dried 1-2h is calcined at 450-500 DEG C after dry, room temperature is cooled to；
（2）According to solid-to-liquid ratio 1:20-30 is by step（1）The attapulgite of processing is added in distilled water, is added equivalent to bumps Rod soil property amount 2-4% PVP K-30, stirs 30-40min, the ultrasonic disperse 20- under 200-250W power 30min, obtains attapulgite suspension；
By indium metal and metallic tin In in mass ratio2O3:SnO2=9:1 mixing, then according to solid-to-liquid ratio 1:6-8 adds hybrid metal Enter to mass fraction in 40% hydrochloric acid solution, heating water bath stirs 20-30min, obtain indium tin-salt solution to 60-70 DEG C；
（4）By step（3）Obtained solution is added to step（2）In obtained attapulgite suspension, 20-30min is stirred, so Add the sodium hydroxide solution that mass fraction is 25% under agitation afterwards, when system pH=7-8, stop addition sodium hydroxide molten Liquid, filtering, is washed with distilled water to no Cl-, after drying under an argon atmosphere in oil bath heat, temperature be 280-320 DEG C, Pressure is temperature-resistant under conditions of 1.5-2MPa, to heat 2-4h, pressure then being down into 0.8-1.2MPa, continues to heat 0.5-1.5h, naturally cools to room temperature, produces attapulgite/indium tin oxide composite；
（5）According to mass ratio 1:3-6 weighs CNT and attapulgite/indium tin oxide composite, described CNT It is less than 6nm for multi-walled carbon nanotube and caliber；
（6）According to solid-to-liquid ratio 1:CNT is added to by mass fraction the concentrated nitric acid and mass fraction that are 70% by 30-40 75% concentrated sulfuric acid is according to volume ratio 1:In the mixed acid solution that 2-4 is mixed, heating water bath stirs 4-6h to 60-70 DEG C, Take out according still further to solid-to-liquid ratio 1:The CNT of carboxylated is added in thionyl chloride by 20-30, heating water bath to 80-90 DEG C, 3-5h is stirred, the CNT of chloride is obtained；
（7）According to solid-to-liquid ratio 1:Attapulgite/indium tin oxide composite is added to 3- (2- aminoethylaminos) third by 8-10 In ylmethyl dimethoxysilane, heating water bath stirs 8-10h, obtains attapulgite/oxygen of Aminosilylation to 90-100 DEG C Change indium tin composite material；
（8）According to solid-to-liquid ratio 1:The CNT of chloride is added in tetrahydrofuran by 20-25, is stirred, then is added Enter attapulgite/indium tin oxide composite of Aminosilylation, the water after ultrasonic disperse 0.5-1h under 100-150W power Bath is heated to 70-80 DEG C, stirs 4-6h, and filtering, with water washing is distilled 2-3 times, is dried, obtains doped carbon nanometer pipe and indium oxide Tin composite conducting attapulgite, is required conductive attapulgite.
4. a kind of preparation method of middle-high voltage power cable shield semiconductors layer sizing according to claim 1, it is special Levy and be, the plasticizer is dioctyl phthalate, diisobutyl phthalate, phthalic acid two（2- ethyl hexyls Base）One or more groups in ester, acetyl ricinoleic acid methoxyethyl ester, tetrahydrofurfuryl oleate, trichloroethyl phosphate Compound.
5. a kind of preparation method of middle-high voltage power cable shield semiconductors layer sizing according to claim 1, it is special Levy and be, the vulcanizing agent is according to mass ratio 2.5-3.5 by peroxide and assistant crosslinking agent:1 mixes；The peroxidating Thing is cumyl peroxide, dual-tert-butyl peroxy isopropyl base benzene, benzoyl peroxide, 2,5- dimethyl -2,5- two（The tert-butyl group Peroxidating）Hexane, 4,4- bis-（Tert-butyl hydroperoxide）One kind in n-butyl pentanoate；The assistant crosslinking agent is triallyl isocyanide Urea acid esters, TAC, trimethyol propane triacrylate, trihydroxy methyl propane trimethyl acrylate, two Penylene BMI, dizinc acrylate resin, dimethyl between acrylic acid glycol ester, GDMA, N, N'- One kind in zinc acrylate resin.
6. a kind of preparation method of middle-high voltage power cable shield semiconductors layer sizing according to claim 1, it is special Levy and be, the lubricant is that chlorinated paraffin, microcrystalline wax, n-butyl stearate, 12- hydroxy lithium stearates, three stearic acid are sweet One or more compositions in grease, di-2-ethylhexylphosphine oxide stearamide, N- hydroxymethylstear amides, pentaerythritol monooleate.
7. a kind of preparation method of middle-high voltage power cable shield semiconductors layer sizing according to claim 1, it is special Levy and be, the processing aid is according to mass ratio 1-2 by accelerator and age resistor:1 mixes；The accelerator is two sulphur Change Thiuram, tetra-sulfurized pair pentamethylene thiuram, 4,4'- dithio morpholines, N, N'- di-o-tolyls thiocarbamide, 2-（4- Morpholinodithio）One or more compositions in benzothiazole, N tert butyl benzothiazole 2 sulfenamide；It is described anti- Old agent is N, N'- bis-（Betanaphthyl）P-phenylenediamine, 3 methy 6 tert butyl phenol, N- cyclohexyl p-ethoxyaniline, three nonyls One or more compositions in base phenyl phosphites, styrenated phenol.
CN201710590576.1A 2017-07-19 2017-07-19 A kind of preparation method of middle-high voltage power cable shield semiconductors layer sizing Pending CN107286455A (en)

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CN113539557A (en) * 2021-07-26 2021-10-22 安徽电缆股份有限公司 Anti-interference corrosion-resistant military invisible cable
CN115838511A (en) * 2023-02-23 2023-03-24 四川大学 High-voltage cable semi-conductive shielding material and preparation method thereof

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CN101544790A (en) * 2009-04-17 2009-09-30 安徽纵横高科电缆股份有限公司 125 DEG C resistance low smoke non-halogen rubber-sheathed cable shielding material
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CN113539557A (en) * 2021-07-26 2021-10-22 安徽电缆股份有限公司 Anti-interference corrosion-resistant military invisible cable
CN115838511A (en) * 2023-02-23 2023-03-24 四川大学 High-voltage cable semi-conductive shielding material and preparation method thereof

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Application publication date: 20171024