CN108017914A - A kind of silicon rubber based non-linear cable accessory material and preparation method thereof - Google Patents
A kind of silicon rubber based non-linear cable accessory material and preparation method thereof Download PDFInfo
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- CN108017914A CN108017914A CN201810019383.5A CN201810019383A CN108017914A CN 108017914 A CN108017914 A CN 108017914A CN 201810019383 A CN201810019383 A CN 201810019383A CN 108017914 A CN108017914 A CN 108017914A
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- 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
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- C08K3/24—Acids; Salts thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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Abstract
The invention belongs to direct current cables APPENDIX MATERIALSThe field, and in particular to a kind of silicon rubber based non-linear cable accessory material and preparation method thereof.The present invention passes through sol-gal process first, the CaCu 3 Ti 4 O particle of certain grain size is made after high-temperature calcination crystallization, ball milling, CaCu 3 Ti 4 O particle is dispersed in double-component liquid silicon rubber by in-situ polymerization again, then is molded through hot-press vulcanization and silicon rubber based non-linear cable accessory material is made.Cable accessory material prepared by the present invention has the non-linear and relatively stable dc breakdown electric field strength of excellent conductance, it can effectively improve the electrical conductivity gradients between different materials, increase the transport capacity of carrier, slacken cumulative effect of the space charge in interface, so as to fulfill internal field's distortion is eliminated, the internal electric field distribution of homogenizing cable accessory, strengthens annex insulation performance, failure occurrence probability is reduced, extends the service life of cable accessory.Preparation method technique of the present invention and required equipment are simple, of low cost, easily implement.
Description
Technical field
The invention belongs to direct current cables APPENDIX MATERIALSThe field, and in particular to a kind of silicon rubber based non-linear cable accessory material
And preparation method thereof.
Background technology
In recent years, since urbanization, modernization are constantly accelerated, urban population is continuously increased, power demand also with day
It is all to increase, and traditional overhead transmission line has been unable to meet the process of Modern Urban Planning.Direct current cables is because transmitted power is big, line
Path loss consumption is small and is widely adopted.But in direct current cables circuit, 70% failure all occurs in cable accessory.Cable is attached
Stress cone root in part is collectively formed by semiconductor stresses cone material, reinforced insulation material and cable major insulation material.Due to
The electrical conductivity of these three materials differs greatly, and is easily formed electrical conductivity gradients, and induces and internal field's distortion occurs, in addition, three
The interface of kind material can form space charge, aggravate electric field distortion degree.This electric field distortion can reduce the exhausted of APPENDIX MATERIALSThe
Edge performance, increases failure occurrence probability, accelerates the aging of cable accessory insulating materials, influences the service life of cable accessory.
Silicon rubber is a kind of high polymer for having and stablizing chemical constitution, because with good electrical insulating property, ageing resistance, temperature
Spend characteristic and mechanical performance and be widely used in direct current cables annex.Electrical conductivity is added in silicon rubber to rely on field strength
Property inorganic fill mutually non-linear dielectric materials can be made, its outstanding advantages can be voluntarily homogenized under uneven DC electric field
Electric field is distributed, therefore the Intelligent insulation material that is otherwise known as.
At present, when preparing non-linear cable APPENDIX MATERIALSThe, often the non-linear property of cable accessory conductivity of material is being improved
Cable accessory material breakdown intensity is reduced while energy, have impact on the overall performance of cable accessory material.
The content of the invention
To solve above-mentioned the deficiencies in the prior art, the present invention provides a kind of non-linear silicon rubber base cable accessory material and
Its preparation method.
A kind of preparation method step of silicon rubber based non-linear cable accessory material is as follows：
First, nitrate trihydrate copper and four water-calcium nitrate are weighed respectively by certain mol proportion and measures positive four butyl ester of metatitanic acid；Again
Ethylene glycol monomethyl ether and dust technology are measured according to the volume of positive four butyl ester of metatitanic acid respectively according to a certain volume；By ethylene glycol monomethyl ether, dilute
Nitric acid pours into beaker and stirs evenly successively, and nitrate trihydrate copper is added above-mentioned mixed solution and is completely dissolved it, then to mixed
Close in solution and add four water-calcium nitrate, four water-calcium nitrate is completely dissolved the mixed solution clarified；By the mixed of the clarification
Close solution to be cooled to room temperature and add positive four butyl ester of metatitanic acid thereto, lasting stirring makes positive four butyl ester of metatitanic acid be dispersed in mixing
In solution, CaCu 3 Ti 4 O sol solutions are made, the CaCu 3 Ti 4 O sol solutions lucifuge is stood；
2nd, step is positioned in constant temperature oven once the CaCu 3 Ti 4 O sol solutions that lucifuge is stood and is heat-treated, is made
Amorphous state CaCu 3 Ti 4 O gel；The amorphous state CaCu 3 Ti 4 O gel is put into Muffle furnace and is calcined, the copper titanate of crystallization is made
Calcium；The CaCu 3 Ti 4 O of the crystallization is put into ball milling instrument, and the titanium of alcohol and ball milling pearl to the crystallization is added into ball milling instrument
Sour copper calcium carries out wet-milling, and the mixing liquid obtained by wet-milling certain time is put into constant temperature oven and is heat-treated, and crystallization is made
CaCu 3 Ti 4 O particle；
3rd, A, the B two-component liquid silastic for measuring equal volume respectively are poured into different beakers, accurately weigh two parts together
The step of etc. quality two made crystallization CaCu 3 Ti 4 O particle and be added separately in A, B two-component liquid silastic, at room temperature
Lasting stirring makes CaCu 3 Ti 4 O even particulate dispersion in liquid silastic respectively, then A, B two-component liquid silastic are mixed
Together and continue to stir certain time, the volume ratio content that CaCu 3 Ti 4 O particle is made is the uniformly mixed of 1-10vol.%
Liquid adulterates silicon rubber；
4th, the made liquid doping silicon rubber of step 3 is placed under vacuum condition and certain time is stirred at room temperature, then fallen
Enter in mould and be placed in vacuum drying oven and carry out vacuumize process at room temperature；
5th, the mould equipped with liquid doping silicon rubber of evacuated processing is taken out from vacuum drying oven, above and below mould
Two sides is with Interal fixation and is put into compression molding instrument and carries out high temperature vulcanized forming processes, and the silicon rubber base that sulfidization molding is made is non-
Linear cable APPENDIX MATERIALSThe；The silicon rubber based non-linear cable accessory material of the sulfidization molding is removed from the molds and is put into
Post-cure processing is carried out in constant temperature oven, it is more non-than the silicon rubber base that content is 1-10vol.% that CaCu 3 Ti 4 O particle volume is made
Linear cable APPENDIX MATERIALSThe finished product.
Further, molar ratio described in step 1 is：Nitrate trihydrate copper:Four water-calcium nitrate:Positive four butyl ester=1 of metatitanic acid:3:
4, the volume ratio is positive four butyl ester of metatitanic acid:Ethylene glycol monomethyl ether:Dust technology=100:400:1；The lasting stirring is with 100-
The speed of agitator stirring 40min of 300r/min；It is that lucifuge stands 12-36h at room temperature that the lucifuge, which is stood,.
Further, the temperature that CaCu 3 Ti 4 O sol solutions described in step 2 are heat-treated is 80 DEG C, processing time 8-12h；
The Muffle furnace calcine technology is that temperature is risen to 300 DEG C with the speed of 5 DEG C/min, and temperature keeps the temperature 1-2h after reaching 300 DEG C, then
Temperature is risen to 1050 DEG C by 300 DEG C with the speed of 5 DEG C/min, temperature keeps the temperature 1-8h after reaching 1050 DEG C.
Further, the rotating speed of ball milling instrument described in step 2 is 580r/min, and the wet-milling time is 8-12h；The ball
The heat treatment temperature of gained mixing liquid is 80 DEG C after mill, processing time 4-6h.
Further, the particle diameter of the CaCu 3 Ti 4 O particle of crystallization made from step 2 is 300-500nm.
Further, A, B two-component liquid silastic described in step 3 are the model of German Wacker Chemical Co., Ltd's productionDual composition addition type liquid silastic.
Further, persistently A is stirred respectively at room temperature described in step 3, the speed of agitator of B two-component liquid silastic is
100-300r/min, mixing time 60min, continue the rotating speed of stirring after A, B two-component liquid silastic are mixed
For 100-300r/min, mixing time 30min.
Further, the rotating speed that liquid doping silicon rubber described in step 4 is stirred at room temperature under vacuum is 100-
300r/min, mixing time 60min；The die size is 100 × 100 × 0.2mm；The vacuumize process time is
30min。
Further, plate size described in step 5 is 250 × 176 × 8mm, is vulcanized in the high temperature vulcanized moulding process
Temperature is 120-150 DEG C, vulcanization time 10-15min, and hot pressing pressure is 10-15MPa, and the post-cure treatment temperature is
200 DEG C, processing time 4h.
A kind of silicon rubber based non-linear made from preparation method based on above-mentioned silicon rubber based non-linear cable accessory material
Cable accessory material, CaCu 3 Ti 4 O particle volume is 1- than content in the silicon rubber based non-linear cable accessory material
10vol.%, the particle diameter of the CaCu 3 Ti 4 O particle is 300-500nm.
By regulating and controlling to fill the pattern of phase the CaCu 3 Ti 4 O particle of even particle size has been made, by it with low in the present invention
Filling content adds liquid silastic and prepares silicon rubber based non-linear cable accessory material, has both improved the electricity of cable accessory material
Lead non-linear, while also ensure that the APPENDIX MATERIALSThe has good breakdown strength.
The present invention fills phase by being doped with the nonlinear CaCu 3 Ti 4 O Particulate inorganics of high I-V into silicon rubber, makes institute
Obtained silicon rubber based non-linear cable accessory material has excellent conductance non-linear, can effectively improve stress cone and cable master
Electrical conductivity gradients between insulation, increase the transport capacity of carrier, slacken cumulative effect of the space charge in interface, so that real
Internal field's distortion is now eliminated, the internal electric field distribution of homogenizing cable accessory, strengthens annex insulation performance, reduces failure occurrence probability,
Extend the service life of cable accessory.
Preparation method of the present invention can make the silicon rubber based non-linear cable accessory material prepared by it have relatively low threshold value
Field strength, larger electrical conductivity nonlinear factor and relatively stable dc breakdown electric field strength, and preparation process of the present invention and institute
Need equipment simple, it is of low cost, easily implement.
Brief description of the drawings
Fig. 1 is the XRD spectrum of the CaCu 3 Ti 4 O particle obtained by embodiment 2；
Fig. 2 be CaCu 3 Ti 4 O particle volume obtained by embodiment 2- embodiments 5 than content be respectively 3,5,8,
The XRD spectrum of the silicon rubber based non-linear cable accessory material of 10vol.%；
Fig. 3 be CaCu 3 Ti 4 O particle volume obtained by embodiment 2- embodiments 5 than content be respectively 3,5,8,
The electrical conductivity of the silicon rubber based non-linear cable accessory material of 10vol.% changes collection of illustrative plates with electric field strength；
Fig. 4 be CaCu 3 Ti 4 O particle volume obtained by embodiment 2- embodiments 5 than content be respectively 3,5,8,
The dc breakdown Weibull distribution collection of illustrative plates of the silicon rubber based non-linear cable accessory material of 10vol.%.
Embodiment
Technical scheme is described further with reference to embodiment, but is not limited thereto, it is every right
Technical solution of the present invention technical scheme is modified or replaced equivalently, without departing from the spirit and scope of technical solution of the present invention, should all contain
Cover in protection scope of the present invention.
Embodiment 1
A kind of preparation method step of silicon rubber based non-linear cable accessory material is as follows：
First, it is in molar ratio nitrate trihydrate copper:Four water-calcium nitrate:Positive four butyl ester=1 of metatitanic acid:3:4, and according to metatitanic acid just
The volume of four butyl esters is by volume：Positive four butyl ester of metatitanic acid:Ethylene glycol monomethyl ether:Dust technology=100:400:1,160ml is measured respectively
Positive four butyl ester of ethylene glycol monomethyl ether, 0.4ml dust technologies, 41ml metatitanic acids and 21.744g nitrate trihydrates copper and 7.0845g are weighed respectively
Four water-calcium nitrate；Ethylene glycol monomethyl ether, dust technology are poured into beaker successively and stirred evenly, nitrate trihydrate copper is added into above-mentioned mixing
Solution is simultaneously completely dissolved it, then four water-calcium nitrate is added into mixed solution, is completely dissolved four water-calcium nitrate and is clarified
Mixed solution；The mixed solution of the clarification is cooled to room temperature and adds positive four butyl ester of metatitanic acid thereto, with 100-300r/
The rotating speed of min, which persistently stirs 40min, makes positive four butyl ester of metatitanic acid be dispersed in mixed solution, and CaCu 3 Ti 4 O sol solutions are made；
Lucifuge stands 12-36h to the CaCu 3 Ti 4 O sol solutions at room temperature.
2nd, it is 80 DEG C step to be positioned over temperature in constant temperature oven once the CaCu 3 Ti 4 O sol solutions that lucifuge is stood, processing
Time is 8-12h, and amorphous state CaCu 3 Ti 4 O gel is made after solvent therein all evaporation；By the amorphous state CaCu 3 Ti 4 O
Gel is put into Muffle furnace and calcines, and calcine technology is that temperature is risen to 300 DEG C, after temperature reaches 300 DEG C with the speed of 5 DEG C/min
1-2h is kept the temperature, then temperature is risen to 1050 DEG C by 300 DEG C with the speed of 5 DEG C/min, temperature keeps the temperature 1-8h after reaching 1050 DEG C, system
Obtain the CaCu 3 Ti 4 O of crystallization；
The CaCu 3 Ti 4 O of the crystallization is put into ball milling instrument, and alcohol and ball milling pearl are added to the crystallization into ball milling instrument
CaCu 3 Ti 4 O carry out wet-milling, the rotating speed of ball milling instrument is 580r/min, wet-milling 8-12h；The mixing liquid of gained is put into constant temperature
80 DEG C of heat treatment time 4-6h of baking oven, until alcohol volatilizees completely, are made the CaCu 3 Ti 4 O for the crystallization that particle diameter is 300-500nm
Grain.
3rd, A, the B two-component liquid silastic for measuring 50ml respectively are poured into different beakers, the A, B two-component liquid
Silicon rubber is the model of German Wacker Chemical Co., Ltd's productionDual composition addition type liquid silastic.
The CaCu 3 Ti 4 O particle of accurate two made crystallization of the step of weighing two parts of equal qualities is simultaneously added separately to the double groups of A, B
In part liquid silastic, persistently stirring 60min respectively with the speed of 100-300r/min at room temperature makes CaCu 3 Ti 4 O particle uniform
It is dispersed therein, then A, B two-component liquid silastic is mixed to and continued the speed stirring with 100-300r/min
30min, makes CaCu 3 Ti 4 O particle be dispersed in by in-situ polymerization in double-component liquid silicon rubber, and CaCu 3 Ti 4 O particle is made
Volume ratio content be 1-10vol.% uniformly mixed liquid adulterate silicon rubber；
4th, the made liquid doping silicon rubber of step 3 is placed under vacuum condition with the speed of agitator room of 100-300r/min
The lower stirring 60min of temperature, to discharge the bubble in liquid doped silicon rubber, is poured into size as 100 again after bubble to be discharged
In the mould of × 100 × 0.2mm and vacuumize process 30min at room temperature is placed in vacuum drying oven；
5th, the mould equipped with liquid doping silicon rubber of evacuated processing is taken out from vacuum drying oven, above and below mould
Two sides is with the Interal fixation that size is 250 × 176 × 8mm and is put into compression molding instrument and carries out high temperature vulcanized forming processes, sulphur
Chemical industry skill is that curing temperature is 120-150 DEG C, vulcanization time 10-15min, and hot pressing pressure is 10-15MPa, is made and is sulfided into
The silicon rubber based non-linear cable accessory material of type；By the silicon rubber based non-linear cable accessory material of the sulfidization molding from mould
It is removed and placed in tool in constant temperature oven and handles 4h with 200 DEG C of post-cures, it is 1- that CaCu 3 Ti 4 O particle volume, which is made, than content
10vol.% silicon rubber based non-linear cable accessory finished materials.
Based on CaCu 3 Ti 4 O granule in silicon rubber based non-linear cable accessory material made from the present embodiment preparation method
Product is 1-10vol.% than content, and the particle diameter of the CaCu 3 Ti 4 O particle is 300-500nm.
Embodiment 2
A kind of preparation method step of silicon rubber based non-linear cable accessory material is as follows：
First, it is in molar ratio nitrate trihydrate copper:Four water-calcium nitrate:Positive four butyl ester=1 of metatitanic acid:3:4, and according to metatitanic acid just
The volume of four butyl esters is by volume：Positive four butyl ester of metatitanic acid:Ethylene glycol monomethyl ether:Dust technology=100:400:1,160ml is measured respectively
Positive four butyl ester of ethylene glycol monomethyl ether, 0.4ml dust technologies, 41ml metatitanic acids and 21.744g nitrate trihydrates copper and 7.0845g are weighed respectively
Four water-calcium nitrate；Ethylene glycol monomethyl ether, dust technology are poured into beaker successively and stirred evenly, nitrate trihydrate copper is added into above-mentioned mixing
Solution is simultaneously completely dissolved it, then four water-calcium nitrate is added into mixed solution, is completely dissolved four water-calcium nitrate and is clarified
Mixed solution；The mixed solution of the clarification is cooled to room temperature and adds positive four butyl ester of metatitanic acid thereto, with 200r/min
Rotating speed persistently stir 40min and positive four butyl ester of metatitanic acid is dispersed in mixed solution, CaCu 3 Ti 4 O sol solutions are made；It is described
Lucifuge stands 24h to CaCu 3 Ti 4 O sol solutions at room temperature.
2nd, it is 80 DEG C step to be positioned over temperature in constant temperature oven once the CaCu 3 Ti 4 O sol solutions that lucifuge is stood, processing
Time is 8-12h, and amorphous state CaCu 3 Ti 4 O gel is made after solvent therein all evaporation；By the amorphous state CaCu 3 Ti 4 O
Gel is put into Muffle furnace and calcines, and calcine technology is that temperature is risen to 300 DEG C, after temperature reaches 300 DEG C with the speed of 5 DEG C/min
1-2h is kept the temperature, then temperature is risen to 1050 DEG C by 300 DEG C with the speed of 5 DEG C/min, temperature keeps the temperature 1-8h after reaching 1050 DEG C, system
Obtain the CaCu 3 Ti 4 O of crystallization；
The CaCu 3 Ti 4 O of the crystallization is put into ball milling instrument, and alcohol and ball milling pearl are added to the crystallization into ball milling instrument
CaCu 3 Ti 4 O carry out wet-milling, the rotating speed of ball milling instrument is 580r/min, wet-milling 10h；The mixing liquid of gained is put into constant temperature to dry
80 DEG C of heat treatment time 5h of case, until alcohol volatilizees completely, are made the CaCu 3 Ti 4 O particle for the crystallization that particle diameter is 300-500nm.
3rd, A, the B two-component liquid silastic for measuring 50ml respectively are poured into different beakers, the A, B two-component liquid
Silicon rubber is the model of German Wacker Chemical Co., Ltd's productionDual composition addition type liquid silastic.
It is accurate weigh the CaCu 3 Ti 4 O particle of two made crystallization of the step of two parts of quality are 13.3g and be added separately to A,
In B two-component liquid silastic, persistently stirring 60min respectively with the speed of 200r/min at room temperature makes CaCu 3 Ti 4 O particle uniform
It is dispersed therein, then A, B two-component liquid silastic is mixed and continued 30min is stirred with the speed of 200r/min,
CaCu 3 Ti 4 O particle is dispersed in by in-situ polymerization in double-component liquid silicon rubber, the volume of CaCu 3 Ti 4 O particle is made
The uniformly mixed liquid for being 3vol.% than content adulterates silicon rubber；
4th, the made liquid doping silicon rubber of step 3 is placed under vacuum condition with the speed of agitator of 200r/min at room temperature
60min is stirred, to discharge the bubble in liquid doped silicon rubber, is poured into size after bubble to be discharged again as 100 × 100
In the mould of × 0.2mm and vacuumize process 30min at room temperature is placed in vacuum drying oven；
5th, the mould equipped with liquid doping silicon rubber of evacuated processing is taken out from vacuum drying oven, above and below mould
Two sides is with the Interal fixation that size is 250 × 176 × 8mm and is put into compression molding instrument and carries out high temperature vulcanized forming processes, sulphur
Chemical industry skill is that curing temperature is 135 DEG C, vulcanization time 12min, and hot pressing pressure is 12MPa, and the silicon rubber of sulfidization molding is made
Based non-linear cable accessory material；The silicon rubber based non-linear cable accessory material of the sulfidization molding is removed from the molds simultaneously
It is put into constant temperature oven and handles 4h with 200 DEG C of post-cures, it is 3vol.% silicon rubber that CaCu 3 Ti 4 O particle volume, which is made, than content
Based non-linear cable accessory finished material.
Based on CaCu 3 Ti 4 O granule in silicon rubber based non-linear cable accessory material made from the present embodiment preparation method
Product is 3vol.% than content, and the particle diameter of the CaCu 3 Ti 4 O particle is 300-500nm.
Embodiment 3
The present embodiment accurately weighs the step of two parts of quality are 22.2g with differing only in for embodiment 2 in step 3
The CaCu 3 Ti 4 O particle of two made crystallization is simultaneously added separately in A, B two-component liquid silastic so that CaCu 3 Ti 4 O particle exists
Content in liquid doping silicon rubber is 5vol.%, and the present embodiment is finally made CaCu 3 Ti 4 O particle volume and is than content
The silicon rubber based non-linear cable accessory finished material of 5vol.%.
Embodiment 4
The present embodiment accurately weighs the step of two parts of quality are 35.5g with differing only in for embodiment 2 in step 3
The CaCu 3 Ti 4 O particle of two made crystallization is simultaneously added separately in A, B two-component liquid silastic so that CaCu 3 Ti 4 O particle exists
Content in liquid doping silicon rubber is 8vol.%, and the present embodiment is finally made CaCu 3 Ti 4 O particle volume and is than content
The silicon rubber based non-linear cable accessory finished material of 8vol.%.
Embodiment 5
The present embodiment accurately weighs the step of two parts of quality are 44.3g with differing only in for embodiment 2 in step 3
The CaCu 3 Ti 4 O particle of two made crystallization is simultaneously added separately in A, B two-component liquid silastic so that CaCu 3 Ti 4 O particle exists
Content in liquid doping silicon rubber is 10vol.%, and the present embodiment is finally made CaCu 3 Ti 4 O particle volume and is than content
The silicon rubber based non-linear cable accessory finished material of 10vol.%.
Fig. 1 is the XRD spectrum of the CaCu 3 Ti 4 O particle obtained by embodiment 2, and abscissa represents angle of diffraction, and scope is 2 θ
=10-90 °, ordinate represents diffracted intensity, and CCTO represents CaCu 3 Ti 4 O in figure.This it appears that CaCu 3 Ti 4 O from Fig. 1
Characteristic diffraction peak, without other miscellaneous peaks, illustrate that CaCu 3 Ti 4 O made from step 2 of the present invention exists without other crystal forms.
Fig. 2 be CaCu 3 Ti 4 O particle volume obtained by embodiment 2- embodiments 5 than content be respectively 3,5,8,
The XRD spectrum of the silicon rubber based non-linear cable accessory material of 10vol.%, abscissa represent angle of diffraction, scope for 2 θ=
10-90 °, ordinate represents diffracted intensity, and LSR represents silicon rubber in figure, and CCTO represents CaCu 3 Ti 4 O.Can be obvious from Fig. 2
Find out the characteristic diffraction peak of silicon rubber and CaCu 3 Ti 4 O, without other miscellaneous peaks, illustrate inorganic fill phase and the silicon rubber as matrix
Between be combined simply by the mode of physical mixed, without chemically reacting.
Fig. 3 be CaCu 3 Ti 4 O particle volume obtained by embodiment 2- embodiments 5 than content be respectively 3,5,8,
The electrical conductivity of the silicon rubber based non-linear cable accessory material of 10vol.% changes collection of illustrative plates with electric field strength, and abscissa represents electric field
Intensity (kV/mm), ordinate represent electrical conductivity (S/m), and CCTO/LSR represents that corresponding CaCu 3 Ti 4 O nano particle volume compares content
Silicon rubber based non-linear cable accessory material.As can be seen from Figure 3 silicon rubber base is non-thread made from preparation method of the present invention
Property cable accessory material electrical conductivity obvious nonlinear change is presented with electric field strength increase, and as CaCu 3 Ti 4 O particle adds
Add the raising of ratio, the nonlinear threshold electric field strength of electrical conductivity of the cable accessory material reduces, and nonlinear factor also increases
Greatly.
Fig. 4 be CaCu 3 Ti 4 O particle volume obtained by embodiment 2- embodiments 5 than content be respectively 3,5,8,
The dc breakdown Weibull distribution collection of illustrative plates of the silicon rubber based non-linear cable accessory material of 10vol.%, abscissa represent LnE values,
Ordinate represents Ln (- Ln (1-P)) value, and CCTO/LSR represents silicon rubber base of the corresponding CaCu 3 Ti 4 O nano particle volume than content
Non-linear cable APPENDIX MATERIALSThe.Silicon rubber based non-linear cable accessory material made from preparation method of the present invention as can be seen from Figure 4
The dc breakdown electric-field intensity distribution of material is more concentrated, and with the raising of CaCu 3 Ti 4 O particle adding proportion, the cable accessory
The breakdown field strength of material is without the decline occurred by a relatively large margin.
It can be seen that preparation method of the present invention can make prepared silicon rubber based non-linear cable accessory material by Fig. 3 and Fig. 4
Material has relatively low threshold field strength, larger electrical conductivity nonlinear factor and relatively stable dc breakdown electric field strength.
Claims (10)
1. a kind of preparation method of silicon rubber based non-linear cable accessory material, it is characterised in that the preparation method step is such as
Under：
First, nitrate trihydrate copper and four water-calcium nitrate are weighed respectively by certain mol proportion and measures positive four butyl ester of metatitanic acid；Further according to
The volume of positive four butyl ester of metatitanic acid measures ethylene glycol monomethyl ether and dust technology respectively according to a certain volume；By ethylene glycol monomethyl ether, dust technology
Beaker is poured into successively and is stirred evenly, and nitrate trihydrate copper is added into above-mentioned mixed solution and is completely dissolved it, then it is molten to mixing
Four water-calcium nitrate is added in liquid, four water-calcium nitrate is completely dissolved the mixed solution clarified；The mixing of the clarification is molten
Liquid is cooled to room temperature and adds positive four butyl ester of metatitanic acid thereto, and lasting stirring makes positive four butyl ester of metatitanic acid be dispersed in mixed solution
In, CaCu 3 Ti 4 O sol solutions are made, the CaCu 3 Ti 4 O sol solutions lucifuge is stood；
2nd, step is positioned in constant temperature oven once the CaCu 3 Ti 4 O sol solutions that lucifuge is stood and is heat-treated, amorphous is made
State CaCu 3 Ti 4 O gel；The amorphous state CaCu 3 Ti 4 O gel is put into Muffle furnace and is calcined, the CaCu 3 Ti 4 O of crystallization is made；Will
The CaCu 3 Ti 4 O of the crystallization is put into ball milling instrument, and the CaCu 3 Ti 4 O of alcohol and ball milling pearl to the crystallization is added into ball milling instrument
Wet-milling is carried out, the mixing liquid obtained by wet-milling certain time is put into constant temperature oven and is heat-treated, the copper titanate of crystallization is made
Calcium particle；
3rd, A, the B two-component liquid silastic for measuring equal volume respectively are poured into different beakers, accurately weigh two parts of equal matter
The step of amount two made crystallization CaCu 3 Ti 4 O particle and be added separately in A, B two-component liquid silastic, distinguish at room temperature
Lasting stirring makes CaCu 3 Ti 4 O even particulate dispersion in liquid silastic, then A, B two-component liquid silastic are blended in one
Rise and continue to stir certain time, the volume ratio content that CaCu 3 Ti 4 O particle is made is the uniformly mixed liquid of 1-10vol.%
Adulterate silicon rubber；
4th, the made liquid doping silicon rubber of step 3 is placed under vacuum condition and certain time is stirred at room temperature, then be poured into mould
In tool and it is placed in vacuum drying oven and carries out vacuumize process at room temperature；
5th, the mould equipped with liquid doping silicon rubber of evacuated processing is taken out from vacuum drying oven, by mould upper and lower surface
With Interal fixation and it is put into compression molding instrument and carries out high temperature vulcanized forming processes, the silicon rubber based non-linear of sulfidization molding is made
Cable accessory material；The silicon rubber based non-linear cable accessory material of the sulfidization molding is removed from the molds and is put into constant temperature
Post-cure processing is carried out in baking oven, it is 1-10vol.% silicon rubber based non-linear electricity that CaCu 3 Ti 4 O particle volume, which is made, than content
Cable fittings finished material.
A kind of 2. preparation method of silicon rubber based non-linear cable accessory material according to claim 1, it is characterised in that step
A rapid molar ratio is：Nitrate trihydrate copper:Four water-calcium nitrate:Positive four butyl ester=1 of metatitanic acid:3:4, the volume ratio for metatitanic acid just
Four butyl esters:Ethylene glycol monomethyl ether:Dust technology=100:400:1；The lasting stirring is stirred with the speed of agitator of 100-300r/min
Mix 40min；It is that lucifuge stands 12-36h at room temperature that the lucifuge, which is stood,.
A kind of 3. preparation method of silicon rubber based non-linear cable accessory material according to claim 1 or claim 2, it is characterised in that
The temperature that CaCu 3 Ti 4 O sol solutions described in step 2 are heat-treated is 80 DEG C, processing time 8-12h；The Muffle furnace calcine technology
For temperature is risen to 300 DEG C with the speed of 5 DEG C/min, temperature keeps the temperature 1-2h after reaching 300 DEG C, then will with the speed of 5 DEG C/min
Temperature rises to 1050 DEG C by 300 DEG C, and temperature keeps the temperature 1-8h after reaching 1050 DEG C.
A kind of 4. preparation method of silicon rubber based non-linear cable accessory material according to claim 3, it is characterised in that step
The rotating speed of the rapid two ball milling instrument is 580r/min, and the wet-milling time is 8-12h；The heat of gained mixing liquid after the ball milling
Treatment temperature is 80 DEG C, processing time 4-6h.
A kind of 5. preparation method of silicon rubber based non-linear cable accessory material according to claim 4, it is characterised in that step
The particle diameter of the CaCu 3 Ti 4 O particle of crystallization made from rapid two is 300-500nm.
A kind of 6. preparation method of silicon rubber based non-linear cable accessory material according to claim 5, it is characterised in that step
Rapid three A, B two-component liquid silastic are double groups of zero R737 of model POWERSIL of German Wacker Chemical Co., Ltd's production
Part add-on type liquid silicon rubber.
A kind of 7. preparation method of silicon rubber based non-linear cable accessory material according to claim 6, it is characterised in that step
It is 100-300r/min persistently to stir A, the speed of agitator of B two-component liquid silastic described in rapid three respectively at room temperature, during stirring
Between be 60min, continue after A, B two-component liquid silastic are mixed stirring rotating speed be 100-300r/min, stir
Time is 30min.
A kind of 8. preparation method of silicon rubber based non-linear cable accessory material according to claim 7, it is characterised in that step
The rotating speed that the rapid four liquid doping silicon rubber is stirred at room temperature under vacuum is 100-300r/min, and mixing time is
60min；The die size is 100 × 100 × 0.2mm.
A kind of 9. preparation method of silicon rubber based non-linear cable accessory material according to claim 8, it is characterised in that step
Rapid five plate size is 250 × 176 × 8mm, and curing temperature is 120-150 DEG C in the high temperature vulcanized moulding process, sulphur
The change time is 10-15min, and hot pressing pressure is 10-15MPa, and the post-cure treatment temperature is 200 DEG C, processing time 4h.
It is 10. a kind of made from the preparation method based on any silicon rubber based non-linear cable accessory materials of claim 1-9
Silicon rubber based non-linear cable accessory material, it is characterised in that CaCu 3 Ti 4 O in the silicon rubber based non-linear cable accessory material
Particle volume is 1-10vol.% than content, and the particle diameter of the CaCu 3 Ti 4 O particle is 300-500nm.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109665755A (en) * | 2019-01-22 | 2019-04-23 | 华南理工大学 | A kind of room temperature vulcanized silicone rubber base ac cable APPENDIX MATERIALSThe and preparation method thereof |
| CN114806177A (en) * | 2021-10-08 | 2022-07-29 | 中国电力科学研究院有限公司 | Preparation method of liquid silicone rubber |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101891460A (en) * | 2010-07-08 | 2010-11-24 | 桂林理工大学 | Method for preparing calcium copper titanium oxide powder by sol-gel method |
| CN104945645A (en) * | 2015-06-23 | 2015-09-30 | 绥化学院 | Preparation method of polyethylene composite material |
| CN104985738A (en) * | 2015-06-23 | 2015-10-21 | 哈尔滨理工大学 | Preparation method of polyvinylidene fluoride matrix composite material |
| CN106747413A (en) * | 2017-02-23 | 2017-05-31 | 四川环碳科技有限公司 | CaCu 3 Ti 4 O nano crystal powder and preparation method thereof |
-
2018
- 2018-01-09 CN CN201810019383.5A patent/CN108017914A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101891460A (en) * | 2010-07-08 | 2010-11-24 | 桂林理工大学 | Method for preparing calcium copper titanium oxide powder by sol-gel method |
| CN104945645A (en) * | 2015-06-23 | 2015-09-30 | 绥化学院 | Preparation method of polyethylene composite material |
| CN104985738A (en) * | 2015-06-23 | 2015-10-21 | 哈尔滨理工大学 | Preparation method of polyvinylidene fluoride matrix composite material |
| CN106747413A (en) * | 2017-02-23 | 2017-05-31 | 四川环碳科技有限公司 | CaCu 3 Ti 4 O nano crystal powder and preparation method thereof |
Non-Patent Citations (5)
| Title |
|---|
| 李文虎，艾桃桃主编: "《材料科学与工程专业实验教程》", 30 November 2015, 北京邮电大学出版社 * |
| 王迎军主编: "《新型材料科学与技术 无机材料卷 中》", 31 October 2016, 华南理工大学出版社 * |
| 董飞翎: "《CaCu3Ti4O12基陶瓷的介电性能研究》", 《中国优秀硕士学位论文全文数据库（电子期刊）.工程科技I辑》 * |
| 蔡雅楠: "《CCTO/橡胶复合材料制备及其介电性能研究》", 《中国优秀硕士学位论文全文数据库（电子期刊）.工程科技Ⅱ辑》 * |
| 贾成厂等编著: "《陶瓷基复合材料导论》", 31 August 1998, 冶金工业出版社 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109665755A (en) * | 2019-01-22 | 2019-04-23 | 华南理工大学 | A kind of room temperature vulcanized silicone rubber base ac cable APPENDIX MATERIALSThe and preparation method thereof |
| CN109665755B (en) * | 2019-01-22 | 2020-02-18 | 华南理工大学 | Room-temperature vulcanized silicone rubber-based alternating-current cable accessory material and preparation method thereof |
| CN114806177A (en) * | 2021-10-08 | 2022-07-29 | 中国电力科学研究院有限公司 | Preparation method of liquid silicone rubber |
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