CN108034260A - Field operation compounded rubber and preparation method thereof - Google Patents

Field operation compounded rubber and preparation method thereof Download PDF

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Publication number
CN108034260A
CN108034260A CN201810034849.9A CN201810034849A CN108034260A CN 108034260 A CN108034260 A CN 108034260A CN 201810034849 A CN201810034849 A CN 201810034849A CN 108034260 A CN108034260 A CN 108034260A
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mixing
preparation
parts
solvent
aging
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蔡青青
米春海
何源
周太平
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Wuhu Spaceflight Special Cable Factory Co Ltd
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Wuhu Spaceflight Special Cable Factory Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L83/00Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
    • C08L83/04Polysiloxanes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29BPREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00Mixing; Kneading
    • B29B7/002Methods
    • B29B7/005Methods for mixing in batches
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29BPREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00Mixing; Kneading
    • B29B7/02Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type
    • B29B7/22Component parts, details or accessories; Auxiliary operations
    • B29B7/28Component parts, details or accessories; Auxiliary operations for measuring, controlling or regulating, e.g. viscosity control
    • B29B7/283Component parts, details or accessories; Auxiliary operations for measuring, controlling or regulating, e.g. viscosity control measuring data of the driving system, e.g. torque, speed, power
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29BPREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00Mixing; Kneading
    • B29B7/02Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type
    • B29B7/22Component parts, details or accessories; Auxiliary operations
    • B29B7/28Component parts, details or accessories; Auxiliary operations for measuring, controlling or regulating, e.g. viscosity control
    • B29B7/286Component parts, details or accessories; Auxiliary operations for measuring, controlling or regulating, e.g. viscosity control measuring properties of the mixture, e.g. temperature, density
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C35/00Heating, cooling or curing, e.g. crosslinking or vulcanising; Apparatus therefor
    • B29C35/02Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould
    • B29C35/08Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould by wave energy or particle radiation
    • B29C35/0805Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould by wave energy or particle radiation using electromagnetic radiation
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C35/00Heating, cooling or curing, e.g. crosslinking or vulcanising; Apparatus therefor
    • B29C35/02Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould
    • B29C35/08Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould by wave energy or particle radiation
    • B29C35/0805Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould by wave energy or particle radiation using electromagnetic radiation
    • B29C2035/0855Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould by wave energy or particle radiation using electromagnetic radiation using microwave
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2296Oxides; Hydroxides of metals of zinc
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/08Stabilised against heat, light or radiation or oxydation

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Polymers & Plastics (AREA)
  • Medicinal Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electromagnetism (AREA)
  • Toxicology (AREA)
  • Oral & Maxillofacial Surgery (AREA)
  • Thermal Sciences (AREA)
  • Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)

Abstract

The present invention relates to cable rubber, specifically discloses a kind of field operation compounded rubber and preparation method thereof.The present invention is mixed using boron fibre with silane coupling agent, obtains pretreatment enhancers, then by a mixing, secondary mixing, and flash process is combined, and extrusion molding, microwave vulcanization are combined, obtain field operation compounded rubber.Using the preparation method, the glutinous roller phenomenon during mixing (the first mixing, the second mixing) can substantially be mitigated, reduce actual operating time, the risk of raw material aging can be reduced on the basis of preparation efficiency is increased, and obtained product is low temperature resistant, high intensity, the balancing performance such as anti-aging, obtained field operation compounded rubber has the advantages that low temperature resistant, high intensity and anti-aging.The preparation method of the present invention is workable, and positive effect, has highly application value.

Description

Field operation compounded rubber and preparation method thereof
Technical field
The present invention relates to cable rubber, and in particular, to a kind of field operation compounded rubber and preparation method thereof.
Background technology
At present, with the development of science and technology, either industry or the daily life of the mankind, towards electrified side To development, then in industry and power domain, its status is also gradually increased cable.Cable have power cable, control cable, Compensating cable, shielded cable, high-temperature cable, computer cable, signal cable, coaxial cable, fire-resisting cable, cable for ship, aluminium Alloy cable etc..Cable is typically by several or the cable of at least two similar ropes being twisted of several groups of every group of conducting wires, Mutually insulated between every group of conducting wire, and be often twisted into around a center, whole outside is surrounded by the outer jacket of high-insulation, is used for Connect circuit, electric appliance etc..
Field operation military training is more in extremely cold area, and temperature is very low (particularly winter), and ultraviolet light is strong, general instrument Sheath and insulation can crack at low temperature for line and extended line, lose to the protective effect of transmission of electricity and fail.It is and relatively cold regional ultraviolet Light is strong, and general organic high polymer material is unable to bear ultraviolet light and aging and fails.Since instrument line can use outdoors, and And often movement is needed, high to the softness requirements of cable, the softness requirements particularly under extremely low temperature are high, while require to produce Product have good weatherability.
Protective coverings of cable made of protective coverings of cable can follow the string under extremely low temperature at present, and brittleness becomes larger, warp Incessantly repeatedly mobile or bending, so that cable is discarded and cannot used.
Chinese patent document 201710430886.7 discloses a kind of field operation low temperature resistant cable outer jacket and its preparation side Method, and specifically disclose and comprise the following steps:(1) by boron fibre, ethyl orthosilicate, dimethicone, cage-type silsesquioxane, Mixing, drying, obtains M1;(2) by polypropylene, lauryl mercaptan, epoxy resin E44, rare earth nitrades, peroxidating diisopropyl Benzene mixes, and obtains M2;(3) by fluorubber, carbon black, white carbon, triethyl aluminum, Fe-series catalyst, lanthana, trimethylolpropane Triacrylate, zinc oxide, magnesium hydroxide, M1, M2 carry out mixing, obtain M3;(4) M3 is extruded.
But due in preparation process, with the addition of substantial amounts of auxiliary agent, filler, cause occur glutinous roller in preparation process Phenomenon, and glutinous roller further results in mixing inequality, rubber performance is uneven, and in addition preparation process is glutinous due to repeatedly to clear up Roller, causes preparation time very long, and the extension of mixing time can further result in the aging of rubber raw materials again, increases the rubber of preparation The risk of product strength hydraulic performance decline, on the other hand, glutinous roller can cause raw material mixing uneven, cause rubber partial properties compared with It is good, and part performance cannot be met the requirements.And if reduce the additive amount of filler, although glutinous roller phenomenon mitigates, can lead The hydraulic performance decline of rubber is caused, does not meet that field operation requires anti-aging, high intensity with compounded rubber and low temperature resistant etc. performance will Ask.
Therefore, how on the basis of ensureing that field operation compounded rubber has the performance such as low temperature resistant, high intensity, anti-aging, It is a technical problem to be solved urgently that the glutinous roller phenomenon in preparation process, which is reduced, to obtain the rubber product of balancing performance.
The content of the invention
The object of the present invention is to provide a kind of field operation compounded rubber and preparation method thereof, which can reduce mixed Glutinous roller phenomenon during sweetening process, reduces actual operating time, it is old raw material can be reduced on the basis of preparation efficiency is increased The risk of change, obtained igniter motor rubber have the advantages that low temperature resistant, high intensity, anti-aging, and balancing performance.The present invention Preparation method it is workable, positive effect, has highly application value.
To achieve these goals, the present invention provides a kind of preparation method of field operation compounded rubber, the method bag Include following steps:(1) boron fibre is mixed with silane coupling agent, obtains pretreatment enhancers;(2) by polypropylene, the first solvent, first Base vinylsiloxane rubber, carbon black, pretreatment enhancers, zinc oxide, Fe-series catalyst and antioxidant carry out a mixing, Ran Houjing Put;(3) the second solvent, white carbon and vulcanizing agent are added in a mixing thing after standing and carries out secondary mixing;(4) with by The solvent total amount that one solvent and the second solvent are formed is a hundred percent, and secondary mixing thing is flashed, boils off the molten of 60-80% Agent;(5) the secondary mixing thing after flash distillation is subjected to stone roller page, cutting, film is made, film extrusion is molded, microwave vulcanization;Its In, the particle size range of white carbon is -800 mesh of 600 mesh, and the weight ratio of carbon black and methyl vinyl silicone rubber is 1:3-5.
The present invention also provides a kind of field operation compounded rubber being prepared according to previously described preparation method.
Through the above technical solutions, the present invention is mixed using boron fibre with silane coupling agent, pretreatment enhancers are obtained, then pass through A mixing, secondary mixing are crossed, and combines flash process, and combines extrusion molding, microwave vulcanization, has obtained field operation with compound rubber Glue.It using the preparation method, can substantially mitigate the glutinous roller phenomenon during mixing (the first mixing, the second mixing), reduce actual Operating time, can reduce the risk of raw material aging on the basis of preparation efficiency is increased, and obtained product is low temperature resistant, high The balancing performance such as intensity, anti-aging, obtained field operation compounded rubber have the advantages that low temperature resistant, high intensity and anti-aging.This The preparation method of invention is workable, and positive effect, has highly application value.
Embodiment
The embodiment of the present invention is described in detail below.It is it should be appreciated that described herein specific Embodiment is merely to illustrate and explain the present invention, and is not intended to limit the invention.
The endpoint of disclosed scope and any value are not limited to the accurate scope or value herein, these scopes or Value should be understood to comprising the value close to these scopes or value.For number range, between the endpoint value of each scope, respectively It can be combined with each other between the endpoint value of a scope and single point value, and individually between point value and obtain one or more New number range, these number ranges should be considered as specific open herein.
The present invention provides a kind of preparation method of field operation compounded rubber, the described method comprises the following steps:(1) by boron Fiber is mixed with silane coupling agent, obtains pretreatment enhancers;(2) by polypropylene, the first solvent, methyl vinyl silicone rubber, charcoal Black, pretreatment enhancers, zinc oxide, Fe-series catalyst and antioxidant carry out a mixing, then stand;(3) after standing The second solvent, white carbon and vulcanizing agent are added in mixing thing and carries out secondary mixing;(4) with by the first solvent and the second solvent The solvent total amount of formation is a hundred percent, and secondary mixing thing is flashed, boils off the solvent of 60-80%;(5) by after flash distillation Secondary mixing thing carries out stone roller page, cutting, and film is made, film extrusion is molded, microwave vulcanization;Wherein, the particle diameter model of white carbon Enclose for -800 mesh of 600 mesh, the weight ratio of carbon black and methyl vinyl silicone rubber is 1:3-5.
Through the above technical solutions, the present invention is mixed using boron fibre with silane coupling agent, pretreatment enhancers are obtained, then pass through A mixing, secondary mixing are crossed, and combines flash process, and combines extrusion molding, microwave vulcanization, has obtained field operation with compound rubber Glue.It using the preparation method, can substantially mitigate the glutinous roller phenomenon during mixing (the first mixing, the second mixing), reduce actual Operating time, can reduce the risk of raw material aging on the basis of preparation efficiency is increased, and obtained product is low temperature resistant, high The balancing performance such as intensity, anti-aging, obtained field operation compounded rubber have the advantages that low temperature resistant, high intensity and anti-aging.This The preparation method of invention is workable, and positive effect, has highly application value.
In a kind of more preferred embodiment of the present invention, in order to mitigate (the first mixing, the second mixing) process of mixing In glutinous roller phenomenon, reduce actual operating time, with the basis of preparation efficiency increase reduction raw material aging risk, and Obtained product is low temperature resistant, high intensity, the balancing performance such as anti-aging and has the advantages that low temperature resistant, high intensity and anti-aging open country War compounded rubber, it is preferable that in parts by weight, 30-40 parts of polypropylene, 50-80 parts of the first solvent, methyl vinyl silicone rubber 100-120 parts, 25-35 parts of carbon black, 10-20 parts of pretreatment enhancers, 5-8 parts of zinc oxide, 2-3 parts of Fe-series catalyst, antioxidant 5-8 parts, 7-12 parts of the second 50-80 parts of solvent, 18-25 parts of white carbon and vulcanizing agent.
In a kind of more preferred embodiment of the present invention, in order to mitigate (the first mixing, the second mixing) process of mixing In glutinous roller phenomenon, reduce actual operating time, with the basis of preparation efficiency increase reduction raw material aging risk, and Obtained product is low temperature resistant, high intensity, the balancing performance such as anti-aging and has the advantages that low temperature resistant, high intensity and anti-aging open country War compounded rubber, it is preferable that the weight ratio of boron fibre and silane coupling agent is 2:1-3.
In a kind of more preferred embodiment of the present invention, in order to mitigate (the first mixing, the second mixing) process of mixing In glutinous roller phenomenon, reduce actual operating time, with the basis of preparation efficiency increase reduction raw material aging risk, and Obtained product is low temperature resistant, high intensity, the balancing performance such as anti-aging and has the advantages that low temperature resistant, high intensity and anti-aging open country War compounded rubber, it is preferable that the one or more in silane coupling agent KH550, KH560, KH570.
In a kind of more preferred embodiment of the present invention, in order to mitigate (the first mixing, the second mixing) process of mixing In glutinous roller phenomenon, reduce actual operating time, with the basis of preparation efficiency increase reduction raw material aging risk, and Obtained product is low temperature resistant, high intensity, the balancing performance such as anti-aging and has the advantages that low temperature resistant, high intensity and anti-aging open country War compounded rubber, it is preferable that
In a kind of more preferred embodiment of the present invention, in order to mitigate (the first mixing, the second mixing) process of mixing In glutinous roller phenomenon, reduce actual operating time, with the basis of preparation efficiency increase reduction raw material aging risk, and Obtained product is low temperature resistant, high intensity, the balancing performance such as anti-aging and has the advantages that low temperature resistant, high intensity and anti-aging open country War compounded rubber, it is preferable that silane coupling agent is the mixture of KH550 and KH570, wherein, the weight of KH550 and KH570 Than for 2:2-3.
In a kind of more preferred embodiment of the present invention, in order to mitigate (the first mixing, the second mixing) process of mixing In glutinous roller phenomenon, reduce actual operating time, with the basis of preparation efficiency increase reduction raw material aging risk, and Obtained product is low temperature resistant, high intensity, the balancing performance such as anti-aging and has the advantages that low temperature resistant, high intensity and anti-aging open country War compounded rubber, it is preferable that in step (1), mixing condition includes:In the condition that 130-180 DEG C of rotating speed is 500-800rpm Lower mixing 30-50min.
In a kind of more preferred embodiment of the present invention, in order to mitigate (the first mixing, the second mixing) process of mixing In glutinous roller phenomenon, reduce actual operating time, with the basis of preparation efficiency increase reduction raw material aging risk, and Obtained product is low temperature resistant, high intensity, the balancing performance such as anti-aging and has the advantages that low temperature resistant, high intensity and anti-aging open country War compounded rubber, it is preferable that the condition of a mixing includes:Under conditions of 190-200 DEG C of rotating speed is 200-300r/min Mixing 15-20min.
In a kind of more preferred embodiment of the present invention, in order to mitigate (the first mixing, the second mixing) process of mixing In glutinous roller phenomenon, reduce actual operating time, with the basis of preparation efficiency increase reduction raw material aging risk, and Obtained product is low temperature resistant, high intensity, the balancing performance such as anti-aging and has the advantages that low temperature resistant, high intensity and anti-aging open country War compounded rubber, it is preferable that the condition of standing includes:30-40min is stood in 120-140 DEG C.
In a kind of more preferred embodiment of the present invention, in order to mitigate (the first mixing, the second mixing) process of mixing In glutinous roller phenomenon, reduce actual operating time, with the basis of preparation efficiency increase reduction raw material aging risk, and Obtained product is low temperature resistant, high intensity, the balancing performance such as anti-aging and has the advantages that low temperature resistant, high intensity and anti-aging open country War compounded rubber, it is preferable that the condition of secondary mixing includes:Under conditions of 170-180 DEG C of rotating speed is 400-500r/min Mixing 8-10min.
In a kind of more preferred embodiment of the present invention, in order to mitigate (the first mixing, the second mixing) process of mixing In glutinous roller phenomenon, reduce actual operating time, with the basis of preparation efficiency increase reduction raw material aging risk, and Obtained product is low temperature resistant, high intensity, the balancing performance such as anti-aging and has the advantages that low temperature resistant, high intensity and anti-aging open country War compounded rubber, it is preferable that extrusion condition includes:Extrusion temperature is 190-195 DEG C, and steam pressure controls in extrusion In 0.6-0.8MPa.
In a kind of more preferred embodiment of the present invention, in order to mitigate (the first mixing, the second mixing) process of mixing In glutinous roller phenomenon, reduce actual operating time, with the basis of preparation efficiency increase reduction raw material aging risk, and Obtained product is low temperature resistant, high intensity, the balancing performance such as anti-aging and has the advantages that low temperature resistant, high intensity and anti-aging open country War compounded rubber, it is preferable that microwave vulcanization includes successively:One section of microwave vulcanization, two sections of hot-air cures.
In a kind of more preferred embodiment of the present invention, in order to mitigate (the first mixing, the second mixing) process of mixing In glutinous roller phenomenon, reduce actual operating time, with the basis of preparation efficiency increase reduction raw material aging risk, and Obtained product is low temperature resistant, high intensity, the balancing performance such as anti-aging and has the advantages that low temperature resistant, high intensity and anti-aging open country War compounded rubber, it is preferable that one section of microwave vulcanization section temperature is 190-200 DEG C, and one section of temperature of two sections of hot-air cures is 180-185 DEG C, two sections of temperature of two sections of hot-air cures are 165-175 DEG C.
In a kind of more preferred embodiment of the present invention, in order to mitigate (the first mixing, the second mixing) process of mixing In glutinous roller phenomenon, reduce actual operating time, with the basis of preparation efficiency increase reduction raw material aging risk, and Obtained product is low temperature resistant, high intensity, the balancing performance such as anti-aging and has the advantages that low temperature resistant, high intensity and anti-aging open country War compounded rubber, it is preferable that the condition of flash distillation includes:Temperature is 90-120 DEG C, pressure 0.025-0.030MPa.
In a kind of more preferred embodiment of the present invention, in order to mitigate (the first mixing, the second mixing) process of mixing In glutinous roller phenomenon, reduce actual operating time, with the basis of preparation efficiency increase reduction raw material aging risk, and Obtained product is low temperature resistant, high intensity, the balancing performance such as anti-aging and has the advantages that low temperature resistant, high intensity and anti-aging open country War compounded rubber, it is preferable that Fe-series catalyst is one in the organoiron compound such as triacetyl acetone iron and isooctyl acid iron Kind is a variety of.
In a kind of more preferred embodiment of the present invention, in order to mitigate (the first mixing, the second mixing) process of mixing In glutinous roller phenomenon, reduce actual operating time, with the basis of preparation efficiency increase reduction raw material aging risk, and Obtained product is low temperature resistant, high intensity, the balancing performance such as anti-aging and has the advantages that low temperature resistant, high intensity and anti-aging open country War compounded rubber, it is preferable that the first solvent is the one or more in lauryl alcohol, ethyl acetate, glycerine and hexamethylene.
In a kind of more preferred embodiment of the present invention, in order to mitigate (the first mixing, the second mixing) process of mixing In glutinous roller phenomenon, reduce actual operating time, with the basis of preparation efficiency increase reduction raw material aging risk, and Obtained product is low temperature resistant, high intensity, the balancing performance such as anti-aging and has the advantages that low temperature resistant, high intensity and anti-aging open country War compounded rubber, it is preferable that the second solvent is ethyl acetate and the mixture of hexamethylene.
In a kind of more preferred embodiment of the present invention, in order to mitigate (the first mixing, the second mixing) process of mixing In glutinous roller phenomenon, reduce actual operating time, with the basis of preparation efficiency increase reduction raw material aging risk, and Obtained product is low temperature resistant, high intensity, the balancing performance such as anti-aging and has the advantages that low temperature resistant, high intensity and anti-aging open country War compounded rubber, it is preferable that the weight ratio of ethyl acetate and hexamethylene is 2 in the second solvent:1-3.
In a kind of more preferred embodiment of the present invention, in order to mitigate (the first mixing, the second mixing) process of mixing In glutinous roller phenomenon, reduce actual operating time, with the basis of preparation efficiency increase reduction raw material aging risk, and Obtained product is low temperature resistant, high intensity, the balancing performance such as anti-aging and has the advantages that low temperature resistant, high intensity and anti-aging open country War compounded rubber, it is preferable that antioxidant is irgasfos 168 and/or antioxidant 264.
In a kind of more preferred embodiment of the present invention, in order to mitigate (the first mixing, the second mixing) process of mixing In glutinous roller phenomenon, reduce actual operating time, with the basis of preparation efficiency increase reduction raw material aging risk, and Obtained product is low temperature resistant, high intensity, the balancing performance such as anti-aging and has the advantages that low temperature resistant, high intensity and anti-aging open country War compounded rubber, it is preferable that vulcanizing agent elects the one or more in sulphur, benzoyl peroxide and urethanes as.
In a kind of more preferred embodiment of the present invention, in order to mitigate (the first mixing, the second mixing) process of mixing In glutinous roller phenomenon, reduce actual operating time, with the basis of preparation efficiency increase reduction raw material aging risk, and Obtained product is low temperature resistant, high intensity, the balancing performance such as anti-aging and has the advantages that low temperature resistant, high intensity and anti-aging open country War compounded rubber, it is preferable that polyacrylic weight average molecular weight is 10000-30000.
In the above-mentioned technical solutions, conventional boron fibre, i.e. filament diameter are that 100-200 μm of boron fibre can realize this Invention.
In the above-mentioned technical solutions, this hair can be achieved in the methyl vinyl silicone rubber of conventional average molecular weight 35-70 ten thousand It is bright, model 110-1 is selected in embodiment later, the methyl vinyl silicone rubber that average molecular weight is 50-70 ten thousand carries out Illustrate.
The present invention also provides a kind of field operation compounded rubber being prepared according to previously described preparation method.
Through the above technical solutions, the present invention is mixed using boron fibre with silane coupling agent, pretreatment enhancers are obtained, then pass through A mixing, secondary mixing are crossed, and combines flash process, and combines extrusion molding, microwave vulcanization, has obtained field operation with compound rubber Glue.It using the preparation method, can substantially mitigate the glutinous roller phenomenon during mixing (the first mixing, the second mixing), reduce actual Operating time, can reduce the risk of raw material aging on the basis of preparation efficiency is increased, and obtained product is low temperature resistant, high The balancing performance such as intensity, anti-aging, obtained field operation compounded rubber have the advantages that low temperature resistant, high intensity and anti-aging.This The preparation method of invention is workable, and positive effect, has highly application value.
The present invention will be described in detail by way of examples below.In following embodiments, mixer turns over for strong pressurizing Rotatable mixer, is in universe Machinery Co., Ltd. purchased from Shanghai;150 μm of boron fibre filament diameter, purchased from brilliant hundred million ceramics in Zibo Co., Ltd;Methyl vinyl silicone rubber is model 110-1;Fe-series catalyst is isooctyl acid iron;First solvent is hexamethylene; Antioxidant is irgasfos 168;Vulcanizing agent is benzoyl peroxide;Polyacrylic weight average molecular weight is 20000;Other are conventional city Sell product.
Preparation example 1
Boron fibre is mixed into 50min with silane coupling agent under conditions of 180 DEG C of rotating speeds are 800rpm, wherein, boron fibre Weight ratio with silane coupling agent is 2:1, silane coupling agent is the mixture of KH550 and KH570, wherein, KH550 and KH570 Weight ratio be 2:2, obtain pretreatment enhancers.
Preparation example 2
Boron fibre is mixed into 30min with silane coupling agent under conditions of 130 DEG C of rotating speeds are 500rpm, wherein, boron fibre Weight ratio with silane coupling agent is 2:3, silane coupling agent is the mixture of KH550 and KH570, wherein, KH550 and KH570 Weight ratio be 2:3, obtain pretreatment enhancers.
Preparation example 3
Boron fibre is mixed into 40min with silane coupling agent under conditions of 155 DEG C of rotating speeds are 650rpm, wherein, boron fibre Weight ratio with silane coupling agent is 2:2, silane coupling agent is the mixture of KH550 and KH570, wherein, KH550 and KH570 Weight ratio be 2:2.5, obtain pretreatment enhancers.
Embodiment 1
The preparation method of field operation compounded rubber, comprises the following steps:
In parts by weight, 30 parts of polypropylene, 50 parts of the first solvent, 100 parts of methyl vinyl silicone rubber, 25 parts of carbon black, system 5 parts of 10 parts of pretreatment enhancers, 5 parts of zinc oxide, 2 parts of Fe-series catalyst and antioxidant in standby example 1 are in 200 DEG C of rotating speeds A mixing 20min is carried out under conditions of 300r/min, then stands 40min in 140 DEG C;
7 parts of 50 parts of the second solvent, 18 parts of white carbon and vulcanizing agent is added in a mixing thing after standing in 170 DEG C to turn Speed carries out secondary mixing 10min under conditions of being 500r/min;Wherein, the second solvent is the mixing of ethyl acetate and hexamethylene The weight ratio of thing, ethyl acetate and hexamethylene is 2:1;
, as absolutely, to be in temperature by secondary mixing thing by the solvent total amount that the first solvent and the second solvent are formed 120 DEG C, pressure is flashed under conditions of being 0.030MPa, boils off 80% solvent;
Secondary mixing thing after flash distillation is subjected to stone roller page, cutting, film is made, film extrusion is molded, wherein, extrusion temperature Spend for 195 DEG C, steam pressure is controlled and included successively in 0.8MPa, then microwave vulcanization, microwave vulcanization in extrusion:One section Microwave vulcanization, two sections of hot-air cures, wherein, one section of microwave vulcanization section temperature is 200 DEG C, one section of temperature of two sections of hot-air cures Spend for 185 DEG C, two sections of temperature of two sections of hot-air cures are 175 DEG C;
Wherein, the particle size range of white carbon is -800 mesh of 600 mesh.
Embodiment 2
The preparation method of field operation compounded rubber, comprises the following steps:
In parts by weight, 40 parts of polypropylene, 80 parts of the first solvent, 120 parts of methyl vinyl silicone rubber, 35 parts of carbon black, system 8 parts of 20 parts of pretreatment enhancers, 8 parts of zinc oxide, 3 parts of Fe-series catalyst and antioxidant in standby example 2 are in 190 DEG C of rotating speeds A mixing 15min is carried out under conditions of 200r/min, then stands 30min in 120 DEG C;
12 parts of 80 parts of the second solvent, 25 parts of white carbon and vulcanizing agent are added in a mixing thing after standing in 170 DEG C Rotating speed carries out secondary mixing 8min under conditions of being 400r/min;Wherein, the second solvent is the mixing of ethyl acetate and hexamethylene The weight ratio of thing, ethyl acetate and hexamethylene is 2:3;
Using by the solvent total amount that the first solvent and the second solvent are formed as absolutely, by secondary mixing thing in temperature be 90 DEG C, pressure is flashed under conditions of being 0.025MPa, boils off 60% solvent;
Secondary mixing thing after flash distillation is subjected to stone roller page, cutting, film is made, film extrusion is molded, wherein, extrusion temperature Spend for 190 DEG C, steam pressure is controlled and included successively in 0.6MPa, then microwave vulcanization, microwave vulcanization in extrusion:One section Microwave vulcanization, two sections of hot-air cures, wherein, one section of microwave vulcanization section temperature is 190 DEG C, one section of temperature of two sections of hot-air cures Spend for 180 DEG C, two sections of temperature of two sections of hot-air cures are 165 DEG C;
Wherein, the particle size range of white carbon is -800 mesh of 600 mesh.
Embodiment 3
The preparation method of field operation compounded rubber, comprises the following steps:
In parts by weight, 35 parts of polypropylene, 65 parts of the first solvent, 110 parts of methyl vinyl silicone rubber, 30 parts of carbon black, system 6.5 parts of 15 parts of pretreatment enhancers, 6.5 parts of zinc oxide, 2.5 parts of Fe-series catalyst and antioxidant in standby example 3 are in 195 DEG C of rotating speeds To carry out a mixing 18min under conditions of 250r/min, then 35min is stood in 130 DEG C;
9.5 parts of 65 parts of the second solvent, 21 parts of white carbon and vulcanizing agent are added in a mixing thing after standing in 175 DEG C Rotating speed carries out secondary mixing 9min under conditions of being 450r/min;Wherein, the second solvent is the mixing of ethyl acetate and hexamethylene The weight ratio of thing, ethyl acetate and hexamethylene is 2:2;
, as absolutely, to be in temperature by secondary mixing thing by the solvent total amount that the first solvent and the second solvent are formed 105 DEG C, pressure is flashed under conditions of being 0.028MPa, boils off 70% solvent;
Secondary mixing thing after flash distillation is subjected to stone roller page, cutting, film is made, film extrusion is molded, wherein, extrusion temperature Spend for 193 DEG C, steam pressure is controlled and included successively in 0.7MPa, then microwave vulcanization, microwave vulcanization in extrusion:One section Microwave vulcanization, two sections of hot-air cures, wherein, one section of microwave vulcanization section temperature is 195 DEG C, one section of temperature of two sections of hot-air cures Spend for 183 DEG C, two sections of temperature of two sections of hot-air cures are 170 DEG C;
Wherein, the particle size range of white carbon is -800 mesh of 600 mesh.
Comparative example 1
Field operation compounded rubber is prepared according to the method for embodiment 3, unlike, the particle size range of white carbon is 1000 The mesh of mesh -1200, the second solvent is ethyl acetate, and the additive amount of carbon black is changed to 40 parts.
Comparative example 2
Field operation compounded rubber is prepared according to the method for embodiment 3, unlike, the particle size range of white carbon is 1000 The mesh of mesh -1200, the second solvent is ethyl acetate, and the additive amount of carbon black is changed to 40 parts, in addition, by pretreatment enhancers 10 Part is replaced with the mixture of 10 parts of boron fibres and silane coupling agent, wherein, boron fibre and each 5 parts of silane coupling agent.
Comparative example 3
The preparation method of field operation compounded rubber, comprises the following steps:
In parts by weight, the pre- place in 35 parts of polypropylene, 110 parts of methyl vinyl silicone rubber, 30 parts of carbon black, preparation example 3 6.5 parts of 15 parts of reinforcing agent, 6.5 parts of zinc oxide, 2.5 parts of Fe-series catalyst and antioxidant are managed in 195 DEG C of rotating speeds as 250r/min's Under the conditions of carry out a mixing 18min, then in 130 DEG C stand 35min;
Added in a mixing thing after standing 9.5 parts of 21 parts of white carbon and vulcanizing agent in 175 DEG C of rotating speeds be 450r/ Secondary mixing 9min is carried out under conditions of min;Wherein, the second solvent is the mixture of ethyl acetate and hexamethylene, ethyl acetate Weight ratio with hexamethylene is 2:2;
Secondary mixing thing is subjected to stone roller page, cutting, film is made, film extrusion is molded, wherein, extrusion temperature 193 DEG C, steam pressure is controlled and included successively in 0.7MPa, then microwave vulcanization, microwave vulcanization in extrusion:One section of microwave sulphur Change, two sections of hot-air cures, wherein, one section of microwave vulcanization section temperature is 195 DEG C, and one section of temperature of two sections of hot-air cures is 183 DEG C, two sections of temperature of two sections of hot-air cures are 170 DEG C;
Wherein, the particle size range of white carbon is -800 mesh of 600 mesh.
Comparative example 4
The preparation method of field operation compounded rubber, comprises the following steps:
In parts by weight, 35 parts of polypropylene, 65 parts of the first solvent, 110 parts of methyl vinyl silicone rubber, 30 parts of carbon black, system 6.5 parts of 15 parts of pretreatment enhancers, 6.5 parts of zinc oxide, 2.5 parts of Fe-series catalyst and antioxidant in standby example 3 are in 195 DEG C of rotating speeds To carry out a mixing 18min under conditions of 250r/min, then 35min is stood in 130 DEG C;
9.5 parts of 65 parts of the second solvent, 21 parts of white carbon and vulcanizing agent are added in a mixing thing after standing in 175 DEG C Rotating speed carries out secondary mixing 9min under conditions of being 450r/min;Wherein, the second solvent is the mixing of ethyl acetate and hexamethylene The weight ratio of thing, ethyl acetate and hexamethylene is 2:2;
, as absolutely, to be in temperature by secondary mixing thing by the solvent total amount that the first solvent and the second solvent are formed 105 DEG C, pressure is flashed under conditions of being 0.028MPa, boils off 40% solvent;
Secondary mixing thing after flash distillation is subjected to stone roller page, cutting, film is made, film extrusion is molded, wherein, extrusion temperature Spend for 193 DEG C, steam pressure is controlled and included successively in 0.7MPa, then microwave vulcanization, microwave vulcanization in extrusion:One section Microwave vulcanization, two sections of hot-air cures, wherein, one section of microwave vulcanization section temperature is 195 DEG C, one section of temperature of two sections of hot-air cures Spend for 183 DEG C, two sections of temperature of two sections of hot-air cures are 170 DEG C;
Wherein, the particle size range of white carbon is -800 mesh of 600 mesh.
Detect example 1
In embodiment 1-3 and comparative example 1-4, it is divided into activity duration and actual operating time.Activity duration is according to system The effective operation time that Preparation Method carries out, and actual operating time includes because the time of the shutdown such as glutinous roller of cleaning, is from going into operation To the total time for preparing completion.
In preparation process, the mixing situation in embodiment 1-3 and comparative example 1-4 is observed, it is timely to there is glutinous roller phenomenon Cleaning is shut down, continues operation after cleaning, downtime is not counted in the activity duration.
It was found that in embodiment 1-3, comparative example 4, substantially without glutinous roller phenomenon, material is uniform, mixes all right, embodiment 1- 3rd, the activity duration in comparative example 4 is actual operating time.And in comparative example 1-3, repeatedly there is glutinous roller phenomenon, phenomenon is thing Expect into bulk, sticking cannot drop on roller, it is necessary to operating personnel repeatedly shuts down cleaning gets off, according to statistics, the reality in comparative example 2,3 The border operating time increases significantly than the activity duration, and wherein the activity duration increases 60% in comparative example 2, is actually grasped in comparative example 3 It is longer by 50% than activity duration to make the time, and the actual operating time in comparative example 1 is longer by 45% than activity duration.
Detect example 2
Composite rubber material in embodiment 1-3 and comparative example 1-4 is tested according to the method in national standard GB/T1040-2006 Tensile strength, the AG-20KNG of puller system model Shimadzu Corporation production;Rate of extension is 500mm/min, test temperature 23 ℃.It is according to the tensile strength retention rate after UL62-2001 tests ultraviolet light (argon arc lamp) aging 720h and -70 DEG C of low-temperature bendings No cracking.Single sampling is no less than 10.
It was found that tensile strength, tensile strength retention rate compare between each sample of composite rubber material in embodiment 1-3 Uniformly, and the tensile strength being above in comparative example 1-4 and at least the 5% of tensile strength retention rate.In wherein embodiment 1-3, Minimum with the performance of embodiment 1, the average tensile strength in embodiment 1 is 21.3N/mm2, ultraviolet light and aging 720h (argon arc lamp) Tensile strength retention rate is 94% afterwards.
Although the peak of the tensile strength and tensile strength retention rate in comparative example 1-3 differs not with embodiment 1 Greatly, still, the detection parameters difference of each sample is larger in comparative example 1-3, the most obvious with the performance of sample in comparative example 2,3, The tensile strength that wherein there is sample in comparative example 2,3 can reach 19.5N/mm2, and the tensile strength of minimum sample only has 16.1N/mm2
Moreover, it is observed that under -70 DEG C of low temperature bend tests, the not cracking feelings of sample in embodiment 1-3 Condition, and cracking situation in comparative example 1-3, cracking ratio is in 30-70%.
It can be seen from the above that the present invention not only solves the glutinous roller phenomenon in preparation process, and obtained compounded rubber The performance of sample is more uniform, this is uniformly undivided with being kneaded in preparation process.
And roller phenomenon is sticked in comparative example 1-3 and is repeatedly occurred, cause actual operating time not only to be grown, but also obtained compound rubber The performance of glue is uneven, the tensile strength some of sample have greatly it is small, this with preparation process raw material it is blocking, it is impossible to be uniformly mixed It is undivided.Moreover, although addO-on therapy is not much different with embodiment 3, the tensile strength and anti-tensile of sample are strong Retention rate is spent compared with having declined in embodiment 3, is traced it to its cause, it may be possible to which the extension of actual operating time, causes raw material in height Cracked in the case of heat.
And although comparative example 4 does not stick roller in preparation process, the tensile strength of sample is relatively low, its tensile strength only has 18.9N/mm2, under -70 DEG C of low temperature bend tests, cracking ratio is 20%.As it can be seen that the additive amount of simple adjusting solvent, not It can obtain the compounded rubber of better performances.
The preferred embodiment of the present invention described in detail above, still, during present invention is not limited to the embodiments described above Detail, in the range of the technology design of the present invention, a variety of simple variants can be carried out to technical scheme, this A little simple variants belong to protection scope of the present invention.
It is further to note that each particular technique feature described in above-mentioned embodiment, in not lance In the case of shield, can be combined by any suitable means, in order to avoid unnecessary repetition, the present invention to it is various can The combination of energy no longer separately illustrates.
In addition, various embodiments of the present invention can be combined randomly, as long as it is without prejudice to originally The thought of invention, it should equally be considered as content disclosed in this invention.

Claims (10)

1. a kind of preparation method of field operation compounded rubber, it is characterised in that the described method comprises the following steps:
(1) boron fibre is mixed with silane coupling agent, obtains pretreatment enhancers;
(2) by polypropylene, the first solvent, methyl vinyl silicone rubber, carbon black, pretreatment enhancers, zinc oxide, Fe-series catalyst A mixing is carried out with antioxidant, is then stood;
(3) the second solvent, white carbon and vulcanizing agent are added in a mixing thing after standing and carries out secondary mixing;
(4) by the solvent total amount that the first solvent and the second solvent are formed, as absolutely, secondary mixing thing to be flashed, is steamed Remove the solvent of 60-80%;
(5) the secondary mixing thing after flash distillation is subjected to stone roller page, cutting, film is made, film extrusion is molded, microwave vulcanization;
Wherein, the particle size range of white carbon is -800 mesh of 600 mesh, and the weight ratio of carbon black and methyl vinyl silicone rubber is 1:3-5.
2. preparation method according to claim 1, wherein, in parts by weight, 30-40 parts of polypropylene, the first solvent 50-80 Part, 100-120 parts of methyl vinyl silicone rubber, 25-35 parts of carbon black, 10-20 parts of pretreatment enhancers, 5-8 parts of zinc oxide, iron system 2-3 parts of catalyst, 5-8 parts of antioxidant, 7-12 parts of the second 50-80 parts of solvent, 18-25 parts of white carbon and vulcanizing agent.
3. preparation method according to claim 1 or 2, wherein, the weight ratio of boron fibre and silane coupling agent is 2:1-3; And/or
Silane coupling agent is KH550, the one or more in KH560, KH570;Preferably,
Silane coupling agent is the mixture of KH550 and KH570, wherein, the weight ratio of KH550 and KH570 are 2:2-3.
4. preparation method according to claim 1 or 2, wherein, in step (1), mixing condition includes:In 130-180 DEG C Rotating speed mixes 30-50min under conditions of being 500-800rpm.
5. preparation method according to claim 1 or 2, wherein, the condition of a mixing includes:In 190-200 DEG C of rotating speed For mixing 15-20min under conditions of 200-300r/min;And/or
The condition of standing includes:30-40min is stood in 120-140 DEG C.
6. preparation method according to claim 1 or 2, wherein, the condition of secondary mixing includes:In 170-180 DEG C of rotating speed For mixing 8-10min under conditions of 400-500r/min;And/or
Extrusion condition includes:Extrusion temperature is 190-195 DEG C, and steam pressure control is in 0.6-0.8MPa in extrusion.
7. preparation method according to claim 1 or 2, wherein, microwave vulcanization includes successively:One section of microwave vulcanization, two sections Hot-air cure;Preferably,
One section of microwave vulcanization section temperature is 190-200 DEG C, and one section of temperature of two sections of hot-air cures is 180-185 DEG C, two sections of heat Two sections of temperature of air cure are 165-175 DEG C.
8. preparation method according to claim 1 or 2, wherein, the condition of flash distillation includes:Temperature is 90-120 DEG C, pressure For 0.025-0.030MPa.
9. preparation method according to claim 1 or 2, wherein, Fe-series catalyst is triacetyl acetone iron and isooctyl acid One or more in the organoiron compounds such as iron;And/or
First solvent is the one or more in lauryl alcohol, ethyl acetate, glycerine and hexamethylene;And/or
Second solvent is ethyl acetate and the mixture of hexamethylene;Preferably, the weight of ethyl acetate and hexamethylene in the second solvent Amount is than being 2:1-3;And/or
Antioxidant is irgasfos 168 and/or antioxidant 264;And/or
Vulcanizing agent is the one or more in sulphur, benzoyl peroxide and urethanes;And/or
Polyacrylic weight average molecular weight is 10000-30000.
10. the field operation compounded rubber being prepared according to claim 1-9 any one of them preparation methods.
CN201810034849.9A 2018-01-15 2018-01-15 Field operation compounded rubber and preparation method thereof Pending CN108034260A (en)

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Publication number Priority date Publication date Assignee Title
CN108623924A (en) * 2018-05-23 2018-10-09 芜湖航天特种电缆厂股份有限公司 Igniter motor composite cable sealing sheath and preparation method thereof
CN108641244A (en) * 2018-05-23 2018-10-12 芜湖航天特种电缆厂股份有限公司 Igniter motor compounded rubber and preparation method thereof
CN108659415A (en) * 2018-05-23 2018-10-16 芜湖航天特种电缆厂股份有限公司 Aerospace composite cable and preparation method thereof
CN108707287A (en) * 2018-05-23 2018-10-26 芜湖航天特种电缆厂股份有限公司 Igniter motor composite cable and preparation method thereof
CN108892871A (en) * 2018-05-23 2018-11-27 芜湖航天特种电缆厂股份有限公司 Composite cable and preparation method thereof

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CN107400369A (en) * 2017-09-12 2017-11-28 芜湖航天特种电缆厂股份有限公司 Undersea detection corrosion resistant compounded rubber and preparation method thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107400369A (en) * 2017-09-12 2017-11-28 芜湖航天特种电缆厂股份有限公司 Undersea detection corrosion resistant compounded rubber and preparation method thereof

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108623924A (en) * 2018-05-23 2018-10-09 芜湖航天特种电缆厂股份有限公司 Igniter motor composite cable sealing sheath and preparation method thereof
CN108641244A (en) * 2018-05-23 2018-10-12 芜湖航天特种电缆厂股份有限公司 Igniter motor compounded rubber and preparation method thereof
CN108659415A (en) * 2018-05-23 2018-10-16 芜湖航天特种电缆厂股份有限公司 Aerospace composite cable and preparation method thereof
CN108707287A (en) * 2018-05-23 2018-10-26 芜湖航天特种电缆厂股份有限公司 Igniter motor composite cable and preparation method thereof
CN108892871A (en) * 2018-05-23 2018-11-27 芜湖航天特种电缆厂股份有限公司 Composite cable and preparation method thereof

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Application publication date: 20180515