CN105860288A - Ozone-proof and anti-aging modified ethylene propylene rubber cable material and preparation method thereof - Google Patents

Ozone-proof and anti-aging modified ethylene propylene rubber cable material and preparation method thereof Download PDF

Info

Publication number
CN105860288A
CN105860288A CN201610402924.3A CN201610402924A CN105860288A CN 105860288 A CN105860288 A CN 105860288A CN 201610402924 A CN201610402924 A CN 201610402924A CN 105860288 A CN105860288 A CN 105860288A
Authority
CN
China
Prior art keywords
parts
ethylene propylene
rubber
ozone
powder
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201610402924.3A
Other languages
Chinese (zh)
Inventor
产俊涛
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Individual
Original Assignee
Individual
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Individual filed Critical Individual
Priority to CN201610402924.3A priority Critical patent/CN105860288A/en
Publication of CN105860288A publication Critical patent/CN105860288A/en
Pending legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L23/00Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
    • C08L23/02Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L23/16Elastomeric ethene-propene or ethene-propene-diene copolymers, e.g. EPR and EPDM rubbers
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01BCABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B3/00Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
    • H01B3/18Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances
    • H01B3/28Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances natural or synthetic rubbers
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00Applications
    • C08L2203/20Applications use in electrical or conductive gadgets
    • C08L2203/202Applications use in electrical or conductive gadgets use in electrical wires or wirecoating
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/02Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/03Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C08L2205/035Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend

Landscapes

  • Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Organic Insulating Materials (AREA)
  • Inorganic Insulating Materials (AREA)

Abstract

The invention discloses an ozone-proof and anti-aging modified ethylene propylene rubber cable material. The ozone-proof and anti-aging modified ethylene propylene rubber cable material is prepared from ethylene propylene diene terpolymer, ethylene propylene monomer, fluororubber, epichlorohydrin rubber, hydrogenated butadiene-acrylonitrile rubber, phenylene silicone rubber, calcium stearate, zirconium fluoride, molybdenum disulfide, sulphur, zinc borate, magnesium hydroxide, ammonium molybdate, antimonous oxide, a silane coupling agent, triallyl cyanurate, resorcinol, fumed silica, maleic anhydride, azodiisobutyronitrile, dimethylbenzene, cyclohexane, acetyl tributyl citrate, epoxidized soybean oil, an antioxidant, an anti-aging agent CPPD, an antiozonant CTU and an additive. The invention further discloses a preparation method of the ozone-proof and anti-aging modified ethylene propylene rubber cable material. The obtained cable material has the excellent aging resistance and ozone resistance and has the wide market prospect.

Description

Modified epr cable compound that a kind of resistance to ozone is ageing-resistant and preparation method thereof
Technical field
The present invention relates to electric power field of material technology, modified epr cable compound that a kind of resistance to ozone is ageing-resistant and Preparation method.
Background technology
Wires and cables industry is the second largest industry that China is only second to automobile industry, and product variety Service Efficiency and domestic market are occupied Rate is all more than 90%.Worldwide, China's electric wire gross output value has exceeded the U.S., becomes the first big electric wire in the world Cable manufacturing country.Along with China's wires and cables industry high speed development, creation of new enterprise quantity constantly rises, industry overall technology Level is largely increased.
China's economic growth continuously and healthily, provides the huge market space for cable products, the temptation that Chinese market is strong Power so that the world all focuses on Chinese market sight, in the decades that reform and opening-up is short, cable manufacturing industry institute of China shape The huge production capacity become allows the world regard with special esteem.Along with China electric power industry, data communication industry, urban track traffic industry, The continuous expansion of the industry size such as car industry and shipbuilding, also will increase rapidly the demand of electric wire, following electric wire Industry also has huge development potentiality.
CABLE MATERIALS is wire cable insulating and sheath plastics.CABLE MATERIALS is the most of many uses, and its performance indications are had spy Different requirement, such as insulating properties, hot strength, use temperature, the index such as fire resistance all to have strict requirements, constantly Improve the performance of CABLE MATERIALS, be the urgent needs of economy and social development.
EP rubbers is the copolymer synthesized for primary raw material with ethylene and propylene, is also the important materials of CABLE MATERIALS, second the third rubber Glue performance in terms of ageing-resistant, ozone resistance is good, with its for the CABLE MATERIALS that material is made also have good ageing-resistant, Ozone resistance.Along with the development of society, market proposes higher requirement to the performance of CABLE MATERIALS, as some special occasions are wanted Asking CABLE MATERIALS to have higher resistance to ozone, ageing-resistant performance, existing CABLE MATERIALS the most gradually cannot meet the demand in market.
Summary of the invention
It is an object of the invention to provide ageing-resistant modified epr cable compound of a kind of resistance to ozone and preparation method thereof, to solve The problem certainly proposed in above-mentioned background technology.
For achieving the above object, the present invention provides following technical scheme:
The modified epr cable compound that a kind of resistance to ozone is ageing-resistant, is made up of according to the raw material of weight portion following: EPDM Rubber 45-49 part, ethylene propylene monomer 18-22 part, fluorubber 20-25 part, epichlorohydrin rubber 13-16 part, hydrogenated butyronitrile Rubber 5-8 part, phenylene silicone rubber 10-15 part, calcium stearate 3-6 part, Zirconium tetrafluoride. 1-3 part, molybdenum bisuphide 1-3 part, Sulfur 1-2 part, Firebrake ZB 4-6 part, magnesium hydroxide 13-17 part, ammonium molybdate 2-5 part, antimony oxide 0.8-2.0 part, Silane coupler 3-5 part, triallyl cyanurate 1.5-3.0 part, resorcinol 1.2-1.8 part, gas-phase silica 16-20 Part, maleic anhydride 6-10 part, azodiisobutyronitrile 0.5-0.8 part, dimethylbenzene 12-17 part, hexamethylene 7-11 part, second Acyl tributyl citrate 2-5 part, epoxy soybean oil 3-6 part, irgasfos 168 2.0-2.8 part, age resistor CPPD 3-5 Part, antiozonant CTU 1.5-2.5 part, additive 5-8 part;Described additive is made up of according to the raw material of weight portion following: Kyanite 8-11 part, Maifanitum 3-5 part, carborundum 4-7 part, beryllium oxide 1-3 part, zinc stearate 2-5 part, crosslinking Agent DCP 1-3 part, ferrocene 1.0-1.5 part, fluorographite 0.6-1.4 part, methyl vinyl silicon oil 1.8-2.5 part, Titanate coupling agent 2.5-3.2 part, polyvinyl butyral 1-3 part.
As the further scheme of the present invention: be made up of according to the raw material of weight portion following: ethylene propylene diene rubber 46-48 part, Ethylene propylene monomer 19-21 part, fluorubber 21-24 part, epichlorohydrin rubber 14-15 part, hydrogenated nitrile-butadiene rubber 6-7 part, benzene Support silicone rubber 11-14 part, calcium stearate 4-5 part, Zirconium tetrafluoride. 1.2-2.5 part, molybdenum bisuphide 1.5-2.7 part, sulfur 1.3-1.8 Part, Firebrake ZB 4.2-5.7 part, magnesium hydroxide 14-16 part, ammonium molybdate 3-4 part, antimony oxide 0.9-1.8 part, silicon Alkane coupling agent 3.5-4.5 part, triallyl cyanurate 1.7-2.8 part, resorcinol 1.3-1.6 part, gas-phase silica 17-19 part, maleic anhydride 7-9 part, azodiisobutyronitrile 0.6-0.7 part, dimethylbenzene 13-16 part, hexamethylene 8-10 part, Tributyl 2-acetylcitrate 3-4 part, epoxy soybean oil 4-5 part, irgasfos 168 2.2-2.7 part, age resistor CPPD 3.2-4.6 Part, antiozonant CTU 1.7-2.3 part, additive 6-7 part;Described additive is made up of according to the raw material of weight portion following: Kyanite 9-10 part, Maifanitum 3.3-4.6 part, carborundum 5-6 part, beryllium oxide 1.2-2.9 part, zinc stearate 3-4 Part, crosslink agent DCP 1.5-2.5 part, ferrocene 1.1-1.4 part, fluorographite 0.8-1.2 part, methyl vinyl silicon oil 1.9-2.4 part, titanate coupling agent 2.7-3.1 part, polyvinyl butyral 1.5-2.5 part.
As the present invention further scheme: be made up of according to the raw material of weight portion following: ethylene propylene diene rubber 47 parts, Ethylene propylene monomer 20 parts, fluororubber 23 part, epichlorohydrin rubber 14.5 parts, hydrogenated nitrile-butadiene rubber 6.8 parts, penylene silicon rubber 12 parts of glue, calcium stearate 4.2 parts, Zirconium tetrafluoride. 1.9 parts, molybdenum bisuphide 2.1 parts, 1.5 parts of sulfur, Firebrake ZB 4.7 Part, 15 parts of magnesium hydroxide, ammonium molybdate 3.4 parts, antimony oxide 1.4 parts, silane coupler 4 parts, cyanuric acid three Allyl ester 2.3 parts, resorcinol 1.4 parts, gas-phase silica 18 parts, maleic anhydride 8 parts, azodiisobutyronitrile 0.6 Part, dimethylbenzene 15 parts, hexamethylene 9 parts, tributyl 2-acetylcitrate 3.6 parts, epoxy soybean oil 4 parts, irgasfos 168 2.5 parts, age resistor CPPD 3.7 parts, antiozonant CTU 1.9 parts, additive 7 parts;Described additive is pressed by following Raw material according to weight portion forms: kyanite 9 parts, Maifanitum 3.8 parts, carborundum 5.5 parts, beryllium oxide 2.1 parts, tristearin Acid 3.4 parts of zinc, crosslink agent DCP 2 parts, ferrocene 1.3 parts, fluorographite 1.1 parts, methyl vinyl silicon oil 2.2 parts, Titanate coupling agent 2.9 parts, polyvinyl butyral 2 parts.
The preparation method of the modified epr cable compound that described resistance to ozone is ageing-resistant, step is as follows:
1) weigh kyanite, Maifanitum, carborundum and beryllium oxide, after pulverizing, cross 150-200 mesh sieve, and add to ball In grinding machine, using sodium hydroxide solution as ball milling liquid, ball milling mixing 3-5h, after ball milling, filter, dry, it is thus achieved that the One mixed-powder;
2) the first mixed-powder is added to calcining furnace, calcination processing 1-2h at 850-900 DEG C, it is thus achieved that microcrystalline powder;
3), after being pulverized by microcrystalline powder, zinc stearate, ferrocene and fluorographite, dry ball milling 3-5h are added, it is thus achieved that the Two mixed-powders;
4) weigh crosslink agent DCP, methyl vinyl silicon oil, titanate coupling agent and polyvinyl butyral, after merging, add Second mixed-powder, puts into agitating device, stirring mixing 1-2h under 2500-3000r/min, it is thus achieved that additive, Standby;
5) calcium stearate, Zirconium tetrafluoride., molybdenum bisuphide, sulfur, Firebrake ZB, magnesium hydroxide, ammonium molybdate and three oxidations are weighed Two antimony, after pulverizing, 150-200 mesh sieve excessively, dry ball milling 3-5h, it is thus achieved that the 3rd mixed-powder, standby;
6) ethylene propylene diene rubber, ethylene propylene monomer, fluorubber, epichlorohydrin rubber, hydrogenated nitrile-butadiene rubber, penylene silicon are weighed Rubber, gas-phase silica, maleic anhydride, azodiisobutyronitrile, dimethylbenzene and hexamethylene, put into banbury, heat up To 70-75 DEG C, banburying 20-25min, it is warming up to 82-86 DEG C, is subsequently adding additive, the 3rd mixed-powder, silane occasionally Join agent, triallyl cyanurate, resorcinol, tributyl 2-acetylcitrate, epoxy soybean oil, irgasfos 168, prevent Old agent CPPD and antiozonant CTU, banburying 10-15min, it is thus achieved that banburying product;
7) by the feeding mill of banburying product thin logical 3-5 time, it is thus achieved that granulation material;
8) granulation material is put in screw extruder, extruding pelletization, then drying, screen, pack after i.e. obtain CABLE MATERIALS.
Compared with prior art, the invention has the beneficial effects as follows:
CABLE MATERIALS prepared by the present invention is performance excellence in terms of ageing-resistant, ozone resistance, it is possible to meet market in specific occasion Under demand to CABLE MATERIALS performance, there is wide market prospect.
Detailed description of the invention
Below in conjunction with detailed description of the invention, technical scheme is described in more detail.
Embodiment 1
The modified epr cable compound that a kind of resistance to ozone is ageing-resistant, is made up of according to the raw material of weight portion following: EPDM Rubber 45 parts, ethylene propylene monomer 18 parts, fluorubber 20 parts, epichlorohydrin rubber 13 parts, hydrogenated nitrile-butadiene rubber 5 parts, benzene Support 10 parts of silicone rubber, calcium stearate 3 parts, Zirconium tetrafluoride. 1 part, molybdenum bisuphide 1 part, 1 part of sulfur, Firebrake ZB 4 parts, 13 parts of magnesium hydroxide, ammonium molybdate 2 parts, antimony oxide 0.8 part, silane coupler 3 parts, triallyl cyanurate 1.5 parts, resorcinol 1.2 parts, gas-phase silica 16 parts, maleic anhydride 6 parts, azodiisobutyronitrile 0.5 part, diformazan Benzene 12 parts, hexamethylene 7 parts, tributyl 2-acetylcitrate 2 parts, epoxy soybean oil 3 parts, irgasfos 168 2 parts, anti- Old agent CPPD 3 parts, antiozonant CTU 1.5 parts, additive 5 parts;Described additive is by following former according to weight portion Material composition: kyanite 8 parts, Maifanitum 3 parts, carborundum 4 parts, beryllium oxide 1 part, zinc stearate 2 parts, crosslink agent DCP 1 part, ferrocene 1 part, fluorographite 0.6 part, methyl vinyl silicon oil 1.8 parts, titanate coupling agent 2.5 parts, poly- Butyral 1 part.
The preparation method of the modified epr cable compound that resistance to ozone described in the present embodiment is ageing-resistant, step is as follows:
1) weigh kyanite, Maifanitum, carborundum and beryllium oxide, after pulverizing, cross 150 mesh sieves, and add to ball mill In, using sodium hydroxide solution as ball milling liquid, ball milling mixing 3h, after ball milling, filter, dry, it is thus achieved that the first mixing Powder;
2) the first mixed-powder is added to calcining furnace, calcination processing 1h at 850 DEG C, it is thus achieved that microcrystalline powder;
3), after being pulverized by microcrystalline powder, zinc stearate, ferrocene and fluorographite, dry ball milling 3h, it is thus achieved that second are added Mixed-powder;
4) weigh crosslink agent DCP, methyl vinyl silicon oil, titanate coupling agent and polyvinyl butyral, after merging, add Second mixed-powder, puts into agitating device, stirring mixing 1h under 2500r/min, it is thus achieved that additive, standby;
5) calcium stearate, Zirconium tetrafluoride., molybdenum bisuphide, sulfur, Firebrake ZB, magnesium hydroxide, ammonium molybdate and three oxidations are weighed Two antimony, after pulverizing, 150 mesh sieves excessively, dry ball milling 3h, it is thus achieved that the 3rd mixed-powder, standby;
6) ethylene propylene diene rubber, ethylene propylene monomer, fluorubber, epichlorohydrin rubber, hydrogenated nitrile-butadiene rubber, penylene silicon are weighed Rubber, gas-phase silica, maleic anhydride, azodiisobutyronitrile, dimethylbenzene and hexamethylene, put into banbury, heat up To 70 DEG C, banburying 20min, it is warming up to 82 DEG C, is subsequently adding additive, the 3rd mixed-powder, silane coupler, trimerization Cyanic acid triallyl, resorcinol, tributyl 2-acetylcitrate, epoxy soybean oil, irgasfos 168, age resistor CPPD and Antiozonant CTU, banburying 10min, it is thus achieved that banburying product;
7) banburying product is sent into thin in mill leading to 3 times, it is thus achieved that granulation material;
8) granulation material is put in screw extruder, extruding pelletization, then drying, screen, pack after i.e. obtain CABLE MATERIALS.
Embodiment 2
The modified epr cable compound that a kind of resistance to ozone is ageing-resistant, is made up of according to the raw material of weight portion following: EPDM Rubber 46 parts, ethylene propylene monomer 19 parts, fluorubber 24 parts, epichlorohydrin rubber 15 parts, hydrogenated nitrile-butadiene rubber 6 parts, benzene Support 11 parts of silicone rubber, calcium stearate 6 parts, Zirconium tetrafluoride. 1 part, molybdenum bisuphide 1.5 parts, 1 part of sulfur, Firebrake ZB 6 parts, 14 parts of magnesium hydroxide, ammonium molybdate 2 parts, antimony oxide 0.9 part, silane coupler 3.2 parts, cyanuric acid three allyl Ester 1.8 parts, resorcinol 1.5 parts, gas-phase silica 20 parts, maleic anhydride 6 parts, azodiisobutyronitrile 0.6 part, Dimethylbenzene 14 parts, hexamethylene 9 parts, tributyl 2-acetylcitrate 3 parts, epoxy soybean oil 4 parts, irgasfos 168 2.2 Part, age resistor CPPD 3 parts, antiozonant CTU 1.7 parts, additive 6 parts;Described additive by following according to weight The raw material composition of part: kyanite 10 parts, Maifanitum 3.5 parts, carborundum 4.5 parts, beryllium oxide 1 part, zinc stearate 2 Part, crosslink agent DCP 1.3 parts, ferrocene 1.1 parts, fluorographite 0.8 part, methyl vinyl silicon oil 1.9 parts, metatitanic acid Ester coupling agent 3 parts, polyvinyl butyral 1.5 parts.
The preparation method of the modified epr cable compound that resistance to ozone described in the present embodiment is ageing-resistant, step is as follows:
1) weigh kyanite, Maifanitum, carborundum and beryllium oxide, after pulverizing, cross 200 mesh sieves, and add to ball mill In, using sodium hydroxide solution as ball milling liquid, ball milling mixing 3.5h, after ball milling, filter, dry, it is thus achieved that first mixes Close powder;
2) the first mixed-powder is added to calcining furnace, calcination processing 1.5h at 860 DEG C, it is thus achieved that microcrystalline powder;
3), after being pulverized by microcrystalline powder, zinc stearate, ferrocene and fluorographite, dry ball milling 3.5h are added, it is thus achieved that the Two mixed-powders;
4) weigh crosslink agent DCP, methyl vinyl silicon oil, titanate coupling agent and polyvinyl butyral, after merging, add Second mixed-powder, puts into agitating device, stirring mixing 1h under 2700r/min, it is thus achieved that additive, standby;
5) calcium stearate, Zirconium tetrafluoride., molybdenum bisuphide, sulfur, Firebrake ZB, magnesium hydroxide, ammonium molybdate and three oxidations are weighed Two antimony, after pulverizing, 150 mesh sieves excessively, dry ball milling 3.5h, it is thus achieved that the 3rd mixed-powder, standby;
6) ethylene propylene diene rubber, ethylene propylene monomer, fluorubber, epichlorohydrin rubber, hydrogenated nitrile-butadiene rubber, penylene silicon are weighed Rubber, gas-phase silica, maleic anhydride, azodiisobutyronitrile, dimethylbenzene and hexamethylene, put into banbury, heat up To 72 DEG C, banburying 21min, it is warming up to 83 DEG C, is subsequently adding additive, the 3rd mixed-powder, silane coupler, trimerization Cyanic acid triallyl, resorcinol, tributyl 2-acetylcitrate, epoxy soybean oil, irgasfos 168, age resistor CPPD and Antiozonant CTU, banburying 12min, it is thus achieved that banburying product;
7) banburying product is sent into thin in mill leading to 4 times, it is thus achieved that granulation material;
8) granulation material is put in screw extruder, extruding pelletization, then drying, screen, pack after i.e. obtain CABLE MATERIALS.
Embodiment 3
The modified epr cable compound that a kind of resistance to ozone is ageing-resistant, is made up of according to the raw material of weight portion following: EPDM Rubber 47 parts, ethylene propylene monomer 20 parts, fluororubber 23 part, epichlorohydrin rubber 14.5 parts, hydrogenated nitrile-butadiene rubber 6.8 parts, Phenylene silicone rubber 12 parts, calcium stearate 4.2 parts, Zirconium tetrafluoride. 1.9 parts, molybdenum bisuphide 2.1 parts, 1.5 parts of sulfur, boron Acid 4.7 parts of zinc, 15 parts of magnesium hydroxide, ammonium molybdate 3.4 parts, antimony oxide 1.4 parts, silane coupler 4 parts, three Paracyanogen acid triallyl 2.3 parts, resorcinol 1.4 parts, gas-phase silica 18 parts, maleic anhydride 8 parts, azo two are different Butyronitrile 0.6 part, dimethylbenzene 15 parts, hexamethylene 9 parts, tributyl 2-acetylcitrate 3.6 parts, epoxy soybean oil 4 parts, Irgasfos 168 2.5 parts, age resistor CPPD 3.7 parts, antiozonant CTU 1.9 parts, additive 7 parts;Described interpolation Agent is made up of according to the raw material of weight portion following: kyanite 9 parts, Maifanitum 3.8 parts, carborundum 5.5 parts, beryllium oxide 2.1 Part, zinc stearate 3.4 parts, crosslink agent DCP 2 parts, ferrocene 1.3 parts, fluorographite 1.1 parts, methyl ethylene silicon Oil 2.2 parts, titanate coupling agent 2.9 parts, polyvinyl butyral 2 parts.
The preparation method of the modified epr cable compound that resistance to ozone described in the present embodiment is ageing-resistant, step is as follows:
1) weigh kyanite, Maifanitum, carborundum and beryllium oxide, after pulverizing, cross 200 mesh sieves, and add to ball mill In, using sodium hydroxide solution as ball milling liquid, ball milling mixing 4h, after ball milling, filter, dry, it is thus achieved that the first mixing Powder;
2) the first mixed-powder is added to calcining furnace, calcination processing 1.5h at 880 DEG C, it is thus achieved that microcrystalline powder;
3), after being pulverized by microcrystalline powder, zinc stearate, ferrocene and fluorographite, dry ball milling 4h, it is thus achieved that second are added Mixed-powder;
4) weigh crosslink agent DCP, methyl vinyl silicon oil, titanate coupling agent and polyvinyl butyral, after merging, add Second mixed-powder, puts into agitating device, stirring mixing 1.5h under 2800r/min, it is thus achieved that additive, standby;
5) calcium stearate, Zirconium tetrafluoride., molybdenum bisuphide, sulfur, Firebrake ZB, magnesium hydroxide, ammonium molybdate and three oxidations are weighed Two antimony, after pulverizing, 180 mesh sieves excessively, dry ball milling 4h, it is thus achieved that the 3rd mixed-powder, standby;
6) ethylene propylene diene rubber, ethylene propylene monomer, fluorubber, epichlorohydrin rubber, hydrogenated nitrile-butadiene rubber, penylene silicon are weighed Rubber, gas-phase silica, maleic anhydride, azodiisobutyronitrile, dimethylbenzene and hexamethylene, put into banbury, heat up To 72 DEG C, banburying 23min, it is warming up to 84 DEG C, is subsequently adding additive, the 3rd mixed-powder, silane coupler, trimerization Cyanic acid triallyl, resorcinol, tributyl 2-acetylcitrate, epoxy soybean oil, irgasfos 168, age resistor CPPD and Antiozonant CTU, banburying 13min, it is thus achieved that banburying product;
7) banburying product is sent into thin in mill leading to 4 times, it is thus achieved that granulation material;
8) granulation material is put in screw extruder, extruding pelletization, then drying, screen, pack after i.e. obtain CABLE MATERIALS.
Embodiment 4
The modified epr cable compound that a kind of resistance to ozone is ageing-resistant, is made up of according to the raw material of weight portion following: EPDM Rubber 48 parts, ethylene propylene monomer 21 parts, fluorubber 20 parts, epichlorohydrin rubber 16 parts, hydrogenated nitrile-butadiene rubber 7 parts, benzene Support 13 parts of silicone rubber, calcium stearate 6 parts, Zirconium tetrafluoride. 2.5 parts, molybdenum bisuphide 3 parts, 1.5 parts of sulfur, Firebrake ZB 5 Part, 15 parts of magnesium hydroxide, ammonium molybdate 5 parts, antimony oxide 1.6 parts, silane coupler 4.3 parts, cyanuric acid three Allyl ester 2.7 parts, resorcinol 1.5 parts, gas-phase silica 16 parts, maleic anhydride 10 parts, azodiisobutyronitrile 0.7 Part, dimethylbenzene 16 parts, hexamethylene 10 parts, tributyl 2-acetylcitrate 4 parts, epoxy soybean oil 5 parts, irgasfos 168 2.5 Part, age resistor CPPD 4 parts, antiozonant CTU 2 parts, additive 6 parts;Described additive by following according to weight portion Raw material composition: kyanite 10 parts, Maifanitum 4.5 parts, carborundum 6 parts, beryllium oxide 1.5 parts, zinc stearate 4 parts, Crosslink agent DCP 1 part, ferrocene 1.2 parts, fluorographite 1.2 parts, methyl vinyl silicon oil 2.2 parts, titanate esters coupling Agent 3 parts, polyvinyl butyral 2.5 parts.
The preparation method of the modified epr cable compound that resistance to ozone described in the present embodiment is ageing-resistant, step is as follows:
1) weigh kyanite, Maifanitum, carborundum and beryllium oxide, after pulverizing, cross 200 mesh sieves, and add to ball mill In, using sodium hydroxide solution as ball milling liquid, ball milling mixing 4.5h, after ball milling, filter, dry, it is thus achieved that first mixes Close powder;
2) the first mixed-powder is added to calcining furnace, calcination processing 1.5h at 890 DEG C, it is thus achieved that microcrystalline powder;
3), after being pulverized by microcrystalline powder, zinc stearate, ferrocene and fluorographite, dry ball milling 4h, it is thus achieved that second are added Mixed-powder;
4) weigh crosslink agent DCP, methyl vinyl silicon oil, titanate coupling agent and polyvinyl butyral, after merging, add Second mixed-powder, puts into agitating device, stirring mixing 1.5h under 2900r/min, it is thus achieved that additive, standby;
5) calcium stearate, Zirconium tetrafluoride., molybdenum bisuphide, sulfur, Firebrake ZB, magnesium hydroxide, ammonium molybdate and three oxidations are weighed Two antimony, after pulverizing, 200 mesh sieves excessively, dry ball milling 4h, it is thus achieved that the 3rd mixed-powder, standby;
6) ethylene propylene diene rubber, ethylene propylene monomer, fluorubber, epichlorohydrin rubber, hydrogenated nitrile-butadiene rubber, penylene silicon are weighed Rubber, gas-phase silica, maleic anhydride, azodiisobutyronitrile, dimethylbenzene and hexamethylene, put into banbury, heat up To 74 DEG C, banburying 23min, it is warming up to 85 DEG C, is subsequently adding additive, the 3rd mixed-powder, silane coupler, trimerization Cyanic acid triallyl, resorcinol, tributyl 2-acetylcitrate, epoxy soybean oil, irgasfos 168, age resistor CPPD and Antiozonant CTU, banburying 14min, it is thus achieved that banburying product;
7) banburying product is sent into thin in mill leading to 5 times, it is thus achieved that granulation material;
8) granulation material is put in screw extruder, extruding pelletization, then drying, screen, pack after i.e. obtain CABLE MATERIALS.
Embodiment 5
The modified epr cable compound that a kind of resistance to ozone is ageing-resistant, is made up of according to the raw material of weight portion following: EPDM Rubber 49 parts, ethylene propylene monomer 22 parts, fluorubber 25 parts, epichlorohydrin rubber 16 parts, hydrogenated nitrile-butadiene rubber 8 parts, benzene Support 15 parts of silicone rubber, calcium stearate 6 parts, Zirconium tetrafluoride. 3 parts, molybdenum bisuphide 3 parts, 2 parts of sulfur, Firebrake ZB 6 parts, 17 parts of magnesium hydroxide, ammonium molybdate 5 parts, antimony oxide 2.0 parts, silane coupler 5 parts, triallyl cyanurate 3.0 parts, resorcinol 1.8 parts, gas-phase silica 20 parts, maleic anhydride 10 parts, azodiisobutyronitrile 0.8 part, two Toluene 17 parts, hexamethylene 11 parts, tributyl 2-acetylcitrate 5 parts, epoxy soybean oil 6 parts, irgasfos 168 2.8 parts, Age resistor CPPD 5 parts, antiozonant CTU 2.5 parts, additive 8 parts;Described additive by following according to weight portion Raw material forms: kyanite 11 parts, Maifanitum 5 parts, carborundum 7 parts, beryllium oxide 3 parts, zinc stearate 5 parts, crosslinking Agent DCP 3 parts, ferrocene 1.5 parts, fluorographite 1.4 parts, methyl vinyl silicon oil 2.5 parts, titanate coupling agent 3.2 Part, polyvinyl butyral 3 parts.
The preparation method of the modified epr cable compound that resistance to ozone described in the present embodiment is ageing-resistant, step is as follows:
1) weigh kyanite, Maifanitum, carborundum and beryllium oxide, after pulverizing, cross 200 mesh sieves, and add to ball mill In, using sodium hydroxide solution as ball milling liquid, ball milling mixing 5h, after ball milling, filter, dry, it is thus achieved that the first mixing Powder;
2) the first mixed-powder is added to calcining furnace, calcination processing 2h at 900 DEG C, it is thus achieved that microcrystalline powder;
3), after being pulverized by microcrystalline powder, zinc stearate, ferrocene and fluorographite, dry ball milling 5h, it is thus achieved that second are added Mixed-powder;
4) weigh crosslink agent DCP, methyl vinyl silicon oil, titanate coupling agent and polyvinyl butyral, after merging, add Second mixed-powder, puts into agitating device, stirring mixing 2h under 3000r/min, it is thus achieved that additive, standby;
5) calcium stearate, Zirconium tetrafluoride., molybdenum bisuphide, sulfur, Firebrake ZB, magnesium hydroxide, ammonium molybdate and three oxidations are weighed Two antimony, after pulverizing, 200 mesh sieves excessively, dry ball milling 5h, it is thus achieved that the 3rd mixed-powder, standby;
6) ethylene propylene diene rubber, ethylene propylene monomer, fluorubber, epichlorohydrin rubber, hydrogenated nitrile-butadiene rubber, penylene silicon are weighed Rubber, gas-phase silica, maleic anhydride, azodiisobutyronitrile, dimethylbenzene and hexamethylene, put into banbury, heat up To 75 DEG C, banburying 25min, it is warming up to 86 DEG C, is subsequently adding additive, the 3rd mixed-powder, silane coupler, trimerization Cyanic acid triallyl, resorcinol, tributyl 2-acetylcitrate, epoxy soybean oil, irgasfos 168, age resistor CPPD and Antiozonant CTU, banburying 15min, it is thus achieved that banburying product;
7) banburying product is sent into thin in mill leading to 5 times, it is thus achieved that granulation material;
8) granulation material is put in screw extruder, extruding pelletization, then drying, screen, pack after i.e. obtain CABLE MATERIALS.
CABLE MATERIALS prepared by embodiment 1-5 is carried out performance test, and result is: hot strength is 17.9-18.5Mpa, disconnected Splitting percentage elongation is 328-376%, and after 136 DEG C × 168h hot air aging, stretching strength retentivity is 99.0-99.8%, Extension at break conservation rate is 98.3-99.4%, and under the conditions of 25 DEG C × 30h, ozone concentration 0.025-0.030%, flawless occurs.
CABLE MATERIALS prepared by the present invention is performance excellence in terms of ageing-resistant, ozone resistance, it is possible to meet market in specific occasion Under demand to CABLE MATERIALS performance, there is wide market prospect.
Above the better embodiment of the present invention is explained in detail, but the present invention is not limited to above-mentioned embodiment, In the ken that those of ordinary skill in the art is possessed, it is also possible to make each on the premise of without departing from present inventive concept Plant change.

Claims (4)

1. the modified epr cable compound that a resistance to ozone is ageing-resistant, it is characterised in that by following former according to weight portion Material composition: ethylene propylene diene rubber 45-49 part, ethylene propylene monomer 18-22 part, fluorubber 20-25 part, epichlorohydrin rubber 13-16 Part, hydrogenated nitrile-butadiene rubber 5-8 part, phenylene silicone rubber 10-15 part, calcium stearate 3-6 part, Zirconium tetrafluoride. 1-3 part, two sulfur Change molybdenum 1-3 part, sulfur 1-2 part, Firebrake ZB 4-6 part, magnesium hydroxide 13-17 part, ammonium molybdate 2-5 part, three oxidations two Antimony 0.8-2.0 part, silane coupler 3-5 part, triallyl cyanurate 1.5-3.0 part, resorcinol 1.2-1.8 part, Gas-phase silica 16-20 part, maleic anhydride 6-10 part, azodiisobutyronitrile 0.5-0.8 part, dimethylbenzene 12-17 part, Hexamethylene 7-11 part, tributyl 2-acetylcitrate 2-5 part, epoxy soybean oil 3-6 part, irgasfos 168 2.0-2.8 part, Age resistor CPPD 3-5 part, antiozonant CTU 1.5-2.5 part, additive 5-8 part;Described additive by following according to The raw material composition of weight portion: kyanite 8-11 part, Maifanitum 3-5 part, carborundum 4-7 part, beryllium oxide 1-3 part, hard Fat acid zinc 2-5 part, crosslink agent DCP 1-3 part, ferrocene 1.0-1.5 part, fluorographite 0.6-1.4 part, ethylene methacrylic Base silicone oil 1.8-2.5 part, titanate coupling agent 2.5-3.2 part, polyvinyl butyral 1-3 part.
The modified epr cable compound that resistance to ozone the most according to claim 1 is ageing-resistant, it is characterised in that by with Under according to weight portion raw material form: ethylene propylene diene rubber 46-48 part, ethylene propylene monomer 19-21 part, fluorubber 21-24 Part, epichlorohydrin rubber 14-15 part, hydrogenated nitrile-butadiene rubber 6-7 part, phenylene silicone rubber 11-14 part, calcium stearate 4-5 part, Zirconium tetrafluoride. 1.2-2.5 part, molybdenum bisuphide 1.5-2.7 part, sulfur 1.3-1.8 part, Firebrake ZB 4.2-5.7 part, hydroxide Magnesium 14-16 part, ammonium molybdate 3-4 part, antimony oxide 0.9-1.8 part, silane coupler 3.5-4.5 part, cyanuric acid Triallyl 1.7-2.8 part, resorcinol 1.3-1.6 part, gas-phase silica 17-19 part, maleic anhydride 7-9 part, idol Nitrogen bis-isobutyronitrile 0.6-0.7 part, dimethylbenzene 13-16 part, hexamethylene 8-10 part, tributyl 2-acetylcitrate 3-4 part, Epoxy soybean oil 4-5 part, irgasfos 168 2.2-2.7 part, age resistor CPPD 3.2-4.6 part, antiozonant CTU 1.7-2.3 Part, additive 6-7 part;Described additive is made up of according to the raw material of weight portion following: kyanite 9-10 part, Maifanitum 3.3-4.6 part, carborundum 5-6 part, beryllium oxide 1.2-2.9 part, zinc stearate 3-4 part, crosslink agent DCP 1.5-2.5 Part, ferrocene 1.1-1.4 part, fluorographite 0.8-1.2 part, methyl vinyl silicon oil 1.9-2.4 part, titanate esters coupling Agent 2.7-3.1 part, polyvinyl butyral 1.5-2.5 part.
The modified epr cable compound that resistance to ozone the most according to claim 2 is ageing-resistant, it is characterised in that by with Under according to weight portion raw material form: ethylene propylene diene rubber 47 parts, ethylene propylene monomer 20 parts, fluororubber 23 part, chlorine Ether rubber 14.5 parts, hydrogenated nitrile-butadiene rubber 6.8 parts, phenylene silicone rubber 12 parts, calcium stearate 4.2 parts, Zirconium tetrafluoride. 1.9 Part, molybdenum bisuphide 2.1 parts, 1.5 parts of sulfur, Firebrake ZB 4.7 parts, 15 parts of magnesium hydroxide, ammonium molybdate 3.4 parts, three Aoxidize 1.4 parts of two antimony, silane coupler 4 parts, triallyl cyanurate 2.3 parts, resorcinol 1.4 parts, gas phase white White carbon black 18 parts, maleic anhydride 8 parts, azodiisobutyronitrile 0.6 part, dimethylbenzene 15 parts, hexamethylene 9 parts, acetyl Fructus Citri Limoniae Acid tributyl 3.6 parts, epoxy soybean oil 4 parts, irgasfos 168 2.5 parts, age resistor CPPD 3.7 parts, antiozonant CTU 1.9 parts, additive 7 parts;Described additive is made up of according to the raw material of weight portion following: kyanite 9 parts, wheat meal 3.8 parts of stone, carborundum 5.5 parts, beryllium oxide 2.1 parts, zinc stearate 3.4 parts, crosslink agent DCP 2 parts, ferrocene 1.3 Part, fluorographite 1.1 parts, methyl vinyl silicon oil 2.2 parts, titanate coupling agent 2.9 parts, polyvinyl butyral 2 parts.
4. a preparation method for the modified epr cable compound that resistance to ozone as described in claim 1-3 is arbitrary is ageing-resistant, It is characterized in that, step is as follows:
1) weigh kyanite, Maifanitum, carborundum and beryllium oxide, after pulverizing, cross 150-200 mesh sieve, and add to ball In grinding machine, using sodium hydroxide solution as ball milling liquid, ball milling mixing 3-5h, after ball milling, filter, dry, it is thus achieved that the One mixed-powder;
2) the first mixed-powder is added to calcining furnace, calcination processing 1-2h at 850-900 DEG C, it is thus achieved that microcrystalline powder;
3), after being pulverized by microcrystalline powder, zinc stearate, ferrocene and fluorographite, dry ball milling 3-5h are added, it is thus achieved that the Two mixed-powders;
4) weigh crosslink agent DCP, methyl vinyl silicon oil, titanate coupling agent and polyvinyl butyral, after merging, add Second mixed-powder, puts into agitating device, stirring mixing 1-2h under 2500-3000r/min, it is thus achieved that additive, Standby;
5) calcium stearate, Zirconium tetrafluoride., molybdenum bisuphide, sulfur, Firebrake ZB, magnesium hydroxide, ammonium molybdate and three oxidations are weighed Two antimony, after pulverizing, 150-200 mesh sieve excessively, dry ball milling 3-5h, it is thus achieved that the 3rd mixed-powder, standby;
6) ethylene propylene diene rubber, ethylene propylene monomer, fluorubber, epichlorohydrin rubber, hydrogenated nitrile-butadiene rubber, penylene silicon are weighed Rubber, gas-phase silica, maleic anhydride, azodiisobutyronitrile, dimethylbenzene and hexamethylene, put into banbury, heat up To 70-75 DEG C, banburying 20-25min, it is warming up to 82-86 DEG C, is subsequently adding additive, the 3rd mixed-powder, silane occasionally Join agent, triallyl cyanurate, resorcinol, tributyl 2-acetylcitrate, epoxy soybean oil, irgasfos 168, prevent Old agent CPPD and antiozonant CTU, banburying 10-15min, it is thus achieved that banburying product;
7) by the feeding mill of banburying product thin logical 3-5 time, it is thus achieved that granulation material;
8) granulation material is put in screw extruder, extruding pelletization, then drying, screen, pack after i.e. obtain CABLE MATERIALS.
CN201610402924.3A 2016-06-08 2016-06-08 Ozone-proof and anti-aging modified ethylene propylene rubber cable material and preparation method thereof Pending CN105860288A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201610402924.3A CN105860288A (en) 2016-06-08 2016-06-08 Ozone-proof and anti-aging modified ethylene propylene rubber cable material and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610402924.3A CN105860288A (en) 2016-06-08 2016-06-08 Ozone-proof and anti-aging modified ethylene propylene rubber cable material and preparation method thereof

Publications (1)

Publication Number Publication Date
CN105860288A true CN105860288A (en) 2016-08-17

Family

ID=56677319

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201610402924.3A Pending CN105860288A (en) 2016-06-08 2016-06-08 Ozone-proof and anti-aging modified ethylene propylene rubber cable material and preparation method thereof

Country Status (1)

Country Link
CN (1) CN105860288A (en)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106674826A (en) * 2016-12-12 2017-05-17 天长市康宁塑胶科技有限公司 High-temperature-resistant and aging-resistant fluororubber material
CN106810722A (en) * 2016-12-20 2017-06-09 广西华锑科技有限公司 A kind of Mobyneb antimony oxide compound flame retardant and preparation method thereof
CN107033413A (en) * 2017-06-13 2017-08-11 江西吉恩重工有限公司 Ageing-resistant cable for ship material of a kind of resistance to ozone and preparation method thereof
CN107383473A (en) * 2017-07-24 2017-11-24 安徽超越电缆科技有限公司 A kind of wear-resisting ageing-resistant cable material
CN108059740A (en) * 2017-12-12 2018-05-22 雷春生 A kind of preparation method of ageing-resistant rubber

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103923403A (en) * 2014-05-10 2014-07-16 任新年 Zero-halogen low-smoke and flame-retardant rubber for electric wires and cables and preparing method for zero-halogen low-smoke and flame-retardant rubber
CN104151720A (en) * 2014-08-20 2014-11-19 江西电缆有限责任公司 Terpolymer EP rubber insulation formula and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103923403A (en) * 2014-05-10 2014-07-16 任新年 Zero-halogen low-smoke and flame-retardant rubber for electric wires and cables and preparing method for zero-halogen low-smoke and flame-retardant rubber
CN104151720A (en) * 2014-08-20 2014-11-19 江西电缆有限责任公司 Terpolymer EP rubber insulation formula and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
北京航空材料研究院主编: "《航空材料技术》", 31 December 2013 *

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106674826A (en) * 2016-12-12 2017-05-17 天长市康宁塑胶科技有限公司 High-temperature-resistant and aging-resistant fluororubber material
CN106810722A (en) * 2016-12-20 2017-06-09 广西华锑科技有限公司 A kind of Mobyneb antimony oxide compound flame retardant and preparation method thereof
CN107033413A (en) * 2017-06-13 2017-08-11 江西吉恩重工有限公司 Ageing-resistant cable for ship material of a kind of resistance to ozone and preparation method thereof
CN107033413B (en) * 2017-06-13 2019-02-15 江西吉恩重工有限公司 A kind of cable for ship material and preparation method thereof that resistance to ozone is ageing-resistant
CN107383473A (en) * 2017-07-24 2017-11-24 安徽超越电缆科技有限公司 A kind of wear-resisting ageing-resistant cable material
CN108059740A (en) * 2017-12-12 2018-05-22 雷春生 A kind of preparation method of ageing-resistant rubber

Similar Documents

Publication Publication Date Title
CN105860288A (en) Ozone-proof and anti-aging modified ethylene propylene rubber cable material and preparation method thereof
CN105017684B (en) The preparation method of flame retardant type high reliability CABLE MATERIALS
CN105778266A (en) High-strength oil resistant cable material and preparation method thereof
CN103013133B (en) A kind of automobile V-shaped circle sizing material and preparation method thereof
CN102746549A (en) Polyethylene insulation power cable material for coal and method for preparing the same
CN102153308A (en) Cement liquid grinding aid and preparation method thereof
CN105936707A (en) Oil resistant and high temperature resistant polyvinyl chloride cable material for automobiles and preparation method thereof
CN102965033B (en) Nano-mica powder modified compound adhesive for packaging
CN102965050B (en) A kind of adhesive for packaging of nano diatomite modification
CN104327394A (en) High-weather-resistance cable material and preparation method thereof
CN105885301A (en) Fatigue-resistant data transmission line and method for preparing same
CN103333380B (en) A kind of Sun-proof cable sheath material
CN104311937A (en) Acid and alkali resistant cable material with strong stability and preparation method thereof
CN105778206B (en) A kind of softness PE cable protective cover material and preparation method thereof
CN104311917A (en) Impact-resistant anti-aging cable material and preparation method thereof
CN105462080A (en) Anti-deformation heat preservation compound ethylene propylene diene monomer cable material and preparation method thereof
CN110698801A (en) High-fluidity graphene modified polystyrene composite material and preparation method thereof
CN110791027A (en) High-strength corrosion-resistant flame-retardant cable material
CN106832893B (en) A kind of isomerism recycling nylon of the crosslinking agent containing L-POSS and preparation method thereof
CN108070181A (en) A kind of PVC cable material of heat resistant and preparation method thereof
CN108047600A (en) A kind of polyvinyl chloride cable material of excellent fireproof performance and preparation method thereof
CN113462057A (en) Environment-friendly color master batch and preparation method thereof
CN104387801A (en) Modified calcium carbonate with enhanced anti-aging effect and preparation method thereof
CN112321956A (en) Rubber wire outer sheath for outdoor electrical appliance and preparation method thereof
CN105017603A (en) Easily processable cable material for large power and preparation method thereof

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication

Application publication date: 20160817

RJ01 Rejection of invention patent application after publication