CN109571825A - A kind of dedicated static conductive rubber of propellants machine and preparation method of sample - Google Patents

A kind of dedicated static conductive rubber of propellants machine and preparation method of sample Download PDF

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Publication number
CN109571825A
CN109571825A CN201811364375.0A CN201811364375A CN109571825A CN 109571825 A CN109571825 A CN 109571825A CN 201811364375 A CN201811364375 A CN 201811364375A CN 109571825 A CN109571825 A CN 109571825A
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static conductive
parts
conductive rubber
rubber
preparation
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Inventor
祁贝贝
张建功
李琨
王兴平
金龙
王俊峰
王昊
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INNER MONGOLIA SPACE HONGXIA CHEMICAL Co Ltd
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INNER MONGOLIA SPACE HONGXIA CHEMICAL Co Ltd
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Priority to CN201811364375.0A priority Critical patent/CN109571825A/en
Publication of CN109571825A publication Critical patent/CN109571825A/en
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C35/00—Heating, cooling or curing, e.g. crosslinking or vulcanising; Apparatus therefor
    • B29C35/02—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
    • C08K13/02—Organic and inorganic ingredients
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/02—Elements
    • C08K3/04—Carbon
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/001—Conductive additives

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Oral & Maxillofacial Surgery (AREA)
  • Thermal Sciences (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The invention discloses a kind of preparation method of sample of the dedicated static conductive rubber of propellants machine: being fabricated to 120mm × 150 mm × 2mm vulcanization test piece using mechanics sheet mold；Mechanics test piece is put into vulcanizing press, 150 DEG C~160 DEG C of curing temperature, sulfide stress 10MPa, vulcanization time is the min of 60min~70；Vulcanization terminates, and is cooled to room temperature, and test piece is cut into standard test piece size with special (purpose) rubber film cutter.Using sample prepared by static conductive rubber performance preparation method of sample of the invention, the test and indication of the performances such as resistance value, mechanical property, hardness, the density of static conductive rubber of the invention can be effectively used for.

Description

A kind of dedicated static conductive rubber of propellants machine and preparation method of sample
Technical field
The present invention relates to solid propellant manufacturing fields, and in particular to mixing of solid propellants process uses static conductive rubber The production of performance sample.
Background technique
Currently, domestic overwhelming majority solid propellant manufacturer has used vertical mixer to carry out propellants, The charging process of the energetic materials such as middle AP, RDX and HMX is automatically fed into the mixing kettle of mixing machine by deflector chute.Mixing When charging, there is the dust mixture of these types of component on the top of mixing kettle, since there is also other in propellant slurry Volatile components, therefore form in mixing kettle the explosion danger object of polynary multiphase.The moment that material is separated with deflector chute will Generate electrostatic, when static charge accumulation to a certain extent when, it may appear that spark discharge may excite dust and other volatile components Mixture kindling, and then cause the burning or explosion of a large amount of propellants.
The one kind of static conductive rubber as conductive polymer composites is to add conduction as matrix using rubber elastomer to fill out Material is prepared, and has not only remained the elasticity of base rubber, but also the electric conductivity with conductive filler.It feeds in mixing of solid propellants Electro-insulating rubber is replaced with static conductive rubber in system, the electric conductivity on charging system surface can be improved, electrostatic hazard is reduced, plays The effect of electrostatic protection.In the selection of static conductive rubber material, be capable of technique require refer mainly to indicate, sheet resistance value≤ 1.0×104Ω, soft, shore hardness≤60 °.Static conductive rubber surface resistance value standard currently on the market is wanted mostly Ask≤5 × 104Ω, 60~75 ° of shore hardness, wherein relative performance preferably HG2949-1999 static conductive rubber, through detecting table Surface resistance can satisfy≤1.0 × 104Ω requirement, but shore hardness is mostly more than 65 °.For characterizing the static conductive rubbery Can, because of the change of rubber material formula and technique, the made sample of other rubber performance preparation method of sample can not be applicable in.
Summary of the invention
To meet mixing of solid propellants manufacturing technique requirent, the present invention static conductive rubber matrix small by preferred hardness Rubber, reasonably optimizing conductive filler proportion increase softening agent proportion, improve calendering process performance, optimization sulfidization molding technique, add Add solid packing identical with current static conductive rubber, activator, vulcanizing system and anti-aging agent, by production sample and tests table Surface resistance guarantees that static conductive rubber electric conductivity meets current propellant and produces and uses index, according to mechanical property, hardness, The performance test results such as density produce shore hardness≤60 °, soft, sheet resistance value≤1.0 × 104Ω, and it is comprehensive The static conductive rubber compounding haveing excellent performance.Meet technique for propellants charging system after the static conductive rubber curing forming It is required that.
The specific technical solution that the present invention uses is as follows:
One, the dedicated static conductive rubber compounding of propellants machine
Base rubber is butyronitrile 4155, including vulcanizing agent, vulcanizing activator, vulcanization accelerator, plasticizer, anti-aging agent, conduction are filled out Material.
Prescription quality number are as follows: base rubber, 100；Vulcanizing agent, 1.0~1.8；Vulcanizing activator, 1.5~2.5；Vulcanization Promotor, 1.5~2.3；Plasticizer, 15~25；Anti-aging agent, 3~5；Conductive filler, 15~35.
Above-mentioned vulcanizing agent is sulphur or cumyl peroxide or lead peroxide, and vulcanizing activator is stearic acid and oxidation Zinc, vulcanization accelerator are altax or Vulcanization accelerator TMTD or accelerant CZ, and plasticizer is dibutyl phthalate or adjacent benzene Dioctyl phthalate dibutyl ester or tricresyl phosphate, anti-aging agent are antioxidant D or anti-aging agent RD or anti-aging agent BL, and conductive filler is conduction Carbon black and acetylene carbon black.In vulcanizing activator the prescription quality number of stearic acid and zinc oxide may respectively be 0.5~2 and 1.0~ 2.5.The prescription quality number of conductive black and acetylene carbon black may respectively be 10~20 and 5~15 in conductive filler.
Two, the dedicated static conductive rubber compounding preparation of propellants machine
The dedicated static conductive rubber compounding preparation of the propellants machine, including three process of preparing:
A kind of process 1, dedicated static conductive rubber compounding preparation method of propellants machine, is completed by following steps:
Step 1, using double roller opening rubber mixing machine, roll spacing≤0.5mm, 30 DEG C~40 DEG C of roller water flowing temperature, by butyronitrile 4155 100 parts of addition rubber mixing machines of base rubber, plasticate the time >=1min;
Step 2, roll spacing are gradually amplified to the mm of 2 mm~5,30 DEG C~40 DEG C of roller water flowing temperature, are slowly added to vulcanization accelerator, Mixing time >=2min;
Step 3, the roll spacing mm of 2 mm~5, are slowly added to vulcanizing activator, anti-aging agent by 30 DEG C~40 DEG C of roller water flowing temperature, are kneaded Time >=3min;
Step 4, the roll spacing mm of 2 mm~5, are slowly added to conductive filler, plasticizer by 30 DEG C~40 DEG C of roller water flowing temperature, be kneaded >= 30min;
Step 5, the roll spacing mm of 2 mm~5, are slowly added to vulcanizing agent, mixing time >=3min by 30 DEG C~40 DEG C of roller water flowing temperature;
Step 6, the roll spacing mm of 2 mm~5,30 DEG C~40 DEG C of roller water flowing temperature, cutting is thin logical, and thin logical number is no less than 10 times, mixes Refine time >=20min；
Step 7, slice.
A kind of process 2, dedicated static conductive rubber compounding preparation method of propellants machine, is completed by following steps:
Step 1, using double roller opening rubber mixing machine, roll spacing≤0.5mm, 30 DEG C~40 DEG C of roller water flowing temperature, by butyronitrile 4155 100 parts of addition rubber mixing machines of base rubber, plasticate the time >=1min;
Step 2, roll spacing are gradually amplified to the mm of 2 mm~5,30 DEG C~40 DEG C of roller water flowing temperature, are slowly added to vulcanization accelerator, Mixing time >=2min;
Step 3, the roll spacing mm of 2 mm~5, are slowly added to vulcanizing activator, anti-aging agent by 30 DEG C~40 DEG C of roller water flowing temperature, are kneaded Time >=3min;
Step 4, the roll spacing mm of 2 mm~5,30 DEG C~40 DEG C of roller water flowing temperature, the conductive charcoal being slowly alternately added in conductive filler Black, acetylene carbon black and plasticizer, mixing >=30min;
Step 5, the roll spacing mm of 2 mm~5, are slowly added to vulcanizing agent, mixing time >=3min by 30 DEG C~40 DEG C of roller water flowing temperature;
Step 6, the roll spacing mm of 2 mm~5,30 DEG C~40 DEG C of roller water flowing temperature, cutting is thin logical, and thin logical number is no less than 10 times, mixes Refine time >=20min；
Step 7, slice.
A kind of process 3, dedicated static conductive rubber compounding preparation method of propellants machine, is completed by following steps:
Step 1, using double roller opening rubber mixing machine, roll spacing≤0.5mm, 30 DEG C~40 DEG C of roller water flowing temperature, by butyronitrile 4155 100 parts of addition rubber mixing machines of base rubber, plasticate time 1min;
Step 2, roll spacing are gradually amplified to the mm of 2 mm~5,30 DEG C~40 DEG C of roller water flowing temperature, are slowly added to vulcanization accelerator, Mixing time 2min;
Step 3, the roll spacing mm of 2 mm~5, are slowly added to vulcanizing activator, anti-aging agent by 30 DEG C~40 DEG C of roller water flowing temperature, are kneaded 3 min of time~5min;
Step 4, the roll spacing mm of 2 mm~5,30 DEG C~40 DEG C of roller water flowing temperature, the conductive charcoal being slowly alternately added in conductive filler Black, acetylene carbon black and plasticizer are kneaded 30min;
Step 5, the roll spacing mm of 2 mm~5, are slowly added to vulcanizing agent, mixing time 3min by 30 DEG C~40 DEG C of roller water flowing temperature;
Step 6, the roll spacing mm of 2 mm~5,30 DEG C~40 DEG C of roller water flowing temperature, cutting is thin logical, and thin logical number is no less than 10 times, mixes Refine 20 min of time~30min；
Step 7, slice.
Four, the preparation method of performance sample prepared by the dedicated static conductive rubber compounding of propellants machine
The preparation method of performance sample prepared by the dedicated static conductive rubber compounding of the propellants machine, it is complete by following steps At:
Step 1 is fabricated to 120mm × 150 mm × 2mm mechanics test piece using mechanics sheet mold；
Vulcanization test piece is put into vulcanizing press, 150 DEG C~160 DEG C of curing temperature, sulfide stress 10MPa, vulcanization by step 2 Time is the min of 60min~70；
Step 3, vulcanization terminate, and are cooled to room temperature, and test piece is cut into standard test piece size with special (purpose) rubber film cutter.
Five, static conductive rubber performance preparation method of sample
For static conductive rubber mechanical property and sheet resistance value prepared by Efficient Characterization, corresponding performance sample need to be prepared, it should Rubber performance preparation method of sample, is completed by following steps:
Step 1 is fabricated to 120mm × 150 mm × 2mm mechanics test piece using mechanics sheet mold；
Vulcanization test piece is put into curing cage, 150 DEG C~160 DEG C of curing temperature by step 2, and vulcanization time is 60min~70 min；
Test piece is cut into standard test piece size with special (purpose) rubber film cutter after vulcanization terminates discharging cooling by step 3.
The invention has the benefit that
Static conductive rubber surface resistance value≤1.0 × 10 prepared by the present invention4Ω, shore hardness≤60 °, tensile strength >= 6MPa, elongation at break >=300%, density≤1.25g/cm3 are applied in mixing of solid propellants charging system, test electrostatic Voltage is lower than electrostatic potential safety margin, and static conductive works well.Using static conductive rubber performance sample preparation side of the invention Sample prepared by method can be effectively used for the performances such as resistance value, mechanical property, hardness, the density of static conductive rubber of the invention Test and indication.
Specific embodiment
Embodiment one, a kind of mutatis mutandis static conductive rubber in mixing machine sizing material system static protection, mass fraction:
4,155 100 parts of butyronitrile, 15 parts of Plasticized with Dibutyl Phthalate agent, 10 parts of conductive black, 5 parts of acetylene carbon black, zinc oxide 1.0 parts, 0.5 part of stearic acid, 1.5 parts of altax, 1.0 parts of sulfur vulcanizing agent, 3 parts of antioxidant D.Using process 1, one The kind dedicated static conductive rubber compounding preparation method rubber material of propellants machine, using above-mentioned static conductive rubber performance sample system Preparation Method rubber performance sample.Static conductive offset plate performance obtained is respectively as follows: density 1.10g/cm3, 52 ° of shore hardness, tension Intensity 17.9MPa, elongation at break 511%, sheet resistance 4.52 × 103Ω。
Embodiment two, a kind of mutatis mutandis static conductive rubber in mixing machine sizing material system static protection, mass fraction:
4,155 100 parts of butyronitrile, 20 parts of Plasticized with Dibutyl Phthalate agent, 15 parts of conductive black, 10 parts of acetylene carbon black, oxidation 1.5 parts of zinc, 1 part of stearic acid, 2.0 parts of altax, 1.5 parts of sulfur vulcanizing agent, 4 parts of antioxidant D.Using process 1, one The kind dedicated static conductive rubber compounding preparation method rubber material of propellants machine, using above-mentioned static conductive rubber performance sample system Preparation Method rubber performance sample.Static conductive offset plate performance obtained is respectively as follows: density 1.15g/cm3, 55 ° of shore hardness, tension Intensity 15.6MPa, elongation at break 477%, sheet resistance 1.57 × 103Ω。
Embodiment three, a kind of mutatis mutandis static conductive rubber in mixing machine sizing material system static protection, mass fraction:
4,155 100 parts of butyronitrile, 25 parts of Plasticized with Dibutyl Phthalate agent, 20 parts of conductive black, 10 parts of acetylene carbon black, oxidation 2.5 parts of zinc, 2 parts of stearic acid, 2.3 parts of altax, 1.8 parts of sulfur vulcanizing agent, 5 parts of antioxidant D.Using process 2, one The kind dedicated static conductive rubber compounding preparation method rubber material of propellants machine, using above-mentioned static conductive rubber performance sample system Preparation Method rubber performance sample.Static conductive offset plate performance obtained is respectively as follows: density 1.20g/cm3, 58 ° of shore hardness, tension Intensity 13.2MPa, elongation at break 358%, sheet resistance 1.05 × 103Ω。
Example IV, a kind of mutatis mutandis static conductive rubber in mixing machine sizing material system static protection, mass fraction:
4,155 100 parts of butyronitrile, 15 parts of Plasticized with Dibutyl Phthalate agent, 10 parts of conductive black, 10 parts of acetylene carbon black, oxidation 1.0 parts of zinc, 0.5 part of stearic acid, 1.5 parts of altax, 1.0 parts of sulfur vulcanizing agent, 3 parts of antioxidant D.Using process 2, A kind of dedicated static conductive rubber compounding preparation method rubber material of propellants machine, using above-mentioned static conductive rubber performance sample Preparation method rubber performance sample.Static conductive offset plate performance obtained is respectively as follows: density 1.17g/cm3, 56 ° of shore hardness, resist Tensile strength 16.9MPa, elongation at break 498%, sheet resistance 5.01 × 103Ω。
Embodiment five, a kind of mutatis mutandis static conductive rubber in mixing machine sizing material system static protection, mass fraction:
4,155 100 parts of butyronitrile, 20 parts of Plasticized with Dibutyl Phthalate agent, 10 parts of conductive black, 15 parts of acetylene carbon black, oxidation 1.5 parts of zinc, 1 part of stearic acid, 2.0 parts of altax, 1.5 parts of sulfur vulcanizing agent, 4 parts of antioxidant D.Using process 3, one The kind dedicated static conductive rubber compounding preparation method rubber material of propellants machine, using above-mentioned static conductive rubber performance sample system Preparation Method rubber performance sample.Static conductive offset plate performance obtained is respectively as follows: density 1.21g/cm3, 57 ° of shore hardness, tension Intensity 13.2MPa, elongation at break 457%, sheet resistance 4.13 × 103Ω。
Embodiment six, a kind of mutatis mutandis static conductive rubber in mixing machine sizing material system static protection, mass fraction:
4,155 100 parts of butyronitrile, 25 parts of Plasticized with Dibutyl Phthalate agent, 15 parts of conductive black, 15 parts of acetylene carbon black, oxidation 2.5 parts of zinc, 2 parts of stearic acid, 2.3 parts of altax, 1.8 parts of sulfur vulcanizing agent, 5 parts of antioxidant D.Using process 3, one The kind dedicated static conductive rubber compounding preparation method rubber material of propellants machine, using above-mentioned static conductive rubber performance sample system Preparation Method rubber performance sample.Static conductive offset plate performance obtained is respectively as follows: density 1.24g/cm3, 58 ° of shore hardness, tension Intensity 11.12MPa, elongation at break 358%, sheet resistance 1.21 × 103Ω。
Embodiment seven, a kind of mutatis mutandis static conductive rubber in mixing machine sizing material system static protection, mass fraction:
4,155 100 parts of butyronitrile, 15 parts of o-phthalic acid dibutyl ester plasticizer, 10 parts of conductive black, 5 parts of acetylene carbon black, zinc oxide 1.0 parts, 0.5 part of stearic acid, 1.5 parts of Vulcanization accelerator TMTD, 1.0 parts of cumyl peroxide vulcanizing agent, 3 parts of anti-aging agent RD.It adopts With process 2, a kind of dedicated static conductive rubber compounding preparation method rubber material of propellants machine, using above-mentioned static conductive Rubber performance preparation method of sample rubber performance sample.Static conductive offset plate performance obtained is respectively as follows: density 1.10g/cm3, Shao 57 ° of family name's hardness, tensile strength 9.17MPa, elongation at break 327%, sheet resistance 6.82 × 103Ω。
Embodiment eight, a kind of mutatis mutandis static conductive rubber in mixing machine sizing material system static protection, mass fraction:
4,155 100 parts of butyronitrile, 15 parts of phosphate trimethylbenzene ester plasticiser, 10 parts of conductive black, 5 parts of acetylene carbon black, zinc oxide 1.0 Part, 0.5 part of stearic acid, 1.5 parts of accelerant CZ, 1.0 parts of lead peroxide vulcanizing agent, 3 parts of anti-aging agent BL.Using process 3, A kind of dedicated static conductive rubber compounding preparation method rubber material of propellants machine, using above-mentioned static conductive rubber performance sample Preparation method rubber performance sample.Static conductive offset plate performance obtained is respectively as follows: density 1.10g/cm3, 59 ° of shore hardness, resist Tensile strength 7.21MPa, elongation at break 311%, sheet resistance 7.35 × 103Ω。

Claims (1)

1. a kind of dedicated static conductive rubber performance preparation method of sample of propellants machine, which is characterized in that the preparation method It is completed by following steps:
Step 1 is fabricated to 120mm × 150 mm × 2mm mechanics test piece using mechanics sheet mold；
Vulcanization test piece is put into vulcanizing press, 150 DEG C~160 DEG C of curing temperature, sulfide stress 10MPa, vulcanization by step 2 Time is the min of 60min~70；
Step 3, vulcanization terminate, and are cooled to room temperature, and test piece is cut into standard test piece size with special (purpose) rubber film cutter.
CN201811364375.0A 2018-11-16 2018-11-16 A kind of dedicated static conductive rubber of propellants machine and preparation method of sample Pending CN109571825A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102504358A (en) * 2011-11-22 2012-06-20 广东石油化工学院 High-heat-conductivity rubber composite material and preparation method thereof
CN102816355A (en) * 2011-06-10 2012-12-12 北京橡胶工业研究设计院 Electroconductive rubber and preparation method thereof
CN104479231A (en) * 2014-12-04 2015-04-01 中国航天科工集团第六研究院四十六所 Electrostatic conductive rubber material prepared from hydroxy-terminated polybutadiene propellant residue and preparation method of electrostatic conductive rubber material
CN104987555A (en) * 2015-07-25 2015-10-21 中国航天科工集团第六研究院四十六所 Rubber material prepared by using discarded HTPB propellant residue and preparation method
CN106519349A (en) * 2016-11-23 2017-03-22 安徽美腾特种电缆材料有限公司 Wear-resistant and anti-static rubber floor and preparation method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102816355A (en) * 2011-06-10 2012-12-12 北京橡胶工业研究设计院 Electroconductive rubber and preparation method thereof
CN102504358A (en) * 2011-11-22 2012-06-20 广东石油化工学院 High-heat-conductivity rubber composite material and preparation method thereof
CN104479231A (en) * 2014-12-04 2015-04-01 中国航天科工集团第六研究院四十六所 Electrostatic conductive rubber material prepared from hydroxy-terminated polybutadiene propellant residue and preparation method of electrostatic conductive rubber material
CN104987555A (en) * 2015-07-25 2015-10-21 中国航天科工集团第六研究院四十六所 Rubber material prepared by using discarded HTPB propellant residue and preparation method
CN106519349A (en) * 2016-11-23 2017-03-22 安徽美腾特种电缆材料有限公司 Wear-resistant and anti-static rubber floor and preparation method thereof

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