CN110183856A - A kind of heat conductive flame-retarding protection silicone rubber compound and preparation method thereof - Google Patents

A kind of heat conductive flame-retarding protection silicone rubber compound and preparation method thereof Download PDF

Info

Publication number
CN110183856A
CN110183856A CN201910573935.1A CN201910573935A CN110183856A CN 110183856 A CN110183856 A CN 110183856A CN 201910573935 A CN201910573935 A CN 201910573935A CN 110183856 A CN110183856 A CN 110183856A
Authority
CN
China
Prior art keywords
retarding
rubber compound
heat conductive
silicone rubber
silicone
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.)
Withdrawn
Application number
CN201910573935.1A
Other languages
Chinese (zh)
Inventor
尹志平
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.)
Dongguan Liqun Rongxing Polymer Technology Co Ltd
Original Assignee
Dongguan Liqun Rongxing Polymer Technology Co Ltd
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 Dongguan Liqun Rongxing Polymer Technology Co Ltd filed Critical Dongguan Liqun Rongxing Polymer Technology Co Ltd
Priority to CN201910573935.1A priority Critical patent/CN110183856A/en
Publication of CN110183856A publication Critical patent/CN110183856A/en
Withdrawn legal-status Critical Current

Links

Classifications

    • 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
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K5/00Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
    • C09K5/08Materials not undergoing a change of physical state when used
    • C09K5/14Solid materials, e.g. powdery or granular
    • 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
    • C08K2003/2217Oxides; Hydroxides of metals of magnesium
    • C08K2003/222Magnesia, i.e. magnesium oxide
    • 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
    • C08K2003/2217Oxides; Hydroxides of metals of magnesium
    • C08K2003/2224Magnesium hydroxide
    • 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
    • C08K2003/2227Oxides; Hydroxides of metals of aluminium
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/02Flame or fire retardant/resistant
    • 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
    • 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

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Polymers & Plastics (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Combustion & Propulsion (AREA)
  • Thermal Sciences (AREA)
  • Materials Engineering (AREA)
  • Organic Insulating Materials (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The present invention relates to the technical fields of silastic material, and in particular to a kind of heat conductive flame-retarding protection silicone rubber compound and preparation method thereof in power cable connection accessory.This protects the raw material of silicone rubber compound to have methyl vinyl silicone raw rubber, Siloxane-Oxyalkylene Copolymers, white carbon black, conductive filler, silane coupling agent, silicone oil, zinc stearate, composite flame-proof filler, hardenable composite material, peroxide vulcanizing agent for the heat conductive flame-retarding in cable connector plugging member.It wherein, is that and using Siloxane-Oxyalkylene Copolymers as auxiliary material, obtained silicone rubber compound can be made to have higher tensile strength and elongation at break using methyl vinyl silicone raw rubber as major ingredient.The heat conductive flame-retarding protects silicone rubber compound by the synergistic effect between each component, has excellent thermally conductive and flame retardant property, can harden protection at high temperature, can effectively reduce accident or prevent secondary safety accident from occurring.

Description

A kind of heat conductive flame-retarding protection silicone rubber compound and preparation method thereof
Technical field
The present invention relates to the technical fields of silastic material, and in particular to a kind of for leading in power cable connection accessory Hot flame protection silicone rubber compound and preparation method thereof.
Background technique
Silastic material is a kind of novel high molecular material, has been carried out largely to silastic material at home in recent years Depth research and development and production application, silicone rubber products are widely used in the fields such as civilian, industrial, medical, military project.With domestic city The acceleration of change process, the facilities such as various skyscrapers, supermarket, hospital, airport, sport place, matched electric power are continuously increased, silicon Application of the rubber in power cable field is also more and more.The silicon rubber Protection Product of early stage is used in electric power facility surface and only serves Insulation protection, heat is not easy to disperse when high temperature, or occurs that second protection cannot be played the role of when fire, exists Applied defect.
Summary of the invention
It is an object of the present invention in view of the deficiencies of the prior art, provide a kind of heat conductive flame-retarding protection rubber composition Object, the heat conductive flame-retarding protect silicone rubber compound to have excellent thermally conductive and flame retardant property, can harden protection at high temperature, can It effectively reduces accident or prevents secondary safety accident from occurring.
The second object of the present invention is in view of the deficiencies of the prior art, to provide a kind of heat conductive flame-retarding protection rubber composition The preparation method of object.
One of to achieve the goals above, the present invention adopts the following technical scheme:
A kind of heat conductive flame-retarding protection silicone rubber compound is provided, is prepared from the following raw materials in parts by weight:
Wherein, the hardenable composite material is the composition of silicon powder, clay and clay.
Preferably, a kind of heat conductive flame-retarding protects silicone rubber compound, is prepared from the following raw materials in parts by weight:
More preferably, a kind of heat conductive flame-retarding protects silicone rubber compound, by the raw material system of following parts by weight At:
The methyl vinyl silicone raw rubber is the raw rubber with methyl blocking or ethenyl blocking, the methyl ethylene The content of organic silicon raw rubber medium vinyl is 0.03~3.0%;
The molecular weight of the methyl vinyl silicone raw rubber is 450,000~700,000, the methyl vinyl silicone raw rubber Fugitive constituent be 1.0%~1.5%;
The Siloxane-Oxyalkylene Copolymers are double-end amino Siloxane-Oxyalkylene Copolymers.
The heat filling is one of aluminium oxide, magnesia, silicon nitride or graphene or any two or more group Close object;
The white carbon black is that specific surface area is 100m2/ g~300m2The precipitated silica or/and gas-phase silica of/g;
The silicone oil is one of hydroxy silicon oil, methyl-silicone oil or vinyl silicone oil or any two or more combination Object;
The composite flame-proof filler is in aluminium hydroxide, magnesium hydroxide, zinc carbonate, diphosphorus trioxide or antimony oxide A kind of or any two or more composition;
The peroxide vulcanizing agent is cumyl peroxide, dibenzoyl peroxide, 2,4 dichlorobenzoperoxides Or one of di-tert-butyl peroxide or any two or more composition.
To achieve the goals above two, the present invention adopts the following technical scheme:
A kind of preparation method of heat conductive flame-retarding protection silicone rubber compound is provided, comprising the following steps:
Step 1, it is dry: the composite flame-proof filler of formula ratio and hardenable composite material to be put into drying box do respectively It is dry, to remove moisture, obtain dried powder;
Grinding: step 2 is ground being put into grinder after powder cooling dried in step 1, to prevent powder group It is poly-;
Step 3, heat treatment: by the heat filling investment mixing plant of formula ratio, the silane that formula ratio is then added is even Connection agent is heat-treated, cooling stand-by after be heat-treated, the heat filling that obtains that treated;
Step 4, mixing: by methyl vinyl silicone raw rubber, Siloxane-Oxyalkylene Copolymers, white carbon black, the silicon of formula ratio Oil and zinc stearate, which are successively put into, carries out mixing in mixer, carry out high-temperature vacuum processing again after agglomerating, obtain the good base of mixing Plinth sizing material;
Step 5, mill: the good sizing of the mixing that step 4 is obtained, further mill processing, to promote to disperse, Internal stress is eliminated, the good base rubber of mill is obtained;
Step 6: mixing processing: the good base rubber of mill in step 5 is sequentially added in open mill or in batch mixer Powder, step 3 treated heat filling after step 2 grinding, finally add the peroxide vulcanizing agent of formula ratio, after mixing Obtain the heat conductive flame-retarding protection silicone rubber compound.
In above-mentioned technical proposal, in the step 1, the temperature of the drying is 90 DEG C~110 DEG C, the drying when Between be 3h~5h.
In above-mentioned technical proposal, in the step 3, the temperature of the heat treatment is 75 DEG C~85 DEG C, the heat treatment Time is 40min~80min.
In above-mentioned technical proposal, in the step 4, the temperature of the high-temperature vacuum processing is 140 DEG C~160 DEG C, described The time of high-temperature vacuum processing is 40min~80min.
In above-mentioned technical proposal, in the step 5, the mill adds man-hour requirement to adjust open mill roll spacing gap width For 0.5mm~1.0mm.
Compared with prior art, beneficial effect is the present invention:
(1) a kind of heat conductive flame-retarding provided by the invention protects silicone rubber compound, with methyl vinyl silicone raw rubber work For major ingredient, and using Siloxane-Oxyalkylene Copolymers as auxiliary material, obtained silicone rubber compound can be made to have higher anti-tensile strong Degree and elongation at break;By the way that heat filling is added, to meet the thermally conductive requirement of silicone rubber compound;Silane coupling agent makes group The inorganic filler surface closed in object wraps up one layer of organic group, to increase heat filling and methyl vinyl silicone raw rubber, gather The blending intersolubility of ether modified polyorganosiloxane;White carbon black need to have certain specific surface area, specific surface area as reinforced filling Too LR low reinforcing is poor, and the too high meeting of specific surface causes hybrid process difficult so that hardening effect is obvious;Silicone oil is used as plasticizer In improvement processability, or as structuring inorganic agent, to improve the blended with substrate;Zinc stearate takes off in being primarily used to The effect of mould agent;Composite flame-proof filler, and two or more is with there is synergistic effect, to reach optimal flameproof effect; Hardenable composite material, which can reach a high temperature, sinters the effect of sterosome into;Peroxide vulcanizing agent can be squeezed out convenient for product Molding or compression molding.The heat conductive flame-retarding protects silicone rubber compound by the synergistic effect between each component, has excellent Different thermally conductive and flame retardant property, can harden protection at high temperature, can effectively reduce accident or prevent secondary safety accident from occurring.
(2) a kind of heat conductive flame-retarding provided by the invention protects silicone rubber compound, and there is preferable tensile strength, fracture to stretch Long rate, hardness, tearing strength, thermal coefficient, heat setting effect and flame retardant rating, wherein porcelain effect is 800 DEG C of high temperature combustions It is hardened after burning, lump does not drip.Wherein, flame retardant rating reaches the grade of UL94V-0.
(3) a kind of heat conductive flame-retarding provided by the invention protects silicone rubber compound, is by special types such as addition heat conductive flame-retardings Filler, be prepared into thermally conductive fire prevention can reduce accident occur or realize secondary protection silastic material, be widely used in require compared with High electric power facility field.Special silicone rubber material of the present invention is applied particularly to power cable connecting piece, in operation power process In shield, if equipment for a long time in a high voltage state operation temperature raising can play heat spreading function, if colleague occur fire Calamity accident can play the role of combustion, and in addition the product of high-temp combustion can be hardened quickly, play the role of second protection, and electric power is greatly improved The safety guarantee coefficient of facility.
(4) preparation method of a kind of heat conductive flame-retarding protection silicone rubber compound provided by the invention, the present invention is for existing The not fire-retardant or not thermally conductive equal not satisfactory situation of protection effects existing for protection silastic material is changed in power cable field Into using the multiple working procedure that mixing, mill and mixing are processed, making each component by drying, grinding, the heat treatment to raw material It is fully dispersed uniform, finally prepare the silicone rubber compound for meeting particular/special requirement.
Specific embodiment
In order to which the technical problems, technical solutions and beneficial effects solved by the present invention is more clearly understood, below in conjunction with Embodiment, the present invention will be described in further detail.It should be appreciated that specific embodiment described herein is only used to explain The present invention is not intended to limit the present invention.
Embodiment 1.
A kind of heat conductive flame-retarding protection silicone rubber compound, is prepared from the following raw materials in parts by weight:
Wherein, hardenable composite material is the composition of silicon powder, clay and clay.
In the present embodiment, methyl vinyl silicone raw rubber is the raw rubber with methyl blocking, and methyl vinyl silicone is raw The content of glue medium vinyl is 2.0%;
In the present embodiment, the molecular weight of methyl vinyl silicone raw rubber is 500,000, methyl vinyl silicone raw rubber Fugitive constituent is 1.2%;
Wherein, Siloxane-Oxyalkylene Copolymers are double-end amino Siloxane-Oxyalkylene Copolymers, and then can be improved by amino Cross-linking reaction.
In the present embodiment, heat filling is aluminium oxide.
In the present embodiment, white carbon black is that specific surface area is 200m2The precipitated silica of/g.
In the present embodiment, silicone oil is hydroxy silicon oil.
In the present embodiment, composite flame-proof filler is aluminium hydroxide.
In the present embodiment, peroxide vulcanizing agent is cumyl peroxide.
A kind of preparation method of above-mentioned heat conductive flame-retarding protection silicone rubber compound, comprising the following steps:
Step 1, it is dry: the composite flame-proof filler of formula ratio and hardenable composite material to be put into drying box do respectively It is dry, to remove moisture, obtain dried powder;In the present embodiment, dry temperature is 100 DEG C, and the dry time is 4h;
Grinding: step 2 is ground being put into grinder after powder cooling dried in step 1, to prevent powder group It is poly-;
Step 3, heat treatment: by the heat filling investment mixing plant of formula ratio, the silane that formula ratio is then added is even Connection agent is heat-treated, cooling stand-by after be heat-treated, the heat filling that obtains that treated;In the present embodiment, the temperature of heat treatment Degree is 80 DEG C, and the time of heat treatment is 60min;
Step 4, mixing: by methyl vinyl silicone raw rubber, Siloxane-Oxyalkylene Copolymers, white carbon black, the silicon of formula ratio Oil and zinc stearate, which are successively put into, carries out mixing in mixer, carry out high-temperature vacuum processing again after agglomerating, obtain the good base of mixing Plinth sizing material;In the present embodiment, the temperature of high-temperature vacuum processing is 150 DEG C, and the time of high-temperature vacuum processing is 60min;
Step 5, mill: the good sizing of the mixing that step 4 is obtained, further mill processing, to promote to disperse, Internal stress is eliminated, the good base rubber of mill is obtained;Wherein, mill add man-hour requirement adjustment open mill roll spacing gap width be 0.7mm;
Step 6: mixing processing: the good base rubber of mill in step 5 is sequentially added in open mill or in batch mixer Powder, step 3 treated heat filling after step 2 grinding, finally add the peroxide vulcanizing agent of formula ratio, after mixing Obtain the heat conductive flame-retarding protection silicone rubber compound.
Embodiment 2.
A kind of heat conductive flame-retarding protection silicone rubber compound, is prepared from the following raw materials in parts by weight:
Wherein, hardenable composite material is the composition of silicon powder, clay and clay.
In the present embodiment, methyl vinyl silicone raw rubber is the raw rubber with ethenyl blocking, methyl vinyl silicone The content of raw rubber medium vinyl is 0.03%;
In the present embodiment, the molecular weight of methyl vinyl silicone raw rubber is 450,000, methyl vinyl silicone raw rubber Fugitive constituent is 1.0%;
Wherein, Siloxane-Oxyalkylene Copolymers are double-end amino Siloxane-Oxyalkylene Copolymers, and then can be improved by amino Cross-linking reaction.
In the present embodiment, heat filling is magnesia.
In the present embodiment, white carbon black is that specific surface area is 100m2The gas-phase silica of/g.
In the present embodiment, silicone oil is methyl-silicone oil.
In the present embodiment, composite flame-proof filler is magnesium hydroxide.
In the present embodiment, peroxide vulcanizing agent is dibenzoyl peroxide.
A kind of preparation method of above-mentioned heat conductive flame-retarding protection silicone rubber compound, comprising the following steps:
Step 1, it is dry: the composite flame-proof filler of formula ratio and hardenable composite material to be put into drying box do respectively It is dry, to remove moisture, obtain dried powder;In the present embodiment, dry temperature is 90 DEG C, and the dry time is 5h;
Grinding: step 2 is ground being put into grinder after powder cooling dried in step 1, to prevent powder group It is poly-;
Step 3, heat treatment: by the heat filling investment mixing plant of formula ratio, the silane that formula ratio is then added is even Connection agent is heat-treated, cooling stand-by after be heat-treated, the heat filling that obtains that treated;In the present embodiment, the temperature of heat treatment Degree is 75 DEG C, and the time of heat treatment is 80min;
Step 4, mixing: by methyl vinyl silicone raw rubber, Siloxane-Oxyalkylene Copolymers, white carbon black, the silicon of formula ratio Oil and zinc stearate, which are successively put into, carries out mixing in mixer, carry out high-temperature vacuum processing again after agglomerating, obtain the good base of mixing Plinth sizing material;In the present embodiment, the temperature of high-temperature vacuum processing is 140 DEG C, and the time of high-temperature vacuum processing is 80min;
Step 5, mill: the good sizing of the mixing that step 4 is obtained, further mill processing, to promote to disperse, Internal stress is eliminated, the good base rubber of mill is obtained;Wherein, mill add man-hour requirement adjustment open mill roll spacing gap width be 0.5mm;
Step 6: mixing processing: the good base rubber of mill in step 5 is sequentially added in open mill or in batch mixer Powder, step 3 treated heat filling after step 2 grinding, finally add the peroxide vulcanizing agent of formula ratio, after mixing Obtain the heat conductive flame-retarding protection silicone rubber compound.
Embodiment 3.
A kind of heat conductive flame-retarding protection silicone rubber compound, is prepared from the following raw materials in parts by weight:
Wherein, hardenable composite material is the composition of silicon powder, clay and clay.
In the present embodiment, methyl vinyl silicone raw rubber is the raw rubber with methyl blocking, and methyl vinyl silicone is raw The content of glue medium vinyl is 3.0%;
In the present embodiment, the molecular weight of methyl vinyl silicone raw rubber is 700,000, methyl vinyl silicone raw rubber Fugitive constituent is 1.5%;
Wherein, Siloxane-Oxyalkylene Copolymers are double-end amino Siloxane-Oxyalkylene Copolymers, and then can be improved by amino Cross-linking reaction.
In the present embodiment, heat filling is the composition of silicon nitride and graphene.
In the present embodiment, white carbon black is that specific surface area is 300m2The precipitated silica of/g and the composition of gas-phase silica.
In the present embodiment, silicone oil is the composition of methyl-silicone oil and vinyl silicone oil.
In the present embodiment, composite flame-proof filler is the composition of zinc carbonate and diphosphorus trioxide.
In the present embodiment, the group of peroxide vulcanizing agent 2,4 dichlorobenzoperoxide and di-tert-butyl peroxide Close object.
A kind of preparation method of above-mentioned heat conductive flame-retarding protection silicone rubber compound, comprising the following steps:
Step 1, it is dry: the composite flame-proof filler of formula ratio and hardenable composite material to be put into drying box do respectively It is dry, to remove moisture, obtain dried powder;In the present embodiment, dry temperature is 110 DEG C, and the dry time is 3h;
Grinding: step 2 is ground being put into grinder after powder cooling dried in step 1, to prevent powder group It is poly-;
Step 3, heat treatment: by the heat filling investment mixing plant of formula ratio, the silane that formula ratio is then added is even Connection agent is heat-treated, cooling stand-by after be heat-treated, the heat filling that obtains that treated;In the present embodiment, the temperature of heat treatment Degree is 85 DEG C, and the time of heat treatment is 40min;
Step 4, mixing: by methyl vinyl silicone raw rubber, Siloxane-Oxyalkylene Copolymers, white carbon black, the silicon of formula ratio Oil and zinc stearate, which are successively put into, carries out mixing in mixer, carry out high-temperature vacuum processing again after agglomerating, obtain the good base of mixing Plinth sizing material;In the present embodiment, the temperature of high-temperature vacuum processing is 160 DEG C, and the time of high-temperature vacuum processing is 40min;
Step 5, mill: the good sizing of the mixing that step 4 is obtained, further mill processing, to promote to disperse, Internal stress is eliminated, the good base rubber of mill is obtained;Wherein, mill add man-hour requirement adjustment open mill roll spacing gap width be 1.0mm;
Step 6: mixing processing: the good base rubber of mill in step 5 is sequentially added in open mill or in batch mixer Powder, step 3 treated heat filling after step 2 grinding, finally add the peroxide vulcanizing agent of formula ratio, after mixing Obtain the heat conductive flame-retarding protection silicone rubber compound.
Embodiment 4.
A kind of heat conductive flame-retarding protection silicone rubber compound, is prepared from the following raw materials in parts by weight:
Wherein, hardenable composite material is the composition of silicon powder, clay and clay.
In the present embodiment, methyl vinyl silicone raw rubber is the raw rubber with ethenyl blocking, methyl vinyl silicone The content of raw rubber medium vinyl is 0.5%;
In the present embodiment, the molecular weight of methyl vinyl silicone raw rubber is 500,000, methyl vinyl silicone raw rubber Fugitive constituent is 1.1%;
Wherein, Siloxane-Oxyalkylene Copolymers are double-end amino Siloxane-Oxyalkylene Copolymers, and then can be improved by amino Cross-linking reaction.
In the present embodiment, heat filling is the composition of aluminium oxide, magnesia and silicon nitride.
In the present embodiment, white carbon black is that specific surface area is 150m2The precipitated silica 5 of/g.
In the present embodiment, silicone oil is the composition of hydroxy silicon oil, methyl-silicone oil and vinyl silicone oil.
In the present embodiment, composite flame-proof filler is the composition of zinc carbonate, diphosphorus trioxide and antimony oxide.
In the present embodiment, peroxide vulcanizing agent is cumyl peroxide, dibenzoyl peroxide and 2,4 dichloro peroxides Change the composition of benzoyl.
A kind of preparation method of above-mentioned heat conductive flame-retarding protection silicone rubber compound, comprising the following steps:
Step 1, it is dry: the composite flame-proof filler of formula ratio and hardenable composite material to be put into drying box do respectively It is dry, to remove moisture, obtain dried powder;In the present embodiment, dry temperature is 95 DEG C, and the dry time is 4.5h;
Grinding: step 2 is ground being put into grinder after powder cooling dried in step 1, to prevent powder group It is poly-;
Step 3, heat treatment: by the heat filling investment mixing plant of formula ratio, the silane that formula ratio is then added is even Connection agent is heat-treated, cooling stand-by after be heat-treated, the heat filling that obtains that treated;In the present embodiment, the temperature of heat treatment Degree is 78 DEG C, and the time of heat treatment is 70min;
Step 4, mixing: by methyl vinyl silicone raw rubber, Siloxane-Oxyalkylene Copolymers, white carbon black, the silicon of formula ratio Oil and zinc stearate, which are successively put into, carries out mixing in mixer, carry out high-temperature vacuum processing again after agglomerating, obtain the good base of mixing Plinth sizing material;In the present embodiment, the temperature of high-temperature vacuum processing is 145 DEG C, and the time of high-temperature vacuum processing is 70min;
Step 5, mill: the good sizing of the mixing that step 4 is obtained, further mill processing, to promote to disperse, Internal stress is eliminated, the good base rubber of mill is obtained;Wherein, mill add man-hour requirement adjustment open mill roll spacing gap width be 0.6mm;
Step 6: mixing processing: the good base rubber of mill in step 5 is sequentially added in open mill or in batch mixer Powder, step 3 treated heat filling after step 2 grinding, finally add the peroxide vulcanizing agent of formula ratio, after mixing Obtain the heat conductive flame-retarding protection silicone rubber compound.
Embodiment 5.
A kind of heat conductive flame-retarding protection silicone rubber compound, is prepared from the following raw materials in parts by weight:
Wherein, hardenable composite material is the composition of silicon powder, clay and clay.
In the present embodiment, methyl vinyl silicone raw rubber is the raw rubber with ethenyl blocking, methyl vinyl silicone The content of raw rubber medium vinyl is 2.5%;
In the present embodiment, the molecular weight of methyl vinyl silicone raw rubber is 600,000, methyl vinyl silicone raw rubber Fugitive constituent is 1.4%;
Wherein, Siloxane-Oxyalkylene Copolymers are double-end amino Siloxane-Oxyalkylene Copolymers, and then can be improved by amino Cross-linking reaction.
In the present embodiment, heat filling is the composition of aluminium oxide and magnesia.
In the present embodiment, white carbon black is that specific surface area is 250m2The gas-phase silica of/g.
In the present embodiment, silicone oil is the composition of hydroxy silicon oil and methyl-silicone oil.
In the present embodiment, composite flame-proof filler is the composition of aluminium hydroxide and magnesium hydroxide.
In the present embodiment, peroxide vulcanizing agent is the composition of cumyl peroxide and dibenzoyl peroxide.
A kind of preparation method of above-mentioned heat conductive flame-retarding protection silicone rubber compound, comprising the following steps:
Step 1, it is dry: the composite flame-proof filler of formula ratio and hardenable composite material to be put into drying box do respectively It is dry, to remove moisture, obtain dried powder;In the present embodiment, dry temperature is 105 DEG C, and the dry time is 3.5h;
Grinding: step 2 is ground being put into grinder after powder cooling dried in step 1, to prevent powder group It is poly-;
Step 3, heat treatment: by the heat filling investment mixing plant of formula ratio, the silane that formula ratio is then added is even Connection agent is heat-treated, cooling stand-by after be heat-treated, the heat filling that obtains that treated;In the present embodiment, the temperature of heat treatment Degree is 82 DEG C, and the time of heat treatment is 50min;
Step 4, mixing: by methyl vinyl silicone raw rubber, Siloxane-Oxyalkylene Copolymers, white carbon black, the silicon of formula ratio Oil and zinc stearate, which are successively put into, carries out mixing in mixer, carry out high-temperature vacuum processing again after agglomerating, obtain the good base of mixing Plinth sizing material;In the present embodiment, the temperature of high-temperature vacuum processing is 155 DEG C, and the time of high-temperature vacuum processing is 50min;
Step 5, mill: the good sizing of the mixing that step 4 is obtained, further mill processing, to promote to disperse, Internal stress is eliminated, the good base rubber of mill is obtained;Wherein, mill add man-hour requirement adjustment open mill roll spacing gap width be 0.9mm;
Step 6: mixing processing: the good base rubber of mill in step 5 is sequentially added in open mill or in batch mixer Powder, step 3 treated heat filling after step 2 grinding, finally add the peroxide vulcanizing agent of formula ratio, after mixing Obtain the heat conductive flame-retarding protection silicone rubber compound.
Measuring:
To a kind of heat conductive flame-retarding made from embodiment 1 to embodiment 5 protection silicone rubber compound carry out respectively tensile strength, The measurement of elongation at break, hardness, tearing strength, thermal coefficient, heat setting effect and flame retardant rating.Wherein, tensile strength Test method according to GB/T528-2009, the test method of elongation at break is according to GB/T528-2009, the test side of hardness Method is according to GB/T531.1-2008, and the test method of tearing strength is according to GB/T529-2008, the test method root of thermal coefficient According to GB/T10294-2008.Its measurement result refers to table 1.
1 embodiment 1 of table to embodiment 5 silicone rubber compound performance measurement table
By the determination data of above-mentioned table 1 it is found that heat conductive flame-retarding produced by the present invention protection silicone rubber compound has preferably Tensile strength, elongation at break, hardness, tearing strength, thermal coefficient, heat setting effect and flame retardant rating.
Finally it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention, rather than the present invention is protected The limitation of range is protected, although explaining in detail referring to preferred embodiment to the present invention, those skilled in the art are answered Work as understanding, it can be with modification or equivalent replacement of the technical solution of the present invention are made, without departing from the reality of technical solution of the present invention Matter and range.

Claims (10)

1. a kind of heat conductive flame-retarding protects silicone rubber compound, it is characterised in that: be prepared from the following raw materials in parts by weight:
Wherein, the hardenable composite material is the composition of silicon powder, clay and clay.
2. a kind of heat conductive flame-retarding according to claim 1 protects silicone rubber compound, it is characterised in that: by following parts by weight Several raw materials are made:
3. a kind of heat conductive flame-retarding according to claim 1 protects silicone rubber compound, it is characterised in that: by following parts by weight Several raw materials are made:
4. a kind of heat conductive flame-retarding according to claim 1 protects silicone rubber compound, it is characterised in that: the ethylene methacrylic The organic silicon raw rubber of base is the raw rubber with methyl blocking or ethenyl blocking, the methyl vinyl silicone raw rubber medium vinyl Content is 0.03~3.0%;
The molecular weight of the methyl vinyl silicone raw rubber is 450,000~700,000, and the methyl vinyl silicone raw rubber is waved Sending out part is 1.0%~1.5%;
The Siloxane-Oxyalkylene Copolymers are double-end amino Siloxane-Oxyalkylene Copolymers.
5. a kind of heat conductive flame-retarding according to claim 1 protects silicone rubber compound, it is characterised in that:
The heat filling is one of aluminium oxide, magnesia, silicon nitride or graphene or any two or more composition;
The white carbon black is that specific surface area is 100m2/ g~300m2The precipitated silica or/and gas-phase silica of/g;
The silicone oil is one of hydroxy silicon oil, methyl-silicone oil or vinyl silicone oil or any two or more composition;
The composite flame-proof filler is one of aluminium hydroxide, magnesium hydroxide, zinc carbonate, diphosphorus trioxide or antimony oxide Or any two or more composition;
The peroxide vulcanizing agent is cumyl peroxide, dibenzoyl peroxide, 2,4 dichlorobenzoperoxides or two One of tert-butyl peroxide or any two or more composition.
6. a kind of preparation method of heat conductive flame-retarding protection silicone rubber compound, feature described in claim 1 to 5 any one It is: the following steps are included:
Step 1, dry: the composite flame-proof filler of formula ratio and hardenable composite material are put into drying in drying box respectively, with Moisture is removed, dried powder is obtained;
Grinding: step 2 is ground being put into grinder after powder cooling dried in step 1, to prevent powder reuniting;
Heat treatment: by the heat filling investment mixing plant of formula ratio, the silane coupling agent of formula ratio is then added in step 3 It is heat-treated, cooling stand-by after being heat-treated, the heat filling that obtains that treated;
Step 4, mixing: by the methyl vinyl silicone raw rubber of formula ratio, Siloxane-Oxyalkylene Copolymers, white carbon black, silicone oil and Zinc stearate successively puts into and carries out mixing in mixer, carries out high-temperature vacuum processing again after agglomerating, obtains the good basic glue of mixing Material;
Step 5, mill: the good sizing of the mixing that step 4 is obtained, further mill processing are eliminated with promoting to disperse Internal stress obtains the good base rubber of mill;
Step 6: the good base rubber of mill in step 5 mixing processing: is sequentially added into open mill or in batch mixer step Powder, step 3 treated heat filling after two grindings finally add the peroxide vulcanizing agent of formula ratio, make after mixing It obtains the heat conductive flame-retarding and protects silicone rubber compound.
7. a kind of preparation method of heat conductive flame-retarding protection silicone rubber compound according to claim 6, it is characterised in that: institute It states in step 1, the temperature of the drying is 90 DEG C~110 DEG C, and the time of the drying is 3h~5h.
8. a kind of preparation method of heat conductive flame-retarding protection silicone rubber compound according to claim 6, it is characterised in that: institute It states in step 3, the temperature of the heat treatment is 75 DEG C~85 DEG C, and the time of the heat treatment is 40min~80min.
9. a kind of preparation method of heat conductive flame-retarding protection silicone rubber compound according to claim 6, it is characterised in that: institute It states in step 4, the temperature of the high-temperature vacuum processing is 140 DEG C~160 DEG C, and the time of the high-temperature vacuum processing is 40min ~80min.
10. a kind of preparation method of heat conductive flame-retarding protection silicone rubber compound according to claim 6, it is characterised in that: In the step 5, the mill adds man-hour requirement adjustment open mill roll spacing gap width to be 0.5mm~1.0mm.
CN201910573935.1A 2019-06-28 2019-06-28 A kind of heat conductive flame-retarding protection silicone rubber compound and preparation method thereof Withdrawn CN110183856A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201910573935.1A CN110183856A (en) 2019-06-28 2019-06-28 A kind of heat conductive flame-retarding protection silicone rubber compound and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201910573935.1A CN110183856A (en) 2019-06-28 2019-06-28 A kind of heat conductive flame-retarding protection silicone rubber compound and preparation method thereof

Publications (1)

Publication Number Publication Date
CN110183856A true CN110183856A (en) 2019-08-30

Family

ID=67723984

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201910573935.1A Withdrawn CN110183856A (en) 2019-06-28 2019-06-28 A kind of heat conductive flame-retarding protection silicone rubber compound and preparation method thereof

Country Status (1)

Country Link
CN (1) CN110183856A (en)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110791105A (en) * 2019-09-26 2020-02-14 无锡市华美电缆有限公司 Low-temperature flame-retardant silica gel outer sheath for cable and preparation method thereof
CN114213850A (en) * 2021-12-28 2022-03-22 江苏达胜高聚物股份有限公司 High-thermal-conductivity silicone rubber cable material and preparation method and application thereof
CN114989610A (en) * 2022-06-01 2022-09-02 深圳市华天启科技有限公司 Plastic flame-retardant heat conduction material and preparation method thereof
CN115850977A (en) * 2022-12-21 2023-03-28 蚌埠壹石通聚合物复合材料有限公司 Normal-temperature heat-conducting and high-temperature flame-retardant heat-insulating silicone rubber and preparation method thereof
CN116640450A (en) * 2023-06-15 2023-08-25 安徽工业大学 Rubber based on sulfur-containing industrial solid waste and preparation method thereof

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH07157664A (en) * 1993-12-03 1995-06-20 Fuji Kobunshi Kogyo Kk Thermally conductive silicone rubber sheet and its production
CN101747631A (en) * 2008-12-01 2010-06-23 中国科学院过程工程研究所 Flame-retardant room temperature vulcanized silicone rubber composition
CN107163585A (en) * 2017-04-05 2017-09-15 华南理工大学 It is a kind of can low-temp ceramics silicon rubber and preparation method thereof
CN107936566A (en) * 2017-11-30 2018-04-20 泰州日顺电器发展有限公司 It is a kind of for flame retardant cable can Ceramic silicon rubber composite material and its manufacture method
CN108059834A (en) * 2017-12-19 2018-05-22 大连理工常州研究院有限公司 A kind of battery cell case material with fire protecting performance
CN108165015A (en) * 2017-12-29 2018-06-15 常州市沃科科技有限公司 A kind of fire-resistant thermal conductivity factor changeable material, preparation method and application
CN109021576A (en) * 2018-08-20 2018-12-18 镇江创达新材料科技有限公司 A kind of preparation method of the Flame-retardant ceramic silicone rubber for safety cable

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH07157664A (en) * 1993-12-03 1995-06-20 Fuji Kobunshi Kogyo Kk Thermally conductive silicone rubber sheet and its production
CN101747631A (en) * 2008-12-01 2010-06-23 中国科学院过程工程研究所 Flame-retardant room temperature vulcanized silicone rubber composition
CN107163585A (en) * 2017-04-05 2017-09-15 华南理工大学 It is a kind of can low-temp ceramics silicon rubber and preparation method thereof
CN107936566A (en) * 2017-11-30 2018-04-20 泰州日顺电器发展有限公司 It is a kind of for flame retardant cable can Ceramic silicon rubber composite material and its manufacture method
CN108059834A (en) * 2017-12-19 2018-05-22 大连理工常州研究院有限公司 A kind of battery cell case material with fire protecting performance
CN108165015A (en) * 2017-12-29 2018-06-15 常州市沃科科技有限公司 A kind of fire-resistant thermal conductivity factor changeable material, preparation method and application
CN109021576A (en) * 2018-08-20 2018-12-18 镇江创达新材料科技有限公司 A kind of preparation method of the Flame-retardant ceramic silicone rubber for safety cable

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
来国桥,等: "《有机硅产品合成工艺及应用》", 31 January 2010, 化学工业出版社 *

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110791105A (en) * 2019-09-26 2020-02-14 无锡市华美电缆有限公司 Low-temperature flame-retardant silica gel outer sheath for cable and preparation method thereof
CN114213850A (en) * 2021-12-28 2022-03-22 江苏达胜高聚物股份有限公司 High-thermal-conductivity silicone rubber cable material and preparation method and application thereof
CN114989610A (en) * 2022-06-01 2022-09-02 深圳市华天启科技有限公司 Plastic flame-retardant heat conduction material and preparation method thereof
CN115850977A (en) * 2022-12-21 2023-03-28 蚌埠壹石通聚合物复合材料有限公司 Normal-temperature heat-conducting and high-temperature flame-retardant heat-insulating silicone rubber and preparation method thereof
CN115850977B (en) * 2022-12-21 2023-10-20 蚌埠壹石通聚合物复合材料有限公司 Silicon rubber with normal-temperature heat conduction, high-temperature flame retardance and heat insulation and preparation method thereof
CN116640450A (en) * 2023-06-15 2023-08-25 安徽工业大学 Rubber based on sulfur-containing industrial solid waste and preparation method thereof

Similar Documents

Publication Publication Date Title
CN110183856A (en) A kind of heat conductive flame-retarding protection silicone rubber compound and preparation method thereof
CN1241207C (en) Halogen-free non-phosphorus flame-retarded cable sheath material
CN106349555B (en) Halogen-free high flame-retardant cable material, cable and preparation method thereof
CN110746706B (en) Low-smoke halogen-free ethylene propylene diene monomer composition and preparation method thereof
CN102964696A (en) Ethylene propylene diene copolymer flame retardant cable material and preparation method thereof
CN110093039A (en) A kind of silicone rubber compound and its manufacturing method of conductive anti-energy ceramic of fighting
CN104910477A (en) High strength low smoke halogen-free flame retardant cable material for buildings and preparation method thereof
CN102964698A (en) High cold-resistance ethylene propylene diene copolymer insulated cable material and preparation method thereof
CN111205565B (en) Dynamic vulcanized halogen-free flame-retardant insulator sheath, umbrella skirt composite material and preparation method
CN109957248A (en) It is used to form the composition and flame-proof silicon rubber of flame-proof silicon rubber
CN108976813A (en) A kind of cable closure fire proofing material and preparation method thereof
CN111592765A (en) Flame-retardant and fire-resistant protective material and preparation method thereof
CN104788832A (en) Nano boron fiber reinforced low-smoke zero-halogen flame-retardant cable material for buildings as well as preparation method of cable material
CN109054196A (en) A kind of High-temperature-rescablet cablet material of high tenacity
CN107446368B (en) Using silane-modified boehmite as wood plastic composite of fire retardant and preparation method thereof
CN106479190A (en) A kind of fire-resisting ceramic silicone rubber that can be used for middle temperature sulfuration and preparation method thereof
CN112094502A (en) High-temperature-resistant mixed silicone rubber and preparation method thereof
CN105968414B (en) A kind of fire retardant and its method of modifying, fire proofing and preparation method thereof
CN106589760A (en) Phenolic resin smokeless flame-retardant data cable sheath material and preparation method thereof
CN110343302A (en) A kind of potent fire protection flame retarding cable cover(ing) and preparation method thereof
CN112920461B (en) Ceramic filler, preparation method thereof and EPDM (ethylene-propylene-diene monomer) composite material
CN105462080A (en) Anti-deformation heat preservation compound ethylene propylene diene monomer cable material and preparation method thereof
CN107177078A (en) A kind of flame retardant cable
CN105924708A (en) Environment-friendly silica gel material
WO2018209825A1 (en) Maleic anhydride grafted poe cable material and preparation method therefor

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
WW01 Invention patent application withdrawn after publication

Application publication date: 20190830

WW01 Invention patent application withdrawn after publication