CN106380860A - Self-adhesion silicon rubber material and preparation method thereof - Google Patents

Self-adhesion silicon rubber material and preparation method thereof Download PDF

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CN106380860A
CN106380860A CN201610863836.3A CN201610863836A CN106380860A CN 106380860 A CN106380860 A CN 106380860A CN 201610863836 A CN201610863836 A CN 201610863836A CN 106380860 A CN106380860 A CN 106380860A
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parts
autohension
minutes
silicone rubber
room temperature
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CN106380860B (en
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宋宏涛
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Institute of Nuclear Physics and Chemistry China Academy of Engineering Physics
Southwest University of Science and Technology
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Institute of Nuclear Physics and Chemistry China Academy of Engineering Physics
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L83/00Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
    • C08L83/04Polysiloxanes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C71/00After-treatment of articles without altering their shape; Apparatus therefor
    • B29C71/04After-treatment of articles without altering their shape; Apparatus therefor by wave energy or particle radiation, e.g. for curing or vulcanising preformed articles
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F251/00Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/08Stabilised against heat, light or radiation or oxydation
    • 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
    • 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
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2312/00Crosslinking
    • C08L2312/06Crosslinking by radiation
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/50Improvements relating to the production of bulk chemicals
    • Y02P20/54Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids

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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)
  • Compositions Of Macromolecular Compounds (AREA)
  • Processes Of Treating Macromolecular Substances (AREA)

Abstract

The invention discloses a self-adhesion silicon rubber material and a preparation method thereof. The preparation method is characterized in that 100 parts of silicon rubber, 10 to 80 parts of a reinforcing agent, 1 to 9 parts of a controlling agent and 0 to 5 parts of a sensitizing agent are mixed and formed, and then are subjected to gamma-ray radiation to be crosslinked to obtain the self-adhesion silicon rubber material with excellent performance, wherein the radiation absorbed dose is 30 to 100 kGy. The self-adhesionsilicon rubber material and the preparation method thereof have the advantages that the process is simple, complex chemical raw materials and process control or professional auxiliary equipment are not needed, and the cost is relatively low; and the prepared silicon rubber material can be well adhered to various components or assemblies, such as metal, glass, polyethylene, polytetrafluoroethylene and the like, can maintain lasting adhesion, and can effectively prevent the components or the assemblies from falling off or sliding.

Description

There is silastic material of autohension and preparation method thereof
Technical field
The invention belongs to technical field of rubber material is and in particular to a kind of silastic material with autohension and its preparation Method.
Background technology
Silastic material is widely used in the assemblings of articles for use such as electronic devices and components, equipment parts and produces.A lot In the case of it is desirable to have good adhesion property between silicone rubber and components and parts, parts, to reach preferable effect.Existing Assembling in technology and the mode of production typically coat binding agent on components and parts or parts in advance, or in silicone rubber material Material surface attachment last layer pressure sensitive adhesive, to reach preferable bonding each other, but this mode shortcoming is that manufacturing procedure is loaded down with trivial details, And the requirement to binding agent is higher, binding agent typically requires has good combination property, such as heat-resisting etc..At present, open source information The autohension silastic material of display typically requires in preparatory phase and causes crosslinked, high-temperature vacuum heat treatment using peroxide, And essentially metal autohension, such as patent CN201210437042.2 etc..Therefore, research has wide spectrum autohension and prepares work The silastic material of the simple and direct environmental protection of skill has very positive meaning.
Content of the invention
As the result of various extensive and careful researchs and experiment, it has been found by the inventor that using radiation Crosslinked method can prepare the silastic material with wide spectrum autohension, not only crosslinked uniform, easy to control, energy-saving ring Protect, and technique is simple and direct, favorable reproducibility, production efficiency high, this material mechanical performance is excellent simultaneously.Based on this discovery, complete The present invention.
It is an object of the invention to solving at least the above and/or defect, and provide at least will be described later excellent Point.
A further object of the invention is the method by crosslinking with radiation, improves the life of the silastic material with autohension Produce efficiency, and excellent performance and the silastic material of the simple and direct environmental protection of preparation technology are obtained with this.
In order to realize according to object of the present invention and further advantage, there is provided a kind of silicone rubber material with autohension Material, wherein, the formula of described silastic material forms by weight:100 parts of silicone rubber, 10~80 parts of reinforcing agent, controlling agent 1 ~9 parts, 0~5 part of sensitizer.
Preferably, wherein, the formula composition of described silastic material also includes:1~5 part of viscosifier, antibacterial 1~5 Part, 1~3 part of fire retardant, 1~3 part of antioxidant.
Preferably, wherein, the formula of described material forms by weight:100 parts of silicone rubber base material, reinforcing agent 30 Part, 3 parts of controlling agent, 4 parts of sensitizer, 4 parts of viscosifier, 4 parts of antibacterial, 2 parts of fire retardant, 2 parts of antioxidant.
Preferably, wherein, described autohension silastic material shore hardness 22~67, tensile strength be 3.21~ 35.7MPa, elongation at break 200~912%, tearing strength 12.6~41.3MPa.
Preferably, wherein,
Described silicone rubber is dimethyl silicone rubber, methyl vinyl silicone rubber, appointing in methyl phenyl vinyl silicone rubber Meaning is a kind of;
Described reinforcing agent is precipitated silica, any one in fume colloidal silica;
Described constitution controller is high molecular weight hydroxy silicone oil, any one in low molecule hydroxy silicon oil;
Described sensitizer is triallyl cyanurate, triallyl isocyanurate, trimethylol propane trimethyl third Any one in olefin(e) acid ester, diacrylate -1,6-HD ester;
Described antibacterial is chitin, zinc oxide, any one in copper oxide;
Described fire retardant is weight ratio for 3:1 magnesium hydroxide and aluminium hydroxide;
Described antioxidant is weight ratio for 3:2:1 phenyl silicone oil, MethylethoxylsiliconFluid Fluid and 2,6- di-t-butyl are to first Phenol.
Preferably, wherein, the preparation method of described viscosifier is:By weight, take 100 parts of starch, add 100 parts of water With 10 parts of weight than for 2:1 tripolycyanamide and ammonium carbonate, stir, and adjust pH to 9 with the carbamide of 1.5mol/L, add 50 Part epoxychloropropane, under conditions of 30~40 DEG C of temperature, stirring reaction 4~5 hours, filters, with washing with alcohol, is dried, obtains Crosslinked starch;Add weight ratio for 1 in supercritical reaction apparatus:1 crosslinked starch and 30~35 parts of carrageenan, acrylic acid fourth 20~25 parts of ester, 3~5 parts of acrylamide, 0.02~0.08 part of Ammonium persulfate., 200~250 parts of water, stir, then by body System sealing, be passed through carbon dioxide to 25~45MPa, 60~75 DEG C of temperature under conditions of react 5~8 hours, then use ethanol Precipitation, is vacuum dried at 70 DEG C, obtains reacting coarse product, with apparatus,Soxhlet'ses by the elution of crude product acetone until removing anti- The homopolymer that should produce, is vacuum dried 24 hours at 65 DEG C, obtains viscosifier.
Preferably, wherein, the molecular weight of described silicone rubber is 50~700,000, methyl vinyl silicone rubber medium vinyl Molar content be 0.04~0.60%, in methyl phenyl vinyl silicone rubber the molar content of phenyl be 1.0~ 30.0%.
The present invention also provides a kind of preparation method of the above-mentioned silastic material with autohension, wherein, methods described Comprise the following steps:
Step one, by weight, takes silicone rubber to add in two-roll mill, plasticates at room temperature 5~10 minutes, Ran Houjia Enter reinforcing agent, constitution controller, knead 5~10 minutes, obtain just mixed sizing material, quiet storage 12~24 hours, afterwards by just under room temperature Mixed sizing material back mixing 10~15 minutes, adds sensitizer, continues mixing 5~10 minutes, obtains mixing materials, and quiet storage 24~48 is little again When, afterwards again under room temperature by sizing material back mixing 10~15 minutes, under room temperature by mixing materials on tablet machine compression molding be sheet material Or bulk;The rotating cylinder rotating speed of described two-roll mill is set to 200~600r.min-1
Step 2, the sheet material after molding or bulk are wrapped up through plastic packaging or aluminium foil after, in the air at room temperature, be placed in60Co Carry out crosslinking with radiation in gamma radiation field, absorbed dose are 30~100kGy, make sizing material disposably complete crosslinking, that is, obtain that there is oneself The silastic material of viscosity.
Preferably, wherein, 1~5 part of viscosifier, 1~5 part of antibacterial, fire-retardant are added while described addition sensitizer 1~3 part of agent and 1~3 part of antioxidant.
Preferably, wherein, in described step 260In Co gamma radiation field, the sheet material after sealing or the placement position of bulk Put from 50~200Gy.min-1Absorbed dose rate.
In the present invention, the mould being molded employing in described step one is in rustless steel, polyethylene or polytetrafluoro mould A kind of;
In the present invention constitution controller be high molecular weight hydroxy silicone oil, any one in low molecule hydroxy silicon oil, by weight Part is taken as 1~9 part, and every part is 1mL.
It is different that the sensitizer adopting in the present invention is commercially available environmental-protecting chemical reagent triallyl cyanurate, triallyl Cyanurate, trimethylol-propane trimethacrylate, diacrylate -1, any one in 6- hexanediol ester, above-mentionedization Learn reagent and can produce free radical when by x radiation x.
In the preparation method of the present invention, in step one, mould is rustless steel, polyethylene or polytetrafluoro mould, using front Keep mould cleaning afterwards.
In the preparation method of the present invention, in step 2, disposably complete cross-linking reaction, secondary cross-linking need not be carried out, inhale simultaneously Receive close rate unrestricted, in the case of taking into account timeliness, placement location selects 50~200Gy.min-1Absorbed dose rate.
The silastic material with autohension of the present invention, to without the metal of special handling, plastics, glass etc. all There is good autohension, can be used as filling positioning, sealing course, also there is in weaponry important use.
The present invention at least includes following beneficial effect:
(1) present invention adopts radiation cross-linking process, not only crosslinked uniform, easy to control, energy-conserving and environment-protective, and technique simple and direct, Favorable reproducibility, production efficiency are high, simultaneously, it is to avoid using body phase crosslinking degree during peroxide cure and Density inhomogeneity, system The problems such as product Properties Control is complex or even needs high temperature, this process is not related to the higher temperature higher than 100 DEG C.
(2) silastic material with autohension prepared by the present invention has excellent combination property, can be well Adhere on multiple components and parts such as metal, glass, polyethylene, politef or parts, and lasting adhesiveness can be kept, And quality is pliable and tough, there is the mechanical properties such as preferable tensile strength and elongation at break (being shown in Table 1).
(3) present invention is a kind of method for optimizing of the silastic material with autohension, and the method is comprehensive for studying further The silastic material that the multipurpose of conjunction excellent performance has wide spectrum autohension provides the very simple and direct and good technology of repeatability Path.
Part is embodied by the further advantage of the present invention, target and feature by description below, and part also will be by this Invention research and practice and be understood by the person skilled in the art.
Specific embodiment:
With reference to embodiment, the present invention is described in further detail, to make those skilled in the art with reference to description Word can be implemented according to this.
It should be appreciated that used herein such as " have ", "comprising" and " inclusion " term do not allot one or many The presence of individual other element or a combination thereof or interpolation.
Embodiment 1:
Step one, take 100 parts of dimethyl silicone rubber to add in two-roll mills, plasticate at room temperature 10 minutes, Ran Houjia Enter 30 parts of precipitated silica, 3 parts of high molecular weight hydroxy silicone oil, knead 10 minutes, mixed sizing material at the beginning of obtaining, quiet storage 12 hours, afterwards Sizing material back mixing 10 minutes will just be mixed under room temperature, add 4 parts of triallyl cyanurate, and continue mixing 10 minutes, obtain mixing materials, Again quiet storage 48 hours, afterwards again under room temperature by sizing material back mixing 10 minutes, under room temperature, mixing materials are molded on tablet machine Type is sheet material or bulk;The rotating cylinder rotating speed of described two-roll mill is set to 200r.min-1
Step 2, the sheet material after molding or bulk are wrapped up through plastic packaging or aluminium foil after, in the air at room temperature, be placed in60Co Carry out crosslinking with radiation, absorbed dose are 50kGy, make sizing material disposably complete crosslinking, that is, obtain with autohension in gamma radiation field Silastic material.
Embodiment 2:
Step one, take 100 parts of methyl vinyl silicone rubber to add in two-roll mills, plasticate at room temperature 5 minutes, then Add 50 parts of fume colloidal silica, 7 parts of low molecule hydroxy silicon oil, knead 10 minutes, mixed sizing material at the beginning of obtaining, quiet storage 24 hours, it Sizing material back mixing 15 minutes will just be mixed afterwards under room temperature, add 5 parts of triallyl cyanurate sensitizer, and continue mixing 10 minutes, obtain To mixing materials, quiet storage 24 hours again, afterwards again under room temperature by sizing material back mixing 10 minutes, by mixing materials in tablet machine under room temperature Upper compression molding is sheet material or bulk;The rotating cylinder rotating speed of described two-roll mill is set to 600r.min-1
Step 2, the sheet material after molding or bulk are wrapped up through plastic packaging or aluminium foil after, in the air at room temperature, be placed in60Co Carry out crosslinking with radiation, absorbed dose are 100kGy, make sizing material disposably complete crosslinking, that is, obtain with autohension in gamma radiation field Silastic material.
Embodiment 3:
Step one, take 100 parts of methyl vinyl silicone rubber to add in two-roll mills, plasticate at room temperature 5 minutes, then Add 10 parts of fume colloidal silica, 1 part of low molecule hydroxy silicon oil, knead 5 minutes, mixed sizing material at the beginning of obtaining, quiet storage 12 hours, afterwards Sizing material back mixing 15 minutes will just be mixed under room temperature, add diacrylate -1,1 part of 6- hexanediol ester, continue mixing 7 minutes, mixed Refining material, again quiet storage 36 hours, afterwards again under room temperature by sizing material back mixing 10 minutes, under room temperature by mixing materials on tablet machine mould Molded for sheet material or bulk;The rotating cylinder rotating speed of described two-roll mill is set to 200r.min-1
Step 2, the sheet material after molding or bulk are wrapped up through plastic packaging or aluminium foil after, in the air at room temperature, be placed in60Co Carry out crosslinking with radiation, absorbed dose are 30kGy, make sizing material disposably complete crosslinking, that is, obtain with autohension in gamma radiation field Silastic material.
Embodiment 4:
Step one, take 100 parts of methyl phenyl vinyl silicone rubber to add in two-roll mills, plasticate at room temperature 8 minutes, It is subsequently adding 80 parts of precipitated silica, 9 parts of high molecular weight hydroxy silicone oil, knead 7 minutes, mixed sizing material at the beginning of obtaining, quiet storage 12 hours, Sizing material back mixing 10 minutes will just be mixed afterwards under room temperature, add 4 parts of triallyl isocyanurate, and continue mixing 10 minutes, obtain Mixing materials, again quiet storage 30 hours, afterwards again under room temperature by sizing material back mixing 15 minutes, under room temperature by mixing materials on tablet machine Compression molding is sheet material or bulk;The rotating cylinder rotating speed of described two-roll mill is set to 500r.min-1
Step 2, the sheet material after molding or bulk are wrapped up through plastic packaging or aluminium foil after, in the air at room temperature, be placed in60Co Carry out crosslinking with radiation, absorbed dose are 70kGy, make sizing material disposably complete crosslinking, obtain sample, that is, had in gamma radiation field There is the silastic material of autohension.
Embodiment 5:
Step one, take 100 parts of methyl vinyl silicone rubber to add in two-roll mills, plasticate at room temperature 7 minutes, then Add 30 parts of fume colloidal silica, 1 part of high molecular weight hydroxy silicone oil, knead 10 minutes, mixed sizing material at the beginning of obtaining, quiet storage 15 hours, it Sizing material back mixing 12 minutes will just be mixed afterwards under room temperature, add 5 parts of trimethylol-propane trimethacrylate, continue 10 points of mixing Clock, obtains mixing materials, again quiet storage 48 hours, afterwards again under room temperature by sizing material back mixing 15 minutes, under room temperature, mixing materials are existed On tablet machine, compression molding is sheet material or bulk;The rotating cylinder rotating speed of described two-roll mill is set to 200r.min-1
Step 2, the sheet material after molding or bulk are wrapped up through plastic packaging or aluminium foil after, in the air at room temperature, be placed in60Co Carry out crosslinking with radiation, absorbed dose are 60kGy, make sizing material disposably complete crosslinking, that is, obtain with autohension in gamma radiation field Silastic material.
Embodiment 6:
Step one, take 100 parts of methyl vinyl silicone rubber to add in two-roll mills, plasticate at room temperature 7 minutes, then Add 30 parts of fume colloidal silica, 1 part of high molecular weight hydroxy silicone oil, knead 10 minutes, mixed sizing material at the beginning of obtaining, quiet storage 15 hours, it Sizing material back mixing 12 minutes will just be mixed afterwards under room temperature, add 5 parts of trimethylol-propane trimethacrylate, 4 parts of viscosifier, antibacterial 4 parts of agent, 2 parts of fire retardant, 2 parts of antioxidant, continue mixing 10 minutes, obtain mixing materials, again quiet storage 48 hours, secondary chamber more afterwards By sizing material back mixing 15 minutes under temperature, under room temperature, by mixing materials, on tablet machine, compression molding is sheet material or bulk;Described double roller is opened The rotating cylinder rotating speed of mill is set to 200r.min-1
Step 2, the sheet material after molding or bulk are wrapped up through plastic packaging or aluminium foil after, in the air at room temperature, be placed in60Co Carry out crosslinking with radiation, absorbed dose are 60kGy, make sizing material disposably complete crosslinking, that is, obtain with autohension in gamma radiation field Silastic material.
Described antibacterial is chitin;Described fire retardant is weight ratio for 3:1 magnesium hydroxide and aluminium hydroxide;Described anti- Oxygen agent is weight ratio for 3:2:1 phenyl silicone oil, MethylethoxylsiliconFluid Fluid and DBPC 2,6 ditertiary butyl p cresol;
The preparation method of described viscosifier is:By weight, 100 parts of starch are taken, 100 parts of water of addition and 10 parts of weight ratios are 2:1 tripolycyanamide and ammonium carbonate, stir, and adjust pH to 9 with the carbamide of 1.5mol/L, add 50 parts of epoxychloropropane, Stirring reaction 5 hours under conditions of 40 DEG C of temperature, filters, and with washing with alcohol, is dried, obtains crosslinked starch;Anti- in supercritical Answer and add weight ratio in device for 1:1 crosslinked starch and 30 parts of carrageenan, 20 parts of butyl acrylate, 3 parts of acrylamide, over cure 0.02 part of sour ammonium, 200 parts of water, stir, then seal system, be passed through the bar to 25MPa, temperature 60 C for the carbon dioxide React under part 5 hours, then use ethanol precipitation, be vacuum dried at 70 DEG C, obtain reacting coarse product, will be thick with apparatus,Soxhlet'ses Product until the homopolymer producing except dereaction, is vacuum dried 24 hours at 65 DEG C, obtains viscosifier with acetone elution.
Embodiment 7:
Step one, take 100 parts of dimethyl silicone rubber to add in two-roll mills, plasticate at room temperature 10 minutes, Ran Houjia Enter 30 parts of precipitated silica, 3 parts of high molecular weight hydroxy silicone oil, knead 10 minutes, mixed sizing material at the beginning of obtaining, quiet storage 12 hours, afterwards Sizing material back mixing 10 minutes will just be mixed under room temperature, add 4 parts of triallyl cyanurate, 4 parts of viscosifier, continue mixing 10 minutes, Obtain mixing materials, again quiet storage 48 hours, afterwards again under room temperature by sizing material back mixing 10 minutes, by mixing materials in tabletting under room temperature On machine, compression molding is sheet material or bulk;The rotating cylinder rotating speed of described two-roll mill is set to 200r.min-1
Step 2, the sheet material after molding or bulk are wrapped up through plastic packaging or aluminium foil after, in the air at room temperature, be placed in60Co Carry out crosslinking with radiation, absorbed dose are 50kGy, make sizing material disposably complete crosslinking, that is, obtain with autohension in gamma radiation field Silastic material;
The preparation method of described viscosifier is:By weight, 100 parts of starch are taken, 100 parts of water of addition and 10 parts of weight ratios are 2:1 tripolycyanamide and ammonium carbonate, stir, and adjust pH to 9 with the carbamide of 1.5mol/L, add 50 parts of epoxychloropropane, Stirring reaction 5 hours under conditions of 40 DEG C of temperature, filters, and with washing with alcohol, is dried, obtains crosslinked starch;Anti- in supercritical Answer and add weight ratio in device for 1:1 crosslinked starch and 30 parts of carrageenan, 20 parts of butyl acrylate, 3 parts of acrylamide, over cure 0.02 part of sour ammonium, 200 parts of water, stir, then seal system, be passed through the bar to 25MPa, temperature 60 C for the carbon dioxide React under part 5 hours, then use ethanol precipitation, be vacuum dried at 70 DEG C, obtain reacting coarse product, will be thick with apparatus,Soxhlet'ses Product until the homopolymer producing except dereaction, is vacuum dried 24 hours at 65 DEG C, obtains viscosifier with acetone elution.
Embodiment 8:
Step one, take 100 parts of dimethyl silicone rubber to add in two-roll mills, plasticate at room temperature 10 minutes, Ran Houjia Enter 30 parts of precipitated silica, 3 parts of high molecular weight hydroxy silicone oil, knead 10 minutes, mixed sizing material at the beginning of obtaining, quiet storage 12 hours, afterwards Sizing material back mixing 10 minutes will just be mixed under room temperature, add 4 parts of triallyl cyanurate, 4 parts of antibacterial, 2 parts of fire retardant, antioxidant 2 parts, continue mixing 10 minutes, obtain mixing materials, again quiet storage 48 hours, afterwards again under room temperature by sizing material back mixing 10 minutes, Under room temperature, by mixing materials, on tablet machine, compression molding is sheet material or bulk;The rotating cylinder rotating speed of described two-roll mill is set to 200r.min-1
Step 2, the sheet material after molding or bulk are wrapped up through plastic packaging or aluminium foil after, in the air at room temperature, be placed in60Co Carry out crosslinking with radiation, absorbed dose are 50kGy, make sizing material disposably complete crosslinking, that is, obtain with autohension in gamma radiation field Silastic material;
Described antibacterial is chitin;Described fire retardant is weight ratio for 3:1 magnesium hydroxide and aluminium hydroxide;Described anti- Oxygen agent is weight ratio for 3:2:1 phenyl silicone oil, MethylethoxylsiliconFluid Fluid and DBPC 2,6 ditertiary butyl p cresol.
Embodiment 9:
Step one, take 100 parts of dimethyl silicone rubber to add in two-roll mills, plasticate at room temperature 10 minutes, Ran Houjia Enter 30 parts of precipitated silica, 3 parts of high molecular weight hydroxy silicone oil, knead 10 minutes, mixed sizing material at the beginning of obtaining, quiet storage 12 hours, afterwards Sizing material back mixing 10 minutes will just be mixed under room temperature, add 4 parts of triallyl cyanurate, 4 parts of viscosifier, 4 parts of antibacterial, fire retardant 2 parts, 2 parts of antioxidant, continue mixing 10 minutes, obtain mixing materials, and sizing material is returned under room temperature by quiet storage 48 hours afterwards again again Refining 10 minutes, under room temperature, by mixing materials, on tablet machine, compression molding is sheet material or bulk;The rotating cylinder of described two-roll mill turns Speed is set to 200r.min-1
Step 2, the sheet material after molding or bulk are wrapped up through plastic packaging or aluminium foil after, in the air at room temperature, be placed in60Co Carry out crosslinking with radiation, absorbed dose are 50kGy, make sizing material disposably complete crosslinking, that is, obtain with autohension in gamma radiation field Silastic material;
Described viscosifier adopt the viscosifier in embodiment 7;Described antibacterial, fire retardant and antioxidant adopt embodiment 8 Described in material.
In order to the effect of the present invention is described, inventor provides contrast experiment as follows:
Comparative example 1:
Patent documentation CN104788967A disclosed " a kind of silicone rubber microporous foamed materialss of mixed type foam structure and The silicone rubber microporous foamed materialss of the mixed type foam structure of preparation in embodiment 1~8 in its preparation method ".
Comparative example 2:
In patent documentation CN104744946A disclosed " a kind of high temperature resistant type silicon rubber foam material and preparation method thereof " The high temperature resistant type silicon rubber foam material of preparation in embodiment 1~5.
Comparative example 3:
Make the quiet storage time first time in step one be less than 12 hours (be respectively provided with 8 hours, 5 hours, 1 hour, 30min, 10min), remaining parameter respectively with identical in embodiment 1~9, technical process is also identical.
Autohension test is carried out to embodiment 1~9 and comparative example 1~3:Take any surface finish, size about 200mm × 20mm × The rustless steel of 5mm, glass, polyethylene, politef material model block, by diameter 25mm, the embodiment 1~9 of thick 4mm and right The test sample of ratio 1~3 is respectively placed on the test surfaces of each model block, and mark position, then each model block is stood on reality Test on platform, keep test surfaces to be 90 degree with the angle of test table top, static 96h, the test sample in embodiment 1~9 does not all take off Fall, also there is no obvious sliding, and the test sample in comparative example 1~3 all comes off;When reaching 240h between when resting, real Slight sliding in the test sample applied in example 1~5 and 8, and the test sample in embodiment 6,7 and 9 does not all fall off, and does not have yet There is obvious sliding;When reaching 720h between when resting, obvious sliding in the test sample in embodiment 1~5 and 8, and The test sample of embodiment 6,7 and 9 does not all fall off, and does not have obvious sliding yet.
Other the performance test results are shown in Table 1:
Table 1
Performance Embodiment 1 Embodiment 2 Embodiment 3 Embodiment 4 Embodiment 5
Shore hardness (HA) 50 61 22 67 51
Tensile strength (MPa) 9.74 3.21 4.25 35.7 6.49
Elongation at break (%) 366 320 912 200 715
Tearing strength (KN.m-1) 19.7 27.1 12.6 41.3 28.8
Although embodiment of the present invention is disclosed as above, it is not restricted to listed in description and embodiment With, it can be applied to various suitable the field of the invention completely, for those skilled in the art, can be easily Realize other modification, therefore under the general concept being limited without departing substantially from claim and equivalency range, the present invention does not limit In specific details with shown here as the example with description.

Claims (10)

1. a kind of silastic material with autohension, wherein, the formula of described silastic material forms by weight:Silicon rubber 100 parts of glue, 10~80 parts of reinforcing agent, 1~9 part of controlling agent, 0~5 part of sensitizer.
2. there is the silastic material of autohension as claimed in claim 1, wherein, the formula composition of described silastic material is also Including:1~5 part of viscosifier, 1~5 part of antibacterial, 1~3 part of fire retardant, 1~3 part of antioxidant.
3. there is the silastic material of autohension as claimed in claim 2, wherein, the formula of described material forms by weight For:100 parts of silicone rubber base material, 30 parts of reinforcing agent, 3 parts of controlling agent, 4 parts of sensitizer, 4 parts of viscosifier, 4 parts of antibacterial, fire retardant 2 Part, 2 parts of antioxidant.
4. the silastic material with autohension as any one of claims 1 to 3, wherein, described autohension silicon rubber Glue material shore hardness 22~67, tensile strength are 3.21~35.7MPa, elongation at break 200~912%, tearing strength 12.6~41.3MPa.
5. there is the silastic material of autohension as claimed in claim 2, wherein,
Described silicone rubber is dimethyl silicone rubber, methyl vinyl silicone rubber, any one in methyl phenyl vinyl silicone rubber Kind;
Described reinforcing agent is precipitated silica, any one in fume colloidal silica;
Described constitution controller is high molecular weight hydroxy silicone oil, any one in low molecule hydroxy silicon oil;
Described sensitizer is triallyl cyanurate, triallyl isocyanurate, trimethylol propane trimethyl acrylic acid Any one in ester, diacrylate -1,6-HD ester;
Described antibacterial is chitin, zinc oxide, any one in copper oxide;
Described fire retardant is weight ratio for 3:1 magnesium hydroxide and aluminium hydroxide;
Described antioxidant is weight ratio for 3:2:1 phenyl silicone oil, MethylethoxylsiliconFluid Fluid and DBPC 2,6 ditertiary butyl p cresol.
6. there is the silastic material of autohension as claimed in claim 2, wherein, the preparation method of described viscosifier is:Press Weight portion, takes 100 parts of starch, adds 100 parts of water and 10 parts of weight ratio for 2:1 tripolycyanamide and ammonium carbonate, stir, and use The carbamide of 1.5mol/L adjusts pH to 9, adds 50 parts of epoxychloropropane, stirring reaction 4~5 under conditions of 30~40 DEG C of temperature Hour, filter, with washing with alcohol, be dried, obtain crosslinked starch;Add weight ratio for 1 in supercritical reaction apparatus:1 friendship Connection starch and 30~35 parts of carrageenan, 20~25 parts of butyl acrylate, 3~5 parts of acrylamide, Ammonium persulfate. 0.02~0.08 Part, 200~250 parts of water, stir, then system sealed, be passed through carbon dioxide to 60~75 DEG C of 25~45MPa, temperature React under conditions of lower 5~8 hours, then use ethanol precipitation, be vacuum dried at 70 DEG C, obtain reacting coarse product, use Soxhlet Crude product is eluted the homopolymer until producing except dereaction by extractor with acetone, is vacuum dried 24 hours, obtains at 65 DEG C Viscosifier.
7. there is the silastic material of autohension as claimed in claim 5, wherein, the molecular weight of described silicone rubber is 50~70 Ten thousand, the molar content of methyl vinyl silicone rubber medium vinyl is 0.04~0.60%, methyl phenyl vinyl silicone rubber The molar content of middle phenyl is 1.0~30.0%.
8. a kind of preparation method of the silastic material as claimed in claim 1 with autohension, wherein, methods described includes Following steps:
Step one, by weight, takes silicone rubber to add in two-roll mill, plasticates at room temperature 5~10 minutes, be subsequently adding benefit Strong agent, constitution controller, knead 5~10 minutes, obtain just mixed sizing material, quiet storage 12~24 hours, will just mix glue afterwards under room temperature Material back mixing 10~15 minutes, adds sensitizer, continues mixing 5~10 minutes, obtains mixing materials, again quiet storage 24~48 hours, Afterwards again under room temperature by sizing material back mixing 10~15 minutes, under room temperature by mixing materials on tablet machine compression molding be sheet material or block Material;The rotating cylinder rotating speed of described two-roll mill is set to 200~600r.min-1
Step 2, the sheet material after molding or bulk are wrapped up through plastic packaging or aluminium foil after, in the air at room temperature, be placed in60Co γ spoke Penetrate and in field, carry out crosslinking with radiation, absorbed dose are 30~100kGy, make sizing material disposably complete crosslinking, that is, obtain with autohension Silastic material.
9. there is the preparation method of the silastic material of autohension as claimed in claim 8, wherein, described addition sensitizer It is simultaneously introduced 1~5 part of viscosifier, 1~5 part of antibacterial, 1~3 part of fire retardant and 1~3 part of antioxidant.
10. there is the preparation method of the silastic material of autohension as claimed in claim 8, wherein, in described step 260In Co gamma radiation field, the sheet material after sealing or the placement location of bulk select 50~200Gy.min-1Absorbed dose rate.
CN201610863836.3A 2016-09-29 2016-09-29 Silastic material and preparation method thereof with tack Expired - Fee Related CN106380860B (en)

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CN107815122A (en) * 2017-11-15 2018-03-20 中国工程物理研究院核物理与化学研究所 High-strength tear-resistant type silicon rubber foam material and preparation method thereof
CN109825088A (en) * 2019-02-22 2019-05-31 中国工程物理研究院核物理与化学研究所 A kind of silicon rubber base flexibility neutron shielding material and preparation method thereof
CN110128827A (en) * 2019-04-09 2019-08-16 兴化市戴窑镇永生橡胶制品厂 A kind of silicon rubber with compared with strong interface adhesive property
CN110256852A (en) * 2019-07-01 2019-09-20 深圳市麟富科技有限公司 The special type composite material and production technology and purposes of a kind of absorption of electromagnetic radiation
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CN104893312A (en) * 2015-07-01 2015-09-09 中国工程物理研究院核物理与化学研究所 Composite enhanced high-flexibility microporous silicone rubber foam material and preparation method thereof
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CN107082965A (en) * 2017-05-24 2017-08-22 北京市射线应用研究中心 A kind of anti-neutron composite shielding material of self-adhering-type and preparation method and application
CN107722638A (en) * 2017-11-15 2018-02-23 中国工程物理研究院核物理与化学研究所 Tear-resistant type silicon rubber composite material and preparation method thereof
CN107815122A (en) * 2017-11-15 2018-03-20 中国工程物理研究院核物理与化学研究所 High-strength tear-resistant type silicon rubber foam material and preparation method thereof
CN107815122B (en) * 2017-11-15 2020-08-25 中国工程物理研究院核物理与化学研究所 High-strength tear-resistant silicone rubber foam material and preparation method thereof
CN109825088A (en) * 2019-02-22 2019-05-31 中国工程物理研究院核物理与化学研究所 A kind of silicon rubber base flexibility neutron shielding material and preparation method thereof
CN110289115A (en) * 2019-02-22 2019-09-27 西南科技大学 A kind of high-strength silicon rubber base flexibility neutron shielding material and preparation method thereof
CN109825088B (en) * 2019-02-22 2021-06-15 中国工程物理研究院核物理与化学研究所 Silicon rubber-based flexible neutron shielding material and preparation method thereof
CN110289115B (en) * 2019-02-22 2022-08-30 中国工程物理研究院核物理与化学研究所 High-strength silicone rubber-based flexible neutron shielding material and preparation method thereof
CN110128827A (en) * 2019-04-09 2019-08-16 兴化市戴窑镇永生橡胶制品厂 A kind of silicon rubber with compared with strong interface adhesive property
CN110256852A (en) * 2019-07-01 2019-09-20 深圳市麟富科技有限公司 The special type composite material and production technology and purposes of a kind of absorption of electromagnetic radiation
CN116082846A (en) * 2023-01-05 2023-05-09 湖南防灾科技有限公司 Composition for composite silicone rubber material, preparation method and application thereof

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