CN106380860B - Silastic material and preparation method thereof with tack - Google Patents

Silastic material and preparation method thereof with tack Download PDF

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Publication number
CN106380860B
CN106380860B CN201610863836.3A CN201610863836A CN106380860B CN 106380860 B CN106380860 B CN 106380860B CN 201610863836 A CN201610863836 A CN 201610863836A CN 106380860 B CN106380860 B CN 106380860B
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parts
tack
minutes
room temperature
silastic material
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CN106380860A (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
Southwest University of Science and Technology
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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 kind of silastic material and preparation method thereof with tack, its main feature is that after 100 parts of silicon rubber, 10~80 parts of reinforcing agent, 1~9 part of controlling agent, 0~5 part of sensitizer are kneaded and are formed, it is allowed to crosslink through gamma Rays, radiation absorbed dose is 30~100kGy, and the tack silastic material haveing excellent performance can be obtained.Present invention process is simple, does not need complicated chemical raw material and process control or professional ancillary equipment, cost is relatively low;And the silastic material of preparation can adhere well on a variety of components such as metal, glass, polyethylene, polytetrafluoroethylene (PTFE) or parts, and be able to maintain lasting adhesiveness, can effectively prevent falling off or sliding for component or parts.

Description

Silastic material and preparation method thereof with tack
Technical field
The invention belongs to technical field of rubber material, and in particular to a kind of silastic material and its preparation with tack Method.
Background technique
Silastic material is widely used in the assembly and production of articles such as electronic component, equipment parts.Very much In the case of, it is desirable that there is good adhesion property, to reach ideal effect between silicon rubber and component, parts.It is existing Assembly and production method in technology usually coat binder in advance on component or parts, or in silicon rubber material Expect that upper one layer of pressure sensitive adhesive is adhered on surface, with the preferable bonding between reaching, but this mode is the disadvantage is that manufacturing procedure is cumbersome, And to the more demanding of binder, binder usually requires have good comprehensive performance, such as heat-resisting.Currently, open source information The tack silastic material of display usually requires to cause crosslinking, high-temperature vacuum heat treatment using peroxide in preparatory phase, And essentially metal tack, such as patent CN201210437042.2 etc..Therefore, research has wide spectrum tack and preparation work The silastic material of the simple and direct environmental protection of skill has very positive meaning.
Summary of the invention
As various extensive and careful research and experiment as a result, it has been found by the inventor that using radiation The silastic material with wide spectrum tack can be prepared in the method for crosslinking, be not only crosslinked uniform, easy to control, energy-saving ring It protects, and technique is simple and direct, favorable reproducibility, high production efficiency, while the material mechanical performance is excellent.Based on this discovery, complete The present invention.
It is excellent it is an object of the invention to solve at least the above problems and/or defect, and provide at least to will be described later Point.
A further object of the invention is the method by crosslinking with radiation, improves the life with the silastic material of tack Efficiency is produced, and is had excellent performance with this and the silastic material of the simple and direct environmental protection of preparation process.
In order to realize these purposes and other advantages according to the present invention, a kind of silicon rubber material with tack is provided Material, wherein the formula composition of the silastic material is by weight are as follows: 100 parts of silicon rubber, 10~80 parts of reinforcing agent, controlling agent 1 ~9 parts, 0~5 part of sensitizer.
Preferably, wherein the formula composition of the silastic material further include: 1~5 part of tackifier, antibacterial agent 1~5 Part, 1~3 part of fire retardant, 1~3 part of antioxidant.
Preferably, wherein the formula composition of the material is by weight are as follows: 100 parts of silicon rubber base-material, reinforcing agent 30 Part, 3 parts of controlling agent, 4 parts of sensitizer, 4 parts of tackifier, 4 parts of antibacterial agent, 2 parts of fire retardant, 2 parts of antioxidant.
Preferably, wherein the tack silastic material shore hardness 22~67, tensile strength be 3.21~ 35.7MPa, elongation at break 200~912%, 12.6~41.3MPa of tearing strength.
Preferably, wherein
The silicon rubber is dimethyl silicone rubber, methyl vinyl silicone rubber, appointing in methyl phenyl vinyl silicone rubber It anticipates one kind;
The reinforcing agent is precipitated silica, any one in fume colloidal silica;
The constitution controller is high molecular weight hydroxy silicone oil, any one in low molecule hydroxy silicon oil;
The sensitizer is triallyl cyanurate, triallyl isocyanurate, trimethylol propane trimethyl third Any one in olefin(e) acid ester, diacrylate -1,6-HD ester;
The antibacterial agent is chitin, zinc oxide, any one in copper oxide;
The fire retardant is the magnesium hydroxide and aluminium hydroxide that weight ratio is 3:1;
The antioxidant be weight ratio be 3:2:1 phenyl silicone oil, MethylethoxylsiliconFluid Fluid and 2,6- di-t-butyl to first Phenol.
Preferably, wherein the tackifier the preparation method comprises the following steps: by weight, take 100 parts of starch, 100 parts of water are added The melamine and ammonium carbonate for being 2:1 with 10 parts of weight ratios, stir evenly, and adjust pH to 9 with the urea of 1.5mol/L, are added 50 Part epoxychloropropane, is stirred to react 4~5 hours under conditions of 30~40 DEG C of temperature, filters, dry with ethanol washing, obtains Crosslinked starch;The crosslinked starch and 30~35 parts of carragheen, acrylic acid fourth that weight ratio is 1:1 are added in supercritical reaction apparatus 20~25 parts of ester, 3~5 parts of acrylamide, 0.02~0.08 part of ammonium persulfate, 200~250 parts of water, stir evenly, then by body System's sealing, reacts 5~8 hours under conditions of being passed through at carbon dioxide to 25~45MPa, 60~75 DEG C of temperature, then uses ethyl alcohol Precipitating, is dried in vacuo at 70 DEG C, obtains reacting coarse product, is eluted crude product acetone until removing anti-with Soxhlet extractor The homopolymer that should be generated is dried in vacuo 24 hours at 65 DEG C, obtains tackifier.
Preferably, wherein the molecular weight of the silicon rubber is 50~700,000, methyl vinyl silicone rubber medium vinyl Molar content is 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 methods of above-mentioned silastic material with tack, wherein the method The following steps are included:
Step 1: by weight, take silicon rubber to be added in two-roll mill, plasticate at room temperature 5~10 minutes, then plus Enter reinforcing agent, constitution controller, be kneaded 5~10 minutes, obtains just mixed sizing material, quiet storage 12~24 hours later at room temperature will be first Mixed sizing material back mixing 10~15 minutes, sensitizer is added, continues mixing 5~10 minutes, obtains mixing materials, quiet storage 24~48 is small again When, mixing materials are pressed and molded as sheet material on tablet press machine at room temperature at room temperature by sizing material back mixing 10~15 minutes again later Or bulk;The rotating cylinder revolving speed of the two-roll mill is set as 200~600r.min-1
Step 2: sheet material after molding or bulk at room temperature in air, are placed in after plastic packaging or aluminium foil package60Co Crosslinking with radiation is carried out in gamma radiation field, absorbed dose is 30~100kGy, and sizing material is made to complete crosslinking disposably to get to certainly The silastic material of viscosity.
Preferably, wherein 1~5 part of tackifier, 1~5 part of antibacterial agent, fire-retardant are added while the addition sensitizer 1~3 part and 1~3 part of antioxidant of agent.
Preferably, wherein in the step 260In Co gamma radiation field, the placement position of sheet material or bulk after sealing Set 50~200Gy.min of selection-1Absorbed dose rate.
In the present invention, the mold used is molded in the step 1 as in stainless steel, polyethylene or polytetrafluoro mold It is a kind of;
Constitution controller is high molecular weight hydroxy silicone oil, any one in low molecule hydroxy silicon oil in the present invention, by weight Part is taken as 1~9 part, and every part is 1mL.
The sensitizer used in the present invention is that commercially available environmental-protecting chemical reagent triallyl cyanurate, triallyl are different Cyanurate, trimethylol-propane trimethacrylate, any one in diacrylate -1,6- hexylene glycol ester, above-mentionedization Learning reagent can generate free radicals when by ray radiation.
In preparation method of the invention, molding die is stainless steel, polyethylene or polytetrafluoro mold in step 1, before use Mold cleaning is kept afterwards.
In preparation method of the invention, cross-linking reaction is disposably completed in step 2, without carrying out secondary cross-linking, is inhaled simultaneously It is unrestricted to receive dosage rate, in the case where taking into account timeliness, placement location selects 50~200Gy.min-1Absorbed dose rate.
Silastic material of the present invention with tack, to metal, plastics, glass for being not necessarily to specially treated etc. With good tack, it can be used as filling positioning, sealing course, also there is important use in weaponry.
The present invention is include at least the following beneficial effects:
(1) present invention uses radiation cross-linking process, is not only crosslinked uniform, easy to control, energy conservation and environmental protection, and technique it is simple and direct, Favorable reproducibility, high production efficiency, meanwhile, it avoids using peroxide cure Shi Tixiang crosslinking degree and Density inhomogeneity, system Moral character can control complex or even the problems such as need high temperature, this process is not related to the higher temperature higher than 100 DEG C.
(2) silastic material with tack prepared by the present invention has excellent comprehensive performance, can be well It adheres on a variety of components such as metal, glass, polyethylene, polytetrafluoroethylene (PTFE) or parts, and is able to maintain lasting adhesiveness, And quality is flexible, has the mechanical properties (being shown in Table 1) such as preferable tensile strength and elongation at break.
(3) present invention is a kind of preferred method of silastic material with tack, and this method is comprehensive further to study Closing the multipurpose haveing excellent performance, there is the silastic material of wide spectrum tack to provide the good technology of very simple and direct and reproducibility Path.
Further advantage, target and feature of the invention will be partially reflected by the following instructions, and part will also be by this The research and practice of invention and be understood by the person skilled in the art.
Specific embodiment:
The present invention will be further described in detail below with reference to the embodiments, to enable those skilled in the art referring to specification Text can be implemented accordingly.
It should be appreciated that such as " having ", "comprising" and " comprising " term used herein do not allot one or more The presence or addition of a other elements or combinations thereof.
Embodiment 1:
Step 1: taking in 100 parts of addition two-roll mills of dimethyl silicone rubber, plasticate at room temperature 10 minutes, then plus Enter 30 parts of precipitated silica, 3 parts of high molecular weight hydroxy silicone oil, be kneaded 10 minutes, obtains just mixing sizing material, quiet storage 12 hours, later It will just mix sizing material back mixing 10 minutes at room temperature, and be added 4 parts of triallyl cyanurate, and continue to be kneaded 10 minutes, obtain mixing materials, Mixing materials, are molded at room temperature by sizing material back mixing 10 minutes by quiet storage 48 hours again on tablet press machine at room temperature again later Type is sheet material or bulk;The rotating cylinder revolving speed of the two-roll mill is set as 200r.min-1
Step 2: sheet material after molding or bulk at room temperature in air, are placed in after plastic packaging or aluminium foil package60Co Crosslinking with radiation is carried out in gamma radiation field, absorbed dose 50kGy makes sizing material complete crosslinking disposably to get to tack Silastic material.
Embodiment 2:
Step 1: taking in 100 parts of addition two-roll mills of methyl vinyl silicone rubber, plasticate at room temperature 5 minutes, then 50 parts of fume colloidal silica, 7 parts of low molecule hydroxy silicon oil is added, is kneaded 10 minutes, obtains just mixed sizing material, it is quiet to store up 24 hours, it It will just mix sizing material back mixing 15 minutes at room temperature afterwards, and be added 5 parts of triallyl cyanurate sensitizer, and continue to be kneaded 10 minutes, obtain It is quiet again to store up 24 hours to mixing materials, later again at room temperature by sizing material back mixing 10 minutes, at room temperature by mixing materials in tablet press machine Upper compression molding is sheet material or bulk;The rotating cylinder revolving speed of the two-roll mill is set as 600r.min-1
Step 2: sheet material after molding or bulk at room temperature in air, are placed in after plastic packaging or aluminium foil package60Co Crosslinking with radiation is carried out in gamma radiation field, absorbed dose 100kGy makes sizing material complete crosslinking disposably to get to tack Silastic material.
Embodiment 3:
Step 1: taking in 100 parts of addition two-roll mills of methyl vinyl silicone rubber, plasticate at room temperature 5 minutes, then 10 parts of fume colloidal silica, 1 part of low molecule hydroxy silicon oil is added, is kneaded 5 minutes, obtains just mixing sizing material, quiet storage 12 hours, later It will just mix sizing material back mixing 15 minutes at room temperature, 1 part of diacrylate -1,6- hexylene glycol ester is added, and continue to be kneaded 7 minutes, be mixed Refining material, it is quiet again to store up 36 hours, later again at room temperature by sizing material back mixing 10 minutes, at room temperature by mixing materials in tablet press machine upper mold Molded is sheet material or bulk;The rotating cylinder revolving speed of the two-roll mill is set as 200r.min-1
Step 2: sheet material after molding or bulk at room temperature in air, are placed in after plastic packaging or aluminium foil package60Co Crosslinking with radiation is carried out in gamma radiation field, absorbed dose 30kGy makes sizing material complete crosslinking disposably to get to tack Silastic material.
Embodiment 4:
Step 1: taking in 100 parts of addition two-roll mills of methyl phenyl vinyl silicone rubber, plasticate at room temperature 8 minutes, Then 80 parts of precipitated silica, 9 parts of high molecular weight hydroxy silicone oil is added, is kneaded 7 minutes, obtains just mixed sizing material, it is quiet to store up 12 hours, It will just mix sizing material back mixing 10 minutes at room temperature later, and be added 4 parts of triallyl isocyanurate, and continue to be kneaded 10 minutes, obtain Mixing materials, it is quiet again to store up 30 hours, later again at room temperature by sizing material back mixing 15 minutes, at room temperature by mixing materials on tablet press machine Compression molding is sheet material or bulk;The rotating cylinder revolving speed of the two-roll mill is set as 500r.min-1
Step 2: sheet material after molding or bulk at room temperature in air, are placed in after plastic packaging or aluminium foil package60Co Crosslinking with radiation is carried out in gamma radiation field, absorbed dose 70kGy makes sizing material disposably complete to be crosslinked, and obtains sample to get tool is arrived There is the silastic material of tack.
Embodiment 5:
Step 1: taking in 100 parts of addition two-roll mills of methyl vinyl silicone rubber, plasticate at room temperature 7 minutes, then 30 parts of fume colloidal silica, 1 part of high molecular weight hydroxy silicone oil is added, is kneaded 10 minutes, obtains just mixed sizing material, it is quiet to store up 15 hours, it It will just mix sizing material back mixing 12 minutes at room temperature afterwards, and be added 5 parts of trimethylol-propane trimethacrylate, and continue to be kneaded 10 points Clock obtains mixing materials, and quiet storage 48 hours, later again at room temperature exist mixing materials at room temperature by sizing material back mixing 15 minutes again Compression molding is sheet material or bulk on tablet press machine;The rotating cylinder revolving speed of the two-roll mill is set as 200r.min-1
Step 2: sheet material after molding or bulk at room temperature in air, are placed in after plastic packaging or aluminium foil package60Co Crosslinking with radiation is carried out in gamma radiation field, absorbed dose 60kGy makes sizing material complete crosslinking disposably to get to tack Silastic material.
Embodiment 6:
Step 1: taking in 100 parts of addition two-roll mills of methyl vinyl silicone rubber, plasticate at room temperature 7 minutes, then 30 parts of fume colloidal silica, 1 part of high molecular weight hydroxy silicone oil is added, is kneaded 10 minutes, obtains just mixed sizing material, it is quiet to store up 15 hours, it It will just mix sizing material back mixing 12 minutes at room temperature afterwards, 5 parts of trimethylol-propane trimethacrylate, 4 parts of tackifier, antibacterial is added 4 parts of agent, 2 parts of fire retardant, 2 parts of antioxidant continue to be kneaded 10 minutes, obtain mixing materials, again quiet storage 48 hours, later secondary chamber again By sizing material back mixing 15 minutes under temperature, mixing materials are pressed and molded on tablet press machine at room temperature as sheet material or bulk;The double roller is opened The rotating cylinder revolving speed of mill is set as 200r.min-1
Step 2: sheet material after molding or bulk at room temperature in air, are placed in after plastic packaging or aluminium foil package60Co Crosslinking with radiation is carried out in gamma radiation field, absorbed dose 60kGy makes sizing material complete crosslinking disposably to get to tack Silastic material.
The antibacterial agent is chitin;The fire retardant is the magnesium hydroxide and aluminium hydroxide that weight ratio is 3:1;It is described anti- Oxygen agent is phenyl silicone oil, MethylethoxylsiliconFluid Fluid and the DBPC 2,6 ditertiary butyl p cresol that weight ratio is 3:2:1;
The tackifier the preparation method comprises the following steps: by weight, take 100 parts of starch, 100 parts of water are added and 10 parts of weight ratios are The melamine and ammonium carbonate of 2:1, stirs evenly, and adjusts pH to 9 with the urea of 1.5mol/L, 50 parts of epoxychloropropane are added, It is stirred to react 5 hours, filters under conditions of 40 DEG C of temperature, it is dry with ethanol washing, obtain crosslinked starch;Overcritical anti- Answer the crosslinked starch and 30 parts of carragheen, 20 parts of butyl acrylate, 3 parts of acrylamide, over cure for being added that weight ratio is 1:1 in device 0.02 part of sour ammonium, 200 parts of water, stir evenly, then seal system, the item being passed through under carbon dioxide to 25MPa, temperature 60 C It is reacted under part 5 hours, then uses ethanol precipitation, be dried in vacuo at 70 DEG C, obtain reacting coarse product, it will be thick with Soxhlet extractor Homopolymer of the product acetone elution up to removing dereaction generation, is dried in vacuo 24 hours at 65 DEG C, obtains tackifier.
Embodiment 7:
Step 1: taking in 100 parts of addition two-roll mills of dimethyl silicone rubber, plasticate at room temperature 10 minutes, then plus Enter 30 parts of precipitated silica, 3 parts of high molecular weight hydroxy silicone oil, be kneaded 10 minutes, obtains just mixing sizing material, quiet storage 12 hours, later It will just mix sizing material back mixing 10 minutes at room temperature, and be added 4 parts of triallyl cyanurate, 4 parts of tackifier, continue to be kneaded 10 minutes, Mixing materials are obtained, again quiet storage 48 hours, later again at room temperature by sizing material back mixing 10 minutes, at room temperature by mixing materials in tabletting Compression molding is sheet material or bulk on machine;The rotating cylinder revolving speed of the two-roll mill is set as 200r.min-1
Step 2: sheet material after molding or bulk at room temperature in air, are placed in after plastic packaging or aluminium foil package60Co Crosslinking with radiation is carried out in gamma radiation field, absorbed dose 50kGy makes sizing material complete crosslinking disposably to get to tack Silastic material;
The tackifier the preparation method comprises the following steps: by weight, take 100 parts of starch, 100 parts of water are added and 10 parts of weight ratios are The melamine and ammonium carbonate of 2:1, stirs evenly, and adjusts pH to 9 with the urea of 1.5mol/L, 50 parts of epoxychloropropane are added, It is stirred to react 5 hours, filters under conditions of 40 DEG C of temperature, it is dry with ethanol washing, obtain crosslinked starch;Overcritical anti- Answer the crosslinked starch and 30 parts of carragheen, 20 parts of butyl acrylate, 3 parts of acrylamide, over cure for being added that weight ratio is 1:1 in device 0.02 part of sour ammonium, 200 parts of water, stir evenly, then seal system, the item being passed through under carbon dioxide to 25MPa, temperature 60 C It is reacted under part 5 hours, then uses ethanol precipitation, be dried in vacuo at 70 DEG C, obtain reacting coarse product, it will be thick with Soxhlet extractor Homopolymer of the product acetone elution up to removing dereaction generation, is dried in vacuo 24 hours at 65 DEG C, obtains tackifier.
Embodiment 8:
Step 1: taking in 100 parts of addition two-roll mills of dimethyl silicone rubber, plasticate at room temperature 10 minutes, then plus Enter 30 parts of precipitated silica, 3 parts of high molecular weight hydroxy silicone oil, be kneaded 10 minutes, obtains just mixing sizing material, quiet storage 12 hours, later It will just mix sizing material back mixing 10 minutes at room temperature, and be added 4 parts of triallyl cyanurate, 4 parts of antibacterial agent, 2 parts of fire retardant, antioxidant 2 parts, continue to be kneaded 10 minutes, obtain mixing materials, again quiet storage 48 hours, later again at room temperature by sizing material back mixing 10 minutes, Mixing materials are pressed and molded on tablet press machine at room temperature as sheet material or bulk;The rotating cylinder revolving speed of the two-roll mill is set as 200r.min-1
Step 2: sheet material after molding or bulk at room temperature in air, are placed in after plastic packaging or aluminium foil package60Co Crosslinking with radiation is carried out in gamma radiation field, absorbed dose 50kGy makes sizing material complete crosslinking disposably to get to tack Silastic material;
The antibacterial agent is chitin;The fire retardant is the magnesium hydroxide and aluminium hydroxide that weight ratio is 3:1;It is described anti- Oxygen agent is phenyl silicone oil, MethylethoxylsiliconFluid Fluid and the DBPC 2,6 ditertiary butyl p cresol that weight ratio is 3:2:1.
Embodiment 9:
Step 1: taking in 100 parts of addition two-roll mills of dimethyl silicone rubber, plasticate at room temperature 10 minutes, then plus Enter 30 parts of precipitated silica, 3 parts of high molecular weight hydroxy silicone oil, be kneaded 10 minutes, obtains just mixing sizing material, quiet storage 12 hours, later It will just mix sizing material back mixing 10 minutes at room temperature, 4 parts of triallyl cyanurate of addition, 4 parts of tackifier, 4 parts of antibacterial agent, fire retardant 2 parts, 2 parts of antioxidant continue to be kneaded 10 minutes, obtain mixing materials, and quiet storage 48 hours, later again at room temperature return sizing material again Mixing materials, are pressed and molded at room temperature as sheet material or bulk by refining 10 minutes on tablet press machine;The rotating cylinder of the two-roll mill turns Speed is set as 200r.min-1
Step 2: sheet material after molding or bulk at room temperature in air, are placed in after plastic packaging or aluminium foil package60Co Crosslinking with radiation is carried out in gamma radiation field, absorbed dose 50kGy makes sizing material complete crosslinking disposably to get to tack Silastic material;
The tackifier are using the tackifier in embodiment 7;The antibacterial agent, fire retardant and antioxidant use embodiment 8 Described in material.
In order to illustrate effect of the invention, it is as follows that inventor provides comparative experiments:
Comparative example 1:
Disclosed in patent document CN104788967A " a kind of silicon rubber microporous foamed material of mixed type foam structure and The silicon rubber microporous foamed material of the mixed type foam structure prepared in Examples 1 to 8 in preparation method ".
Comparative example 2:
In " a kind of high temperature resistant type silicon rubber foam material and preparation method thereof " disclosed in patent document CN104744946A The high temperature resistant type silicon rubber foam material prepared in Examples 1 to 5.
Comparative example 3:
Make the quiet storage time of the first time in step 1 less than 12 hours (be respectively set 8 hours, 5 hours, 1 hour, 30min, 10min), remaining parameter respectively with it is identical in Examples 1 to 9, technical process is also identical.
Tack test is carried out to Examples 1 to 9 and comparative example 1~3: take any surface finish, size about 200mm × 20mm × The stainless steel of 5mm, glass, polyethylene, polytetrafluoroethylene (PTFE) material model block, by diameter 25mm, the Examples 1 to 9 of thickness 4mm and right The test sample of ratio 1~3 is respectively placed on the test surfaces of each model block, and mark position, and each model block is then stood on reality It tests on platform, keeps test surfaces and test the angle of table top to be 90 degree, static 96h, the test sample in Examples 1 to 9 does not take off It falls, does not also slide significantly, and the test sample in comparative example 1~3 all falls off;It is real when reaching 240h between when resting It applies the test sample in example 1~5 and 8 and slight sliding occurs, and the test sample in embodiment 6,7 and 9 is not fallen off, is not had yet There is apparent sliding;When reaching 720h between when resting, there is apparent sliding in the test sample in Examples 1 to 5 and 8, and The test sample of embodiment 6,7 and 9 is not fallen off, is not slid significantly 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 the embodiments of the present invention have been disclosed as above, but its is not only in the description and the implementation listed With it can be fully applied to various fields suitable for the present invention, for those skilled in the art, can be easily Realize other modification, therefore without departing from the general concept defined in the claims and the equivalent scope, the present invention is simultaneously unlimited In specific details and example shown and described herein.

Claims (5)

1. a kind of silastic material with tack, wherein the formula composition of the silastic material is by weight are as follows: silicon rubber 100 parts of glue, 10~80 parts of reinforcing agent, 1~9 part of controlling agent, 0~5 part of sensitizer, 1~5 part of tackifier, 1~5 part of antibacterial agent, resistance Fire 1~3 part of agent, 1~3 part of antioxidant;
The silicon rubber is dimethyl silicone rubber, any one in methyl phenyl vinyl silicone rubber;
The reinforcing agent is precipitated silica, any one in fume colloidal silica;
The controlling agent is high molecular weight hydroxy silicone oil, any one in low molecule hydroxy silicon oil;
The sensitizer is triallyl cyanurate, triallyl isocyanurate, trimethylol propane trimethyl acrylic acid Any one in ester;
The antibacterial agent is chitin, zinc oxide, any one in copper oxide;
The fire retardant is the magnesium hydroxide and aluminium hydroxide that weight ratio is 3:1;
The antioxidant is phenyl silicone oil, MethylethoxylsiliconFluid Fluid and the DBPC 2,6 ditertiary butyl p cresol that weight ratio is 3:2:1;
The tackifier the preparation method comprises the following steps: by weight, take 100 parts of starch, it is 2:1 that 100 parts of water and 10 parts of weight ratios, which are added, Melamine and ammonium carbonate, stir evenly, adjust pH to 9 with the urea of 1.5mol/L, 50 parts of epoxychloropropane are added, in temperature It is stirred to react 4~5 hours, filters under conditions of 30~40 DEG C of degree, it is dry with ethanol washing, obtain crosslinked starch;Overcritical The crosslinked starch and 30~35 parts of carragheen, 20~25 parts of butyl acrylate, acryloyl that weight ratio is 1:1 are added in reaction unit 3~5 parts of amine, 0.02~0.08 part of ammonium persulfate, 200~250 parts of water, stir evenly, then seal system, be passed through titanium dioxide It is reacted under conditions of at carbon to 25~45MPa, 60~75 DEG C of temperature 5~8 hours, then uses ethanol precipitation, the vacuum at 70 DEG C It is dry, reacting coarse product is obtained, crude product acetone is eluted into the homopolymer up to removing dereaction generation with Soxhlet extractor, It is dried in vacuo 24 hours at 65 DEG C, obtains tackifier.
2. as described in claim 1 with the silastic material of tack, wherein the formula composition of the silastic material is pressed Poidometer are as follows: 100 parts of silicon rubber base-material, 30 parts of reinforcing agent, 3 parts of controlling agent, 4 parts of sensitizer, 4 parts of tackifier, 4 parts of antibacterial agent, 2 parts of fire retardant, 2 parts of antioxidant.
3. as described in claim 1 with the silastic material of tack, wherein the tack silastic material shore is hard Degree 22~67, tensile strength are 3.21~35.7MPa, elongation at break 200~912%, 12.6~41.3MPa of tearing strength.
4. as described in claim 1 with the silastic material of tack, wherein the molecular weight of the silicon rubber is 50~70 Ten thousand, the molar content of phenyl is 1.0~30.0% in methyl phenyl vinyl silicone rubber.
5. a kind of preparation method of the silastic material with tack as described in claim 1, wherein the method includes Following steps:
Step 1: by weight, taking silicon rubber to be added in two-roll mill, plasticating at room temperature 5~10 minutes, then it is added and mends Strong agent, controlling agent, are kneaded 5~10 minutes, obtain just mixed sizing material, and quiet storage 12~24 hours later at room temperature returns first mixed sizing material Refining 10~15 minutes is added sensitizer, tackifier, antibacterial agent, fire retardant and antioxidant, continues mixing 5~10 minutes, mixed Refining material, quiet storage 24~48 hours, are later again at room temperature pressing mixing materials at room temperature by sizing material back mixing 10~15 minutes again Compression molding is sheet material or bulk on piece machine;The rotating cylinder revolving speed of the two-roll mill is set as 200~600r.min-1
Step 2: sheet material after molding or bulk at room temperature in air, are placed in after plastic packaging or aluminium foil package60Co γ spoke It penetrates and carries out crosslinking with radiation in field, absorbed dose is 30~100kGy, and sizing material is made to complete crosslinking disposably to get to tack Silastic material, wherein60In Co gamma radiation field, the placement location of sheet material or bulk after sealing selects 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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