CN100422263C - Obturator-type silicone rubber foam material, and its preparing method and use - Google Patents
Obturator-type silicone rubber foam material, and its preparing method and use Download PDFInfo
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- CN100422263C CN100422263C CNB2006100210768A CN200610021076A CN100422263C CN 100422263 C CN100422263 C CN 100422263C CN B2006100210768 A CNB2006100210768 A CN B2006100210768A CN 200610021076 A CN200610021076 A CN 200610021076A CN 100422263 C CN100422263 C CN 100422263C
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Abstract
The present invention discloses a closed-pore silicone rubber foamed material and a preparation method thereof and an application thereof. The silicon rubber foamed material is characterized in that 100 parts by weight of silicon rubber, 15 to 80 parts by weight of reinforcing agent, 2 to 15 parts by weight of constitution control agent, 3 to 15 parts by weight of foaming agent, 0 to 3 parts by weight of auxiliary foaming agent and 0 to 4 parts by weight of auxiliary cross-linking agent are mixed and moulded to obtain silicon rubber; the silicon rubber generates cross-linking reaction after being radiated by a cathode beam or a gamma ray with a radiation dose of 5 to 20kGy, and then the foaming agent is decomposed for foaming the silicon rubber by heating; then the silicon rubber cathode beam and gamma ray are immediately adopted for secondary radiation to generate cross-linking reaction with a radiation dose of 20 to 50kGy after the silicon rubber is foamed to further increase the combination properties of the silicon rubber foamed material. The silicon rubber foamed material can be used as a material for sealing, shock absorption, insulation, acoustic insulation and heat insulation.
Description
Technical field
The present invention relates to a kind of obturator-type silicone rubber foam material and its production and use, belong to field of high polymer material processing.
Background technology
Silicon rubber foam material is a silicon rubber through the porousness macromolecular material of foaming back preparation, can be divided into closed pore, perforate and mix aperture silicon rubber foam according to the difference of foam structure.According to the type of preparation method and used silicon rubber, silicon rubber foam material can be divided into room temperature vulcanized silicone rubber foam and high-temperature silicon disulfide rubber foam, Lv Bailing, Liu Dengxiang, " practical rubber handbook, Beijing, Chemical Industry Press, 2001.It is base material that the room temperature vulcanized silicone rubber foam adopts the hydroxy-end capped silicon rubber of condensed type usually, and hydroxy silicon oil is a whipping agent, and platinum complex is a catalyzer, and sulfur foam obtains spongy elastomerics with holes under the room temperature.The room temperature vulcanized silicone rubber foam is applicable to the foam-in-site moulding, plays effects such as filling, sealing, damping; The traditional preparation process method of high temperature vulcanized foam silicone rubber is that silicon rubber, whipping agent and the vulcanizing agent uniform mixing that will contain microgranular inorganic filler make rubber unvulcanizate, by baking, foaming, make silicon rubber foam then.
The high temperature vulcanizable silicone foam, the characteristic of silicon rubber and foam materials is incorporated into one, the good characteristic that not only has silicon rubber, also have lower density, good absorption mechanical vibration or ballistic physical property, functions such as sound insulation, heat insulation, sealing, can be used as sealing, damping, insulation, sound insulation, heat insulation contour performance materials, have been widely used in fields such as communications and transportation, petrochemical complex, electronic industry, national defence and aerospace, Zhouning County's beautiful jade, " organosilicon polymer introduction ", Science Press, Beijing, 2000.Simultaneously, silicon rubber foam also has physiology inertia, nontoxic, odorless, nothing corrosion, and modulus is little, and softness and high resilience can be used as pharmaceutical factory, food factory is dry with liquid product or the sealing of large-scale drying plant and various filler rods etc.In automobile industry, automobile progressively improves with the requirement of weather strip to compression set, winter hardiness at present, and weather strip is tending towards lightweight, and feasible cry with the alternative existing terpolymer EP rubber foam materials of silicon rubber foam material increases day by day.Because silicon rubber foam anti-combustion in light weight, heat-resisting is the excellent material of fabric liner, can be used for the field that has heat and steam transmission and other foam materials can not satisfy performance requriements.
The preparation of high-temperature silicon disulfide rubber foam materials normally adopts superoxide to carry out sulfur foam, sulfidation and foaming process coupling are the keys of the foam materials of preparation foam structure and excellent property, but accomplish that this point is not easy very much, because whipping agent and peroxide vulcanizing agent are all very responsive to temperature, every rising 10 degree of temperature, the decomposition rate of vulcanization rate and whipping agent all is multiplied; In addition, peroxide vulcanizing agent is subject to the influence of whipping agent decompose residues, and the free radical passivation that acidic substance and the easy material that produces hydrogen make superoxide produce easily reduces cross-linking efficiency.In order to regulate the rate of crosslinking of superoxide, often need to add one or more vulcanization accelerators, the research with technology of filling a prescription repeatedly is to reach the coupling of rate of crosslinking and expansion rate.In addition, the homogeneity of peroxide crosslinking is subjected to the influence of its dispersion state in silicon rubber, particularly for rubber foam, thermal conduction is poor, and inside is heated and is slower than the top layer, often causes the top layer of sizing material and internal crosslinking degree varies to cause, foamy density is also inhomogeneous, and epidermis is thicker.
Summary of the invention
The objective of the invention is provides a kind of obturator-type silicone rubber foam material and preparation method thereof at the deficiencies in the prior art.Be characterized in silicon rubber is mixed with strengthening agent, whipping agent and other auxiliary agent and moulding, silicon rubber generation crosslinking reaction after electron beam or gamma-rays radiation, by heating whipping agent is reduced foaming then, it is crosslinked to adopt electron beam or gamma-rays to carry out secondary rays immediately after the silicon rubber foaming, with the over-all properties of further raising silicon rubber foam material.The silicon rubber foam material of present method preparation can be used as sealing, damping, insulation, sound insulation, lagging material.
Purpose of the present invention is realized that by following technical measures wherein said raw material umber is parts by weight except that specified otherwise.
Obturator-type silicone rubber foam material, the recipe ingredient of this foam materials is by weight: 100 parts in silicon rubber, 15~80 parts of white carbon blacks, 2~15 parts of constitution controllers, 3~15 parts of whipping agents, 0~3 part of blowing promotor, 0~4 part of additional crosslinker;
Silicon rubber is at least a in dimethyl silicone rubber, methyl vinyl silicone rubber, the methyl phenyl vinyl silicone rubber.
White carbon black is any one in precipitated silica, the thermal silica.
Constitution controller is any one in hydroxy silicon oil, Diphenylsilanediol, hexamethyldisilazane, octamethylcyclotetrasiloxane, the γ-An Bingjisanyiyangjiguiwan.
Whipping agent is any one in Cellmic C 121, Diisopropyl azodicarboxylate, dinitrosopentamethylene tetramine, the two benzol sulfohydrazide ethers.
Blowing promotor is any one in Zinic stearas, zinc oxide, the urea.
Additional crosslinker is any one in trimethylolpropane trimethacrylate (TMPTMA), cyanacrylate (TAIC), the triallylcyanurate (TAC) etc.
The preparation of obturator-type silicone rubber foam material:
1, the preparation of silicone rubber compounds
With the silicon rubber of 100 weight parts, the white carbon black of 15~80 weight parts, the constitution controller of 2~15 weight parts, the whipping agent of 3~15 weight parts, the blowing promotor of 0~3 weight part, the additional crosslinker of 0~4 weight part, adopt mill or Banbury mixer at room temperature mixing, mixing time is 8~15 minutes, then with the sizing material that mixes under the room temperature on vulcanizing press compression molding be shaped to sheet material.
2, the radiation crosslinking of silicone rubber compounds
Adopt
60Co gamma-radiation source or electron electrostatic accelerator at room temperature carry out radiation to silicon rubber in the air, and radiation dose is 5~20kGy, make silicon rubber generation crosslinking reaction.
3, the foaming of radiation crosslinking silicon rubber
Radiation crosslinking silicon rubber is adopted vulcanizing press, warm air or glycerol bath foamable, and blowing temperature is 140~210 ℃, and foamed time is 5~10 minutes.
4, the secondary rays after the silicon rubber foaming is crosslinked
After the silicon rubber foaming, adopt immediately
60It is crosslinked that Co gamma-radiation source or electron electrostatic accelerator carry out secondary rays, and radiation dose is 20~50kGy.
Experimental result shows, the present invention adopts the obturator-type silicone rubber foam material of radiation crosslinking method preparation to have excellent comprehensive performances, compare with U.S. Diversified silicone products company product of the same type, the silicon rubber foam material tensile strength and the elongation at break of the present invention's preparation are higher, compression set less (seeing Table 1).
The present invention has following advantage: adopt the method for radiation crosslinking to prepare silicon rubber foam material, make crosslinked and the foaming process proceed step by step, technology is simple, easy and simple to handle, when having avoided common employing peroxide vulcanizing agent, need sulfidation and foaming process to be complementary, problems such as the control more complicated of preparation process and product properties.The abscess of the prepared silicon rubber foam material of the present invention is tiny evenly, smooth surface, tensile strength and elongation at break height, and compression set is low.
Embodiment
Below by embodiment the present invention is carried out concrete description; be necessary to be pointed out that at this following examples can only be used for the present invention is further specified; can not be interpreted as limiting the scope of the invention, the person skilled in the art in this field can make some nonessential improvement and adjustment according to the content of the invention described above.
Embodiment:
1. with 100 gram dimethyl silicone rubbers, 15 gram thermal silicas, 2 gram hydroxy silicon oils, adopt at room temperature mixing 4 minutes of two roller mills, add 3 gram Cellmic C 121s, 3 gram zinc oxide, 4 gram cyanacrylates, continued mixing 4 minutes, then under the room temperature on vulcanizing press compression molding be shaped to sheet material.Adopt right cylinder formula Co
60Gamma ray projector at room temperature in the air, carries out radiation crosslinking to silicone rubber compounds, and radiation dose is 6kGy.Silicon rubber after crosslinked is foamed in warm air, and hot air temperature is 200 ℃, and foamed time is 5 minutes.After the silicon rubber foaming, adopt immediately
60It is crosslinked that secondary rays is carried out in Co gamma-radiation source, and radiation dose is 50kGy.
2. with 100 gram methyl vinyl silicone rubbers, 30 gram thermal silicas, 6 gram Diphenylsilanediols, adopted Banbury mixer at room temperature mixing 7 minutes, add 8 gram dinitrosopentamethylene tetramines, 2 gram urea, 2 gram trimethylolpropane trimethacrylates, continued mixing 5 minutes, then under the room temperature on vulcanizing press compression molding be shaped to sheet material.Adopt JJ-2 type electrostatic accelerator, at room temperature in the air, silicone rubber compounds is carried out radiation crosslinking, irradiation dose is 10kGy.Film after crosslinked is foamed in warm air, and hot air temperature is 190 ℃, and foamed time is 8 minutes.After the silicon rubber foaming, it is crosslinked to adopt JJ-2 type electrostatic accelerator to carry out secondary rays immediately, and radiation dose is 30kGy.
3. with 50 gram methyl vinyl silicone rubbers, 50 gram dimethyl silicone rubbers, 35 gram thermal silicas, 10 gram hydroxy silicon oils, adopted Banbury mixer at room temperature mixing 8 minutes, add 10 gram Diisopropyl azodicarboxylates, continued mixing 3 minutes, then under the room temperature on vulcanizing press compression molding be shaped to sheet material.Adopt right cylinder formula Co
60Gamma ray projector at room temperature in the air, carries out radiation crosslinking to silicone rubber compounds, and irradiation dose is 20kGy.Film after crosslinked is placed in the glycerol bath, and oil bath temperature is 140 ℃, and foamed time is 7 minutes.After the silicon rubber foaming, it is crosslinked to adopt JJ-2 type electrostatic accelerator to carry out secondary rays immediately, and radiation dose is 35kGy.
4. with 100 gram methyl phenyl vinyl silicone rubbers, 80 gram precipitated silicas, 12 gram γ-An Bingjisanyiyangjiguiwans, adopt at room temperature mixing 10 minutes of two roller mills, add 15 grams, two benzol sulfohydrazide ethers, 1 the gram triallylcyanurate, continued mixing 5 minutes, then under the room temperature on vulcanizing press compression molding be shaped to sheet material.Adopt JJ-2 type electrostatic accelerator, at room temperature in the air, silicone rubber compounds is carried out radiation crosslinking, irradiation dose is 10kGy.Place vulcanizing press to foam on the film after crosslinked, blowing temperature is 150 ℃, foamed time 10 minutes.After the silicon rubber foaming, it is crosslinked to adopt JJ-2 type electrostatic accelerator to carry out secondary rays immediately, and radiation dose is 25kGy.
The performance of table 1 obturator-type silicone rubber foam material of the present invention
Performance | Foam materials 1 | Foam materials 2 | Foam materials 3 | Foam materials 4 | DSP124 (Diversified silicone products,Inc) |
Density (g/cm 3) | 0.28 | 0.33 | 0.45 | 0.53 | 0.32-0.4 |
Abscess mean diameter (μ m) | 40 | 33 | 28 | 31 | - |
Tensile strength (MPa) | 1.06 | 1.01 | 1.4 | 1.57 | 0.35-0.53 |
Elongation at break (%) | 340 | 240 | 280 | 250 | >80 |
Compressive strength, 25% (kPa) | 50 | 61 | 70 | 128 | 56-84 |
Compression set, compression 50%@23 ℃ * 22h (%) | 6 | 2 | 4 | 6 | <10 |
Claims (9)
1. obturator-type silicone rubber foam material, the recipe ingredient that it is characterized in that this foam materials is by weight: 100 parts in silicon rubber, 15~80 parts of white carbon blacks, 2~15 parts of constitution controllers, 3~15 parts of whipping agents, 0~3 part of blowing promotor, 0~4 part of additional crosslinker, the foam density 0.28~0.53g/cm of this foam materials
3, tensile strength is that 1.01~1.57Mpa, elongation are 240~340%, compressive strength 50~128kPa, compression set is less than 6%.
2. according to the described obturator-type silicone rubber foam material of claim 1, the silicon rubber that it is characterized in that this foam materials is at least a in dimethyl silicone rubber, methyl vinyl silicone rubber, the methyl phenyl vinyl silicone rubber.
3. according to the described obturator-type silicone rubber foam material of claim 1, it is characterized in that white carbon black is precipitated silica or thermal silica.
4. according to the described obturator-type silicone rubber foam material of claim 1, it is characterized in that constitution controller is any one in hydroxy silicon oil, Diphenylsilanediol, hexamethyldisilazane, octamethylcyclotetrasiloxane or the γ-An Bingjisanyiyangjiguiwan.
5. according to the described obturator-type silicone rubber foam material of claim 1, it is characterized in that whipping agent is any one in Cellmic C 121, Diisopropyl azodicarboxylate, dinitrosopentamethylene tetramine or the two benzol sulfohydrazide ethers.
6. according to the described obturator-type silicone rubber foam material of claim 1, it is characterized in that the used blowing promotor of foam materials is any one in Zinic stearas, zinc oxide or the urea.
7. according to the described obturator-type silicone rubber foam material of claim 1, it is characterized in that additional crosslinker is any one in trimethylolpropane trimethacrylate, cyanacrylate or the triallylcyanurate.
8. according to the preparation method of the described obturator-type silicone rubber foam material of one of claim 1~7, it is characterized in that:
A. the preparation of silicone rubber compounds
With the silicon rubber of 100 weight parts, the white carbon black of 15~80 weight parts, the constitution controller of 2~15 weight parts, the whipping agent of 3~15 weight parts, the blowing promotor of 0~3 weight part, the additional crosslinker of 0~4 weight part, adopt mill or Banbury mixer at room temperature mixing evenly, mixing time is 8~15 minutes, is sheet material with the sizing material that mixes is molded under room temperature then;
B. the radiation crosslinking of silicone rubber compounds
Adopt
60Co gamma-radiation source or electron electrostatic accelerator at room temperature carry out radiation to silicon rubber in the air, and radiation dose is 5~20kGy, make silicon rubber generation crosslinking reaction;
C. the foaming of radiation crosslinking silicon rubber
Radiation crosslinking silicon rubber is adopted vulcanizing press, warm air or glycerol bath foamable, and blowing temperature is 140~210 ℃, and foamed time is 5~10 minutes;
D. the secondary rays after the silicon rubber foaming is crosslinked
After the silicon rubber foaming, adopt immediately
60It is crosslinked that Co gamma-radiation source or electron electrostatic accelerator carry out secondary rays, and radiation dose is 20~50kGy.
9. according to the purposes of the described obturator-type silicone rubber foam material of claim 1, it is characterized in that this foam materials is as sealing, damping, insulation, sound insulation, lagging material.
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