WO2015146743A1 - 遮音材 - Google Patents
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- WO2015146743A1 WO2015146743A1 PCT/JP2015/058049 JP2015058049W WO2015146743A1 WO 2015146743 A1 WO2015146743 A1 WO 2015146743A1 JP 2015058049 W JP2015058049 W JP 2015058049W WO 2015146743 A1 WO2015146743 A1 WO 2015146743A1
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- sound insulating
- insulating material
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- resin
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- G—PHYSICS
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- G10K—SOUND-PRODUCING DEVICES; METHODS OR DEVICES FOR PROTECTING AGAINST, OR FOR DAMPING, NOISE OR OTHER ACOUSTIC WAVES IN GENERAL; ACOUSTICS NOT OTHERWISE PROVIDED FOR
- G10K11/00—Methods or devices for transmitting, conducting or directing sound in general; Methods or devices for protecting against, or for damping, noise or other acoustic waves in general
- G10K11/16—Methods or devices for protecting against, or for damping, noise or other acoustic waves in general
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- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
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- C08L53/02—Compositions of block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers of vinyl-aromatic monomers and conjugated dienes
- C08L53/025—Compositions of block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers of vinyl-aromatic monomers and conjugated dienes modified
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- G—PHYSICS
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- G10K—SOUND-PRODUCING DEVICES; METHODS OR DEVICES FOR PROTECTING AGAINST, OR FOR DAMPING, NOISE OR OTHER ACOUSTIC WAVES IN GENERAL; ACOUSTICS NOT OTHERWISE PROVIDED FOR
- G10K11/00—Methods or devices for transmitting, conducting or directing sound in general; Methods or devices for protecting against, or for damping, noise or other acoustic waves in general
- G10K11/16—Methods or devices for protecting against, or for damping, noise or other acoustic waves in general
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Definitions
- the present invention relates to a sound insulating material, and more particularly, to a light insulating material that is lightweight and has excellent sound insulating properties.
- the frequency of wind noise is said to be approximately 2 to 10 kHz.
- a technology that can further insulate tire pattern noise and motor-derived noise.
- it is necessary to develop a sound insulating material capable of insulating sound in a high frequency range of 1 to 6 kHz, which is sensitively detected by human ears, with a good balance.
- Patent Documents 4 and 5 disclose shock absorbers characterized by combining two or more kinds of polymer materials having different tan ⁇ temperature ranges measured by dynamic viscoelasticity. Not doing.
- Patent Document 1 discloses a technique for improving sound insulation by mixing inorganic substances such as high specific gravity metals and metal oxides as a technique for improving sound insulation characteristics.
- the sound insulating material according to this technology has excellent sound insulating performance, since it uses an inorganic substance having a specific gravity of 4.0 or more, it is inevitably heavy and does not satisfy the demand for weight reduction.
- Patent Documents 2 and 3 also disclose techniques for improving sound insulation using a filler having a large specific gravity.
- the object of the present invention is to provide a sound insulation material that is both lightweight and improved in sound insulation characteristics without depending on a complicated structure.
- the present inventors use a combination of materials having a loss tangent tan ⁇ peak obtained by dynamic viscoelasticity measurement in a specific temperature range.
- a sound insulating material that is lightweight and has excellent sound insulating properties can be obtained.
- the present invention relates to a soft material (A) in which a peak of loss tangent tan ⁇ determined by dynamic viscoelasticity measurement is in a temperature range of ⁇ 60 ° C. or higher and lower than 0 ° C., and loss determined by dynamic viscoelasticity measurement.
- the soft material (A) includes at least one selected from ethylene rubber, natural rubber, and diene rubber.
- the soft material (A) preferably contains an ethylene / ⁇ -olefin / non-conjugated polyene copolymer (a).
- the content of structural units derived from ethylene is 40 to 72 mass%, and the content of structural units derived from nonconjugated polyene is 2%. It is preferably ⁇ 15% by mass.
- the resin (B) is an aromatic polymer, 4-methyl-1-pentene / ⁇ -olefin copolymer (b), polyvinyl acetate, polyester, polyurethane, poly (meth) acrylate, epoxy resin. And at least one selected from polyamides.
- the resin (B) is a structural unit (i) derived from 4-methyl-1-pentene of 16 to 95 mol%, and ⁇ - of 2 to 20 carbon atoms excluding 4-methyl-1-pentene.
- Structural unit (ii) derived from at least one ⁇ -olefin selected from olefins (ii) 5 to 84 mol% and structural unit (iii) derived from non-conjugated polyene 0 to 10 mol% (provided that structural unit (i) , (Ii) and (iii) is 100 mol%).
- 4-methyl-1-pentene / ⁇ -olefin copolymer (b-1) is preferably included.
- a sound insulating material obtained by crosslinking a composition containing a soft material (A) and a resin (B) with a vulcanizing agent can be preferably exemplified.
- At least a part of the sound insulating material is a foam.
- the sound insulating material of the present invention is a material that realizes excellent sound insulating properties without depending on a complicated shape and without increasing the weight.
- the sound insulating material of the present invention includes building materials (floor lining, walls, ceiling materials, etc.), personal computers, OA equipment, AV equipment, mobile phones and other electrical and electronic equipment, optical equipment, precision equipment, toys, household and office electrical products, etc. It is effective for the parts and housings of the present invention, and is particularly useful as parts and molding materials in the transportation and mobile industries such as railway vehicles, automobiles, ships and aircraft.
- FIG. 1A is a graph showing the relationship between the test piece weight and the average transmission loss at a frequency of 1 to 4 kHz in the sound insulating materials of Example 1 and Comparative Examples 1 to 6.
- FIG. 1B is a diagram showing the relationship between the test piece weight and the average transmission loss at a frequency of 4 to 6 kHz in the sound insulating materials of Example 1 and Comparative Examples 1 to 6.
- FIG. 2A is a graph showing the relationship between the test piece weight and the average transmission loss at frequencies of 1 to 4 kHz in the sound insulating materials of Examples 11 to 16 and Comparative Examples 16 to 20.
- FIG. 2B is a graph showing the relationship between the test piece weight and the average transmission loss at a frequency of 4 to 6 kHz in the sound insulating materials of Examples 11 to 16 and Comparative Examples 16 to 20.
- the present invention relates to a soft material (A) in which a peak of loss tangent tan ⁇ determined by dynamic viscoelasticity measurement is in a temperature range of ⁇ 60 ° C. or higher and lower than 0 ° C., and loss tangent determined by dynamic viscoelasticity measurement.
- a sound insulating material comprising a resin (B) having a tan ⁇ peak in a temperature range of 0 ° C. or more and 60 ° C. or less in a ratio of 1 to 50 parts by mass of the resin (B) with respect to 100 parts by mass of the soft material (A). is there.
- the loss tangent tan ⁇ obtained by dynamic viscoelasticity measurement will be described.
- the dynamic viscoelasticity measurement is performed on the material while continuously changing the ambient temperature, and the storage elastic modulus G ′ (Pa) and the loss elastic modulus G ′′ (Pa) are measured and given by G ′′ / G ′.
- the loss tangent tan ⁇ is obtained.
- the loss tangent tan ⁇ generally has a peak at a specific temperature.
- the temperature at which the peak appears is generally called the glass transition temperature (hereinafter also referred to as tan ⁇ -Tg).
- the temperature at which the peak of loss tangent tan ⁇ appears can be determined based on the dynamic viscoelasticity measurement described in the examples.
- the soft material (A) included in the sound insulating material of the present invention has a loss tangent tan ⁇ peak in a temperature range of ⁇ 60 ° C. or higher and lower than 0 ° C.
- the resin (B) contained in the sound insulating material of the present invention has a loss tangent tan ⁇ peak in the temperature range of 0 ° C. or higher and 60 ° C. or lower.
- the sound insulating material of the present invention contains the soft material (A) and the resin (B) at a ratio of 1 to 50 parts by mass of the resin (B) per 100 parts by mass of the soft material (A).
- the sound insulating material of the present invention that satisfies these conditions has excellent sound insulating properties.
- the sound insulating material of the present invention does not need to contain a filler having a large specific gravity, the weight can be reduced. Further, the sound insulating material of the present invention does not need to be combined with a plurality of members or to have a characteristic structure, and therefore does not need to be processed into a complicated structure.
- the sound insulation material according to the present invention can achieve excellent sound insulation characteristics by satisfying the above-mentioned conditions because a plurality of peaks having loss tangent tan ⁇ in different temperature ranges of ⁇ 60 ° C. to less than 0 ° C. and 0 ° C. to 60 ° C. It is considered that by including the material at a predetermined ratio, it is possible to effectively block the sound of the entire high frequency range of 1 to 6 kHz that is sensitively detected by the human ear.
- the soft material (A) has a loss tangent tan ⁇ peak preferably in the temperature range of ⁇ 55 to ⁇ 5 ° C., more preferably ⁇ 50 to ⁇ 10 ° C.
- the resin (B ) Has a loss tangent tan ⁇ peak in the temperature range of preferably 5 to 55 ° C., more preferably 10 to 50 ° C.
- the sound insulation material of the present invention is preferably a proportion of 5 to 45 parts by mass, more preferably 10 to 40 parts by mass of the resin (B) per 100 parts by mass of the soft material (A). Including.
- the soft material (A) is a material having a loss tangent tan ⁇ peak in a temperature range of ⁇ 60 ° C. or more and less than 0 ° C., excellent sound insulation characteristics can be obtained as described above.
- the soft material (A) include materials containing ethylene rubber, natural rubber, diene rubber, and the like. The soft material (A) can be used by mixing them.
- diene rubber examples include isoprene rubber (IR), butadiene rubber (BR), styrene butadiene rubber (SBR), chloroprene rubber (CR), acrylonitrile diene rubber (NBR), and butyl rubber (IIR).
- IR isoprene rubber
- BR butadiene rubber
- SBR styrene butadiene rubber
- CR chloroprene rubber
- NBR acrylonitrile diene rubber
- IIR butyl rubber
- ethylene rubber examples include an ethylene / ⁇ -olefin copolymer (EPM) and an ethylene / ⁇ -olefin / non-conjugated polyene copolymer (EPDM).
- EPM ethylene / ⁇ -olefin copolymer
- EPDM ethylene / ⁇ -olefin / non-conjugated polyene copolymer
- Examples of the ethylene / ⁇ -olefin copolymer include a copolymer of ethylene and an ⁇ -olefin having 3 to 20 carbon atoms.
- Examples of the ⁇ -olefin include propylene, butene-1,4-methylpentene-1, hexene-1, heptene-1, octene-1, nonene-1, decene-1, undecene-1, dodecene-1, and tridecene.
- ⁇ -olefins can be used alone or in combination of two or more.
- the ⁇ -olefin in the ethylene / ⁇ -olefin / non-conjugated polyene copolymer is the same as the ⁇ -olefin in the ethylene / ⁇ -olefin copolymer.
- non-conjugated polyene in the ethylene / ⁇ -olefin / non-conjugated polyene copolymer examples include non-conjugated polyene having 5 to 20 carbon atoms, preferably 5 to 10 carbon atoms.
- the soft material (A) preferably contains an ethylene / ⁇ -olefin / non-conjugated polyene copolymer (a), particularly in terms of heat aging resistance, weather resistance, and ozone resistance.
- the content of the ethylene / ⁇ -olefin / non-conjugated polyene copolymer (a) in the soft material (A) is preferably 50 to 100% by mass, more preferably 70 to 100% by mass.
- the content of the structural unit derived from ethylene is preferably 40 to 72% by mass, more preferably 42 to 66% by mass, More preferably, it is 44 to 62% by mass, and the content of the structural unit derived from the non-conjugated polyene is preferably 2 to 15% by mass, more preferably 5 to 14% by mass, and further preferably 7 to 12% by mass. .
- ⁇ -olefins having 3 to 10 carbon atoms are preferable, and in particular, propylene, 1-butene, 1-hexene, 1- Octene and the like are particularly preferable.
- non-conjugated polyenes among the above-mentioned non-conjugated polyenes are dicyclopentadiene, 5-vinylidene-2-norbornene, 5-ethylidene-2- Examples include norbornene.
- the crystallized polyolefin content in the soft material (A) is preferably less than 10% by mass.
- the resin (B) is a material having a loss tangent tan ⁇ peak in the temperature range of 0 ° C. or more and 60 ° C. or less, the excellent sound insulation characteristics can be obtained as described above, and the type thereof is not particularly limited.
- the resin (B) include an aromatic polymer, 4-methyl-1-pentene / ⁇ -olefin copolymer (b), polyvinyl acetate, polyester, polyurethane, poly (meth) acrylate, epoxy resin, and polyamide. Etc. As resin (B), these can also be mixed and used.
- the resin (B) preferably contains 4-methyl-1-pentene / ⁇ -olefin copolymer (b) in terms of weather resistance and ozone resistance.
- aromatic polymer examples include polymers of aromatic vinyl monomers such as styrene and alkylstyrene, and copolymers of aromatic vinyl monomers and olefin monomers.
- the ⁇ -olefin in the 4-methyl-1-pentene / ⁇ -olefin copolymer (b) is, for example, an ⁇ -olefin having 2 to 20 carbon atoms, except for 4-methyl-1-pentene. And branched ⁇ -olefins, cyclic olefins, aromatic vinyl compounds, conjugated dienes, and functionalized vinyl compounds.
- the 4-methyl-1-pentene / ⁇ -olefin copolymer does not contain non-conjugated polyene in the ⁇ -olefin.
- linear ⁇ -olefin examples include linear ⁇ -olefins having 2 to 20, preferably 2 to 15, and more preferably 2 to 10 carbon atoms.
- Specific examples include ethylene, propylene, 1 -Butene, 1-pentene, 1-hexene, 1-octene, 1-decene, 1-undecene, 1-dodecene, 1-tetradecene, 1-hexadecene, 1-octadecene, 1-eicocene and the like. Of these, ethylene, propylene, 1-butene, 1-pentene, 1-hexene and 1-octene are preferred.
- the branched ⁇ -olefin is preferably a branched ⁇ -olefin having 5 to 20 carbon atoms, more preferably 5 to 15 carbon atoms, specifically, 3-methyl-1-butene, 3- Methyl-1-pentene, 3-ethyl-1-pentene, 4,4-dimethyl-1-pentene, 4-methyl-1-hexene, 4,4-dimethyl-1-hexene, 4-ethyl-1-hexene, Examples include 3-ethyl-1-hexene.
- cyclic olefin examples include cyclic olefins having 3 to 20 carbon atoms, preferably 5 to 15 carbon atoms. Specifically, cyclopentene, cyclohexene, cycloheptene, norbornene, 5-methyl-2-norbornene, tetracyclodone. Examples include decene and vinylcyclohexane.
- Aromatic vinyl compounds include styrene, ⁇ -methylstyrene, o-methylstyrene, m-methylstyrene, p-methylstyrene, o, p-dimethylstyrene, o-ethylstyrene, m-ethylstyrene, p-ethylstyrene. And mono- or polyalkyl styrene.
- conjugated diene examples include conjugated dienes having 4 to 20 carbon atoms, preferably 4 to 10 carbon atoms. Specific examples include 1,3-butadiene, isoprene, chloroprene, 1,3-pentadiene, 2,3-dimethyl. Examples thereof include butadiene, 4-methyl-1,3-pentadiene, 1,3-hexadiene, and 1,3-octadiene.
- Examples of functionalized vinyl compounds include hydroxyl group-containing olefins, halogenated olefins, (meth) acrylic acid, propionic acid, 3-butenoic acid, 4-pentenoic acid, 5-hexenoic acid, 6-heptenoic acid, 7-octenoic acid, Unsaturated carboxylic acids such as 8-nonenoic acid, 9-decenoic acid and 10-undecenoic acid, unsaturated amines such as allylamine, 5-hexenamine and 6-heptenamine, (2,7-octadienyl) succinic anhydride, penta Propenyl succinic anhydride, unsaturated carboxylic acid anhydride such as anhydride obtained from the above unsaturated carboxylic acid, unsaturated carboxylic acid halide such as halide obtained from the above unsaturated carboxylic acid, 4-epoxy-1 -Butene, 5-epoxy-1-pentene, 6-epoxy
- the hydroxyl group-containing olefin is not particularly limited as long as it is a hydroxyl group-containing olefin compound, and examples thereof include terminal hydroxylated olefin compounds.
- the terminal hydroxylated olefin compounds include vinyl alcohol, allyl alcohol, hydroxyl-1-butene, hydroxyl-1-pentene, hydroxyl-1-hexene, hydroxyl-1-octene, hydroxyl-1-decene, 2 to 20 carbon atoms such as hydroxyl-1-undecene, hydroxyl-1-dodecene, hydroxyl-1-tetradecene, hydroxyl-1-hexadecene, hydroxyl-1-octadecene, hydroxyl-1-eicocene, Preferably 2 to 15 linear hydroxylated ⁇ -olefins; hydroxylated 3-methyl-1-butene, hydroxylated 3-methyl-1-pentene, hydroxylated 4-
- halogenated olefin examples include halogenated- ⁇ -olefins having a group 17 atom of the periodic table such as chlorine, bromine, iodine, and the like.
- the ⁇ -olefin in the 4-methyl-1-pentene / ⁇ -olefin copolymer (b) may be a single type or a combination of two or more types.
- Examples of the ⁇ -olefin in the 4-methyl-1-pentene / ⁇ -olefin copolymer (b) include ethylene, propylene, 1-butene, 1-pentene, 1-hexene, 3-methyl-1-butene, 3-methyl-1-pentene, 1-octene, 1-decene, 1-undecene, 1-dodecene, 1-tetradecene, 1-hexadecene, 1-octadecene, 1-eicocene, norbornene, 5-methyl-2-norbornene, Tetracyclododecene and hydroxyl-1-undecene are preferred.
- a linear ⁇ -olefin having 2 to 10 carbon atoms is preferable from the viewpoint of flexibility, stress absorption, stress relaxation, etc.
- ethylene, propylene, 1-butene, 1-pentene, 1-hexene is preferable.
- 1-octene is more preferred.
- ethylene and propylene are preferable, and propylene is particularly preferable in that high stress absorption and polyolefin modification properties can be obtained.
- the 4-methyl-1-pentene / ⁇ -olefin copolymer (b) may have a structural unit derived from a non-conjugated polyene, if necessary.
- the non-conjugated polyene is the same as the non-conjugated polyene in the aforementioned ethylene / ⁇ -olefin / non-conjugated polyene copolymer (a).
- the 4-methyl-1-pentene / ⁇ -olefin copolymer (b) may contain other copolymerization components as long as the object of the present invention is not impaired.
- the 4-methyl-1-pentene / ⁇ -olefin copolymer (b) includes a structural unit (i) derived from 4-methyl-1-pentene and a carbon number of 2 to 4 excluding 4-methyl-1-pentene.
- the content ratio of the structural unit (ii) derived from at least one ⁇ -olefin selected from 20 ⁇ -olefins and the structural unit (iii) optionally derived from a non-conjugated polyene is 4-methyl- A 1-pentene / ⁇ -olefin copolymer (b-1) is preferred.
- the content ratio of the structural unit (i), the structural unit (ii), and the structural unit (iii) in the 4-methyl-1-pentene / ⁇ -olefin copolymer (b-1) is the structural unit (i).
- (Ii) and (iii) are 100 mol%
- the structural unit (i) is 16 to 95 mol%
- the structural unit (ii) is 5 to 84 mol%
- the structural unit (iii) is 0 to 10 mol%.
- the structural unit (i) is 26 to 90 mol%
- the structural unit (ii) is 10 to 74 mol%
- the structural unit (iii) is 0 to 7 mol%
- the structural unit (i) is 61 to 85 mol%.
- Structural unit (ii) 15 to 39 mol% and structural unit (iii) 0 to 5 mol%.
- the sound insulating material of the present invention includes a softening material, a reinforcing material, a filler, a processing aid, an activator, a hygroscopic agent and the like within a range that does not impair the object of the present invention. It may contain.
- the softening material can be appropriately selected depending on the application, and can be used alone or in combination of two or more.
- Specific examples of softeners include process oils such as paraffin oil (for example, “Diana Process Oil PS-430” (trade name: manufactured by Idemitsu Kosan Co., Ltd.), lubricating oil, liquid paraffin, petroleum asphalt, petrolatum, etc.
- Oil-based softeners such as coal tar and coal tar pitch; fatty oil-based softeners such as castor oil, linseed oil, rapeseed oil, soybean oil, and palm oil; beeswax, carnauba wax, and Waxes such as lanolin; fatty acids such as ricinoleic acid, palmitic acid, stearic acid, barium stearate, calcium stearate, and zinc laurate or salts thereof; naphthenic acid, pine oil, and rosin or derivatives thereof; terpene resins, petroleum resins , Atactic polypropylene, and coumarone indene resin Synthetic polymer materials: ester softeners such as dioctyl phthalate, dioctyl adipate, and dioctyl sebacate; other microcrystalline wax, liquid polybutadiene, modified liquid polybutadiene, liquid thiocol, hydrocarbon synthetic lubricant, tall oil, and Sub (
- the blending amount of the softening material is usually 5 to 150 parts by mass, preferably 10 to 120 parts by mass, and more preferably 20 to 100 parts by mass with respect to 100 parts by mass of the soft material (A).
- “Asahi # 55G” and “Asahi # 50HG” (trade name: manufactured by Asahi Carbon Co., Ltd.), “Seast (trade name)” series: SRF, GPF, FEF are commercially available.
- MAF, HAF, ISAF, SAF, FT, MT, etc. carbon black (manufactured by Tokai Carbon Co., Ltd.), carbon black surface-treated with a silane coupling agent, etc., silica, activated calcium carbonate, fine talc, fine powder Silicic acid or the like can be used.
- carbon black of “Asahi # 55G”, “Asahi # 50HG”, “Seast HAF” is preferable.
- light calcium carbonate As the filler, light calcium carbonate, heavy calcium carbonate, talc, clay or the like can be used. Of these, heavy calcium carbonate is preferred.
- heavy calcium carbonate commercially available “Whiteon SB” (trade name: Shiraishi Calcium Co., Ltd.) or the like can be used.
- the compounding amounts of the reinforcing material and the filler are usually 30 to 300 parts by mass, preferably 50 to 250 parts by mass, and more preferably 70 to 230 parts by mass with respect to 100 parts by mass of the soft material (A).
- processing aids those generally blended into rubber as processing aids can be widely used. Specific examples include ricinoleic acid, stearic acid, palmitic acid, lauric acid, barium stearate, zinc stearate, calcium stearate and esters. Of these, stearic acid is preferred.
- the processing aid is appropriately blended in an amount of usually 10 parts by mass or less, preferably 8.0 parts by mass or less, more preferably 5.0 parts by mass or less with respect to 100 parts by mass of the soft material (A).
- the activator can be appropriately selected depending on the application, and can be used alone or in combination of two or more.
- Specific examples of the activator include di-n-butylamine, dicyclohexylamine, monoelaanolamine, “Acting B” (trade name: manufactured by Yoshitake Pharmaceutical Co., Ltd.), “Acching SL” (trade name: Yoshitsugu Pharmaceutical Co., Ltd.)
- Amines such as diethylene glycol, polyethylene glycol (for example, “PEG # 4000” (manufactured by Lion Corporation)), lecithin, triarylate melitlate, zinc compounds of aliphatic and aromatic carboxylic acids (for example, “Struktolvactivator”) 73 ”,“ Struktol IB 531 ”and“ Struktol FA541 ”(trade name: Schill &Seiler)); Zinc peroxide preparations such as“ ZEONET ZP ”(trade name: manufactured by Nippon Zeon Co., Ltd.)
- the compounding amount of the activator is usually 0.2 to 10 parts by weight, preferably 0.3 to 5 parts by weight, more preferably 0.5 to 4 parts by weight with respect to 100 parts by weight of the soft material (A). .
- the hygroscopic agent can be appropriately selected depending on the application and can be used alone or in combination of two or more.
- Specific examples of the hygroscopic agent include calcium oxide, silica gel, sodium sulfate, molecular sieve, zeolite, white carbon and the like. Of these, calcium oxide is preferred.
- the blending amount of the hygroscopic agent is usually 0.5 to 15 parts by mass, preferably 1.0 to 12 parts by mass, and more preferably 1.0 to 10 parts by mass with respect to 100 parts by mass of the soft material (A). .
- the sound insulating material of the present invention can be obtained by kneading the above components.
- the sound insulating material of the present invention is not particularly limited in shape.
- the sound insulating material of the present invention is formed into a sheet shape by a sheet forming method such as a calendar roll method or a T-die extrusion method.
- the sound insulating material of the present invention can be used as a sound insulating sheet by forming a sheet shape.
- the sound insulation material of a desired shape can be obtained by compression-molding the obtained sheet
- the sound insulating material of the present invention contains crosslinkable components such as ethylene / ⁇ -olefin / non-conjugated polyene copolymer, these components may be cross-linked.
- a vulcanizing agent is added to the crosslinkable component and kneaded. That is, the sound insulating material of the present invention can be obtained by crosslinking a composition containing the soft material (A) and the resin (B) using a vulcanizing agent.
- a sulfur compound As the vulcanizing agent (crosslinking agent), a sulfur compound, an organic peroxide, a phenol resin, an oxime compound, or the like can be used.
- sulfur compounds include sulfur, sulfur chloride, sulfur dichloride, morpholine disulfide, alkylphenol disulfide, tetramethylthiuram disulfide, selenium dithiocarbamate, and the like.
- sulfur compound sulfur and tetramethylthiuram disulfide are preferable.
- the sulfur compound is generally 0.3 to 10 parts by weight, preferably 0.5 to 5.0 parts by weight, more preferably 0.7 to 4.0 parts by weight, based on 100 parts by weight of the soft material (A). Blend.
- organic peroxide examples include dicumyl peroxide, 2,5-dimethyl-2,5-di (t-butylperoxy) hexane, 2,5-dimethyl-2,5-di (benzoylperoxy) hexane, 2, Examples include 5-diethyl-2,5-di (t-butylperoxy) hexyne-3, di-t-butylperoxide, di-t-butylperoxy-3,3,5-trimethylcyclohexane, t-dibutylhydroperoxide, etc. it can.
- dicumyl peroxide, di-t-butyl peroxide, and di-t-butylperoxy-3,3,5-trimethylcyclohexane are preferable.
- the amount of the organic peroxide is usually 0.001 to 0.05 mol, preferably 0.002 to 0.02 mol, more preferably 0.005 to 0.015, per 100 g of the soft material (A). Is a mole.
- Vulcanization accelerators include N-cyclohexyl-2-benzothiazole sulfenamide, N-oxydiethylene-2-benzothiazole sulfenamide, N, N′-diisopropyl-2-benzothiazole sulfenamide, 2-mercapto Benzothiazole (for example, “Sunceller M” (trade name: manufactured by Sanshin Chemical Co., Ltd.)), 2- (4-morpholinodithio) benzothiazole (for example, “Noxeller MDB-P” (trade name: Sanshin) Such as 2- (2,4-dinitrophenyl) mercaptobenzothiazole, 2- (2,6-diethyl-4-morpholinothio) benzothiazole, dibenzothiazyl disulfide; Gua such as diphenyl guanidine, triphen
- Thiuram series zinc dimethyldithiocarbamate, zinc diethyldithiocarbamate, zinc dibutyldithiocarbamate (for example, “Suncellar PZ” (trade name: manufactured by Sanshin Chemical Co., Ltd.), “Suncellor BZ” (trade name: Sanshin Chemical Industries) Etc.), dithioates such as tellurium diethyldithiocarbamate; ethylenethiourea (for example, “Suncellor BUR” (trade name: manufactured by Sanshin Chemical Industry Co., Ltd.), “Suncellor 22-C” (trade name: Thiourea such as N, N'-diethylthiourea; xanthate such as zinc dibutylxatogenate; other zinc white (for example, "META-Z102" (trade name: Inoue Lime Industry) Zinc oxide), etc.
- “Suncellar PZ” trade name: manufactured by Sanshin Chemical Co., Ltd.
- the blending amount of these vulcanization accelerators is usually 0.1 to 20 parts by weight, preferably 0.2 to 15 parts by weight, more preferably 0.5 to 10 parts per 100 parts by weight of the soft material (A). Part by mass.
- a vulcanization aid When vulcanizing, a vulcanization aid can be further used.
- the vulcanization aid can be appropriately selected depending on the application, and can be used alone or in combination of two or more.
- Specific examples of the vulcanization aid include magnesium oxide and zinc white (for example, zinc oxide such as “META-Z102” (trade name: manufactured by Inoue Lime Industry Co., Ltd.)).
- the blending amount is usually 1 to 20 parts by mass with respect to 100 parts by mass of the soft material (A).
- vulcanization aid examples include quinone dioximes such as p-quinonedioxime; acrylics such as ethylene glycol dimethacrylate and trimethylolpropane trimethacrylate; allyls such as diallyl phthalate and triallyl isocyanurate; other maleimides; Examples include divinylbenzene.
- the sound insulating material of the present invention may be entirely or partially foamed.
- the foam may be a vulcanized foam.
- the sound insulating material of the present invention can be effectively used as, for example, a sponge-like seal product of an automobile, particularly a weather strip, by forming at least a part of the foam.
- a foaming agent is added to the above components to cause foaming.
- the foaming agent include inorganic foaming agents such as sodium bicarbonate and sodium carbonate; nitroso compounds such as N, N′-dinitrosopentamethylenetetramine and N, N′-dinitrosotephthalamide; azodicarbonamide and azobisiso Organic foaming agents such as azo compounds such as butyronitrile; hydrazide compounds such as benzenesulfonyl hydrazide and 4,4′-oxybis (benzenesulfonyl hydrazide); azide compounds such as calcium azide and 4,4′-diphenyldisulfonyl azide Can be mentioned.
- the blending amount of the foaming agent is usually 3 to 30 parts by mass, preferably 4 to 20 parts by mass with respect to 100 parts by mass of the soft material (A).
- the foaming agent for example, vinylol AC # 3M (trade name: Eiwa azodicarbonamide (abbreviated as ADCA)), vinylhole AC # 3C-K2 (brand name: Eiwa Azodicarbon Co., Ltd.) commercially available are used.
- Amide (abbreviation ADCA)), Cellmic C-2 (trade name: Sankyo Kasei Co., Ltd. Azodicarbonamide (abbreviation ADCA)), Neoselbon N # 1000M (trade name: Eiwa Kasei Kogyo Co., Ltd. 4,4'-oxybis Sulfonyl hydrazide) (abbreviation OBSH)) and the like can be used.
- a foaming aid may be used together with the foaming agent.
- the foaming aid include organic acids such as salicylic acid, phthalic acid, stearic acid, oxalic acid and citric acid and salts thereof, urea and derivatives thereof, and the like.
- the blending amount of the foaming aid is usually 0.1 to 5 parts by mass, preferably 0.3 to 4 parts by mass with respect to 100 parts by mass of the soft material (A).
- the foaming aid for example, commercially available cell paste K5 (trade name: Eiwa Kasei Kogyo Co., Ltd., Urea), FE-507 (trade name: Eiwa Kasei Kogyo Co., Ltd.) can be used.
- the sound insulating material of the present invention is a vulcanized foam
- a composition containing the above components, a vulcanizing agent and a foaming agent is vulcanized and foamed.
- vulcanization foaming there is a method of extruding the composition using an extruder mounted on a tubular die and forming it into a tubular shape.
- the obtained molded body is introduced into a vulcanizing tank simultaneously with molding, and heated, for example, at 230 ° C. for 5 minutes to perform crosslinking and foaming to obtain a tubular foam (sponge).
- the sound insulating material of the present invention is a material that realizes excellent sound insulating properties while being lightweight without being complicated in shape, and thus can be used for various applications.
- automotive sealing materials, architectural sealing materials, railway vehicle sealing materials, marine sealing materials, aircraft sealing materials, and the like including the sound insulating material of the present invention are excellent sound insulating products.
- A) Soft material A-1) EPDM (trade name: Mitsui EPT 1045 (manufactured by Mitsui Chemicals)), ethylene content: 58 wt%, dicyclopentadiene content: 5.0 wt%, Mooney viscosity [ML 1 + 4 (100 ° C.)]: 38)
- A-2) EPDM (trade name: Mitsui EPT 8030M (manufactured by Mitsui Chemicals)), EPDM, structural unit content derived from ethylene: 47% by mass, structure derived from 5-ethylidene-2-norbornene (ENB) Unit content: 9.5% by mass, Mooney viscosity [ML 1 + 4 (100 ° C.)]: 32)
- the content of structural units derived from ethylene is 46% by mass, and the total content of structural units derived from 5-ethylidene-2-norbornene (ENB) and 5-vinyl-2-norbornene (VNB) is 11%.
- the Mooney viscosity [ML 1 + 4 (160 ° C.)] of this copolymer was 74.
- A-4) Butyl rubber (IIR) (trade name: JSR Butyl 268 (manufactured by JSR Corporation), degree of unsaturation (mol%): 1.5%, Mooney viscosity [ML 1 + 8 (125 ° C.)]: 51)
- A-5) Styrene butadiene rubber (SBR) (trade name: SBR 1502 (manufactured by Nippon Zeon Co., Ltd.), bound styrene content: 23.5%, Mooney viscosity [ML 1 + 4 (100 ° C.)]: 52)
- A-6) Acrylonitrile butadiene rubber (NBR) (trade name: Nipol 1042 (manufactured by Zeon Corporation), amount of bound acrylonitrile: 33.5%, Mooney viscosity [ML 1 + 4 (100 ° C.)]: 77.5 )
- the autoclave was heated to an internal temperature of 60 ° C. and pressurized with propylene so that the total pressure was 0.40 MPa (gauge pressure).
- methylaluminoxane prepared in advance, 1 mmol in terms of Al, diphenylmethylene (1-ethyl-3-t-butyl-cyclopentadienyl) (2,7-di-t-butyl-fluorenyl) zirconium Polymerization was initiated by injecting 0.34 ml of a toluene solution containing 0.01 mmol of dichloride into the autoclave with nitrogen. During the polymerization reaction, the temperature was adjusted so that the internal temperature of the autoclave was 60 ° C.
- the polymer mass containing the solvent obtained by filtering the reaction solution was dried at 100 ° C. under reduced pressure for 12 hours.
- the obtained polymer was 36.9 g, and the content of structural units derived from 4-methyl-1-pentene in the polymer was 72 mol%, and the content of structural units derived from propylene was 28 mol%.
- the weight average molecular weight (Mw) measured by gel permeation chromatography (GPC) was 337,000, tan ⁇ -Tg was 28 ° C., and the maximum tan ⁇ was 2.4.
- the kneading was performed at a rotor rotation speed of 50 rpm, a floating weight pressure of 3 kg / cm 2 and a kneading time of 5 minutes, and the kneading discharge temperature was 148 ° C.
- vulcanization accelerator J-1 tetramethylthiuram disulfide
- vulcanization accelerator J-2 tetramethylthiuram disulfide
- vulcanization accelerator J-2 tetramethylthiuram disulfide
- vulcanization accelerator J-2 tetramethylthiuram disulfide
- vulcanization accelerator J-2 tetramethylthiuram disulfide
- vulcanization accelerator J-2 tetramethylthiuram disulfide
- vulcanization accelerator J-2 tetramethylthiuram disulfide
- Comparative Example 2 instead of the resin (B), an ethylene- ⁇ -olefin copolymer (trade name: Tafmer DF605 (manufactured by Mitsui Chemicals)), tan ⁇ -Tg: ⁇ 46 ° C., tan ⁇ maximum value: 0 .5) was used. The results are shown in Table 1.
- Example 1A shows the results for 1 to 4 kHz
- FIG. 1B shows the results for 4 to 6 kHz.
- Example 1 As shown in Table 1 and FIG. 1, in the frequency ranges of 1 to 4 kHz and 4 to 6 kHz at which sound can be heard with high sensitivity to the human ear, in Comparative Examples 1 to 6, each time the mass of the test piece used for measurement increases Transmission loss is improved. In Example 1, it is confirmed that the sound insulation characteristics are higher than those of Comparative Examples 1 to 6 even when the mass of the test piece is equal to or lighter than that of Comparative Examples 1 to 6. From this result, the sound insulating material of the present invention can be reduced in weight while maintaining the sound insulating properties of the conventional sound insulating material, or the sound insulating properties can be improved while maintaining the light weight of the conventional sound insulating material. I know that there is.
- Example 2 Using an 8-inch two-roll kneader, soft material under kneading conditions of front roll temperature / rear roll temperature: 70 ° C./70° C., rotation speed of front roll 12.5 rpm, rotation speed of rear roll 10.4 rpm 100 parts by weight of A-4 (butyl rubber), 40 parts by weight of resin B-1, 3 parts by weight of vulcanization aid C-1 (zinc oxide), and 1 part by weight of processing aid (stearic acid) were kneaded until uniform.
- A-4 butyl rubber
- resin B-1 butyl rubber
- vulcanization aid C-1 zinc oxide
- processing aid stearic acid
- vulcanization accelerator J-1 tetramethylthiuram disulfide
- vulcanizing agent sulfur
- Comparative Examples 7 and 8 For Comparative Examples 7 and 8, a vulcanized sheet (press sheet) was prepared under the same conditions as in Example 2 except that the blending composition was changed to the blending composition shown in Table 2, and the above measurements and evaluations were performed. However, in Comparative Example 8, instead of the resin (B), an ethylene- ⁇ -olefin copolymer (trade name: Tafmer DF605 (manufactured by Mitsui Chemicals)), tan ⁇ -Tg: ⁇ 46 ° C., tan ⁇ maximum value: 0 .5) was used. The results are shown in Table 2.
- Example 2 From the results of the sound insulation characteristics test, as shown in Table 2, the sound insulation characteristics of Example 2 were compared in the areas of 1 to 4 kHz and 4 to 6 kHz although the mass of the test piece was lighter than those of Comparative Examples 7 and 8. It turns out that it is superior to Examples 7 and 8.
- Example 3 Using an 8-inch two-roll kneader, soft material under kneading conditions of front roll temperature / rear roll temperature: 70 ° C./70° C., rotation speed of front roll 12.5 rpm, rotation speed of rear roll 10.4 rpm 100 parts by weight of A-5 (styrene butadiene rubber), 40 parts by weight of resin B-1, 3 parts by weight of vulcanization aid C-1 (zinc oxide), and 1 part by weight of processing aid (stearic acid) until uniform After kneading, 1 part by mass of vulcanization accelerator J-3 (N- (tert-butyl) -2-benzothiazole sulfenamide) and 1.75 parts by mass of vulcanizing agent (sulfur) are added to make it even more uniform.
- A-5 styrene butadiene rubber
- resin B-1 3 parts by weight of vulcanization aid C-1 (zinc oxide)
- processing aid stearic acid
- Comparative Example 10 instead of the resin (B), an ethylene- ⁇ -olefin copolymer (trade name: Tafmer DF605 (manufactured by Mitsui Chemicals)), tan ⁇ -Tg: ⁇ 46 ° C., tan ⁇ maximum value: 0. 5) was used. The results are shown in Table 3.
- Example 3 From the results of the sound insulation characteristic test, as shown in Table 3, the sound insulation characteristics of Example 3 are comparable in the ranges of 1 to 4 kHz and 4 to 6 kHz even though the mass of the test piece is lighter than those of Comparative Examples 9 and 10. It can be seen that it is superior to Examples 9 and 10.
- Example 4 Using an 8-inch two-roll kneader, soft material under kneading conditions of front roll temperature / rear roll temperature: 70 ° C./70° C., rotation speed of front roll 12.5 rpm, rotation speed of rear roll 10.4 rpm 100 parts by weight of A-6 (acrylonitrile butadiene rubber), 40 parts by weight of resin B-1, 3 parts by weight of vulcanization aid C-1 (zinc oxide), and 1 part by weight of processing aid (stearic acid) until uniform After kneading, 0.7 parts by mass of vulcanization accelerator J-3 (N- (tert-butyl) -2-benzothiazolesulfenamide) and 1.55 parts by mass of vulcanizing agent (sulfur) were added, It kneaded until it became more uniform.
- A-6 acrylonitrile butadiene rubber
- resin B-1 acrylonitrile butadiene rubber
- vulcanization aid C-1 zinc oxide
- processing aid
- Example 4 From the results of the sound insulation characteristics test, as shown in Table 4, the sound insulation characteristics of Example 4 in both the 1 to 4 kHz and 4 to 6 kHz regions were compared, although the test piece mass was lighter than those of Comparative Examples 11 and 12. It turns out that it is superior to Examples 11 and 12.
- Example 5 MIXTRON BB MIXER (manufactured by Kobe Steel, Ltd., BB-4 type, volume 2.95 L, rotor 4WH), soft material A-3 (EPDM) 100 parts by mass, resin B-1 40 parts by mass, Vulcanization aid C-2 (active zinc white) 8 parts by weight, processing aid (stearic acid) 2 parts by weight, reinforcing material (carbon black) 88 parts by weight, filler (calcium carbonate) 50 parts by weight, activator ( 1 part by mass of polyethylene glycol) and 71 parts by mass of a softening material (paraffin oil) were kneaded.
- EPDM soft material A-3
- resin B-1 40 parts by mass resin B-1 40 parts by mass
- Vulcanization aid C-2 active zinc white 8 parts by weight
- processing aid stearic acid
- reinforcing material carbon black
- filler calcium carbonate
- the kneading was performed at a rotor rotation speed of 50 rpm, a floating weight pressure of 3 kg / cm 2 , a kneading time of 5 minutes, and the kneading discharge temperature was 152 ° C.
- vulcanization accelerator J-4 dibenzothiazyl disulfide
- vulcanization accelerator J-5 vulcanization accelerator J-5
- vulcanization accelerator J-6 (2-imidazoline-2-thiol) 1 part by mass
- vulcanization accelerator J-7 tellurium diethyldithiocarbamate
- 1.5 parts by mass of a sulfurizing agent (sulfur) was added and kneaded using a 14-inch two-roll kneader.
- the roll temperature was the front roll / rear roll: 60 ° C./55° C.
- the rotation speed of the front roll was 13 rpm
- the rotation speed of the rear roll was 11.5 rpm.
- Example 6 to 10 For Examples 6 to 10, vulcanized sheets (press sheets) were prepared under the same conditions as in Example 5 except that the blending composition was changed to the blending composition shown in Table 5, and the above measurements and evaluations were performed. The results are shown in Table 5.
- Comparative Examples 13 to 15 For Comparative Examples 13 to 15, vulcanized sheets (press sheets) were prepared under the same conditions as in Example 5 except that the blending composition was changed to the blending composition shown in Table 5, and the above measurements and evaluations were performed.
- Comparative Example 14 instead of the resin (B), an ethylene- ⁇ -olefin copolymer (Tafmer DF605 (manufactured by Mitsui Chemicals), tan ⁇ -Tg: ⁇ 46 ° C., tan ⁇ maximum value: 0.5)
- a polyolefin copolymer (trade name: NOTIO SN0285 (manufactured by Mitsui Chemicals, Inc.), tan ⁇ -Tg: ⁇ 10 ° C., tan ⁇ maximum value: 1.2 instead of the resin (B). ) was used. The results are shown in Table 5.
- Example 11 MIXTRON BB MIXER (manufactured by Kobe Steel, Ltd., BB-4 type, volume 2.95 L, rotor 4WH), soft material A-3 (EPDM) 100 parts by mass, resin B-1 40 parts by mass, Vulcanization aid C-2 (active zinc white) 8 parts by weight, processing aid (stearic acid) 2 parts by weight, reinforcing material (carbon black) 88 parts by weight, filler (calcium carbonate) 50 parts by weight, activator ( 1 part by weight of polyethylene glycol), 71 parts by weight of a softening material (paraffin oil), and 5 parts by weight of a hygroscopic agent (calcium oxide) were kneaded.
- EPDM soft material A-3
- the kneading was performed at a rotor rotation speed of 50 rpm, a floating weight pressure of 3 kg / cm 2 , a kneading time of 5 minutes, and the kneading discharge temperature was 152 ° C.
- vulcanization accelerator J-4 (dibenzothiazyl disulfide) 1.5 parts by mass, vulcanization accelerator J-5 (zinc dibutyldithiocarbamate) 2 parts, vulcanization accelerator J-6 (2-imidazoline-2-thiol) 1 part by mass
- vulcanization accelerator J-7 tellurium diethyldithiocarbamate
- vulcanizing agent sulfur
- the obtained ribbon-shaped composition was extruded under the conditions of a die temperature of 80 ° C. and a cylinder temperature of 60 ° C. using a 60 mm ⁇ extruder equipped with a tubular die (inner diameter 12 mm, wall thickness 1.5 mm), Molded into a tube.
- This molded body is introduced into a microwave vulcanizing tank at 230 ° C. and 1 kHz at the same time as the molding, followed by a linear hot-air vulcanizer (HAV) set at 250 ° C. and heated for 5 minutes for crosslinking and foaming.
- a tube-like sponge molded body was obtained. The sponge molded body was cut out, a test piece was punched out, and the above measurement and evaluation were performed using this test piece.
- Example 6 For Examples 12 to 16, a tube-like sponge molded body was produced under the same conditions as in Example 11 except that the blending composition and vulcanization conditions were changed to the blending composition and vulcanization conditions as shown in Table 6, and a test piece was prepared. Got. The measurement and evaluation were performed using this test piece. The results are shown in Table 6.
- Comparative Examples 16 to 20 For Comparative Examples 16 to 20, a tube-like sponge molded body was produced under the same conditions as in Example 11 except that the blending composition and vulcanization conditions were changed to the blending composition and vulcanization conditions as shown in Table 6, and a test piece was prepared. Got. The measurement and evaluation were performed using this test piece. The results are shown in Table 6.
- FIG. 12 shows the results of the relationship between the test piece mass and the average transmission loss for the sound insulation characteristics of Examples 11 to 16 and Comparative Examples 16 to 20.
- FIG. 2A shows the results for 1 to 4 kHz
- FIG. 2B shows the results for 4 to 6 kHz.
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Abstract
Description
(配合材料)
実施例及び比較例に用いた配合材料は下記の通りである。
A)軟質材
A-1)EPDM(商品名:三井EPT 1045(三井化学(株)製)、エチレン含有量:58wt%、ジシクロペンタジエン含有量:5.0wt%、ムーニー粘度[ML1+4(100℃)]:38)
A-2)EPDM(商品名:三井EPT 8030M(三井化学(株)製)、EPDM、エチレンから導かれる構造単位含有量:47質量%、5-エチリデン-2-ノルボルネン(ENB)から導かれる構造単位含有量:9.5質量%、ムーニー粘度[ML1+4(100℃)]:32)
A-3)下記重合例1により得られたEPDM
[重合例1]
攪拌翼を備えた容積300Lの重合器を用いて連続的に、エチレン、プロピレン、5-エチリデン-2-ノルボルネン(ENB)および5-ビニル-2-ノルボルネン(VNB)からなる四元共重合反応を80℃にて行った。重合溶媒としてヘキサン(最終濃度:90.8重量%)を用いて、エチレン濃度を3.1重量%、プロピレン濃度を4.6重量%、ENB濃度を1.4重量%およびVNB濃度を0.11重量%として、これらを連続供給した。重合圧力を0.8MPaに保ちながら、主触媒としてメタロセン系触媒である[N-(1,1-ジメチルエチル)-1,1-ジメチル-1-[(1,2,3,3A,8A-η)-1,5,6,7-テトラヒドロ-2-メチル-S-インダセン-1-yl]シランアミネート(2-)-κN][(1,2,3,4-η)-1,3-ペンタジエン]-チタニウムを、その濃度が0.0013mmol/Lとなるよう連続的に供給した。また、共触媒として(C6H5)3CB(C6F5)4を、その濃度が0.0066mmol/Lとなるように、有機アルミニウム化合物としてトリイソブチルアルミニウム(TIBA)を、その濃度が0.0154mmol/Lとなるように、それぞれ連続的に供給した。なお、上記メタロセン系触媒は、国際公開第98/49212号パンフレットに記載されている方法に準じて合成して得た。
A-5)スチレンブタジエンゴム(SBR)(商品名:SBR 1502(日本ゼオン(株)製)、結合スチレン量:23.5%、ムーニー粘度[ML1+4(100℃)]:52)
A-6)アクリロニトリルブタジエンゴム(NBR)(商品名:Nipol 1042(日本ゼオン(株)製)、結合アクリロニトリル量:33.5%、ムーニー粘度[ML1+4(100℃)]:77.5)
B)樹脂
B-1)下記重合例2により得られた重合体
[重合例2]
充分窒素置換した容量1.5リットルの攪拌翼付SUS製オートクレーブに、23℃でノルマルヘキサン300ml(乾燥窒素雰囲気、活性アルミナ上で乾燥したもの)、4-メチル-1-ペンテン450mlを入れた。このオートクレーブに、トリイソブチルアルミニウム(TIBAL)の1.0mmol/mlトルエン溶液を0.75ml入れ、攪拌機を回した。
B-3)水素添加スチレン系熱可塑エラストマー(商品名:S.O.E. L605(旭化成(株)製)、tanδ―Tg:16℃、tanδ最大値:1.5)
C)加硫助剤
C-1)酸化亜鉛2種(三井金属鉱業(株)製)
C-2)活性亜鉛華(商品名:META-Z102(井上石灰工業(株)製))
D)加工助剤
ステアリン酸(商品名:粉末ステアリン酸さくら(日油(株)製))
E)補強材
カーボンブラック(商品名:旭#55G(旭カーボン(株)製))
F)充填材
炭酸カルシウム(商品名:ホワイトンSB(白石カルシウム(株)製))
G)活性剤
ポリエチレングリコール(商品名:PEG#4000(ライオン(株)製))
H)軟化材
パラフィンオイル(商品名:ダイアナプロセスオイル PS-430(出光興産(株)製))
I)加硫剤
硫黄(商品名:アルファグランS-50EN(東知(株)製))
J)加硫促進剤
J-1)チウラム系加硫促進剤:テトラメチルチウラムジスルフィド(商品名:サンセラーTT(三新化学工業(株)製))
J-2)チアゾール系加硫促進剤:2-メルカプトベンゾチアゾール(商品名:サンセラーM(三新化学工業(株)製))
J-3)スルフェンアミド系加硫促進剤:N-(tert-ブチル)-2-ベンゾチアゾールスルフェンアミド(商品名:サンセラーNS-G(三新化学工業(株)製))
J-4)チアゾール系加硫促進剤:ジベンゾチアジルジスルフィド(商品名:サンセラーDM(三新化学工業(株)製))
J-5)ジチオカルバメート系加硫促進剤:ジブチルジチオカルバミン酸亜鉛(商品名:サンセラーBZ(三新化学工業(株)製))
J-6)チオウレア系加硫促進剤:2-イミダゾリン-2-チオール(商品名:サンセラー22-C(三新化学工業(株)製))
J-7)ジチオカルバメート系加硫促進剤:ジエチルジチオカルバミン酸テルル(商品名:サンセラーTE-G(三新化学工業(株)製))
K)発泡剤
4,4'-オキシビス(ベンゼンスルホニルヒドラジド)(OBSH)(商品名:ネオセルボンN#1000M(永和化成工業(株)製))
L)吸湿剤
酸化カルシウム(商品名:VESTA-18(井上石灰工業(株)製))
(測定方法および評価方法)
以下の実施例および比較例において、各物性は以下の方法により測定または評価した。
a)動的粘弾性測定
粘弾性測定装置ARES(TA Instrumens JAPAN Inc.社製)を用いて、下記測定条件で各材料の粘度の温度依存性を測定した。当該測定で得られた、貯蔵弾性率(G')と損失弾性率(G")との比(G"/G':損失正接)をtanδとした。tanδを温度に対してプロットすると、上に凸の曲線すなわちピークが得られ、そのピークの頂点の温度をガラス転移温度、すなわちtanδ―Tgとし、その温度における極大値を測定した。tanδにつき2つのピークが観測された場合には、第1および第2のピークとして双方のtanδ―Tgおよび極大値を記録した。
Frequency :1.0Hz
Temperature :-70~80℃
Ramp Rate :4.0℃/分
Strain :0.5%
b)遮音特性試験
プレスシートおよびチューブ状スポンジ成形品から試験片を打ち抜き、内径29mmφの4206-T型音響管(Bruel&Kjaer製)および測定用ソフト(PULSE Material Testing Type7758、Bruel&Kjaer製)を用いて垂直入射透過損失を測定し、1~4kHzおよび4~6kHzにおける平均透過損失を求めた。
c)比重、試験片重量
遮音特性試験に使用した試験片に対し、25℃雰囲気下で自動比重計(東洋精機製作所製:M-1型)を用いて質量測定および、空気中と純水中との質量の差から比重測定を行った。
[実施例1]
MIXTRON BB MIXER((株)神戸製鋼所社製、BB-4型、容積2.95L、ローター4WH)を用いて、軟質材A-1(EPDM)100質量部、樹脂B-1 40質量部、加硫助剤C-1(酸化亜鉛)5質量部、加工助剤(ステアリン酸)1質量部を混練した。混練は、ローター回転数50rpm、フローティングウェイト圧力3kg/cm2、混練時間5分間で行い、混練排出温度は148℃であった。
[比較例1~6]
比較例1~6について、配合組成を表1に示すとおりの配合組成に変更した以外は実施例1と同条件で加硫シート(プレスシート)を作製し、上記測定および評価を行った。ただし、比較例2では、樹脂(B)の替りにエチレン-α-オレフィン共重合体(商品名:タフマーDF605(三井化学(株)製)、tanδ―Tg:-46℃、tanδ最大値:0.5)を用いた。結果を表1に示す。
[実施例2]
8インチ二本ロール混練機を用いて、前ロール温度/後ロール温度:70℃/70℃、前ロールの回転数12.5rpm、後ロールの回転数10.4rpmという混練条件にて、軟質材A-4(ブチルゴム)100質量部、樹脂B-1 40質量部、加硫助剤C-1(酸化亜鉛)3質量部、加工助剤(ステアリン酸)1質量部を均一になるまで混練した後、加硫促進剤J-1(テトラメチルチウラムジスルフィド)1質量部、加硫剤(硫黄)1.75質量部を添加して、さらに均一になるまで混練した。その後、混練物をシート状に分出し、加熱プレスを用いて160℃で30分間加熱加硫することで、厚さ2mmの加硫シート(プレスシート)を得た。この加硫シートを用いて上記測定および評価を行った。結果を表2に示す。
[比較例7、8]
比較例7、8について、配合組成を表2に示すとおりの配合組成に変更した以外は実施例2と同条件で加硫シート(プレスシート)を作製し、上記測定および評価を行った。ただし、比較例8では、樹脂(B)の替りにエチレン-α-オレフィン共重合体(商品名:タフマーDF605(三井化学(株)製)、tanδ―Tg:-46℃、tanδ最大値:0.5)を用いた。結果を表2に示す。
[実施例3]
8インチ二本ロール混練機を用いて、前ロール温度/後ロール温度:70℃/70℃、前ロールの回転数12.5rpm、後ロールの回転数10.4rpmという混練条件にて、軟質材A-5(スチレンブタジエンゴム)100質量部、樹脂B-1 40質量部、加硫助剤C-1(酸化亜鉛)3質量部、加工助剤(ステアリン酸)1質量部を均一になるまで混練した後、加硫促進剤J-3(N-(tert-ブチル)-2-ベンゾチアゾールスルフェンアミド)1質量部、加硫剤(硫黄)1.75質量部を添加して、さらに均一になるまで混練した。その後、混練物をシート状に分出し、加熱プレスを用い160℃で30分間加熱加硫することで、厚さ2mmの加硫シート(プレスシート)を得た。この加硫シートを用いて上記測定および評価を行った。結果を表3に示す。
[比較例9、10]
比較例9、10について、配合組成を表3に示すとおりの配合組成に変更した以外は実施例3と同条件で加硫シート(プレスシート)を作製し、上記測定および評価を行った。ただし、比較例10では、樹脂(B)替りにエチレン-α-オレフィン共重合体(商品名:タフマーDF605(三井化学(株)製)、tanδ―Tg:-46℃、tanδ最大値:0.5)を用いた。結果を表3に示す。
[実施例4]
8インチ二本ロール混練機を用いて、前ロール温度/後ロール温度:70℃/70℃、前ロールの回転数12.5rpm、後ロールの回転数10.4rpmという混練条件にて、軟質材A-6(アクリロニトリルブタジエンゴム)100質量部、樹脂B-1 40質量部、加硫助剤C-1(酸化亜鉛)3質量部、加工助剤(ステアリン酸)1質量部を均一になるまで混練した後、加硫促進剤J-3(N-(tert-ブチル)-2-ベンゾチアゾールスルフェンアミド)0.7質量部、加硫剤(硫黄)1.55質量部を添加して、さらに均一になるまで混練した。その後、混練物をシート状に分出し、加熱プレスを用い160℃で30分間加熱加硫することで、厚さ2mmの加硫シート(プレスシート)を得た。この加硫シートを用いて上記測定および評価を行った。結果を表4に示す。
[比較例11、12]
比較例11、12について、配合組成を表4に示すとおりの配合組成に変更した以外は実施例4と同条件で加硫シート(プレスシート)を作製し、上記測定および評価を行った。ただし、比較例12では、樹脂(B)の替りにエチレン-α-オレフィン共重合体(商品名:タフマーDF605(三井化学(株)製)、tanδ―Tg:-46℃、tanδ最大値:0.5)を用いた。結果を表4に示す。
[実施例5]
MIXTRON BB MIXER((株)神戸製鋼所社製、BB-4型、容積2.95L、ローター4WH)を用いて、軟質材A-3(EPDM)100質量部、樹脂B-1 40質量部、加硫助剤C-2(活性亜鉛華)8質量部、加工助剤(ステアリン酸)2質量部、補強材(カーボンブラック)88質量部、充填材(炭酸カルシウム)50質量部、活性剤(ポリエチレングリコール)1質量部、軟化材(パラフィンオイル)71質量部を混練した。混練は、ローター回転数50rpm、フローティングウェイト圧力3kg/cm2、混練時間5分間で行い、混練排出温度は152℃であった。
[実施例6~10]
実施例6~10について、配合組成を表5に示すとおりの配合組成に変更した以外は実施例5と同条件で加硫シート(プレスシート)を作製し、上記測定および評価を行った。結果を表5に示す。
[比較例13~15]
比較例13~15について、配合組成を表5に示すとおりの配合組成に変更した以外は実施例5と同条件で加硫シート(プレスシート)を作製し、上記測定および評価を行った。ただし、比較例14では、樹脂(B)の替りにエチレン-α-オレフィン共重合体(タフマーDF605(三井化学(株)製)、tanδ―Tg:-46℃、tanδ最大値:0.5)を用い、比較例15では、樹脂(B)の替りにポリオレフィン系共重合体(商品名:ノティオSN0285(三井化学(株)製)、tanδ―Tg:-10℃、tanδ最大値:1.2)を用いた。結果を表5に示す。
[実施例11]
MIXTRON BB MIXER((株)神戸製鋼所社製、BB-4型、容積2.95L、ローター4WH)を用いて、軟質材A-3(EPDM)100質量部、樹脂B-1 40質量部、加硫助剤C-2(活性亜鉛華)8質量部、加工助剤(ステアリン酸)2質量部、補強材(カーボンブラック)88質量部、充填材(炭酸カルシウム)50質量部、活性剤(ポリエチレングリコール)1質量部、軟化材(パラフィンオイル)71質量部、吸湿剤(酸化カルシウム)5質量部を混練した。混練は、ローター回転数50rpm、フローティングウェイト圧力3kg/cm2、混練時間5分間で行い、混練排出温度は152℃であった。
[実施例12~16]
実施例12~16について、配合組成および加硫条件を、表6に示すとおりの配合組成および加硫条件に変更した以外は実施例11と同条件でチューブ状スポンジ成形体を作製し、試験片を得た。この試験片を用いて上記測定および評価を行った。結果を表6に示す。
[比較例16~20]
比較例16~20について、配合組成および加硫条件を、表6に示すとおりの配合組成および加硫条件に変更した以外は実施例11と同条件でチューブ状スポンジ成形体を作製し、試験片を得た。この試験片を用いて上記測定および評価を行った。結果を表6に示す。
Claims (13)
- 動的粘弾性測定により求められた損失正接tanδのピークが-60℃以上0℃未満の温度範囲に存在する軟質材(A)と、動的粘弾性測定により求められた損失正接tanδのピークが0℃以上60℃以下の温度範囲に存在する樹脂(B)とを、軟質材(A)100質量部当たり樹脂(B)1~50質量部の割合で含む遮音材。
- 軟質材(A)がエチレン系ゴム、天然ゴムおよびジエン系ゴムから選ばれる少なくとも1種を含む、請求項1に記載の遮音材。
- 軟質材(A)がエチレン・α-オレフィン・非共役ポリエン共重合体(a)を含む、請求項1に記載の遮音材。
- エチレン・α-オレフィン・非共役ポリエン共重合体(a)は、エチレンから導かれる構成単位の含有量が40~72質量%であり、かつ非共役ポリエンから導かれる構成単位の含有量が2~15質量%である、請求項3に記載の遮音材。
- 樹脂(B)が芳香族系重合体、4-メチル-1-ペンテン・α-オレフィン共重合体(b)、ポリ酢酸ビニル、ポリエステル、ポリウレタン、ポリ(メタ)アクリレート、エポキシ樹脂およびポリアミドから選ばれる少なくとも1種を含む、請求項1~4のいずれかに記載の遮音材。
- 樹脂(B)が、4-メチル-1-ペンテンから導かれる構成単位(i)16~95モル%、4-メチル-1-ペンテンを除く炭素原子数2~20のα-オレフィンから選ばれる少なくとも1種以上のα-オレフィンから導かれる構成単位(ii)5~84モル%および非共役ポリエンから導かれる構成単位(iii)0~10モル%(ただし、構成単位(i)、(ii)および(iii)の合計を100モル%とする)を有する4-メチル-1-ペンテン・α-オレフィン共重合体(b-1)を含む、請求項1~4のいずれかに記載の遮音材。
- 軟質材(A)および樹脂(B)を含む組成物を、加硫剤を用いて架橋して得られる、請求項1~6のいずれかに記載の遮音材。
- 前記遮音材は、少なくともその一部が発泡体であることを特徴とする、請求項1~7のいずれかに記載の遮音材。
- 請求項1~8のいずれかに記載の遮音材を含む自動車用シール材。
- 請求項1~8のいずれかに記載の遮音材を含む建築用シール材。
- 請求項1~8のいずれかに記載の遮音材を含む鉄道車両用シール材。
- 請求項1~8のいずれかに記載の遮音材を含む船舶用シール材。
- 請求項1~8のいずれかに記載の遮音材を含む航空機用シール材。
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JP2022515311A (ja) * | 2018-11-07 | 2022-02-18 | 住友化学株式会社 | エチレン-α-オレフィン-非共役ポリエン共重合体ゴム、及びゴム組成物 |
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KR102039881B1 (ko) | 2019-11-04 |
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