JPWO2020116577A1 - 多孔質吸音材及びその製造方法、並びに、吸音方法 - Google Patents
多孔質吸音材及びその製造方法、並びに、吸音方法 Download PDFInfo
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Classifications
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/06—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent
- C08J9/10—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent developing nitrogen, the blowing agent being a compound containing a nitrogen-to-nitrogen bond
- C08J9/102—Azo-compounds
- C08J9/103—Azodicarbonamide
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0014—Use of organic additives
- C08J9/0023—Use of organic additives containing oxygen
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08J9/0061—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof characterized by the use of several polymeric components
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0066—Use of inorganic compounding ingredients
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0095—Mixtures of at least two compounding ingredients belonging to different one-dot groups
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
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- C08J9/36—After-treatment
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L11/00—Compositions of homopolymers or copolymers of chloroprene
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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- C08L23/04—Homopolymers or copolymers of ethene
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Abstract
Description
(ベース材料)
エチレン−プロピレン−ジエンゴム(以下、「EPDM」という):三井化学株式会社製、「EMB−EPT4021」
クロロプレンゴム(以下、「CR」という):東ソー株式会社製、「スカイプレンB−30」
低密度ポリエチレン(以下、「LDPE」という):日本ポリエチレン株式会社製、「LF640MA」
[金属フィラー]
センダストA:山陽特殊製鋼株式会社製、Fe−Si−Al合金系粉末、比重:8g/cm3、平均粒子径:10μm
センダストB:山陽特殊製鋼株式会社製、Fe−Si−Al合金系粉末、比重:8g/cm3、平均粒子径:30μm
センダストC:山陽特殊製鋼株式会社製、Fe−Si−Al合金系粉末、比重:8g/cm3、平均粒子径:5μm
亜鉛粉末:和光純薬工業株式会社製、亜鉛粉末
鉄合金粉末:三津和化学薬品株式会社製、「sus304L」、ステンレス粉末
タングステン合金粉末:タングステンヘビーメタル粉末
[その他のフィラー]
炭酸カルシウム:白石カルシウム社製、「ホワイトンSB」
充填剤用酸化亜鉛:堺化学工業株式会社製、「酸化亜鉛2種」
ステアリン酸:日油株式会社製、「粉末ステアリン酸さくら」
プロセスオイル:出光興産株式会社製、「ダイアナプロセスオイルPW−90」、パラフィン系プロセスオイル
架橋剤として、ベース材料がEPDMである場合は硫黄を用い、ベース材料がCRである場合は酸化亜鉛(架橋剤用酸化亜鉛)を用い、ベース材料がLDEPである場合は有機過酸化物類を用いた。
硫黄:細井化学工業株式会社製、微粉硫黄S−200メッシュ
架橋剤用酸化亜鉛:堺化学株式会社製、酸化亜鉛2種
有機過酸化物類:日本油脂株式会社製、「パークミルD」、ジクミルパーオキサイド
チアゾール類:大内新興化学工業株式会社製、「ノクセラーM」、2−メルカプトベンゾチアゾール
チウラム類:大内新興化学工業株式会社製、「ノクセラーTT」、テトラメチルチウラムジスルフィド
アゾジカルボンアミド:三協化成株式会社製、「セルマイクC−1」
尿素:永和化成工業株式会社製、「セルペースト101」
(実施例1)
ロール温度40℃のミキシングロール(7インチ、回転数:25rpm)を用いてEPDM(ベース材料)100質量部を5分間素練りした。その後、このEPDMに対して、センダストAを30質量部、炭酸カルシウムを80質量部、充填剤用酸化亜鉛を1質量部、ステアリン酸(加工助剤)を3質量部添加した後に15分間混練した。次いで、プロセスオイル(軟化剤)を60質量部添加した後に5分間混練した。続いて、ロール温度を70℃に上げることにより熱入れを3分間行った。そして、ロール温度を40℃に下げた後、硫黄(架橋剤)を1質量部、架橋促進剤(チアゾール類2質量部、チウラム類1質量部)、アゾジカルボンアミド(発泡剤)を10質量部、尿素(発泡助剤)を1質量部添加した後に10分間混錬することにより発泡前の発泡組成物(混練物)を得た。
表1の種類及び使用量の金属フィラーを用いたこと以外は実施例1と同様に行い、シート状の多孔質吸音材を得た。
金属フィラーを使用せず、チアゾール類の使用量を2.3質量部に変更したこと以外は実施例1と同様に行い、二次発泡体を得た。また、気泡の連通化を行った後にスライス加工を行って厚さ10mmに仕上げること以外は実施例1と同様に行い、シート状の多孔質吸音材を得た。
金属フィラーを使用せず、架橋促進剤をチアゾール類2.3質量部及びチウラム類1.1質量部に変更したこと以外は実施例1と同様に行い、二次発泡体を得た。また、気泡の連通化を行った後にスライス加工を行って厚さ10mmに仕上げること以外は実施例1と同様に行い、シート状の多孔質吸音材を得た。
金属フィラーを使用せず、発泡剤の使用量を15質量部に変更したこと以外は実施例1と同様に行い、二次発泡体を得た。また、気泡の連通化の回数を8回に変更し、スライス加工を行って厚さ10mmに仕上げること以外は実施例1と同様に行い、シート状の多孔質吸音材を得た。
金属フィラーを使用せず、架橋促進剤をチアゾール類2.5質量部及びチウラム類1.2質量部に変更したこと以外は実施例1と同様に行い、二次発泡体を得た。また、気泡の連通化を行った後にスライス加工を行って厚さ10mmに仕上げること以外は実施例1と同様に行い、シート状の多孔質吸音材を得た。
金属フィラーを使用せず、発泡剤の使用量を17質量部に変更したこと以外は実施例1と同様に行い、二次発泡体を得た。また、気泡の連通化の回数を5回に変更し、スライス加工を行って厚さ20mmに仕上げること以外は実施例1と同様に行い、シート状の多孔質吸音材を得た。
気泡の連通化を行った後にスライス加工を行って厚さ30mmに仕上げること以外は実施例9と同様に行い、シート状の多孔質吸音材を得た。
ロール温度40℃のミキシングロール(7インチ、回転数:25rpm)を用いてCR(ベース材料)100質量部を5分間素練りした。その後、このCRに対して、センダストAを30質量部、炭酸カルシウムを50質量部、ステアリン酸(加工助剤)を1質量部添加した後に5分間混練した。次いで、プロセスオイル(軟化剤)を60質量部添加した後に5分間混練した。続いて、ロール温度を70℃に上げることにより熱入れを5分間行った。そして、ロール温度を40℃に下げた後、架橋剤用酸化亜鉛(架橋剤)を5質量部、アゾジカルボンアミド(発泡剤)を15質量部、尿素(発泡助剤)を1.5質量部添加した後に10分間混錬することにより発泡前の発泡組成物(混練物)を得た。
ロール温度40℃のミキシングロール(7インチ、回転数:25rpm)を用いてEPDM(ベース材料)100質量部を5分間素練りした。その後、このEPDMに対して、炭酸カルシウムを20質量部、充填剤用酸化亜鉛を1質量部、ステアリン酸(加工助剤)を3質量部添加した後に15分間混練した。次いで、回転数を40rpmに変更した上で(以降の混練操作も同様の回転数)、プロセスオイル(軟化剤)を60質量部添加した後に20分間混練した。続いて、ロール温度を80℃に上げることにより熱入れを3分間行った。そして、ロール温度を40℃に下げた後、硫黄(架橋剤)を1質量部、架橋促進剤(チアゾール類2質量部、チウラム類1質量部)、アゾジカルボンアミド(発泡剤)を10質量部、尿素(発泡助剤)を1質量部添加した後に20分間混錬することにより発泡前の発泡組成物(混練物)を得た。
気泡の連通化を行った後にスライス加工を行って表2の厚さに仕上げること以外は実施例12と同様に行い、シート状の多孔質吸音材を得た。
発泡剤の使用量を表2の使用量に変更し、気泡の連通化を行わなかったこと以外は実施例12と同様に行い、シート状の多孔質吸音材を得た。
発泡剤の使用量を表2の使用量に変更したこと以外は実施例12と同様に行い、シート状の多孔質吸音材を得た。
架橋促進剤及び発泡剤の使用量を表2の使用量に変更したこと以外は実施例12と同様に行い、シート状の多孔質吸音材を得た。
架橋剤、架橋促進剤及び発泡剤の使用量を表2の使用量に変更したこと以外は実施例12と同様に行い、シート状の多孔質吸音材を得た。
発泡前の発泡組成物(混練物)を次の手順で得たこと以外は実施例12と同様に行い、シート状の多孔質吸音材を得た。すなわち、ロール温度40℃のミキシングロール(7インチ、回転数:25rpm)を用いてCR(ベース材料)100質量部を5分間素練りした。その後、このCRに対して、炭酸カルシウムを20質量部、充填剤用酸化亜鉛を1質量部、ステアリン酸(加工助剤)を3質量部添加した後に15分間混練した。次いで、回転数を40rpmに変更した上で(以降の混練操作も同様の回転数)、プロセスオイル(軟化剤)を60質量部添加した後に20分間混練した。続いて、ロール温度を80℃に上げることにより熱入れを3分間行った。そして、ロール温度を40℃に下げた後、架橋剤用酸化亜鉛(架橋剤)を5質量部、アゾジカルボンアミド(発泡剤)を17質量部、尿素(発泡助剤)を1.5質量部添加した後に20分間混錬することにより発泡前の発泡組成物(混練物)を得た。
架橋剤の使用量を表2の使用量に変更したこと以外は実施例19と同様に行い、シート状の多孔質吸音材を得た。
架橋促進剤の使用量を表3の使用量に変更したこと以外は実施例12と同様に行い、シート状の多孔質吸音材を得た。
架橋促進剤及び発泡剤の使用量を表3の使用量に変更したこと以外は実施例12と同様に行い、シート状の多孔質吸音材を得た。
発泡剤の使用量を表3の使用量に変更したこと以外は実施例19と同様に行い、シート状の多孔質吸音材を得た。
架橋剤及び発泡剤の使用量を表3の使用量に変更したこと以外は実施例19と同様に行い、シート状の多孔質吸音材を得た。
LDPE(ベース材料)100質量部、センダストC(金属フィラー)30質量部、炭酸カルシウム10質量部、充填剤用酸化亜鉛0.2質量部、ステアリン酸(加工助剤)5質量部、ジクミルパーオキサイド(架橋剤)0.7質量部、アゾジカルボンアミド(発泡剤)10質量部、及び、尿素(発泡助剤)1質量部をドライブレンドして混合物を得た後、ニーダーを用いて当該混合物を15分間溶融混練することにより発泡前の発泡性組成物(不定形)を得た。
金属フィラーとしてセンダストAを用いたこと以外は実施例22と同様に行い、シート状の多孔質吸音材を得た。
金属フィラーとしてセンダストBを用いたこと以外は実施例22と同様に行い、シート状の多孔質吸音材を得た。
金属フィラーとしてセンダストAを用いると共に金属フィラーの使用量を表4の使用量に変更したこと以外は実施例22と同様に行い、シート状の多孔質吸音材を得た。
金属フィラーとして鉄合金粉末を用いたこと以外は実施例22と同様に行い、シート状の多孔質吸音材を得た。
金属フィラーとしてタングステン合金粉末を用いたこと以外は実施例22と同様に行い、シート状の多孔質吸音材を得た。
LDPE(ベース材料)100質量部、炭酸カルシウム10質量部、充填剤用酸化亜鉛0.2質量部、ステアリン酸(加工助剤)5質量部、ジクミルパーオキサイド(架橋剤)0.7質量部、アゾジカルボンアミド(発泡剤)2.5質量部、及び、尿素(発泡助剤)1質量部をドライブレンドして混合物を得た後、ニーダーを用いて当該混合物を15分間溶融混練することにより発泡前の発泡性組成物(不定形)を得た。
発泡剤の使用量を表5の使用量に変更したこと以外は実施例29と同様に行い、シート状の多孔質吸音材を得た。
気泡の連通化の回数を5回に変更し、スライス加工を行って表5の厚さに仕上げること以外は実施例30と同様に行い、シート状の多孔質吸音材を得た。
炭酸カルシウム及び発泡剤の使用量を表6の使用量に変更したこと以外は実施例29と同様に行い、シート状の多孔質吸音材を得た。
下記に示す方法で多孔質吸音材(発泡体)の物性を評価した。結果を表1〜表6に示す。
多孔質吸音材の発泡倍率を次の手順で測定した。具体的には、発泡させる前の発泡性組成物から厚さ1cm、縦5cm、横5cmの大きさの試験片を切り出した後、その試験片の質量を計測して発泡前の密度を求めた。そして、後述する多孔質吸音材の見かけ密度(発泡後の密度)で前述の発泡前の密度を除することにより発泡倍率を算出した。
多孔質吸音材のセル径の平均値を測定した。具体的には、卓上走査電子顕微鏡(JCM6000Plusネオスコープ、日本電子株式会社製)を用いて、多孔質吸音材の一つの気泡部の画像を取り込み、その画像を画像解析ソフト(Mac−View、株式会社マウンテック製)に基づいて画像解析(円相当径への換算)することによりセル径(μm)を算出した。多孔質吸音材の100個の気泡部のセル径を取得した後、100個のセル径の算術平均値を平均セル径(μm)として求めた。
多孔質吸音材の見掛け密度をJIS K 6767(1999)「発泡プラスチック−ポリエチレン−試験方法」に準じて測定した。具体的には、多孔質吸音材の厚さを10mmに調整した後、縦5cm、横5cmの板状の試験片を切り出した後、その試験片の質量を測定して、単位体積あたりの質量(見掛け密度)を算出した。
多孔質吸音材の通気度(cm3/cm2・s)を次の手順で測定した。具体的には、JIS L 1096(2010)「織物及び編物の生地試験方法」のA法に従い、フラジール形通気度試験機(フラジールパーミヤメーター、株式会社東洋精機製作所製)を用いて5mm厚のサンプルの通気度を測定した。
ISO 1923(1981)「発泡プラスチック及びゴム−線寸法の測定」に準じて多孔質吸音材の厚さを測定した。具体的には、測定面積が約10cm2となるダイヤルゲージを用いて多孔質吸音材の厚さを測定した。
JIS A 1405:1998「音響−インピーダンス管による吸音率及びインピーダンスの測定−定在波比法」記載の方法により吸音率を測定した。プローブチューブマイクロホンを備える垂直入射吸音率測定器(TYPE10041、電子測器株式会社製)を用いて500Hz及び1000Hzの吸音率を測定した。具体的には、多孔質吸音材を直径29mmに調整して試験片を得た後、当該試験片を試料ホルダーの背面板に密着させて測定した。吸音率の値が高いほど、音を吸収する特性が良好であることを示し、吸音率が0.6以上である場合を「A」と評価し、吸音率が0.4以上0.6未満である場合を「B」と評価し、吸音率が0.4未満である場合を「C」と評価した。
Claims (7)
- 平均セル径が100〜600μmであり、見かけ密度が40〜140kg/m3である、多孔質吸音材。
- 通気度が0.1〜40cm3/cm2・sである、請求項1に記載の多孔質吸音材。
- 厚さ15〜40mmのシート状である、請求項1又は2に記載の多孔質吸音材。
- 樹脂材料及びエラストマーからなる群より選ばれる少なくとも一種のベース材料と、金属フィラーと、を含有し、
前記金属フィラーの含有量が前記ベース材料100質量部に対して5〜50質量部であり、
前記金属フィラーの比重が4〜10であり、
前記金属フィラーの平均粒子径が5〜30μmである、請求項1〜3のいずれか一項に記載の多孔質吸音材。 - 請求項1〜4のいずれか一項に記載の多孔質吸音材を用いて吸音する、吸音方法。
- 1000Hz以下の音を吸音する、請求項5に記載の吸音方法。
- 請求項1〜4のいずれか一項に記載の多孔質吸音材の製造方法であって、
樹脂材料及びエラストマーからなる群より選ばれる少なくとも一種と、発泡剤と、を含有する発泡性組成物を発泡させることにより発泡体を得た後、当該発泡体を圧縮することにより、前記発泡体中に含まれる独立セルの一部又は全部を連通させて連続セルを得る、多孔質吸音材の製造方法。
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