JP6833675B2 - ゴム用組成物及びその用途 - Google Patents
ゴム用組成物及びその用途 Download PDFInfo
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- JP6833675B2 JP6833675B2 JP2017512207A JP2017512207A JP6833675B2 JP 6833675 B2 JP6833675 B2 JP 6833675B2 JP 2017512207 A JP2017512207 A JP 2017512207A JP 2017512207 A JP2017512207 A JP 2017512207A JP 6833675 B2 JP6833675 B2 JP 6833675B2
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- chloroprene
- butadiene
- rubber
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Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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- A—HUMAN NECESSITIES
- A41—WEARING APPAREL
- A41D—OUTERWEAR; PROTECTIVE GARMENTS; ACCESSORIES
- A41D19/00—Gloves
- A41D19/0055—Plastic or rubber gloves
- A41D19/0058—Three-dimensional gloves
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61B—DIAGNOSIS; SURGERY; IDENTIFICATION
- A61B42/00—Surgical gloves; Finger-stalls specially adapted for surgery; Devices for handling or treatment thereof
- A61B42/10—Surgical gloves
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C41/00—Shaping by coating a mould, core or other substrate, i.e. by depositing material and stripping-off the shaped article; Apparatus therefor
- B29C41/02—Shaping by coating a mould, core or other substrate, i.e. by depositing material and stripping-off the shaped article; Apparatus therefor for making articles of definite length, i.e. discrete articles
- B29C41/14—Dipping a core
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/0008—Organic ingredients according to more than one of the "one dot" groups of C08K5/01 - C08K5/59
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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Description
外科手術用手袋に、クロロプレン系重合体ラテックスを使用して柔軟性を改良する方法が提案されている(例えば、特開2007−106994;特許文献1、特表2009−501833(欧州特許第1904569号);特許文献2)。
[1] クロロプレン系重合体ラテックス(A)、金属酸化物(B)、酸化防止剤(C)、界面活性剤(D)及びpH調整剤(E)を含み、加硫促進剤を含まない組成物であって、前記(A)に含まれるクロロプレン系重合体中のテトラハイドロフラン不溶分量が50〜85質量%であり、前記(A)の固形分100質量部に対して、(B)を1〜10質量部、(C)を0.1〜5質量部、(D)を0.1〜10質量部、(E)を0.01〜5質量部の割合で含むゴム用組成物。
[2] クロロプレン系重合体ラテックス(A)、金属酸化物(B)、酸化防止剤(C)、界面活性剤(D)及びpH調整剤(E)からなる組成物である前項1に記載のゴム用組成物。
[3] 前記クロロプレン系重合体ラテックス(A)に含まれる重合体が、2−クロロ−1,3−ブタジエン(クロロプレン)(A−1)と2,3−ジクロロ−1,3−ブタジエン(A−2)とを含む単量体からなる共重合体であって、単量体の割合が前記2−クロロ−1,3−ブタジエン(クロロプレン)(A−1)と前記2,3−ジクロロ−1,3−ブタジエン(A−2)との合計100質量%に対して、2−クロロ−1,3−ブタジエン(クロロプレン)(A−1)76〜93質量%及び2,3−ジクロロ−1,3−ブタジエン(A−2)24〜7質量%である前項1または2に記載のゴム用組成物。
[4] 前記クロロプレン系重合体ラテックス(A)に含まれる重合体が、2−クロロ−1,3−ブタジエン(クロロプレン)(A−1)及び2,3−ジクロロ−1,3−ブタジエン(A−2)に加えてさらにこれらと共重合可能な単量体(A−3)からなる共重合体であって、前記単量体(A−3)の含有量が、前記2−クロロ−1,3−ブタジエン(クロロプレン)(A−1)と前記2,3−ジクロロ−1,3−ブタジエン(A−2)との合計100質量部に対して0.1〜10質量部である前項3に記載のゴム用組成物。
[5] 前項1〜4のいずれかに記載のゴム用組成物を用いて得られる成形物。
[6] 300%弾性率(モデュラス)が0.5〜1.2MPa、引張強度が17MPa以上、引張破断伸びが800%以上、変形率が20%以下である前項5に記載の成形物。
[7] 前項1〜4のいずれかに記載のゴム用組成物を用いて得られるゴム製浸漬製品。
[8] 前記ゴム製浸漬製品が手袋である前項7に記載のゴム製浸漬製品。
[9] 前記手袋が医療用使い捨て手袋である前項8に記載のゴム製浸漬製品。
本発明に係るゴム用組成物としては、クロロプレン系重合体ラテックス(A)、金属酸化物(B)、酸化防止剤(C)、界面活性剤(D)及びpH調整剤(E)からなるものが好ましい。
テトラハイドロフラン不溶分量を上記の範囲にすることにより、加硫促進剤が含まれないことに伴う引張強さ等の機械物性不足を十分改善することができる。
クロロプレン系重合体ラテックス(A)の重合転化率が80〜95%となる範囲で、連鎖移動剤の量を調整することによって、テトラハイドロフラン不溶分量を50〜85質量%に容易にコントロールすることができる。
従来からクロロプレン系重合体ラテックスの加硫に一般に用いられている加硫促進剤は、チウラム系、ジチオカーバメート系、チオウレア系、グアニジン系の加硫促進剤である。チウラム系の加硫促進剤としては、テトラエチルチウラムジスルフィド、テトラブチルチウラムジスルフィドなどが挙げられる。ジチオカーバメート系の加硫促進剤としては、ジブチルチオジカルバミン酸ナトリウム、ジブチルチオジカルバミン酸亜鉛、ジエチルチオジカルバミン酸亜鉛などが挙げられる。チオウレア系の加硫促進剤としては、エチレンチオウレア、ジエチルチオウレア、トリメチルチオウレア、N,N’−ジフェニルチオウレアなどが挙げられる。グアニジン系の加硫促進剤としては、ジフェニルグアニジン、ジオルトトルイルグアニジンなどが挙げられる。また加硫促進剤は上記に挙げたものの2種以上を併用することもあるが、本発明ではこれらの加硫促進剤は一切使用しない。
重合後のエマルジョンを採集し、100℃、2時間乾燥後の固形分から、重合転化率を計算した。
なお、固形分及び重合転化率は下記式にて求めた。
固形分[質量%]
=[(100℃、2時間乾燥後の重量)/(乾燥前のラテックス重量)]×100
重合転化率[%]=[(ポリマー生成量/モノマー仕込み量)]×100」
ここで、ポリマー生成量は、重合後固形分からポリマー以外の固形分を差し引いて求めた。
下記方法にてクロロプレン系重合体ラテックスの物性を評価した。
[測定法]
テトラハイドロフラン不溶分量:
ラテックス1gをTHF(テトラハイドロフラン)溶剤100mlに滴下して、1晩振とうした後、遠心分離機にて上澄みの溶解相を分離し、100℃、1時間かけて溶剤を蒸発・乾固させて、溶解分量を計算し、差引き、テトラハイドロフラン不溶分量を評価した。
重合後のエマルジョン中の残留2−クロロ−1,3−ブタジエン(クロロプレン)単量体及び2,3−ジクロロ−1,3−ブタジエン単量体をガスクロマトグラフによって分析し、仕込み各単量体量から差し引くことによって、ポリマー中の共重合組成を計算した。
スリーワンモーター付きの撹拌槽に上記配合物を仕込み、30分撹拌した。
重合体フィルムの作製:
下記方法にてクロロプレン系重合体ラテックスなどを配合したゴム用組成物から浸漬フィルムを作製した。
凝固、リーチング、乾燥:
25%硝酸カルシウム水溶液を凝固液として、浸漬フィルムを得た後、70℃温水中で、2分間リーチング(浸出)を行い、水溶性成分を除去した。次いで70℃、30分乾燥した。
架橋:
常法のオーブンにて、130℃で、60分加熱し、架橋を行った。
架橋後のシートを評価項目に応じて適宜、切断し、試験片を得た。この試験片を用いて、以下の物性評価を行った。
引張試験:
常態及び熱老化(100℃、22時間)後の引張試験はJIS−K6301に準じた方法で行った。本試験により、室温における300%・500%伸張時のモデュラス、引張強さ、破断伸び及び表面硬度(JIS−A)を測定した。
変形率:
室温において、架橋フィルムから、幅6mm、長さ100mmの短冊状の試験片を抜き出し、10mm幅の標線間を伸び300%まで、引張り、10分間保持した後、解放し、10分後に、標線間の伸びを測定して、初期標線位置からの変位比率として変形率を計算した。
柔軟性の経時安定性:
促進試験として、架橋後のフィルムの低温(−10℃、50日)及び高温(70℃、7日)での貯蔵後の弾性率(モデュラス)をそれぞれ評価した。
内容積60リットルの反応器を使用して、2−クロロ−1,3−ブタジエン(クロロプレン)18.2kg、2,3−ジクロロ−1,3−ブタジエン1.8kg及び純水18kg、不均化ロジン酸(荒川化学工業(株)製、R−300)860g、n−ドデシルメルカプタン2.0g、水酸化カリウム240g、β−ナフタレンスルホン酸ホルマリン縮合物のナトリウム塩160gを仕込み、乳化させ、不均化ロジン酸をロジン石鹸にした後、過硫酸カリウムを開始剤として用い、窒素雰囲気下、40℃で重合を行った。重合転化率が88.1%に達したところで、直ちにフェノチアジンの乳濁液を添加して重合を停止した。次いでその後、未反応の単量体を水蒸気蒸留にて除去し、クロロプレン系重合体のポリマーラテックスを得た。
上記の製造例の方法で得られたクロロプレン系重合体ラテックスを、表1に記載する配合比にて配合物とし、浸漬架橋フィルムを作製した。
上記の製造例において、2,3−ジクロロ−1,3−ブタジエン量、n−ドデシルメルカプタン量、重合転化率を変更したこと以外は実施例1と同様にして、重合を行い、実施例2〜5及び比較例1〜2で使用するクロロプレン系重合体ラテックスを得た。得られたクロロプレン系重合体ラテックスを、表1に記載する配合比にて配合物とし、浸漬架橋フィルムを作製した。
上記の製造例において、2,3−ジクロロ−1,3−ブタジエン量、n−ドデシルメルカプタン量、重合転化率を変更したこと以外は実施例1と同様にして、重合を行い、比較例3〜5で使用する重合体ラテックスを得た。得られたクロロプレン系重合体ラテックスを、下記表2に記載する配合比にて配合物とし、浸漬架橋フィルムを作製した。
また、表3の結果から、比較例1〜2の配合比によって得られた成形物の引張強度は、手術用手袋としては不十分である。
Claims (7)
- クロロプレン系重合体ラテックス(A)、金属酸化物(B)、酸化防止剤(C)、界面活性剤(D)及びpH調整剤(E)を含み、加硫促進剤を含まない組成物であって、前記(A)に含まれるクロロプレン系重合体中のテトラハイドロフラン不溶分量が50〜85質量%であり、前記(A)の固形分100質量部に対して、(B)を1〜10質量部、(C)を0.1〜5質量部、(D)を0.1〜10質量部、(E)を0.01〜5質量部の割合で含み、
前記クロロプレン系重合体ラテックス(A)に含まれる重合体が、単量体が2−クロロ−1,3−ブタジエン(クロロプレン)(A−1)と2,3−ジクロロ−1,3−ブタジエン(A−2)とのみからなる共重合体のみであって、単量体の割合が前記2−クロロ−1,3−ブタジエン(クロロプレン)(A−1)と前記2,3−ジクロロ−1,3−ブタジエン(A−2)との合計100質量%に対して、2−クロロ−1,3−ブタジエン(クロロプレン)(A−1)76〜93質量%及び2,3−ジクロロ−1,3−ブタジエン(A−2)24〜7質量%であるゴム用組成物。 - クロロプレン系重合体ラテックス(A)、金属酸化物(B)、酸化防止剤(C)、界面活性剤(D)及びpH調整剤(E)からなる組成物である請求項1に記載のゴム用組成物。
- 請求項1または2に記載のゴム用組成物を用いて得られる成形物。
- 300%弾性率(モデュラス)が0.5〜1.2MPa、引張強度が17MPa以上、引張破断伸びが800%以上、変形率が20%以下である請求項3に記載の成形物。
- 請求項1または2に記載のゴム用組成物を用いて得られるゴム製浸漬製品。
- 前記ゴム製浸漬製品が手袋である請求項5に記載のゴム製浸漬製品。
- 前記手袋が医療用使い捨て手袋である請求項6に記載のゴム製浸漬製品。
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EP4130079A4 (en) | 2020-03-26 | 2024-02-07 | Denka Company Limited | CHLOROPRENE-BASED BLOCK COPOLYMER LATEX |
CN113715385A (zh) * | 2021-08-31 | 2021-11-30 | 江苏凯瑞斯安全防护用品有限公司 | 一种医用防辐射手套的生产工艺 |
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JP2007106994A (ja) * | 2005-09-15 | 2007-04-26 | Showa Denko Kk | クロロプレン系重合体ラテックス及びその製造方法 |
JP4860252B2 (ja) | 2005-12-01 | 2012-01-25 | 日本エイアンドエル株式会社 | ディップ成形用組成物およびディップ成形品 |
JP2011122141A (ja) * | 2009-11-10 | 2011-06-23 | Showa Denko Kk | クロロプレン系重合体ラテックス及びその製造方法 |
PL2507313T3 (pl) * | 2009-12-01 | 2018-09-28 | Kossan Sdn Bhd | Elastomerowa guma i produkty z gumy uzyskiwane bez stosowania przyspieszaczy wulkanizacji i siarki |
AU2011270682B2 (en) * | 2010-06-25 | 2015-10-08 | Allegiance Corporation | Vulcanization composition having reduced allergenic potential |
CN103459444B (zh) * | 2011-04-06 | 2016-03-23 | 电化株式会社 | 聚氯丁二烯胶乳、橡胶组合物及浸渍成型品 |
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EP2824121B1 (en) * | 2012-03-02 | 2018-06-20 | Denka Company Limited | Polychloroprene latex, polychloroprene latex composition, and molded article |
EP2960293B1 (en) | 2013-02-22 | 2018-12-05 | Zeon Corporation | Latex for dip molding use, composition for dip molding use, and dip-molded article |
US9840600B2 (en) * | 2015-03-30 | 2017-12-12 | Kraton Polymers U.S. Llc | Diene rubber composition configured to be vulcanized at lower temperature; and manufacturing process of rubber article from the same |
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JP7128876B2 (ja) | 2022-08-31 |
CN107429001A (zh) | 2017-12-01 |
AU2016248518B2 (en) | 2018-08-30 |
KR101911303B1 (ko) | 2018-10-24 |
EP3284781B1 (en) | 2020-10-28 |
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EP3284781A4 (en) | 2018-12-05 |
US20180112055A1 (en) | 2018-04-26 |
EP3284781A1 (en) | 2018-02-21 |
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