TWI834844B - 熱可塑性彈性體組成物及其成形體 - Google Patents
熱可塑性彈性體組成物及其成形體 Download PDFInfo
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- TWI834844B TWI834844B TW109108741A TW109108741A TWI834844B TW I834844 B TWI834844 B TW I834844B TW 109108741 A TW109108741 A TW 109108741A TW 109108741 A TW109108741 A TW 109108741A TW I834844 B TWI834844 B TW I834844B
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- thermoplastic elastomer
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- elastomer composition
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- ethylene
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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
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L91/00—Compositions of oils, fats or waxes; Compositions of derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/04—Homopolymers or copolymers of ethene
- C08L23/08—Copolymers of ethene
- C08L23/0807—Copolymers of ethene with unsaturated hydrocarbons only containing more than three carbon atoms
- C08L23/0815—Copolymers of ethene with aliphatic 1-olefins
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/10—Homopolymers or copolymers of propene
- C08L23/12—Polypropene
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B27/08—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/18—Layered products comprising a layer of synthetic resin characterised by the use of special additives
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Abstract
本發明之課題在於提供耐熱老化性優越、硬度及機械特性亦優越、且成物性亦優良的熱可塑性彈性體組成物。
本發明之解決手段為一種熱可塑性彈性體組成物(I),係含有交聯體,該交聯體係乙烯‧α-烯烴‧非共軛多烯共聚合體(A)之經由酚樹脂系交聯劑(E)所得者;且含有結晶性聚烯烴(B)360~460質量份、軟化劑(C)70~140質量份、及滑劑(D)2~6質量份(其中,將上述共聚合體(A)之量設為100質量份)。
Description
本發明係關於熱可塑性彈性體組成物及其成形體。
作為包含含有橡膠成分、樹脂成分等之熱可塑性彈性體材料的成形體,已知有於構成成形體之基體之表面(例如需要滑動性之部位)形成了具有滑動性之被覆體的多層構造者。作為此種多層構造之成形體的例子,可舉例如汽車之窗導槽密封條。
對於汽車之窗導槽密封條的具滑動性之被覆體所使用的材料,係要求均衡佳地具有各種特性。作為此種特性,尤其可舉例如耐油性、高溫下之滲油少(以下亦稱為「耐熱老化性」)、硬度、機械強度等。
關於此耐熱老化性,已知下述見解:在將由含有軟化劑之材料所構成之上述被覆體積層於包含含有軟化劑之材料之上述基體(窗導槽密封條本體)時,由於被覆體中之軟化劑之濃度與基體中之軟化劑之濃度的差,導致軟化劑(油)移行而發生滲出現象。
專利文獻1中,嘗試了藉由改造積體層之構成,具體而言係作成為「油性軟化劑(油)相對於表層材料(滑動材料)中之非晶成分量的比例≧油性軟化劑相對於下層材料中之非晶成分量的比例」,以改良耐熱老化性(抑制曝露於高溫時之表面之黏瘩發生)。作為構成表層材料及下層材料之熱可塑性彈性體,記載有將聚烯烴樹脂10~60重量份、乙烯‧α-烯烴‧非共軛多烯共聚合體30~70重量份、及油性軟化劑5~50
重量份(將此等之合計設為100重量份)於交聯劑存在下動態地進行熱處理者。
再者,於專利文獻2所揭示之基體之表面形成了被覆體的多層構造彈性體成形體中,將「被覆體中之軟化劑(油)之比例/基體中之軟化劑之比例設為0.00以上且未滿0.30」。於實施例之被覆體材料中,相對於EPDM100phr,調配聚丙烯200phr。又,此文獻中並未記載成形體之強度等。
又,專利文獻3揭示有對經完全或部分交聯之熱可塑性彈性體,調配了聚丙烯、填充材、脂肪酸醯胺等之表皮構件用聚丙烯樹脂組成物。又,此文獻中並未記載由組成物所形成之成形體的硬度、機械強度等。
專利文獻1:日本專利特開2001-138440號公報
專利文獻2:日本專利特開2016-000485號公報
專利文獻3:日本專利特開平9-176408號公報
然而,習知之滑動性熱可塑性彈性體組成物及其成形體係於各特性方面仍有進一步改善之空間。例如,於專利文獻1之表層材料中,若油性軟化劑較多則難以提升硬度。
本發明之目的在於提供耐熱老化性優越、硬度及機械物性(拉伸彈性係數、拉伸破斷強度)優越、且成形性亦優越的熱可塑性
彈性體組成物,以及使用其之成形體等。
[1]一種熱可塑性彈性體組成物(I),係含有交聯體,該交聯體係乙烯‧α-烯烴‧非共軛多烯共聚合體(A)(其中,α-烯烴之碳數為3~20)之經由酚樹脂系交聯劑(E)所得者;且上述熱可塑性彈性體組成物(I)含有:結晶性聚烯烴(B)360~460質量份、軟化劑(C)70~140質量份、及滑劑(D)2~6質量份(其中,將上述共聚合體(A)之量設為100質量份)。
[2]如上述[1]之熱可塑性彈性體組成物(I),其中,上述乙烯‧α-烯烴‧非共軛多烯共聚合體(A)係滿足下述要件(a1);要件(a1):來自乙烯之構造單位(e)相對於來自α-烯烴之構造單位(o)的莫耳比[(e)/(o)]為50/50~85/15。
[3]如上述[1]或[2]之熱可塑性彈性體組成物(I),其中,上述結晶性聚烯烴(B)藉示差掃描熱量分析所測定的融點為150~170℃。
[4]如上述[1]至[3]中任一項之熱可塑性彈性體組成物(I),其中,上述結晶性聚烯烴(B)為丙烯系聚合體。
[5]如上述[1]至[4]中任一項之熱可塑性彈性體組成物(I),其中,上述軟化劑(C)為石蠟油。
[6]如上述[1]至[5]中任一項之熱可塑性彈性體組成物(I),其中,上述滑劑(D)為芥酸醯胺。
[7]如上述[1]至[6]中任一項之熱可塑性彈性體組成物(I),其係將上述乙烯‧α-烯烴‧非共軛多烯共聚合體(A)、與上述結晶
性聚烯烴(B)之至少一部分,於上述酚樹脂系交聯劑(E)之存在下進行動態熱處理所得者。
[8]如上述[1]至[7]中任一項之熱可塑性彈性體組成物(I),其中,上述酚樹脂系交聯劑(E)之量相對於上述共聚合體(A)100質量份係為2~9質量份。
[9]一種成形體,係含有上述[1]至[8]中任一項之熱可塑性彈性體組成物(I)。
[10]一種積層體,係將含有上述[1]至[8]中任一項之熱可塑性彈性體組成物(I)之層與含有軟質材料之層進行積層而成。
[11]如上述[10]之積層體,其中,上述軟質材料之硬度(A硬度)為65~95。
[12]如上述[11]之積層體,其中,上述軟質材料係含有熱可塑性彈性體。
[13]如上述[12]之積層體,其中,上述軟質材料係含有包含熱可塑性彈性體之熱可塑性彈性體組成物(II);上述組成物(II)含有軟化劑;上述軟化劑於上述組成物(II)中所佔之質量分率(W2c)為30~50質量%。
[14]如上述[13]之積層體,其中,上述軟化劑(C)於上述熱可塑性彈性體組成物(I)中所佔之質量分率(W1c)相對於上述軟化劑於上述熱可塑性彈性體組成物(II)中所佔之質量分率(W2c)的比(W1c/W2c)為0.60以下。
[15]一種物品,係含有上述[10]至[14]中任一項之積層體。
[16]如上述[15]之物品,其係窗框封條、窗導槽密封條
或建材用墊片。
本發明之熱可塑性彈性體組成物係耐熱老化性優越、硬度及機械物性(拉伸彈性係數、拉伸破斷強度)優越、且成形性亦優越。
又,本發明之成形體及積層體係耐熱老化性優越、硬度及機械物性(拉伸彈性係數、拉伸破斷強度)亦優越。
本發明之熱可塑性彈性體組成物(I)的特徵在於含有:將乙烯‧α-烯烴‧非共軛多烯共聚合體(A)或含有上述共聚合體(A)之混合物,於可將上述共聚合體(A)進行交聯之酚樹脂系交聯劑(E)的存在下,進行動態熱處理而得的熱處理物(上述共聚合體(A)經由上述交聯劑(E)所得的交聯體);且含有結晶性聚烯烴(B)、軟化劑(C)及滑劑(D)。
<乙烯‧α-烯烴‧非共軛多烯共聚合體(A)>
本發明所使用之乙烯‧α-烯烴‧非共軛多烯共聚合體(A)(以下亦記載為「共聚合體(A)」),係含有來自乙烯之構造單位、至少1種之來自碳數3~20之α-烯烴的構造單位、及至少1種之來自非共軛多烯的構造單位的乙烯‧α-烯烴‧非共軛多烯共聚合體。
作為碳數3~20之α-烯烴,可舉例如丙烯(碳數3)、1-丁烯(碳數4)、1-壬烯(碳數9)、1-癸烯(碳數10)、1-十九烯(碳數19)、1-二十烯(碳數20)等之無側鏈之直鏈狀α-烯烴;4-甲基-1-戊烯、9-甲
基-1-癸烯、11-甲基-1-十二烯、12-乙基-1-十四烯等之具側鏈的α-烯烴等。此等α-烯烴可單獨使用1種或組合2種以上使用。此等之中,由耐熱性的觀點而言,較佳為丙烯。
作為非共軛多烯,可舉例如1,4-己二烯、1,6-辛二烯、2-甲基-1,5-己二烯、6-甲基-1,5-庚二烯、7-甲基-1,6-辛二烯等之鏈狀非共軛二烯;環己二烯、二環戊二烯、甲基四氫茚、5-乙烯基-2-降烯、5-亞乙基-2-降烯、5-亞甲基-2-降烯、5-異亞丙基-2-降烯、6-氯甲基-5-異丙烯基-2-降烯等之環狀非共軛二烯;2,3-二異亞丙基-5-降烯、2-亞乙基-3-異亞丙基-5-降烯、2-丙烯基-2,5-降二烯、1,3,7-辛三烯、1,4,9-癸三烯、4,8-二甲基-1,4,8-癸三烯、4-亞乙基-8-甲基-1,7-壬二烯等之三烯等。此等非共軛多烯可單獨使用1種或組合2種以上使用。此等之中,較佳為1,4-己二烯等環狀非共軛二烯、5-亞乙基-2-降烯、5-乙烯基-2-降烯、5-亞乙基-2-降烯及5-乙烯基-2-降烯的混合物,更佳為5-亞乙基-2-降烯、5-乙烯基-2-降烯。
作為共聚合體(A),可舉例如乙烯‧丙烯‧1,4-己二烯共聚合體、乙烯‧1-戊烯‧1,4-己二烯共聚合體、乙烯‧1-己烯‧1,4-己二烯共聚合體、乙烯‧1-庚烯‧1,4-己二烯共聚合體、乙烯‧1-辛烯‧1,4-己二烯共聚合體、乙烯‧1-壬烯‧1,4-己二烯共聚合體、乙烯‧1-癸烯‧1,4-己二烯共聚合體、乙烯‧丙烯‧1-辛烯‧1,4-己二烯共聚合體、乙烯‧丙烯‧5-亞乙基-2-降烯共聚合體、乙烯‧1-戊烯‧5-亞乙基-2-降烯共聚合體、乙烯‧1-己烯‧5-亞乙基-2-降烯共聚合體、乙烯‧1-庚烯‧5-亞乙基-2-降烯共聚合體、乙烯‧1-辛烯‧5-亞乙基-2-降烯共聚合體、乙烯‧1-壬烯‧5-亞乙基-2-降烯共聚合體、乙烯‧1-癸烯‧5-亞乙基-2-降烯共聚合體、乙烯‧丙烯‧1-辛烯‧5-亞乙基-2-降
烯共聚合體、乙烯‧丙烯‧5-亞乙基-2-降烯‧5-乙烯基-2-降烯共聚合體、乙烯‧1-戊烯‧5-亞乙基-2-降烯‧5-乙烯基-2-降烯共聚合體、乙烯‧1-己烯‧5-亞乙基-2-降烯‧5-乙烯基-2-降烯共聚合體、乙烯‧1-庚烯‧5-亞乙基-2-降烯‧5-乙烯基-2-降烯共聚合體、乙烯‧1-辛烯‧5-亞乙基-2-降烯‧5-乙烯基-2-降烯共聚合體、乙烯‧1-壬烯‧5-亞乙基-2-降烯‧5-乙烯基-2-降烯共聚合體、乙烯‧1-癸烯‧5-亞乙基-2-降烯‧5-乙烯基-2-降烯共聚合體、乙烯‧丙烯‧1-辛烯‧5-亞乙基-2-降烯‧5-乙烯基-2-降烯共聚合體等。
共聚合體(A)可單獨使用1種或組合2種以上使用。
共聚合體(A)較佳係滿足下述要件(a1)。更佳係進一步滿足要件(a2),再更佳係連同要件(a1)及(a2)同時滿足要件(a3)。
要件(a1):來自乙烯之構造單位(e)相對於來自α-烯烴之構造單位(o)的莫耳比[(e)/(o)]為50/50~85/15、較佳60/40~80/20。
要件(a2):來自非共軛多烯之構造單位於共聚合體(A)之總構成單位中所佔的比例為0.5~6.0莫耳%。
要件(a3):於135℃十氫萘中所測定之極限黏度[η]為1.0~10dL/g、較佳1.5~8dL/g。
(共聚合體(A)之製造方法)
共聚合體(A)例如可依國際公開第2018/181121號之[0028]~[0145]記載之方法進行製造。
<結晶性聚烯烴(B)>
結晶性聚烯烴(B)若為由烯烴所得之結晶性聚合體則無特別限制,較佳係由將1種以上之單烯烴藉由高壓法或低壓法之任一種進行聚合所得的結晶性之高分子量固體生成物所構成的聚合體。作為此種聚合體,可舉例如同排單烯烴聚合體、對排單烯烴聚合體等。
結晶性聚烯烴(B)可依習知公知之方法進行合成而得,亦可使用市售物。
結晶性聚烯烴(B)可單獨使用1種或組合2種以上使用。
作為成為結晶性聚烯烴(B)之原料的烯烴之例子,可舉例如乙烯、丙烯、1-丁烯、1-戊烯、1-己烯、1-辛烯、1-癸烯、2-甲基-1-丙烯、3-甲基-1-戊烯、4-甲基-1-戊烯、5-甲基-1-己烯等之碳數2~20之α-烯烴(丙烯除外)。此等可單獨使用1種或併用2種以上。
結晶性聚烯烴(B)中,由耐熱性、耐油性的觀點而言,較佳係屬於由以丙烯為主之烯烴所得之丙烯均聚物或丙烯共聚合體的丙烯系(共)聚合體;由拉伸破斷強度之觀點而言,更佳為丙烯均聚物。又,於丙烯共聚合體的情況,來自丙烯之構造單位之含量較佳為40莫耳%以上、更佳50莫耳%以上,作為成為來自丙烯以外之單體的構造單位的烯烴,較佳係碳數2~20之α-烯烴(丙烯除外)、更佳為乙烯、丁烯。
聚合樣式可為無規型或嵌段型。
結晶性聚烯烴(B)之熔融流動速率(MFR)(ASTM D1238-65T、230℃、2.16kg負重),通常為0.01~100g/10分、較佳0.05~50g/10分,由彈性係數之觀點而言,較佳為0.1~9.0g/10分、更佳0.1~6.0g/10分。
結晶性聚烯烴(B)之藉示差掃描熱量分析(DSC)所得的融點(Tm)通常為100℃以上、較佳105℃以上、更佳150~170℃。若融點為此範圍,可表現適合本發明目的之物性(硬度、機械物性及成形性)。
此融點之值係依以下條件進行測定者。
<測定條件>
將試料5mg左右填裝於專用鋁盤,使用Perkin Elmer(股)公司製DSCPyrisl或DSC7,由30℃依320℃/分升溫至200℃,依200℃保持5分鐘後,由200℃依10℃/分降溫至30℃,再依30℃保持5分鐘,接著由依10℃/分進行升溫時之吸熱曲線求得融點。又,於DSC測定時,在檢測到複數波峰時,將於最高溫側所檢測到之波長溫度定義為融點(Tm)。
結晶性聚烯烴(B)係發揮使熱可塑性彈性體組成物之流動性及耐熱性提升的功能。
結晶性聚烯烴(B)係相對於共聚合體(A)100質量份,通常依360~460質量份、較佳370~440質量份、更佳370~420質量份之比例使用。另一方面,結晶性聚烯烴(B)之量若大幅少於上述範圍,則熱可塑性彈性體組成物或其成形體之硬度低;若大幅超過上述範圍,則熱可塑性彈性體組成物之成形性(擠出加工性)劣化。
<軟化劑(C)>
作為軟化劑(C),可使用通常橡膠所使用的軟化劑。作為軟化劑(C),可舉例如:加工處理油、潤滑油、石蠟油、液態石蠟、石油瀝青、凡士林等石油系軟化劑;煤焦油、煤焦瀝青等煤焦油系軟化劑;篦麻油、亞麻仁油、菜籽油、大豆油、椰子油等脂肪油系軟化劑;松油;油膏(硫化油膏);蜜蠟、棕櫚蠟、羊毛脂等蠟類;蓖麻油酸、棕櫚酸、硬脂酸、硬脂酸鋇、硬脂酸鈣、月桂酸鋅等脂肪酸或脂肪酸鹽;環烷酸;松油、松
脂或其衍生物;萜樹脂、石油樹脂、雜排聚丙烯、香豆酮-茚樹脂等合成高分子物質;酞酸二辛酯、己二酸二辛酯、癸二酸二辛酯等酯系軟化劑;微晶蠟、液狀聚丁二烯、改質液狀聚丁二烯、液狀聚硫橡膠、烴系合成潤滑油等。
此等之中較佳為石油系軟化劑、特佳為石蠟油。
軟化劑(C)係相對於共聚合體(A)100質量份,通常為依70~140質量份、較佳80~120質量份、更佳90~110質量份之比例使用。若依此種量使用軟化劑(C),組成物之調製時及成形時之流動性優越,難以使所得成形體之機械物性降低,又,所得成形體之耐熱性、耐熱老化性優越。
<滑劑(D)>
作為滑劑(D),可使用一般廣泛認知之調配於塑膠的公知物。可使用例如化學便覽應用編、改訂2版(日本化學會編,1973年,丸善股份有限公司發行)之1037~1038頁所記載者。作為其具體例,可舉例如有機聚矽氧烷、氟系聚合物、脂肪酸醯胺、金屬皂、酯類、碳酸鈣、矽酸鹽。
作為上述脂肪酸醯胺之具體例,可舉例如硬脂醯胺、氧化硬脂醯胺、油基醯胺、二十二烯基醯胺(別名:芥酸醯胺)、月桂醯胺、棕櫚醯胺及山萮酸醯胺等之高級脂肪酸之單醯胺;羥甲基基醯胺、亞甲基雙硬脂醯胺、伸乙基雙硬脂醯胺、伸乙基雙油基醯胺及伸乙基雙月桂醯胺等之高級脂肪酸之醯胺;硬脂基油基醯胺、N-硬脂基芥酸醯胺及N-油基棕櫚醯胺等之複合型醯胺;以及依Plastrodin及Plastrodin S之商品名(藤澤藥品工業(股))市售的特殊脂肪酸醯胺。
此等可單獨使用1種或併用2種以上。
上述酯類係脂肪族醇、與二羧酸或脂肪酸之酯。作為此種酯類之具體例,可舉例如鯨蠟醇與醋酸之酯、鯨蠟醇與丙酸之酯、鯨蠟醇與酪酸之酯、牛脂醇與醋酸之酯、牛脂醇與丙酸之酯、牛脂醇與酪酸之酯、硬脂醇與醋酸之酯、硬脂醇與丙酸之酯、硬脂醇與酪酸之酯、二硬脂醇與酞酸之酯、甘油單油酸酯、甘油單硬脂酸酯、12-羥化硬脂酸酯、甘油三硬脂酸酯、三羥甲基丙烷三硬脂酸酯、季戊四醇四硬脂酸酯、硬脂酸丁酯、硬脂酸異丁酯、硬脂酸酯、油酸酯、山萮酸酯、含有鈣皂之酯、硬脂酸異十三基酯、棕櫚酸鯨蠟酯、硬脂酸鯨蠟酯、硬脂酸硬脂酯、山萮酸山萮酯、二十八酸乙二醇酯、二十八酸甘油酯、二十八酸季戊四醇酯、含鈣二十八酸酯。
此等之中,較佳為二硬脂醇與酞酸之酯、甘油單油酸酯、甘油單硬脂酸酯、硬脂酸酯、二十八酸甘油酯;特佳為二硬脂醇與酞酸之酯、甘油單硬脂酸酯、二十八酸甘油酯。
作為上述矽酸鹽,可例示式M2O‧mSiO2‧nH2O(式中,M為鹼金屬原子,m及n分別表示M2O每1莫耳中之SiO2或H2O之莫耳數。)所示化合物,作為具體例,可舉例如矽酸鈉、碳酸鉀、碳酸鋰。
此等之中,較佳為脂肪酸醯胺,更佳為高級脂肪酸之單醯胺,特佳為芥酸醯胺。
滑劑(D)係相對於共聚合體(A)100質量份,通常依2~6質量份、較佳3~5質量份之比例使用。若依此種量使用滑劑(D),則本發明之熱可塑性彈性體組成物之機械物性或成型加工性良好。
<酚樹脂系交聯劑(E)>
作為酚樹脂系交聯劑(E)(本發明中亦稱為「交聯劑(E)」),較佳係藉由在屬於可溶酚醛樹脂且烷基取代酚或非取代酚之鹼媒體中之醛內的縮合、更佳係甲醛內的縮合、或二官能性酚二醇類之縮合所製造。烷基取代酚較佳為1~10之碳原子之烷基取代體。更佳係於對位經具有1~10之碳原子的烷基所取代的二羥甲基酚類或酚樹脂。酚樹脂系硬化樹脂典型上為熱交聯性樹脂,亦稱為酚樹脂系交聯劑或酚樹脂。交聯劑(E)通常具有將共聚合體(A)進行交聯的作用。
作為酚樹脂系硬化樹脂(酚樹脂系交聯劑)之例子,可舉例如下述一般式[E1]所示者。
上述式中較佳係Q為二價基-CH2-O-CH2-,m為0或1~10之正整數,R’為具有未滿20之碳原子的有機基。更佳係m為0或1~5之正整數,R’為具有4~12之碳原子的有機基。
具體可舉例如烷基酚甲醛樹脂、羥甲基化烷基酚樹脂、鹵化烷基酚樹脂等;較佳為鹵化烷基酚樹脂、更佳係將末端羥基經溴化者。於酚樹脂系硬化樹脂中,藉下述一般式[E2]表示末端經溴化者之一例。
作為上述酚樹脂系硬化樹脂的製品例,可舉例如TACKIROL(註冊商標)201(烷基酚甲醛樹脂,田岡化學工業(股)公司製)、TACKIROL(註冊商標)250-I(溴化率4%之溴化烷基酚甲醛樹脂,田岡化學工業(股)公司製)、TACKIROL(註冊商標)250-III(溴化烷基酚甲醛樹脂,田岡化學工業(股)公司製)、PR-4507(群榮化學工業(股)公司製)、Vulkaresat510E(Hoechst公司製)、Vulkaresat532E(Hoechst公司製)、Vulkaresen E(Hoechst公司製)、Vulkaresen 105E(Hoechst公司製)、Vulkaresen 130E(Hoechst公司製)、Vulkaresol 315E(Hoechst公司製)、Amberol ST 137X(Rohm&Haas公司製)、SUMILITERESIN(註冊商標)PR-22193(住友Durez(股)公司製)、Symphorm-C-100(Anchor Chem.公司製)、Symphorm-C-1001(Anchor Chem.公司製)、TAMANOL(註冊商標)531(荒川化學(股)公司製)、Schenectady SP1059(Schenectady Chem.公司製)、Schenectady SP1045(Schenectady Chem.公司製)、CRR-0803(U.C.C公司製)、Schenectady SP1055F(Schenectady Chem.公司製,溴化烷基酚甲醛樹脂)、Schenectady SP1056(Schenectady Chem.公司製)、CRM-0803(昭
和Union合成(股)公司製)、Vulkadur A(Bayer公司製)。其中,較佳可使用鹵化酚樹脂系交聯劑,更佳為TACKIROL(註冊商標)250-I、TACKIROL(註冊商標)250-III、Schenectady SP1055F等之溴化烷基酚甲醛樹脂。
又,作為熱可塑性硫化橡膠之經由酚樹脂所進行之交聯的具體例,係記載於美國專利第4,311,628號、美國專利第2,972,600號及美國專利第3,287,440號,此等技術亦可於本發明中使用。
於美國專利第4,311,628號,揭示有包含酚系硬化性樹脂(phenolic curing resin)及硫化活性劑(cure activator)的酚系硫化劑系統(phenolic curative system)。該系統之基本成分係鹼媒體中之取代酚(例如鹵取代酚、C1-C2烷基取代酚)或非取代酚與醛、較佳係與甲醛間之縮合所得、或二官能性酚二醇類(較佳為對位經C5-C10烷基取代之二羥甲基酚類)之縮合所製造的酚樹脂系交聯劑。以藉烷基取代酚樹脂系交聯劑之鹵化所製造的經鹵化之烷基取代酚樹脂系交聯劑為特別適合。可特別推薦使用由羥甲基酚硬化性樹脂、鹵供給物及金屬化合物所構成的酚樹脂系交聯劑,其細節記載於美國專利第3,287,440號及美國專利第3,709,840號說明書。非鹵化酚樹脂系交聯劑係與鹵供給物同時使用、較佳係與鹵化氫去除劑同時使用。鹵化酚樹脂系交聯劑較佳為包含2~10質量%之溴的溴化酚樹脂系交聯劑,雖然鹵供給物並非必要,然而通常與例如氧化鐵、氧化鈦、氧化錳、矽酸鎂、二氧化矽及氧化鋅、較佳為氧化鋅般之金屬氧化物的鹵化氫去除劑同時使用。此等氧化鋅等之鹵化氫去除劑,係相對於酚樹脂系交聯劑100質量份,通常使用1~20質量份。此種去除劑之存在係促進酚樹脂系交聯劑之交聯作用,但在上述共聚合體(A)不容易藉由酚樹脂系交聯劑(E)進行交聯的情況,較佳為
共用鹵供給物及氧化鋅。鹵化酚系硬化性樹脂之製造及使用有氧化鋅之硫化劑系的此等利用,係記載於美國專利第2,972,600號及美國專利第3,093,613號說明書,其揭示係與上述美國專利第3,287,440號及美國專利第3,709,840號說明書之揭示內容一起引用至本說明書中作為參考。作為適當之鹵供給物的例子,可舉例如氯化亞錫、三氯化鐵、或氯化石蠟、氯化聚乙烯、氯碸化聚乙烯及聚氯丁二烯(氯丁二烯橡膠)般之鹵供給性聚合體。適當之酚樹脂系交聯劑及溴化酚樹脂系交聯劑可商業性取得,例如此種交聯劑可由Schenectady Chemicals,Inc.依商品名「SP-1045」、「CRJ-352」、「SP-1055F」及「SP-1056」購入。具相同作用而等價之酚樹脂系交聯劑亦可由其他供應者取得。
酚樹脂系交聯劑(E)由於分解物之發生較少,故由防止成霧(fogging)的觀點而言為較佳交聯劑。
本發明中,於交聯劑(E)存在下進行熱處理時,可調配硫、對醌二肟、p,p’-二苯甲基醌二肟、N-甲基-N,4-二亞硝基苯胺、亞硝基苯、二苯基胍、三羥甲基丙烷-N,N’-間伸苯基二順丁烯二醯亞胺般之過氧化交聯助劑,二乙烯基苯、三烯丙基三聚氰酸酯、乙二醇二甲基丙烯酸酯、二乙二醇二甲基丙烯酸酯、聚乙二醇二甲基丙烯酸酯、三羥甲基丙烷三甲基丙烯酸酯、烯丙基甲基丙烯酸酯等之多官能性甲基丙烯酸酯單體、丁酸乙烯酯、硬脂酸乙烯酯等之多官能性乙烯基單體等的助劑。
又,為了促進交聯劑(E)之分解,亦可使用分散促進劑。作為分散促進劑,可舉例如三乙基胺、三丁基胺、2,4,6-三(二甲基胺基)酚等之三級胺;鋁、鈷、釩、銅、鈣、鋯、錳、鎂、鉛、泵等環烷酸與各種金屬(例如Pb、Co、Mn、Ca、Cu、Ni、Fe、Zn、稀土族)之環烷酸鹽等。
交聯劑(E)係相對於共聚合體(A)100質量份,通常依2~9質量份、較佳2.5~8.5質量份之比例使用。若依此種量使用交聯劑(E),則本發明之熱可塑性彈性體組成物之機械物性或成型加工性良好。又,本發明中,共聚合體(A)之交聯程度並無特別限制,可於本發明範圍內改變交聯劑(E)之量而調整。
<任意之添加劑>
本發明之組成物係除了上述成分以外,在不損及本發明效果之範圍內可調配添加劑。
作為上述添加劑,可舉例如著色劑、抗氧化劑、無機填充劑、補強劑、抗老化劑(穩定劑)、加工助劑、活性劑、吸濕劑、發泡劑、發泡助劑、上述交聯助劑、上述分解促進劑等。
此等添加劑可分別單獨使用1種或組合2種以上使用。
於調配任意之添加劑的情況,穩定劑(抗氧化劑、抗老化劑)、加工助劑等添加劑的調配量,分別相對於上述共聚合體(A)100質量份,為例如0.01~0.80質量份、較佳0.10~0.50質量份左右。著色劑、無機填充劑、補強劑、活性劑、吸濕劑、發泡劑、發泡助劑、上述交聯劑、上述分解促進劑等係調配量並無特別限制,於調配的情況,各添加劑係相對於上述共聚合體(A)100質量份,通常調配0.01~10質量份、較佳1~8質量份。
(熱可塑性彈性體組成物(I)及其製造方法)
本發明之熱可塑性彈性體組成物(I)的特徵在於含有交聯體,該交聯體係上述共聚合體(A)經由酚樹脂系交聯劑(E)交聯而得者;且含有
上述結晶性聚烯烴(B)360~460質量份、上述軟化劑(C)70~140質量份、及上述滑劑(D)2~6質量份(其中,將上述共聚合體(A)之量設為100質量份)。
本發明之熱可塑性彈性體組成物(I)可藉由將上述共聚合體(A)、上述酚樹脂系交聯劑(E)、與上述結晶性聚烯烴(B)中之至少一部分進行動態熱處理而獲得。
動態熱處理較佳於非開放型之裝置中進行,或於氮、二氧化碳氣體等之惰性氣體環境下進行。熱處理之溫度通常為共聚合體(A)之融點至300℃之範圍、較佳為150~280℃、更佳170~270℃。混練時間通常為1~20分鐘、較佳1~10分鐘。
本發明之熱可塑性彈性體組成物(I)由於以上述共聚合體(A)與交聯劑(E)為原料,故於將含有此等之原料進行動態熱處理所得的熱處理物中,通常共聚合體(A)經交聯。
於製造本發明之熱可塑性彈性體組成物(I)時,若對上述共聚合體(A)、及上述交聯劑(E)、與上述結晶性聚烯烴(B)中之至少一部分進行動態熱處理即可,上述結晶性聚烯烴(B)亦可全量供給至該動態熱處理;或者上述軟化劑(C)、上述滑劑(D)及任意之添加劑係分別與上述共聚合體(A)、上述交聯劑(E)、及上述結晶性聚烯烴(B)中之至少一部分一起進行動態熱處理,亦可與上述熱處理物混合,亦可為此等之兩
者(亦即,一部分進行動態熱處理,剩餘者與上述熱處理物混合)。
作為本發明之熱可塑性彈性體組成物(I),較佳係含有石蠟油作為上述軟化劑(C)的組成物。
本發明之成形體的特徵在於含有本發明之熱可塑性彈性體組成物(I)。
本發明之成形體可由本發明之熱可塑性彈性體組成物(I)形成。作為成形方法,可應用習知公知之成形方法。
本發明之成形體係滑動性能、加工性優越。
本發明之積層體的特徵在於使含有本發明之熱可塑性彈性體組成物(I)之層(亦即,本發明之成形體的層)、與含有軟質材料之層進行積層而成。
作為上述軟質材料,可舉例如硬度(A硬度)為65~95、較佳65~85的軟質材料。
作為上述軟質材料,可舉例如熱可塑性彈性體組成物[以下亦記載為「熱可塑性彈性體組成物(II)」]。
作為上述熱可塑性彈性體組成物(II),較佳可舉例如本發明之熱可塑性彈性體組成物(I)、於本發明之熱可塑性彈性體組成物(I)中將酚樹脂系交聯劑(E)取代為其他交聯劑、以及於此等熱可塑性彈性體組成物中變更了原料調配比例者。作為熱可塑性彈性體組成物(II),更佳係交聯劑為酚樹脂系交聯劑(E)者。
作為上述熱可塑性彈性體組成物(II),更佳可舉例如藉由將聚烯烴樹脂(X)10~60質量份、乙烯‧α-烯烴‧非共軛多烯共聚合體樹脂(或對其加入了聚異丁烯、丁基橡膠、丙烯‧乙烯共聚合體等其他橡膠的橡膠成分)(Y)30~70質量份、油性軟化劑(Z)5~50質量份[(X)、(Y)及(Z)之合計為100質量份]於交聯劑存在下進行動態熱處理而製造者。於此(X)、(Y)及(Z)成分係分別意指與本發明之熱可塑性彈性體組成物(I)中所使用之(B)、(A)及(C)成分相同者。
本發明所使用之熱可塑性彈性體組成物中的軟化劑之質量分率(Wc)係定義如下。亦即,本發明所使用之熱可塑性彈性體中,將相對於乙烯‧α-烯烴‧非共軛多烯共聚合體(A)、結晶性聚烯烴(B)、軟化劑(C)及交聯劑(E’)(交聯劑(E’)係亦包括酚樹脂系交聯劑(E)的概念)之質量合計量,依百分率表示軟化劑(C)之質量比例的值設為Wc。再者,將熱可塑性彈性體組成物(I)中之Wc表示為W1c,將熱可塑性彈性體組成物(II)中之Wc表示為W2c。
上述熱可塑性彈性體組成物(II)中之軟化劑(C)的質量分率(W2c),較佳為30~50質量%、更佳33~45質量%。
於此積層體中,於上述熱可塑性彈性體組成物(I)中所佔之質量分率(W1c)相對於上述軟化劑於上述熱可塑性彈性體組成物(II)中所佔之質量分率(W2c)的比(W1c/W2c)較佳為0.60以下、更佳0.50以下。若上述比(W1c/W2c)為上述範圍,則軟化劑(油劑)由含有熱可塑性彈性體組成物(I)之層移行至含有軟質材料(熱可塑性彈性體組成物(II))之層的情況較少,且不妨礙含有熱可塑性彈性體組成物(I)之層的滑動性能。又,W1c/W2c之下限值並無特別限制,較佳為0.30、更佳0.40。
本發明之積層體亦可進一步具有上述2種層以外之層。
雖亦依存於積層體用途,但含有熱可塑性彈性體組成物(I)之層的厚度為例如30μm~1000μm,含有軟質材料(熱可塑性彈性體組成物(II))之層的厚度為例如0.1mm~3.0mm。
本發明之熱可塑性彈性體組成物(I)及其成形體,由於耐熱老化性優越、具有適度之硬度、且機械強度亦優越,故使用其之本發明之積層體,特別可用於汽車用密封構件(窗導槽密封條),認為亦可減低窗導槽密封條於底面部與玻璃較強接觸時的噪音(吱吱聲、嘰嘰聲、嘎嘎聲(軋音(creaking noise)、咔嗒(rattling noise)))。
本發明之積層體係除了窗導槽密封條之外,亦可適合使用於窗框封條、建材用墊片等物品。
接著針對本發明,例示實施例進行更詳細之說明,但本發明並不限定於此等。
<原料>
依以下方法測定原料之物性。
(乙烯‧α-烯烴‧非共軛多烯共聚合體中各構成單位之比例)
乙烯‧α-烯烴‧非共軛多烯共聚合體中所含之來自乙烯之構造單位的比例、來自α-烯烴之構造單位的比例、及來自非共軛多烯之構造單位的比例,係藉由13C-NMR進行測定。
<熱可塑性彈性體組成物>
藉以下方法,測定並評價熱可塑性彈性體組成物。
(MFR)
使用熔融指數儀(東洋精機製作所(股)製),根據JIS K7112,依230℃、10kg負重測定熱可塑性彈性體組成物之顆粒的熔融流動速率(MFR)。
(A硬度)
使用100t電熱自動壓製機(SHOJI公司製),將所得熱可塑性彈性體組成物之顆粒依230℃進行壓製成形6分鐘,其後,於室溫冷卻壓製5分鐘而製作厚2mm之壓製片材。使用該片材,根據ISO7619來使用A型測定器,於押針接觸後立即讀取刻度。
(D硬度)
將由熱可塑性彈性體組成物之顆粒使用50t壓製機所調節的20cm×20cm×2mm之片材樣本作為被試驗料,根據JIS K 6252-3,藉由Durometer D硬度計測定硬度。
(拉伸特性)
將由熱可塑性彈性體組成物之顆粒使用50t壓製機所調節的20cm×20cm×2mm之片材樣本作為被試驗料,根據JIS 6251,依溫度25℃、拉伸速度500mm/分之條件進行拉伸試驗,測定M100(100%伸度時之應力)、TB(拉伸破斷強度)、及EB(拉伸破斷點伸度)。
(凝膠分率)
將由熱可塑性彈性體組成物之顆粒使用50t壓製機所調節的20cm×20cm×2mm之片材樣本作為被試驗料,將被試驗料置入於325網
目之金屬籠中,浸漬於140℃之對二甲苯溶媒中24小時,測定殘存於金屬籠者的重量,由下式算出殘存凝膠分率。
凝膠分率(%)=(殘存物之重量[g]/被試驗料之重量[g])×100
(膨潤率)
將由熱可塑性彈性體組成物之顆粒使用50t壓製機所調節的20cm×20cm×2mm之片材樣本作為被試驗料,浸漬於125℃之石蠟油中72小時。測定浸漬前後之重量,由下式算出膨潤率。
膨潤率(%)=(浸漬後之重量[g])/(浸漬前之重量[g])×100
(耐熱老化性)
將實施例等所製造之積層體,於空氣中、80℃放置72小時,於此積層體中,藉目視及指觸確認滑動層(熱可塑性彈性體組成物(I))側的表面狀態,與放置前之表面狀態進行比較。表1中之符號意義如以下。
○:表面狀態無變化
△:於表面發生光澤,但未發生黏瘩
×:於表面發生光澤、且發生黏瘩
(擠出加工性)
針對熱可塑性彈性體組成物之顆粒,從藉由設定為200℃之L/D=30的毛細管流變計所測定的剪切速度24s-1時之模頭膨脹值、及剪切速度2400s-1時之模頭膨脹值,依下式算出膨脹比。
膨脹比=[剪切速度2400s-1時之模頭膨脹值]/[剪切速度24s-1時之模頭膨脹值]
此膨脹比較大時,表示於低剪切域與高剪切域的模頭膨脹值的差異大、擠出加工性劣化。
作為乙烯‧α-烯烴‧非共軛多烯共聚合體,係使用:於聚合觸媒使用二茂鐵觸媒並藉公知技術所製造,來自乙烯之構造單位(e)相對於來自α-烯烴之構造單位(o)的莫耳比[(e)/(o)]為64/36、來自非共軛多烯之構造單位於總構成單位中所佔的比例為5.4莫耳%、於135℃十氫萘中所測定之極限黏度[η]為2.5dL/g的乙烯‧α-烯烴‧非共軛多烯共聚合體(乙烯‧丙烯‧二烯共聚合體,以下記載為「EPDM-1」)。
作為結晶性聚烯烴(B),係使用藉公知技術所製造之以下之屬於丙烯均聚物的h-PP1~h-PP3。
‧h-PP1:MFR(230℃、2.16kg負重)=0.5g/10分、融點160℃之丙烯均聚物
‧h-PP2:MFR(230℃、2.16kg負重)=2.0g/10分、融點160℃之丙烯均聚物
‧h-PP3:MFR(230℃、2.16kg負重)=9.0g/10分、融點160℃之丙烯均聚物
再者,使用以下原料。
‧軟化劑:PW90(商品名,出光興產(股)製)(石蠟油)
‧滑劑:芥酸醯胺
‧交聯劑:溴化烷基酚甲醛樹脂(商品名,SP-1055F,schenectady公司製)
‧著色劑:碳黑母粒(DIC(股)製,F23287MM)
‧抗氧化劑:酚系抗氧化劑(Irganox 1010(BASF Japan(股)製)),苯并三唑系紫外線吸收劑(Tinuvin 326(BASF Japan(股)製)及受阻胺(HALS)系耐候穩定劑(Tinuvin 770(BASF Japan(股)製))之混合物。
(熱可塑性彈性體組成物-1之製造)
將EPDM-1、h-PP1、軟化劑、滑劑、交聯劑、著色劑及抗氧化劑,依表1記載之比例導入至雙軸擠出機(神戶製鋼所(股)製,HYPER KTX 46),將此等依滾筒溫度:50~250℃(亦即上述「熱可塑性彈性體組成物(I)及其製造方法」處所述之動態熱處理之溫度為250℃)、模頭溫度:200℃、螺桿旋轉數:550rpm、且擠出量:40kg/小時之條件進行熔融混練,得到熱可塑性彈性體組成物(以下亦記載為「熱可塑性彈性體組成物-1」)的顆粒。評價結果示於表1。
(積層體之製造)
作為含有軟質材料(熱可塑性彈性體組成物(II))之層的材料,係準備軟化劑之質量分率(W2c)為33質量%或42質量%的熱可塑性彈性體組成物。
具體而言,將聚烯烴樹脂(上述h-PP1)24質量份、乙烯‧α-烯烴‧非共軛多烯共聚合體(上述EPDM-1)37質量份、與軟化劑33質量份,於6質量份之交聯劑(上述溴化烷基酚甲醛樹脂)之存在下,依與製造上述熱可塑性彈性體組成物-1時相同的條件進行動態熱處理,藉此製造熱可塑性彈性體組成物(以下記載為「TPV-1」)。又,將聚烯烴樹脂(上述h-PP1)19質量份、乙烯‧α-烯烴‧非共軛多烯共聚合體
(上述EPDM-1)33質量份、與軟化劑42質量份,於6質量份之交聯劑(上述溴化烷基酚甲醛樹脂)之存在下,依與製造上述熱可塑性彈性體組成物-1時相同的條件進行動態熱處理,藉此製造熱可塑性彈性體組成物(以下記載為「TPV-2」)。
使用共擠出裝置,製作使含有軟質材料(上述TPV-1或上述TPV-2)之層與含有熱可塑性彈性體組成物-1之滑動層所積層的積層體(滑動層厚度200~250μm,積層體總厚度2mm)。
將此積層體作為被試驗料的耐熱老化性的評價結果示於表1。
除了將原料之種類或量如表1記載般變更以外,其餘與實施例1同樣地進行,得到熱可塑性彈性體組成物之顆粒,進而製作積層體。評價結果示於表1。
實施例之熱可塑性彈性體組成物係各種物性均衡佳且優越。
另一方面,結晶性聚烯烴(B)之量過少的比較例1的熱可塑性彈性體組成物,係硬度較低。
又,結晶性聚烯烴(B)之量過大的比較例2的熱可塑性彈性體組成物,係擠出加工性劣化。
軟化劑(C)之量過大、且未使用交聯劑(E)的比較例3的熱可塑性彈性體組成物,係發生油滲出、且硬度方面劣化。
Claims (14)
- 一種熱可塑性彈性體組成物(I),係含有交聯體,該交聯體係乙烯‧α-烯烴‧非共軛多烯共聚合體(A)之經由酚樹脂系交聯劑(E)所得者;且上述熱可塑性彈性體組成物(I)含有:結晶性聚烯烴(B)360~460質量份、軟化劑(C)70~140質量份、及滑劑(D)2~6質量份;上述共聚合體(A)之量為100質量份;上述共聚合體(A)之α-烯烴之碳數為3~20;上述結晶性聚烯烴(B)為丙烯均聚物或丙烯無規共聚合體。
- 如請求項1之熱可塑性彈性體組成物(I),其中,上述乙烯‧α-烯烴‧非共軛多烯共聚合體(A)係滿足下述要件(a1);要件(a1):來自乙烯之構造單位(e)相對於來自α-烯烴之構造單位(o)的莫耳比[(e)/(o)]為50/50~85/15。
- 如請求項1或2之熱可塑性彈性體組成物(I),其中,上述結晶性聚烯烴(B)藉示差掃描熱量分析所測定的融點為150~170℃。
- 如請求項1或2之熱可塑性彈性體組成物(I),其中,上述結晶性聚烯烴(B)為丙烯均聚物。
- 如請求項1或2之熱可塑性彈性體組成物(I),其中,上述軟化劑(C)為石蠟油。
- 如請求項1或2之熱可塑性彈性體組成物(I),其中,上述滑劑(D)為芥酸醯胺。
- 如請求項1或2之熱可塑性彈性體組成物(I),其中,上述交聯體係將上述乙烯‧α-烯烴‧非共軛多烯共聚合體(A)、與上述結晶性聚烯烴(B)之至少一部分,於上述酚樹脂系交聯劑(E)之存在下進行動態熱處理所得者。
- 如請求項1或2之熱可塑性彈性體組成物(I),其中,上述酚樹脂系交聯劑(E)之量相對於上述共聚合體(A)100質量份係為2~9質量份。
- 一種成形體,係含有請求項1至8中任一項之熱可塑性彈性體組成物(I)。
- 一種積層體,係將含有請求項1至8中任一項之熱可塑性彈性體組成物(I)之層與含有A硬度為65~95之軟質材料之層進行積層而成。
- 如請求項10之積層體,其中,上述軟質材料係含有熱可塑性彈性體。
- 如請求項11之積層體,其中,上述軟質材料係含有包含熱可塑性彈性體之熱可塑性彈性體組成物(II);上述組成物(II)含有軟化劑;上述軟化劑於上述組成物(II)中所佔之質量分率(W2c)為30~50質量%。
- 如請求項12之積層體,其中,上述軟化劑(C)於上述熱可塑性彈性體組成物(I)中所佔之質量分率(W1c)相對於上述軟化劑於上述熱可塑性彈性體組成物(II)中所佔之質量分率(W2c)的比(W1c/W2c)為0.60以下。
- 如請求項10至13中任一項之積層體,其係窗框封條、窗導槽密封條或建材用墊片。
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