TWI656156B - 經處理的塡料、包含該塡料的組成物及由該塡料製造的物件(三) - Google Patents
經處理的塡料、包含該塡料的組成物及由該塡料製造的物件(三) Download PDFInfo
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- TWI656156B TWI656156B TW103134766A TW103134766A TWI656156B TW I656156 B TWI656156 B TW I656156B TW 103134766 A TW103134766 A TW 103134766A TW 103134766 A TW103134766 A TW 103134766A TW I656156 B TWI656156 B TW I656156B
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- acid
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- treated
- unsaturated fatty
- slurry
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- 239000000377 silicon dioxide Substances 0.000 claims description 75
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- 239000000126 substance Substances 0.000 claims description 16
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- DTOSIQBPPRVQHS-PDBXOOCHSA-N alpha-linolenic acid Chemical compound CC\C=C/C\C=C/C\C=C/CCCCCCCC(O)=O DTOSIQBPPRVQHS-PDBXOOCHSA-N 0.000 claims description 7
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Classifications
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
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- C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B60—VEHICLES IN GENERAL
- B60C—VEHICLE TYRES; TYRE INFLATION; TYRE CHANGING; CONNECTING VALVES TO INFLATABLE ELASTIC BODIES IN GENERAL; DEVICES OR ARRANGEMENTS RELATED TO TYRES
- B60C1/00—Tyres characterised by the chemical composition or the physical arrangement or mixture of the composition
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F8/00—Chemical modification by after-treatment
- C08F8/42—Introducing metal atoms or metal-containing 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
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
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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
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
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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
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- C08K3/34—Silicon-containing compounds
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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
- C08K5/00—Use of organic ingredients
- C08K5/54—Silicon-containing compounds
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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
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- C08K5/541—Silicon-containing compounds containing oxygen
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- C08K5/5419—Silicon-containing compounds containing oxygen containing at least one Si—O bond containing at least one Si—C bond
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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
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- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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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
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Abstract
本發明包含一種用於製造經處理的填料之方法,其包含(a)以包含一處理劑之一處理組成物處理包含未經處理的填料之一漿料,其中,此未經處理的填料未被事先乾燥,因此,形成一經處理的填料漿料;及(b)使此經處理的填料漿料乾燥製造經處理的填料。處理劑可包含不飽和脂肪酸、不飽和脂肪酸之衍生物,或其鹽。本發明亦係有關於藉由此方法製備之經處理的填料,與包含此經處理的填料之橡膠混練組成物及輪胎。
Description
本申請案主張2013年10月7日申請之美國臨時申請案第61/887,713號案之利益,此案在此被完整併入以供參考。
本發明係基於美國能源部授予之第DE-EE0005359號合約受政府支持進行。政府於本發明具有某些權利。
本發明係有關於一種用於製備經處理的填料之方法,藉由此方法製造之經處理的填料,及包含此經處理的填料之組成物及物件。
使用二氧化矽/矽烷填料系統降低滾動阻力及改良客車及卡車輪胎抗濕滑性係此項技藝已知。降低滾動阻力造成較少燃料消耗。
滾動阻力、磨耗及牽引力之同時改良,稱為擴大“魔術三角”,需要新的方式發展橡膠複合物。沉澱的二氧化矽於生胎的出現扮演重要角色,其與過去技術相比係自豪於滾動阻力有重大改良。二氧化矽(經由偶合)直接交聯成一經高度交聯之聚合物基質,同時使二氧化矽顆粒間之交互作用達最小,被認為係對於用於製造客車及卡車輪胎的橡膠之合意動力機械性質極其重要。己注意到於天然橡膠(典型上用於製造卡車輪胎),自天然橡膠生物合成而存在之蛋白質優先吸附於二氧化矽表面,干擾於原位之偶合反應。增加之排膠溫度可能改良偶合效率,亦已顯示使天然橡膠降解。因此,於橡膠產業持續需要經改良之二氧化矽-椽膠偶合材料。
再者,已發現使高表面積填料材料併入橡膠組成物內會造成黏度不合意增加,因此,由於處理問題,限制可被包含於橡膠組成物內之高表面積材料的量。因此,需要以材料處理此等高表面材料(例如,沉澱之二氧化矽)的需求,此材料係可作為使高表面材料與將其併入於內的聚合物基質更相容,改良加工黏度,及避免高表面材料與聚合物基質相分離。
依據本發明,提供一種用於製造經處理的填料之方法,其包含:(a)以包含一處理劑之一處理組成物處理包含未經處理的填料之一漿料,其中,此未經處理的填料未
被事先乾燥,因此,形成一經處理的填料漿料;及(b)使此經處理的填料漿料乾燥製造經處理的填料。處理劑可包含一包含一具有至少一個碳-碳雙鍵之線性或分支的選擇性經取代之C4至C38烷基的不飽和脂肪酸;(i)之該不飽和脂肪酸之衍生物,其中,至少一個碳-碳雙鍵反應而包含至少一官能基團;及/或(i)之該不飽和脂肪酸之鹽的至少一者。該不飽和脂肪酸(i)、該衍生物(ii)之該不飽和脂肪酸,及該鹽(iii)之該不飽和脂肪酸於每一情況係相同或不同。
依據本發明,進一步提供一種用於製造經處理的沉澱二氧化矽之方法,其包含:(a)使一鹼金屬矽酸鹽與一酸組合形成一包含未經處理的二氧化矽之漿料,其中,未經處理的二氧化矽未被事先乾燥;(b)以一包含一處理劑之處理組成物處理該漿料,因此,形成一經處理的漿料;及(c)使該經處理的漿料乾燥製造經處理的沉澱二氧化矽。處理劑可包含一包含一具有至少一個碳-碳雙鍵之線性或分支的選擇性經取代之C4至C38烷基的不飽和脂肪酸;(i)之該不飽和脂肪酸之衍生物,其中,至少一個碳-碳雙鍵反應而包含至少一官能基團;及/或(i)之該不飽和脂肪酸之鹽的至少一者。該不飽和脂肪酸(i)、該衍生物(ii)之該不飽和脂肪酸,及該鹽(iii)之該不飽和脂肪酸於每一情況係相同或不同。
依據本發明,進一步提供一種用於製造經處理的沉澱二氧化矽之方法,其包含:(a)使一鹼金屬矽酸鹽頭一酸組合形成一未經處理的漿料,其包含未經處理的二氧化
矽,其中,未經處理的二氧化矽未被事先乾燥;(b)使未經處理的漿料乾燥製造經乾燥之沉澱二氧化矽;(c)以一處理組成物形成經乾燥之沉澱二氧化矽的一水性漿料,此處理組成物包含一處理劑及選擇性之一偶合劑及/或選擇性之一非偶合劑,形成一經處理的沉澱二氧化矽漿料;及(d)使經處理的沉澱二氧化矽漿料乾燥製造一經乾燥之經處理的沉澱二氧化矽。處理劑可包含一包含一具有至少一個碳-碳雙鍵之線性或分支的選擇性經取代之C4至C38烷基的不飽和脂肪酸;(i)之該不飽和脂肪酸之衍生物,其中,至少一個碳-碳雙鍵反應而包含至少一官能基團;及/或(i)之該不飽和脂肪酸之鹽的至少一者。該不飽和脂肪酸(i)、該衍生物(ii)之該不飽和脂肪酸,及該鹽(iii)之該不飽和脂肪酸於每一情況係相同或不同。
依據本發明,亦提供藉由此處所述方法製備之經處理的填料,與包含此經處理的填料之橡膠組成物,諸如,橡膠混練組成物,及包含本發明之經處理的填料之橡膠物件。
如先前所提及,本發明提供一種用於製造經處理的填料之方法。此方法可包含:(a)以一包含一處理劑之處理組成物處理一可包含未經處理的填料之漿料,其中,此
未經處理的填料未被事先乾燥,因此,形成一經處理的填料漿料;及(b)使此經處理的填料漿料乾燥製造經處理的填料。
於此處使用時,有關於填料(諸如,經處理及/或未經處理的填料),術語“未被事先乾燥”意指於處理方法前之填料未被乾燥至少於20重量%之水分含量。為了本發明之目的,未經處理的填料不包含被事先乾燥至少於20重量%之水分含量然後再次水合的填料。
於此處使用時,術語“填料”意指一可用於一聚合物組成物改良此聚合物至少一性質之無機材料,諸如,一無機氧化物。於此處使用時,術語“漿料”意指一含至少包含填料及水之混合物。
於此處使用時,除非其它方式明確及不含糊地限於一個指示物,冠詞"一個"、"一"及"該"包含多數個指示物。
除非其它方式指示,此處揭露之所有範圍或比率需瞭解係包含此處包含之任何及所有子範圍或子比率。例如,"1至10"之陳述範圍或比率需被認為包含最小值1與最大值10間(且包含)的任何及所有子範圍,即,以最小值1或更多開始且以最大值10或更少結束之所有子範圍或子比率,諸如,1至6.1,3.5至7.8,及5.5至10,但不限於此等。
除了於操作範例或其它指示外,說明書及申請專利範圍中使用之表示成份、反應條件等之量的所有數值需瞭解於所有例子係以術語“約”修飾。
於此處使用時,聚合物之分子量值,諸如,重量平均分子量(Mw)及數平均分子量(Mn),係藉由凝膠滲透層析術使用聚苯乙烯標準物判定。
於此處使用時,多分散性指數(PDI)值表示此聚合物之重量平均分子量(Mw)對數平均分子量(Mn)之比率(即,Mw/Mn)。
於此處使用時,術語“聚合物”意指均聚物(例如,自單種單體物種製備)、共聚物(例如,自至少二種單體物種製備),及接枝聚合物。
於此處使用時,術語“(甲基)丙烯酸酯”及相似術語,諸如,“(甲基)丙烯酸酯”,意指甲基丙烯酸酯及/或丙烯酸酯。於此處使用時,術語“(甲基)丙烯酸”意指甲基丙烯酸及/或丙烯酸。
除非其它指示外,此處提及之不受限地諸如核准專利案及專利申請案的所有文件被認為係被完整"併入以供參考"。
於此處使用時,“線性或分支”基團之描述,諸如,線性或分支之烷基,於此處瞭解係包含:一亞甲基基團或一甲基基團;線性基團,諸如,線性C2-C36烷基基團;及適當分支之基團,諸如,分支C3-C36烷基基團。
於此處使用時,“選擇性經取代”之基團的描述意指其中其至少一個氫已選擇性地以一不同於氫之基團替代或取代之一基團,此基團不受限地包含烷基基團、環烷基基團、雜環烷基基團、芳基基團,及/或雜芳基基團,此不
同於氫之基團係不受限地諸如鹵基團(例如,F、Cl、I,及Br)、羥基基團、醚基團、硫醇基團、硫醚基團、羧酸基團、羧酸酯基團、磷酸基團、磷酸酯基團、磺酸基團、磺酸酯基團、硝基基團、氰基基團、烴基基團(不受限地包含:烷基;烯基;炔基;環烷基,包含多稠合環之環烷基及多環狀烷基;雜環烷基;芳基,包含經羥基取代之芳基,諸如,酚,且包含多稠合環之芳基;雜芳基,包含多稠合環之雜芳基;及芳烷基基團),及胺基團,諸如,N(R11 ’)(R12 ’),其中,某些實施例,R11 ’及R12 ’每一者獨立地係選自氫、線性或分支之C1-C20烷基、C3-C12環烷基、C3-C12雜環烷基、芳基,及雜芳基。
可與本發明方法使用之某些化合物包含於每一情況可獨立地選自烴基及/或經取代之烴基及/或官能性烴基(或具有一或多個官能基團之烴基基團)之族群及子族群。於此處使用時,且依據某些實施例,術語“烴基”及相似術語,諸如,“烴基取代基”,意指線性或分支之C1-C36烷基(例如,線性或分支之C1-C10烷基);線性或分支之C2-C36烯基(例如,線性或分支之C2-C10烯基);線性或分支之C2-C36炔基(例如,線性或分支之C2-C10炔基);C3-C12環烷基(例如,C3-C10環烷基);C5-C18芳基(包含多環狀芳基基團)(例如,C5-C10芳基);及C6-C24芳烷基(例如,C6-C10芳烷基)。
代表性之烷基基團不受限地包含甲基、乙基、丙基、異丙基、丁基、異丁基、第二丁基、第三丁基、戊基、新戊基、己基、庚基、辛基、壬基,及癸基。代表性之烯
基基團不受限地包含乙烯基、烯丙基,及丙烯基。代表性之炔基基團不受限地包含乙炔基、1-丙炔基、2-丙炔基、1-丁炔基,及2-丁炔基。代表性之環烷基基團不受限地包含環丙基、環丁基、環戊基、環己基,及環辛基取代基。代表性之芳烷基基團不受限地包含苯甲基及苯乙基。
術語“經取代之烴基”及相似術語,諸如,“官能性烴基”(或具有至少一個官能基團之烴基)於此處使用時係意指其中其至少一個氫已以一不同氫之基團取代之一烴基基團,此不同氫之基團係不受限地諸如鹵基團、羥基基團、醚基團、硫醇基團、硫醚基團、羧酸基團、羧酸酯基團、磷酸基團、磷酸酯基團、磺酸基團、磺酸酯基團、硝基基團、氰基基團、烴基基團(例如,烷基、烯基、炔基、環烷基、芳基,及芳烷基基團)、雜環烷基基團、雜芳基基團,及胺基團,諸如,N(R11 ’)(R12 ’),其中,R11 ’及R12 ’每一者獨立地係選自氫、烴基,及經取代之烴基。
依據某些實施例,術語“烷基”於此處使用時係意指線性或分支之烷基,不受限地諸如線性或分支之C1-C25烷基,或線性或分支之C1-C10烷基,或線性或分支之C2-C10烷基。可選作本發明之各種烷基基團的烷基基團之例子不受限地包含此處於先前描述者。本發明之各種化合物的烷基基團某些實施例可包含一或多個選自-CH=CH-基團及/或一或多個-C≡C-基團之不飽和連接,只要此烷基基團係無二或更多個共軛不飽和連接。某些實施例,烷基基團係無諸如CH=CH基團及-C≡C-基團之不飽和連接。
依據某些實施例,術語“環烷基”於此處使用時係意指為適當環狀之基團,不受限地諸如C3-C12環烷基(不受限地包含環狀C5-C7烷基)基團。環烷基基團之例子不受限地包含此處於先前描述者。依據某些實施例,術語“環烷基”於此處使用時亦包含:橋接環多環烷基基團(或橋接環多環狀烷基基團),不受限地諸如二環[2.2.1]庚基(或降茨基)及二環[2.2.2]辛基;及稠合環多環烷基基團(或稠合環多環狀烷基基團),不受限地諸如八氫-1H-茚基,及十氫萘基。
依據某些實施例,術語“雜環烷基”於此處使用時係意指為適當環狀之基團(於環狀環中具有至少一個雜原子),不受限地諸如C3-C12雜環烷基基團或C5-C7雜環烷基基團,且於環狀環中具有至少一個雜原子,不受限地諸如O、S、N、P,及此等之組合。雜環烷基基團之例子不受限地包含咪唑基、四氫呋喃基、四氫吡喃基,及哌啶基。依據某些實施例,術語“雜環烷基”於此處使用時亦包含:橋接環多環狀雜環烷基基團,不受限地諸如7-氧雜二環[2.2.1]庚基;及稠合環多環狀雜環烷基基團,不受限地諸如八氫環戊[b]吡喃基,及八氫1H異烯基。
於此處使時且依據某些實施例,術語“芳基”包含C5-C18芳基,諸如,C5-C10芳基(且包含多環狀芳基基團,包含多環狀稠合環芳基基團)。代表性之芳基基團不受限地包含苯基、萘基、蒽基,及三蝶烯基。
依據某些實施例,術語“雜芳基”於此處使用時係意指於環中具有至少一個雜原子之芳基基團,且不受限地
包含C5-C18雜芳基,不受限地諸如C5-C10雜芳基(包含稠合環多環狀雜芳基基團),且意指於芳香族環或於稠合環多環狀雜芳基基團之情況中的至少一芳香族環中具有至少一個雜原子之一芳基基團。雜芳基基團之例子不受限地包含呋喃基、吡喃基、吡啶基、異喹啉,及嘧啶基。
於此處使用時,術語“稠合環多環芳基烷基基團”及相似術語,諸如,稠合環多環烷基芳基基團、稠合環多環芳基烷基基團,及稠合環多環烷基芳基基團意指含有至少一個芳基環及至少一個環烷基環稠合在一起形成一稠合環結構的一稠合環多環狀基團。為了非限制性例示之目的,稠合環多環芳基烷基基團之例子不受限地包含茚基、9H-芴基、環五萘基,及二環戊二烯并苯基。
於此處使用時且依據某些實施例,術語“芳烷基”不受限地包含C6-C24芳烷基,不受限地諸如C6-C10芳烷基,且意指以一烷基基團取代之一芳基基團。芳烷基基團之例子不受限地包含此處先前描述者。
用於本發明方法之適合未經處理的填料可包含熟習此項技藝者所知之廣泛各種材料。非限制性之例子可包含於露出表面擁有氧(化學吸附或共價鍵結)或羥基(結合或游離)之諸如無機顆粒及非結晶性固體材料之無機氧化物,不受限地諸如F.Albert Cotton等人之Elements in Advanced Inorganic Chemistry:A Comprehensive Text,第四版,John Wiley and Sons,1980之周期表的第Ib、IIb、IIIa、IIIb、IVa、IVb(碳除外)、Va、VIa、VIIa及VIII族之第2、3、
4、5及6期的金屬之氧化物。適合無機氧化物之非限制性例子可不受限地包含矽酸鋁、二氧化矽,諸如,二氧化矽凝膠、膠體二氧化矽、沉澱二氧化矽,及此等之混合物。
無機氧化物某些實施例可為二氧化矽。例如,於某些實施例,無機氧化物可包含沉積二氧化矽、膠體二氧化矽,及其等之混合物。藉由電子顯微鏡測量時,二氧化矽可具有少於0.1微米,或大於0.001微米,或從0.01至0.05微米,或從0.015至0.02微米之平均最終顆粒尺寸。再者,藉由布魯諾爾艾米特及泰勒(Brunauer,Emmett,and Teller(BET))方法依據ASTM D1993-91判定時,二氧化矽可具有從25至1000平方公尺/克,諸如,從75至250平方公尺/克,或從100至200平方公尺/克之表面積。某些實施例,填料係沉澱二氧化矽。
如先前提及,未經處理的填料漿料係以一包含一處理劑之處理組成物處理。於某些實施例,處理劑可作為一偶合劑。術語“偶合劑”於此處使用時係意指與(i)存在於填料顆粒表面上(諸如,於二氧化矽表面上)的基團與(ii)存在於使填料併入於內之聚合物基質的組份上之官能基團(離子性或共價)結合之一材料。因此,填料顆粒可與聚合物基質內之組份“偶合”。
另外,某些實施例,處理劑可作為一非偶合劑。術語“非偶合劑”於此處使用時係意指用以使經處理的填料與最終使用此經處理的填料之聚合物組成物相容的一材料。即,非偶合劑會影響經處理的填料顆粒之自由表面能,使
經處理的填料顆粒具有與聚合物組成物者相似之表面能量。此促進經處理的填料併入聚合物組成物內,且可用以改良(諸如,減少)組成物之混合黏度。需注意非偶合劑不被預期超過凡得瓦(Van der Waal)交互作用與橡膠基質偶合。於此處使用時,術語“非偶合劑”可與“相容劑”互換地使用。
需注意許多處理劑可同時作為偶合劑及非偶合劑/相容劑。
用於本發明方法之處理劑係包含一不飽和脂肪酸及其鹽者。術語“不飽和脂肪酸”於此處使用時意指具有一烴鏈且於此烴鏈具有至少一個碳-碳雙鍵之羧酸。單不飽和脂肪酸於烴鍵含有單一個碳-碳雙鍵,而多不飽和脂肪酸含有二或更多個碳-碳雙鍵。
某些實施例,不飽和脂肪酸、其衍生物及其鹽可以下列化學式(A)表示:ZO-C(O)-R (A)。關於化學式(A),某些實施例,Z可為H+,且R可為具有至少一個碳-碳雙鍵之一線性或分支之選擇性經取代的C4至C38烷基。於此處使用時,“衍生物”意指二聚物(不受限地例如十一烯酸之二聚物)及經取代之產物。某些其它實施例,不飽和脂肪酸於一或多個不飽和基團(碳-碳雙鍵)可被官能化。藉由“官能化”,其係意指如此處所述之一官能基團可經由一反應加至碳-碳雙鍵處。即,雙鍵可被破壞,且一官能基團可被提供。
某些實施例,有用之不飽和脂肪酸包含於水中至
少可極低極度地分散/溶解者。可用於本發明之不飽和脂肪酸係例如且不受限地包含單不飽和脂肪酸,諸如,油酸(CH3(CH2)7CH=CH(CH2)7COOH)、蓖麻油酸(CH3(CH2)5CH(OH)CH2CH=CH(CH2)7COOH)、棕櫚油酸(CH3(CH2)5CH=CH(CH2)7COOH)、異油酸(CH3(CH2)5CH=CH(CH2)9COOH)、二十烯酸(CH3(CH2)5CH=CH(CH2)11COOH)、反油酸(CH3(CH2)7CH=CH(CH2)7COOH)、11-二十烯酸(CH3(CH2)7CH=CH(CH2)9COOH)、芥酸(CH3(CH2)7CH=CH(CH2)11COOH)、二十四烯酸(CH3(CH2)7CH=CH(CH2)13COOH)、十一烯酸(CH2=CH(CH2)8COOH)。可用於本發明之不飽和脂肪酸係例如且不受限地包含多不飽和脂肪酸,諸如,亞麻油酸(CH3(CH2)4(CH=CHCH2)2(CH2)6COOH)、共軛亞麻油酸、α-亞麻油酸(CH3CH2CH=CHCH2CH=CHCH2CH=CH(CH2)7COOH)、γ-亞麻油酸(CH3(CH2)4CH=CHCH2CH=CHCH2CH=CH(CH2)4COOH)、二均-γ-亞麻油酸(CH3(CH2)4CH=CHCH2CH=CHCH2CH=CH(CH2)6COOH)、次亞麻油酸(CH3CH2(CH=CHCH2)3(CH2)6COOH)、花生四烯酸(CH3(CH2)4(CH=CHCH2)4(CH2)2COOH)、十八碳四烯酸(CH3CH2CH=CHCH2CH=CHCH2CH=CHCH2CH=CH(CH2)4COOH)、二十碳五烯酸
(CH3CH2CH=CHCH2CH=CHCH2CH=CHCH2CH=CHCH2CH=CH(CH2)3COOH)、二十二碳六烯酸(CH3CH2CH=CHCH2CH=CHCH2CH=CHCH2CH=CHCH2CH=CHCH2CH=CH(CH2)2COOH)、二十二碳四烯酸(CH3(CH2)4CH=CHCH2CH=CHCH2CH=CHCH2CH=CH(CH2)5COOH)、α-及β-十八碳三烯酸(CH3(CH2)3(CH=CH)3(CH2)7COOH)、金盞酸(CH3(CH2)4(CH=CH)3(CH2)6COOH),及米德酸(CH3(CH2)7CH=CHCH2CH=CHCH2CH=CH(CH2)3COOH)。於此處使用時,術語不飽和脂肪酸包含其順式及反應異構物。
某些實施例,脂肪酸含有一其內具有至少一個碳-碳雙鍵之線性或分支之選擇性經取代的C10-C18烷基R基團。某些非限制性實施例,不飽和脂肪酸係單不飽和脂肪酸。某些非限制性實施例,不飽和脂肪酸係油酸或其鹽及二十一烯酸或其鹽之至少一者。某些另外非限制性實施例,不飽和脂肪酸係油酸或其鹽。某些另外非限制性實施例,油酸鹽係油酸鈉。某些另外非限制性實施例,不飽和脂肪酸係二十一烯酸或其鹽。某些另外非限制性實施例,二十一烯酸鹽係二十一烯酸鈉。
不飽和脂肪酸或其鹽可自任何適合之商業來源獲得,例如,自Sigma-Aldrich Corp.(St.Louis,MO,USA)及Thermo Fisher Scientific,Inc.(Waltham,MA,USA)。
某些實施例,不飽和脂肪酸之R包含具有一或多
個取代基(或官能基團)之一側鏈。另外,如先前所揭露,某些實施例,不飽和脂肪酸可於一或多個不飽和基團(碳-碳雙鍵)處被官能化。即,雙鍵可被破壞且一取代基團可被提供。R或經官能化之不飽和基團上之取代基的非排它性例子可包含一般類別之烷基、烯基、炔基、苯基、苯甲基、鹵基(包含氟、氯、溴,及碘基團)、羥基、羰基、醛、鹵甲醯基、碳酸酯、羧酸酯、羧基、酯、甲氧基、氫過氧基、過氧基、醚、半縮醛、半縮酮、縮醛、縮酮、原酸酯、亞甲二氧基、原碳酸酯、羧醯胺、一級胺、二級胺、三級胺、四級銨、亞胺(一級酮亞胺、二級酮亞胺、一級醛亞胺、二級醛亞胺)、醯亞胺、疊氮、偶氮、氰酸酯、異氰酸酯、硝酸鹽、亞硝酸鹽、異腈、亞硝氧基、硝基、亞硝基、吡啶基、硫氫基(硫醇)、硫化物、二硫化物、亞磺醯基、磺醯基、亞磺基、磺基、硫氰酸酯、異硫氰酸酯、硫代甲醯基、膦基、膦醯基、磷酸鹽,及其等之衍生物。於此處使用時,“衍生物”意指鹽、開環產物,及經取代之產物。
使不飽和脂肪酸之側鏈或碳-碳雙鍵官能化可依據此項技藝所認知之方法完成。此等方法不受限地包含經過(或對)至少一個碳-碳雙鏈自由基加成、親電子性加成、親核性加成、周環加成,及金屬催化加成。
如前所述,某些實施例,處理劑係不飽和脂肪酸之鹽。再次關於化學式(A):ZO-C(O)-R (A),某些實施例,R可為具有至少一個碳-碳雙鍵之一線性或分
支之選擇性經取代的C4至C38烷基,且Z係一陽離子(不飽和脂肪酸之鹽)且可為任何鹼金屬陽離子、鹼土金屬陽離子、過渡金屬陽離子、氨,或四級銨陽離子。鹼金屬陽離子不受限地包含Na+及K+。鹼土金屬陽離子不受限地包含Mg2+及Ca2+。過渡金屬陽離子不受限地包含Cd2+及Mn2+。四級銨陽離子不受限地包含以下列化學式(B)表示者:+N(R)4 (B)。關於化學式(B),每一R獨立地係一線性或分支之C1-C12烷基基團或一芳基基團。
某些實施例,處理劑包含具有一極性側鏈之一不飽和脂肪酸。可於化學式(A)之R的極性側鏈上或定義此極性側鏈的極性基團之例子不受限地包含羥基、硫醇、羧基、酚、胺、羧醯胺、咪唑,及吲哚基團。熟習此項技藝者會瞭解側鏈無需為了呈極性而帶電荷及足夠的是側鏈被水吸引/對水具吸引性。
某些實施例,可用於本發明之化學式(A)之R的極性側鏈係例如且不受限地具有羥基、酚、硫醇、咪唑、胍、胺,及銨基團之可離子化或經離子化之側鏈。但是,熟習此項技藝者會瞭解前述僅係例示,且具有用於與存在於填料顆粒及/或聚合物基質表面上之基團鍵結、反應,或交互作用之官能性側鏈(不受限地例如極性及/或可離子化/經離子化之側鏈)之不飽和脂肪酸可用於本發明之程序及方法。
某些實施例,除如上列示之處理劑外,處理組成
物可另外包含與此處理劑不同之一第一或另外之偶合劑。於某些實施例,偶合劑可包含各種有機矽烷之任一者。可與本發明某些實施例使用之適合有機矽烷之例子包含以化學式(I)表示者:(R1)a(R2)bSiX4-a-b (I)。有關於化學式(I),R1對於每一“a”獨立地係具有1至36個碳原子且及一官能基團之一烴基基團。烴基基團之官能基團係乙烯基、烯丙基、己烯基、環氧(環氧乙烷)、環氧丙氧基、(甲基)丙烯醯氧基、硫化物、異氰酸基(-NCO)、多硫化物、巰基,或鹵素。有關於化學式(I),R2對於每一“b”獨立地係具有從1至36個碳原子或氫之一烴基基團。化學式(I)之X獨立地係鹵素或具有1至36個碳原子之烷氧基;下標“a”係0、1、2,或3;下標“b”係0、1,或2;(a+b)係1、2,或3。某些實施例,附帶條件係當b係1,(a+b)係2或3。本發明之某些另外實施例,處理組成物進一步包含以化學式(I)表示之一偶合劑,其中,X係烷氧基;a係1;b係0;且R1之烴基的官能基團係鹵素。
諸如以化學式(I)表示者之鹵基官能性有機矽烷的例子不受限地包含(4-氯甲基-苯基)三甲氧基矽烷、(4-氯甲基-苯基)三乙氧基矽烷、[2-(4-氯甲基-苯基)-乙基]三甲氧基矽烷、[2-(4-氯甲基-苯基)-乙基]三乙氧基矽烷、(3-氯-丙烯基)-三甲氧基矽烷、(3-氯-丙烯基)-三乙氧基矽烷、(3-氯-丙基)-三乙氧基矽烷、(3-氯-丙基)-三甲氧基矽烷、三甲氧基-(2-對-甲苯基-乙基)矽烷,及/或三乙氧基-(2-對-甲苯基-
乙基)矽烷。
於某些實施例,以已沉澱之SiO2的總質量為基準,另外偶合劑可以範圍從0.25至30.0重量%,諸如,1至15重量%,或5至10重量%之量存在於漿料中。
於某些實施例,可用於本發明方法之處理組成物亦可進一步包含與諸如以化學式(I)表示之前述選擇性有機矽烷偶合劑不同之一含硫有機矽烷。此等材料之非限制性例子可不受限地包含以下列化學式(II)表示之有機矽烷:(R3)c(R4)dSiY4-c-d (II)。
有關化學式(II),R3對於每一“c”獨立地可為具有1至12個碳原子及一官能基團之一烴基基團。官能基團可為硫化物、多硫化物,或巰基。有關於化學式(II),R4對於每一“d”獨立地可為具有從1至18個碳原子或氫之一烴基基團。每一Y可獨立地係鹵素或具有1至12個碳原子之一烷氧基基團。下標“c”可為0、1、2,或3;下標“b”可為0、1,或2;且c+d可為1、2,或3。某些實施例,附帶條件係當b係1,則a+b係2或3。化學式(II)之R3及R4基團可被選擇,使得其等可與可使經處理的填料併入其中之聚合物組成物反應。另外,含硫之有機矽烷可包含以下列化學式(III)表示之雙(烷氧基矽烷基烷基)多硫化物:Z’-alk-Sn’ -alk-Z’ (III)。有關於化學式(III),“alk”表示具有從1至18個碳原子之一二價烴基團;n'係從2至12之一整數;且Z’係:
其中,R5獨立地係具有從1至4個碳原子之一烷基基團或苯基,且每一R6獨立地係具有從1至8個碳原子之一烷氧基基團,具有從5至8個碳原子之一環烷氧基基團,或具有從1至8個碳原子之一直鏈或分支鏈烷基巰基基團。R5及R6基團可為相同或不同。再者,二價alk基團可為直鏈或分支鏈、一飽和或不飽和脂族烴基團,或一環狀烴基團。雙(烷氧基矽烷基烷基)-多硫化物之非限制性例子可包含雙(2-三烷氧基矽烷基乙基)-多硫化物,其中,三烷氧基基團可為三甲氧基、三乙氧基、三(甲基乙氧基)、三丙氧基、三丁氧基等,最高達三辛氧基;且多硫化物可為二、三、四、五,或六硫化物,或此等之混合物。另外非限制性例子可包含相對應之雙(3-三烷氧基矽烷基丙基)-、雙(3-三烷氧基矽烷基異丁基)、-雙(4-三烷氧基矽烷基丁基)-等,最高達雙(6-三烷氧基矽烷基-己基)-多硫化物。雙(烷氧基矽烷基烷基)-多硫化物之另外非限制性例子係描述於美國專利第3,873,489號案,第6欄,第5-55行,及美國專利第5,580,919號案,第11欄,第11-41行。此等化合物之另外非限制性例子可包含:3,3'雙(三甲氧基矽烷基丙基)二硫化物、3,3'-雙(三乙氧基矽烷基丙基)四硫化物、3,3'-雙(三甲氧基矽烷基丙基)四硫化物、2,2'-雙(三乙氧基矽烷基乙基)四硫化物、3,3'-雙(三甲氧基矽烷基丙基)三硫化物、3,3'-雙(三乙氧基矽烷基丙基)三硫化物、
3,3'-雙(三丁氧基矽烷基丙基)二硫化物、3,3'-雙(三甲氧基矽烷基丙基)六硫化物,及3,3'-雙(三辛氧基矽烷基丙基)四硫化物,及此等之混合物。含硫有機矽烷亦可為以下列化學式(IV)表示之一巰基有機金屬化合物:
有關化學式(IV),M'係矽,L係鹵素或-OR8,Q係氫、C1-C12烷基,或經鹵基取代之C1-C12烷基,R7係C1-C12亞烷基,R8係C1-C12烷基或含有從2至12個碳原子之烷氧基烷基,鹵素或(鹵)基團係氯、溴、碘,或氟,且n係1、2或3。於一非限制性實施例,具有二個巰基基團之巰基有機金屬反應物可被使用。
有用巰基有機金屬化合物之非限制性例子不受限地包含巰基甲基三甲氧基矽烷、巰基乙基三甲氧基矽烷、巰基丙基三甲氧基矽烷、巰基甲基三乙氧基矽烷、巰基乙基三丙氧基矽烷、巰基丙基三乙氧基矽烷、(巰基甲基)二甲基乙氧基矽烷、(巰基甲基)甲基二乙氧基矽烷、3-巰基丙基-甲基二甲氧基矽烷,及此等之混合物。
本發明之某些實施例,含硫有機矽烷可為一巰基有機金屬化合物,諸如,不同於用於步驟(a)之處理組成物中的有機矽烷的巰基矽烷,例如,巰基丙基三甲氧基矽烷及/或巰基甲基三乙氧基矽烷。
再者,被考量係可用於本發明方法之步驟(a)中
之不同於以化學式(I)表示之前述有機矽烷偶合劑的以化學式(IV)表示之含硫有機矽烷可為其中巰基基團被封閉(即,巰基之氫原子係以另外基團替代)之一巰基有機金屬化合物。經封閉之巰基有機金屬化合物可具有經由一單鍵與硫直接結合之一不飽和雜原子或碳。特別之封閉基團的非限制性例子可包含硫代羧酸酯、二硫代氨基甲酸酯、硫代磺酸酯、硫代硫酸酯、硫代磷酸酯、硫代膦酸酯,及硫代亞膦酸酯。
於其中一經阻斷之巰基有機金屬化合物係作為一選擇性偶合材料之某些非限制性實施例,一解封閉劑可添加至聚合物化合物混合物以使經封閉之巰基有機金屬化合物解封閉。於其中水及/或醇存在於混合物中之某些非限制性實施例,諸如三級胺、路易士酸或硫醇之催化劑可被用以藉由水解或醇解起始及促進封閉基團喪失,以釋放相對應之巰基有機金屬化合物。經封閉之巰基矽烷的非限制性例子可不受限地包含2-三乙氧基矽烷基-1-乙基硫代乙酸酯、3-三甲氧基-矽烷基-1-丙基硫代辛酸酯、雙-(3-三乙氧基矽烷基-1-丙基)-甲基二硫代膦酸酯、3-三乙氧基矽烷基-1-丙基二甲基硫代亞膦酸酯、3-三乙氧基矽烷基-1-丙基甲基硫代硫酸酯、3-三乙氧基矽烷基-1-丙基甲苯硫代磺酸酯,及此等之混合物。
此等選擇性之含硫有機矽烷的量可廣泛改變,且可依選擇之特定材料而定。例如,以未經處理的填料之重量為基準,此等選擇性之含硫有機矽烷的量可為大於0.1%,
諸如,以未經處理的填料之重量為基準,係從0.5%至25%,或從1%至20%,或從2%至15%。
於某些實施例,處理組成物可進一步包含一鹵官能性有機矽烷,其包含自如下衍生之擁有鹵素官能性及烷二氧矽烷基官能性之單體、二聚物、寡聚物及/或聚合物之化合物:(i)含多羥基之化合物,其中,烷二氧基團係經由Si-O鍵與單一Si原子共價鍵結形成一環;及/或(ii)烷二氧基團係經由Si-O鍵與至少二個Si原子共價鍵結,形成二聚物、寡聚物,或聚合物,其中,相鄰矽烷基單元係經由橋接烷烷氧基結構彼此鍵結。此等鹵基官能性有機矽烷係詳細描述於2011年1月6日公開之美國公開專利申請案第2011/0003922A1號案,第[0020]至[0057]段,引述部份在此被併入以供參考。
任何前述偶合劑之混合物可用於本發明之方法。
某些實施例,除此處先前所述之處理劑外,處理組成物可選擇性進一步包含不同於此處理劑之一第一或另外非偶合劑/相容劑。此另外之非偶合劑/相容劑可選自飽和生物聚合物、飽和脂肪酸、飽和有機酸、飽和聚合物乳化液、飽和聚合物塗覆組成物,及此等之混合物。此另外之非偶合劑/相容劑可另外或進一步包含一界面活性劑,其係選自陰離子性、非離子性,及兩性之界面活性劑,與其等之混合物。於此處使用時,術語界面活性劑排除不飽和脂肪酸。
某些實施例,以未經處理的填料之總重量,諸如,沉澱之SiO2的總質量為基準,此另外之非偶合劑/相容劑可以從大於1重量%至25重量%之量存在。例如,此另外之非偶合劑/相容劑可選自脂肪酸鹽、烷基肌氨酸酯、烷基肌氨酸鹽,及此等之混合物。此等之特別非限制性例子可於U.S.7,569,107,第5欄第9行至第7欄第21行發現,引述部份在此被併入以供參考。本發明之某些實施例,此另外之非偶合劑/相容劑可包含選自硬脂酸鈉、硬脂酸銨、椰油酸銨、月桂酸鈉、椰油醯基肌氨酸鈉、月桂醯基肌氨酸鈉、牛脂之鈉皂、椰子油之鈉皂、肉荳蔻醯基肌氨酸鈉,及/或硬脂醯基肌氨酸之一或多種陰離子性界面活性劑。
某些實施例,以未經處理的填料總重量,諸如,沉澱之SiO2總質量為基準,此另外之非偶合劑/相容劑係以從大於1重量%至最高且包含25重量%之量存在,例如,2.0重量%至20.0重量%,或4重量%至15重量%,或5重量%至12重量%。
某些實施例,此另外之非偶合劑/相容劑可為一非偶合有機矽烷。某些實施例,可選作此另外之非偶合劑/相容劑之非偶合矽烷的非限制性例子包含十八烷基三乙氧基矽烷、十八烷基三氯矽烷、十八烷基三甲氧基矽烷、丙基三乙氧基矽烷、丙基三甲氧基矽烷、丙基三氯矽烷、正辛基三甲氧基矽烷、正辛基三乙氧基矽烷、正辛基三氯矽烷、正己基三甲氧基矽烷、正己基三乙氧基矽烷,及/或正己基三氯矽烷。
需瞭解為了本發明之目的,某些實施例,包含如上所述之具有結構(I)之有機矽烷的前述有機矽烷之任一者可包含其部份水解物。
與本發明各種不同實施例使用之未經處理的填料可使用此項技藝認知之方法的任一者製備。例如,於其中未經處理的填料係經處理的二氧化矽之例子,未經處理的填料可藉由使可溶性金屬矽酸鹽之水溶液與一酸溶劑混合形成二氧化矽漿料;二氧化矽漿料選擇性地可被老化;酸或鹼可添加至選擇性經老化之二氧化矽漿料以調整漿料之pH;二氧化矽漿料可被過濾,選擇性經清洗,然後,使用此項技藝認知之技術乾燥而製備。依據本發明之各種實施例,於乾燥前,諸如上述任一者之一處理組成物可於上述方法之任一步驟添加。
某些另外實施例,本發明係有關於一種用於製造經處理的沉澱二氧化矽之方法,其包含:(a)使鹼金屬矽酸鹽及酸組合形成一未經處理的漿料;(b)選擇性地以包含此處理劑之此處理組成物處理未經處理的漿料,形成一經處理的漿料;(c)使步驟(a)之未經處理的漿料乾燥,或使(b)之經處理的漿料乾燥,於每一情況產生經乾燥之沉澱二氧化矽;(d)以包含此處理劑之處理組成物形成步驟(c)之經乾燥之沉澱二氧化矽的一水性漿料,形成一經處理的二氧化矽漿料;及(e)使經處理的二氧化矽漿料乾燥產生一經乾燥之經處
理的沉澱二氧化矽。
某些實施例且參考如上概述之方法,無論一處理組成物是否於乾燥前被包含於未經處理的漿料中,經乾燥之沉澱二氧化矽(經處理或未經處理)的水性漿料可被製備,然後,一處理組成物可被添加形成沉澱二氧化矽之經處理的漿料,其後再次乾燥產生一經處理的沉澱二氧化矽。
此外,任何先前實施例之沉澱二氧化矽可被包含於一聚合物摻合物中且與此處先前所述之一處理組成物混練。
用於形成經處理的二氧化矽之方法的更詳細說明可於此處如下之範例中發現。
可與本發明之某些實施例使用的適合金屬矽酸鹽可包含此項技藝所知之廣泛各種材料。非限制性之例子可不受限地包含矽酸鋁、矽酸鋰、矽酸鈉、矽酸鉀,及此等之混合物。金屬矽酸鹽可以下列結構式表示:M2O(SiO2)x,其中,M可為鋁、鋰、鈉,或鉀,且x範圍可為從0.1至4。
可與本發明之某些實施例使用之適合酸可選自此項技藝已知之廣泛各種酸。非限制性之例子可不受限地包含礦物酸、有機酸、二氧化碳、硫酸,及此等之混合物。
藉由本發明方法製備之經處理的填料係適於包含於有機聚合物組成物中。藉由本發明方法製備之經處理的填料材料可與某些實施例用於橡膠混練組成物,諸如,用於製造輪胎及輪胎組件(諸如,輪胎面)之橡膠組成物。
依據本發明方法製備之經處理的填料可包含於
其內之聚合物組成物不受限地包含於Kirk Othmer Encyclopedia of Chemical Technology,第四版,1996,第19冊,881-904頁中所述者,其描述內容在此被併入以供參考。依據本發明各種實施例製備之經處理的填料可與聚合物或其可聚合組份於此聚合物或可聚合組份之物理型式係呈任何液體或可混練型式(諸如,溶液、懸浮液、膠乳、分散液等)時混合。含有本發明之經處理的填料之聚合物組成物可藉由此項技藝已知之任何方式研磨、混合、模製,及選擇性地固化,形成一聚合物物件。聚合物種類可不受限地包含熱塑性及熱固性樹脂、橡膠混練物,及具有彈性體性質之其它聚合物。
前述聚合物可包含,例如,醇酸樹脂、經油改質之醇酸樹脂、不飽和聚酯、天然油(例如,亞麻子、桐油、大豆)、環氧化物、尼龍、熱塑性聚酯(例如,聚對苯二甲酸乙二酯、聚對苯二甲酸丁二酯)、聚碳酸酯,即,熱塑性及熱固性,聚乙烯、聚丁烯、聚苯乙烯、聚丙烯、乙烯丙烯共聚物及三元共聚物、丙烯酸樹脂(丙烯酸、丙烯酸酯、甲基丙烯酸酯、丙烯醯胺、其等之鹽、鹵化氫等之均聚物及共聚物)、酚樹脂、聚縮醛(均聚物及共聚物)、聚胺甲酸酯、聚碸、多硫化物橡膠、硝基纖維素、丁酸乙烯酯、乙烯類(含有氯乙烯及/或乙酸乙烯酯之聚合物)、乙基纖維素、纖維素乙酸酯及丁酸酯、黏膠人造絲、蟲膠、蠟、乙烯共聚物(例如,乙烯-乙酸乙烯酯共聚物、乙烯-丙烯酸共聚物、乙烯丙烯酸酯共聚物)、有機橡膠(合成及天然橡膠)等。
可用於一聚合物組成物中之經處理的填料之量可依聚合物組成物及欲自此聚合物組成物形成之物件的合意性質廣泛變化。例如,以聚合物組成物總重量為基準,存在於聚合物組成物中之經處理的填料之量範圍可為從5最高達70重量%。
某些非限制性實施例,聚合物組成物可包含一有機橡膠。此等橡膠之非限制性例子可不受限地包含天然橡膠;自丁二烯及其同系物及衍生物均聚合反應形成者,諸如:順-1,4-聚異戊二烯;3,4-聚異戊二烯;順-1,4-聚丁二烯;反-1,4-聚丁二烯;1,2-聚丁二烯;及自丁二烯及其同系物及衍生物與一或多種含有乙烯不飽和之可共聚合單體(諸如,苯乙烯及其衍生物、乙烯基-吡啶及其衍生物、丙烯腈、異丁烯,及經烷基取代之丙烯酸酯,諸如,甲基丙烯酸甲酯)共聚合反應形成者。進一步非限制性例子可包含由各種百分率之苯乙烯及丁二烯組成且使用所欲之各種丁二烯異構物之苯乙烯-丁二烯共聚物橡膠(其後稱為"SBR");苯乙烯、異戊二烯及丁二烯聚合物之三元共聚物,及其等之各種異構物;以丙烯腈為主之共聚物及三元共聚物橡膠組成物;及以異丁烯為主之橡膠組成物;及其等之混合物,例如,於美國專利第4,530,959;4,616,065;4,748,199;4,866,131;4,894,420;4,925,894;5,082,901;及5,162,409號案中所述。
適合有機聚合物之非限制性例子可包含乙烯與其它高α烯烴(諸如,丙烯、丁烯-1,及戊烯-1)及二烯單體之共聚物。有機聚合物可為嵌段、無規,或序列,且可藉
由此項技藝所知之方法製備,不受限地諸如,乳化(例如,e-SBR)或溶液聚合反應方法(例如,s-SBR)。用於本發明之聚合物的進一步非限制性例子可包含經部份或完全官能化者,包含經偶合或星狀分支之聚合物。經官能化之有機橡膠的另外非限制性例子可包含聚氯丁二烯、氯丁基及溴丁基橡膠,與溴化異丁烯-共-對甲基苯乙烯橡膠。於一非限制性實施例,有機橡膠可為聚丁二烯、s-SBR,及此等之混合物。
聚合物組成物可為一可固化橡膠。術語"可固化橡膠"係打算包含天然橡膠及其各種未加工及改造型式與各種合成橡膠。於另外非限制性實施例,可固化橡膠可包含SBR與丁二烯橡膠(BR)之組合、SBR、BR與天然橡膠之組合,及先前揭露作為有機橡膠之材料的其它組合。於本發明之說明,除非其它指示外,術語"橡膠"、"彈性體"及“橡膠彈性體”可互換使用。術語"橡膠組成物"、"經混練之橡膠"及"橡膠混練物"可互換使用指與各種成份及材料摻合或混合之橡膠,且此等術語係具有橡膠混合或橡膠混練技藝之技術者所知。
包含藉由本發明方法製造之經處理的填料之橡膠組成物可用於製造無數種橡膠物件,諸如,輪胎(其至少一組件(例如,胎面)包含此經固化之橡膠組成物),與其它橡膠物件,諸如,鞋底、軟管、密封墊、纜線護套、墊片、皮帶等。包含藉由本發明方法製造之經處理的填料之橡膠組成物係特別有利地用於製造輪胎胎面,展現低滾動阻力
且高抗磨性,包含當輪胎胎面係以天然橡膠為主時。再者,某些實施例,對於含有藉由本發明方法製造之經處理的填料之此等天然橡膠組成物可達成較低固化溫度。
本發明之經處理的填料(呈粉末、顆粒、丸粒、漿料、水性懸浮液,或溶劑懸浮液)可與基本材料(即,用於欲製造之產物中的材料)組合形成一稱為母料之混合物。於此母料,經處理的填料可以比於最終產物中更高之濃度存在。此混合物之等分物典型上於混合操作期間添加至生產尺寸量,以助於使極小量之此等添加劑均勻分散至聚合物組成物,例如,塑料、橡膠,及塗覆組成物。
經處理的填料可與乳化及/或溶液聚合物(例如,包含溶液苯乙烯/丁二烯(SBR)之有機橡膠、聚丁二烯橡膠,或其等之混合物)組合形成一母料。一考量到之實施例係包含有機橡膠、水不可溶混之溶劑、經處理的填料,及選擇性之加工油的組合之一母料。此一產物可由一橡膠生產商供應至輪胎製造商。輪胎製造商使用母料之益處係經處理的填料係均勻分散於橡膠,造成使用以製造經混練之橡膠的混合時間達最小。母料可含有每100份橡膠為10至150份(phr)之經處理的二氧化矽,較佳係從20至130phr,更佳係從30至100phr,且最佳係從50至80phr。
本發明於下列範例作更明確說明,此等範例係打算僅作為例示,因為其內之許多修改及變化對熟習此項技藝者係明顯的。除非其它特定外,所有份數及所有百分率係以重量。
本申請專案之範例中報導之二氧化矽CTAB表面積值係使用一CTAB溶液及其後說明之方法判定。分析係使用裝設一Metrohm可互換"Snap-In" 50毫升量管之一Metrohm 751 Titrino自動滴定管,及裝設一550nm過濾器之一Brinkmann探針比色計PC 910型實施。此外,一Mettler Toledo HB43或等化物被用於判定二氧化矽之105℃水分損失,且一Fisher Scientific CentrificTM離心機225型被用以分離二氧化矽及殘餘CTAB溶液。過量CTAB係藉由以AEROSOL® OT(磺基琥珀酸二辛基鈉,可得自Cytec Industries,Inc.)之溶液滴定至達到最大濁度(此係以探針比色計檢測)為止而判定。最大濁度玷被取作為相對應於150毫伏特讀數。獲知一特定重量之二氧化矽吸收之CTAB量及CTAB分子佔據之空間,二氧化矽之外比表面積被計算,且以乾燥重量為基準,以平方公尺/克作報導。
用於測試及製備之溶液包含具pH 9.6之緩衝液、醯基[十六烷基]三甲基溴化銨(CTAB,亦稱為十六烷基三甲基溴化銨,工業級)、AEROSOL® OT,及1N氫氧化鈉。具pH 9.6之緩衝溶液係藉由使3.101克之原硼酸(99%;工業級,結晶)溶於含有500毫升之去離子水及3.708克之氯化鉀固體(Fisher Scientific,Inc.,工業級,結晶)之1公升量瓶而製備。使用一滴管,添加36.85毫升之1N氫氧化鈉溶液。此溶液被混合及稀釋至刻度。
CTAB溶液係使11.0克+/-0.005克之製備的CTAB用於一稱皿上而製備。CTAB顆粒轉移至一2公升燒杯,且稱皿以去離子水沖洗。約700毫升之pH 9.6緩衝溶液及1000毫升之蒸餾水或去離子水添加至2公升燒杯,且以一磁性攪拌棒攪拌。一大的表玻璃置於燒杯上,且燒杯於室溫攪拌至CTAB粉末完全溶解為止。溶液轉移至一2公升量瓶,以去離子水沖洗燒杯及攪拌棒。使氣泡消散,且溶液以去離子水稀釋至刻度。添加一大攪拌棒,且溶液於一磁性攪拌器上混合約10小時。CTAB溶液可於24小時後使用,且僅持續15天。AEROSOL® OT溶液係使用3.46克+/-0.005克置於一稱皿上製備。於稱皿上之AEROSOL® OT沖洗至含有約1500毫升去離子水及一大攪手棒之一2公升燒杯內。AEROSOL® OT溶液被溶液及沖洗至一2公升量瓶內。溶液稀釋至量瓶之2公升體積標記。AEROSOL® OT溶液於使用前老化最少12天。AEROSOL® OT溶液保存期係從製備日起2個月。
於表面積樣品製備前,CTAB溶液之pH被驗證且使用1N氫氧化鈉溶液調整至9.6+/-0.1之pH。對於測試計算,一空白樣品被製備及分析。5毫升CTAB溶液以吸量管吸取且55毫升去離子水添加至一150毫升燒杯,且於一Metrohm 751 Titrino自動滴定器上分析。自動滴定器經程式化,以下列參數判定空白組及樣品:測量點密度=2,信號漂移=20,平衡時間=20秒,起始體積=0毫升,停止體積=35毫升,且固定端點=150mV。滴定管尖端及比色計探針置於剛過溶
液表面下,其等之置放係使得尖端及光探針路徑長度係完全浸入。尖端及光探針二者皆離燒杯底部基本上等距離,且彼此不接觸。以最小攪拌(於Metrohm 728攪拌器上設定為1),於每一空白組及樣品判定前,比色計設定為100% T,且滴定係以AEROSOL® OT溶液起始。端點係以150mV時之滴定劑體積(毫升)記錄。
為了測試樣品製備,約0.30克之粉末狀二氧化矽稱重至含有一攪拌棒之一50毫升容器內。顆粒狀二氧化矽樣品(於研磨及稱重前)翻動獲得一代表性子樣品。一咖啡研磨式研磨器用於研磨顆粒狀材料。然後,30毫升之經pH調整之CTAB溶液以吸量管吸取至含有此0.30克之粉末狀二氧化矽的樣品容器內。然後,二氧化矽及CTAB溶液於一攪拌器上混合35分鐘。混合完全時,二氧化矽及CTAB溶液離心處理20分鐘,使二氧化矽與過量CTAB溶液分離。當離心處理完全時,CTAB溶液以吸量管吸取至一無分離固體(稱為“離心物”)之乾淨容器內。為了樣品分析,50毫升之去離子水置於含有一攪拌棒之一150毫升燒杯內。然後,10毫升之樣品離心物以吸量管吸取至相同燒杯內以供分析。樣品係使用與用於空白組溶液相同之技術及程式化程序分析。
於本申請案之範例中報導之BET表面積值係依據布魯諾爾艾米特及泰勒(BET)方法依據ASTM D1993-03判定。BET表面積係藉由使以一Micromeritics TriStar 3000TM儀器進行之氮吸附等溫測量的五個相對壓力點作擬合而判定。一流動Prep-060TM站提供熱及連續氣流,以製備
供分析之樣品。於氮吸附前,二氧化矽樣品藉由於流動氮氣(P5等級)內加熱至160℃之溫度至少一(1)小時而乾燥。
於本申請案之範例中報導的碳(C)及硫(S)重量百分率值係使用一Flash 2000元素分析器判定。此系統係被安裝監測碳及硫。典型參數包含:燃燒爐係設為950℃,GC爐溫度係設為65℃,載劑氦氣流速係設為140毫升/分鐘,參考氦氣流速係設為100毫升/分鐘,氧流速係設為250毫升/分鐘,且氧注射時間係5秒。對於一特定操作,標正標準物、樣品,及對照組被典型操作。每一者係添加8-10毫克之五氧化二釩(V2O5)。樣品尺寸係於2-4毫克之間,且其等於分析前係密封於錫膠囊中。若對照標準物未於於已知接受值相對±10%內或重複之樣品操作未相配(相對±5%),,整個樣品操作再次分析。
本申請案之範例中報導的硫醇(SH)重量百分率值係使用一反滴定法判定。樣品分散於75毫升之2-丙醇中,其後,添加過量之0.1N碘溶液。然後,測試溶液以氮氣沖刷,封蓋,及使其攪拌15分鐘。其後,未反應之碘以標準化之0.05N硫代硫酸鈉反滴定至無色端點。
水(74.9公升)添加至一150公升之反應槽,且經由
間接水蒸氣線圈加熱而加熱至87℃。矽酸鈉(3.0公升)以560毫升/分鐘之速率添加達成2.6克/公升之Na2O濃度及7.8之酸值。Na2O濃度及酸值係使用上述Na2O滴定方法及酸值滴定方法滴定矽酸鈉/水之混合物而確定。溫度係經由間接水蒸氣線圈加熱維持於87℃,且沉澱步驟被起始。150公升之反應器經由主要槽攪拌器攪拌。主要攪拌器開著,開始一同時附加沉澱步驟。矽酸鈉(50.4公升)及3.2公升之硫酸於90分鐘期間同時添加。矽酸鈉係經由接近槽底部之一開放管以560毫升/分鐘之速率添加,且硫酸於次要高速混合器葉片上直接添加。酸添加速率於90分鐘同時添加步驟期間平均係36.0毫升/分鐘。
於同時添加步驟結束時,起始一30分鐘老化步驟(A.2使用100分鐘老化)。溶液之pH使用硫酸調整至8.5。SILQUEST® A-1891(3-巰基丙基三乙氧基矽烷,可得自Momentive)係以每100份二氧化矽為5.5份(“PHS”,744.3克)添加至反應器。關掉次要高速攪拌器,且表1中指示之脂肪酸於15-20分鐘期間以5.5PHS緩慢噴灑或添加至反應器內。反應混合物於攪拌下完成老化持續該時間(CE-A.1、A.3及A.4係30分鐘,A.2係100分鐘)之剩餘者。溫度維持於87℃。老化步驟完全後,添加硫酸達到4.8之最終批式pH。
混合物泵取至一壓濾機,並且清洗至測得之沖洗水導電度少於1000微西門子(microsiemen)為止。形成之濾餅以水再次漿化形成一可泵取漿料,且使用一Niro噴灑乾燥器(Utility Model 5,具有FU-1型之旋轉霧化器,Niro Inc.)
噴灑乾燥。經噴灑乾燥之粉末使用一Alexanderwerk WP120X40碾壓機以下列條件粒化;螺旋速度=55rpm,碾壓機速度4.5rpm,壓碎機速度=55rpm,液壓=25巴,及篩網尺寸~7篩目。合成二氧化矽之物理性質係綜述於表1。
用於比較範例A本發明及比較之二氧化矽的典型客車胎面配方係顯示於表2。裝設4個翼轉子之一1.89公升(L)Kobelco Stewart Bolling Inc.混合器("00"型)及一Farrel 12英吋雙輥橡膠研磨機被用於依據ASTM D3182-89混合此等成份。
配方係使用一非生產道(non-productive pass)混合,使化合物冷卻,其後於一雙輥研磨機上精磨。對於第一道(first pass),混合速度調整至85rpm,且起始溫度係150℉。可自LANXESS購得之溶液苯乙烯丁二烯橡膠(SBR),BUNA® VSL 5228-2(乙烯基含量:52%;苯乙烯含量:28%;經處理的蒸餾芳香族萃取物(TDAE)油含量:每百分橡膠係
37.5份(phr);幕尼(Mooney)黏度(ML(1+4)100℃):50),及可自The Goodyear Tire & Rubber Company購得之丁二烯橡膠(BR),BUDENETM 1207(順1,4含量98%;幕尼黏度(ML(1+4)100℃):55),聚合物係添加至混合器。進入混合周期內30秒後,一半之測試二氧化矽添加至混合器。進入混合周期內另外30秒後,另一半測試二氧化矽與購自H & R Group Inc.之VIVATEC® 500 TDAE加工油添加至混合器。進入混合周期內另外30秒後,栓塞被升高且滑道被清掃,即,入口滑道上之覆蓋物被升高,且於滑道發現之任何物料被掃回混合器內,且栓塞被下降。進入混合周期內另外30秒後,自Zinc Corporation of America購得之KADOX®-720C經表面處理的氧化鋅、自R.E.Carroll購得之橡膠等級硬脂酸、自Harwick Standard購得且描述為N-(1,3-二甲基丁基)-N'-苯基-對-苯二胺之Stangard SANTOFLEX® 13抗臭氧劑,及自AddivantTM USA,LLC.獲得之SUNPROOF®改良式抗臭氧劑烴蠟之組合添加至混合器。另外30秒後,栓塞被升高且滑道被清掃。從向前進入混合周期內150秒,混合器速度被調整達到及/或維持338℉ +/- 5℉之溫度持續390秒時間範圍。於總混合時間約540秒後,第一道於338℉ +/- 5℉之溫度下降。
購自Taber,Inc.之Rubber Makers硫(“RM硫”),100%活性,自Harwick Standard購得之SANTOCURE® CBS,正環己基-2-苯并噻唑亞磺醯胺,及自Harwick Standard Inc.購得之二苯基胍(DPG)摻合至於一雙輥橡膠研磨機上之冷
卻第一道母料內。研磨進行約5分鐘,實施5次側向切割(side cut)及5次最終道(end pass)。
應力/應變測試樣本於150℃固化30”,而所有其它測試樣本於150℃固化40”。樣本製備及測試使用第2部份(如上)所示之程序及設備實施。化合物性能性質係顯示於表3。
與飽和脂肪酸對照組CE-A.1A相比,關於不飽和度之衝擊的觀察被觀察到。一般,以固定固化包(cure package)(如表3所示),伸長率因使用不飽和脂肪酸而增加。
再者,相對於比較例,此二化合物之韌度增加。
於不飽和脂肪酸之情況,固化劑DPG、CBS及RM硫之相對量可被改變以達成具有無法可由飽和對兆物達成之不同物化性質的化合物。表4證實改變固化劑量的作用。例如,當以與具相同鏈長度之飽和對照組相比為低及高含量改變加速劑CBS,諸如磨耗損失、韌度及硬度之性質會受不飽和型式影響。
水(85.0公升)添加至150公升之反應器槽,且經由間接水蒸氣線圈加熱而加熱至74℃。矽酸鈉(7.7公升)以383毫升/分鐘之速率添加達到7.2克/公升之Na2O濃度。Na2O濃度藉由使用上述Na2O滴定方法滴定矽酸鈉/水之混合物而確認。溫度於需要時經由間接水蒸氣線圈加熱調整至74℃,且沉澱步驟被起始。150公升之反應器經由主要槽攪拌器攪拌。主要攪拌器開著,且開始一同時附加沉澱步驟。矽酸鈉(34.5公升)及2.2公升之硫酸於90分鐘期間同時添加。矽酸鈉係經由接近槽底部之一開放管以383毫升/分鐘之速率添加,且硫酸於次要高速混合器葉片上直接添加。酸添加速率於90分鐘同時添加步驟期間平均係24.0毫升/分鐘。
於同時添加步驟結束時,反應器溫度升至85℃。次要高速攪拌器關掉,且表5所指示之不飽和脂肪酸於15-20分鐘期間以9.5PHS緩慢噴灑於反應器內。添加相容劑後,快速添加硫酸達4.8之最終批次pH。經脂肪酸合成之二氧化矽的性質係顯示於表5。
此程序作些微改變使用如下詳述之脂肪酸鹽合成經處理之二氧化矽。
特別地,水(74.9公升)添加至150公升之反應器槽,且經由間接水蒸氣線圈加熱而加熱至87℃。矽酸鈉(2.5公升)以560毫升/分鐘之速率添加達到2.6克/公升之Na2O濃度及7.8之酸值。Na2O濃度及酸值藉由使用上述Na2O滴定方法及酸值滴定方法滴定矽酸鈉/水之混合物而確認。溫度於需要時經由間接水蒸氣線圈加熱調整至87℃,且沉澱步驟被起
始。150公升之反應器經由主要槽攪拌器攪拌。主要攪拌器開著,且開始一同時附加沉澱步驟。矽酸鈉(50.4公升)及3.2公升之硫酸於90分鐘期間同時添加。矽酸鈉係經由接近槽底部之一開放管以560毫升/分鐘之速率添加,且硫酸於次要高速混合器葉片上直接添加。酸添加速率於90分鐘同時添加步驟期間平均係36.0毫升/分鐘。
於同時添加步驟結束時,起始一100分鐘老化步驟。溶液之pH使用硫酸調整至8.5。關掉次要高速攪拌器,且如表6中指示之脂肪酸鹽於15-20分鐘期間以8.1或9.9PHS緩慢噴灑至反應器內。反應混合物於攪拌下完成老化持續100分鐘之剩餘者。溫度維持於87℃。老化步驟完全後,添加硫酸達到4.8之最終批式pH。
二程序皆依據相同清洗及乾燥方式。混合物泵取至一壓濾機內,並且清洗至測得之沖洗水導電度少於1000微西門子為止。形成之濾餅以水再次漿化形成一可泵取漿料,且使用一Niro噴灑乾燥器(Utility Model 5,具有FU-1型之旋轉霧化器,Niro Inc.)噴灑乾燥。經噴灑乾燥之粉末使用一Alexanderwerk WP120X40碾壓機以下列條件粒化;螺旋速度=55rpm,碾壓機速度4.5rpm,壓碎機速度=55rpm,液壓=25巴,及篩網尺寸~7篩目。
用於比較範例B本發明及比較之二氧化矽的典型客車胎面配方係顯示於表7。裝設4個翼轉子之一1.89公升(L)Kobelco Stewart Bolling Inc.混合器("00"型)及一Farrel 12英吋雙輥橡膠研磨機被用於依據ASTM D3182-89混合此等成份。
配方係使用一非生產道混合,使化合物冷卻,其後於一雙輥研磨機上精磨。對於第一道,混合速度調整至85rpm,且起始溫度係150℉。自LANXESS購得之溶液SBR,Buna® VSL 5228-2(乙烯基含量:52%;苯乙烯含量:28%;TDAE油含量:37.5phr;幕尼黏度(ML(1+4)100℃):50),
及自The Goodyear Tire & Rubber Company獲得之BR,BudeneTM 1207(順1,4含量98%;幕尼黏度(ML(1+4)100℃):55),聚合物皆添加至混合器。進入混合周期內30秒後,一半之測試二氧化矽及全部的可購自Evonik之Si-69添加至混合器。進入混合周期內另外30秒後,另一半測試二氧化矽與購自H & R Group Inc.之Vivatec® 500 TDAE加工油添加至混合器。進入混合周期內另外30秒後,栓塞被升高且滑道被清掃,即,入口滑道上之覆蓋物被升高,且於滑道發現之任何物料被掃回混合器內,且栓塞被下降。於總混合時間約300秒後,第一道於320℉ +/- 5℉之溫度下降。
對於第二道,來自第一道之母料係與購自Zinc Corporation of America之Kadox®-720C經表面處理的氧化鋅裝填回混合器內。於混合周期內另外30秒後,購自R.E.Carroll之橡膠等級硬脂酸、描述為N-(1,3-二甲基丁基)-N'-苯基-對-苯二胺且購自Harwick Standard之Stangard Santoflex® 13抗臭氧劑,及購自AddivantTM USA,LLC之Sunproof®經改良的抗臭氧劑烴蠟之組合物添加至混合器。另外30秒後,栓塞被升高且滑道被清掃。從向前進入混合周期內150秒,混合器速度被調整達到及/或維持320℉ +/- 5℉之溫度持續660秒時間範圍。購自Taber,Inc.之Rubber Makers(RM)硫,100%活性,購自Harwick Standard之Santocure® CBS,正環己基-2-苯并噻唑噻唑亞磺醯胺,及購自Harwick Standard Inc之二苯基胍摻合至於一雙輥橡膠研磨機上之冷卻第二道母料內。研磨進行約5分鐘,實施5
次側向切割及5次最終道)。
應力/應變測試樣本於150℃固化30”,而所有其它測試樣本於150℃固化40”。樣本製備及測試使用第2部份(如上)所示之程序及設備實施。化合物性能性質係顯示於表8。
當相容劑用於較低表面積之二氧化矽上時,相容效果亦於降低之ML(1+4)幕尼黏度觀察到。範例B.2A及B.3A顯示比比較例CE-B.1A者更高之韌度值。鹽型式亦可被用於使此材料與二氧化矽反應。表9顯示混練配方,且表10顯示混練結果。
相關於比較例,觀察到本發明二氧化矽於幕尼黏度ML(1+4)降低。
雖然本發明已關於其某些實施例之特別細節作說明,但除了於申請專利範圍中包含外,不打算此等細節需被視為對本發明範圍之限制。
Claims (17)
- 一種用於製造經處理填料之方法,包含:(a)以一包含一為偶合劑之處理劑的處理組成物,來處理一包含未經處理之填料的漿料,從而形成一經處理填料漿料,其中該未經處理之填料係未被事先乾燥;及(b)使該經處理填料漿料乾燥,以製造經處理填料,其中,該處理劑包含下列之至少一者:(i)一不飽和脂肪酸,其包含一線性或分支的選擇性經取代之C4至C38烷基,其具有至少一個碳-碳雙鍵;及/或(ii)一(i)之該不飽和脂肪酸之衍生物,其中,至少一個碳-碳雙鍵係經反應以使其包含至少一官能基團;其中,該不飽和脂肪酸(i)及該衍生物(ii)之該不飽和脂肪酸於每一情況係相同或不同,且其中,該不飽和脂肪酸(i)及該衍生物(ii)之該不飽和脂肪酸每一者獨立地係選自由十一烯酸、α-亞麻油酸、花生四烯酸、二十二碳六烯烴、二十碳五烯酸、反油酸、芥酸、亞麻油酸、共軛亞麻油酸、反式亞麻油酸、十六碳烯酸、異油酸、肉荳蔻腦酸、棕櫚油酸、油酸、二十碳-9-烯酸、二十四碳烯酸,及其等之組合所組成之組群。
- 如請求項1之方法,其中,該未經處理的填料係選自矽酸鋁、二氧化矽凝膠、膠體二氧化矽、沉澱二氧化矽,及此等之混合物。
- 如請求項1之方法,其中,該填料包含沉澱二氧化矽。
- 一種用於製造經處理的沉澱二氧化矽之方法,包含:(a)使一鹼金屬矽酸鹽與一酸組合,以形成包含未經處理的二氧化矽之一漿料,其中,該未經處理的二氧化矽未被事先乾燥;(b)以包含一為偶合劑之處理劑之一處理組成物來處理該漿料,從而形成一經處理的漿料;及(c)使該經處理的漿料乾燥,以製造一經處理的沉澱二氧化矽,其中,該處理劑包含下列之至少一者:(i)一不飽和脂肪酸,其包含一線性或分支的選擇性經取代之C4至C38烷基,其具有至少一個碳-碳雙鍵;及/或(ii)一(i)之該不飽和脂肪酸之衍生物,其中,至少一個碳-碳雙鍵係經反應而使其包含至少一官能基團;其中,該不飽和脂肪酸(i)及該衍生物(ii)之該不飽和脂肪酸於每一情況係相同或不同,且其中,該不飽和脂肪酸(i)及該衍生物(ii)之該不飽和脂肪酸每一者獨立地係選自由十一烯酸、α-亞麻油酸、花生四烯酸、二十二碳六烯烴、二十碳五烯酸、反油酸、芥酸、亞麻油酸、共軛亞麻油酸、反式亞麻油酸、十六碳烯酸、異油酸、肉荳蔻腦酸、棕櫚油酸、油酸、二十碳-9-烯酸、二十四碳烯酸,及其等之組合所組成之組群。
- 如請求項4之方法,其中,該鹼金屬矽酸鹽包含矽酸鋁、矽酸鋰、矽酸鈉,及/或矽酸鉀。
- 一種用於製造經處理的沉澱二氧化矽之方法,包含:(a)使一鹼金屬矽酸鹽與一酸組合以形成包含未經處理的二氧化矽之一未經處理的漿料,其中,該未經處理的二氧化矽未被事先乾燥;(b)使該未經處理的漿料乾燥以製造經乾燥之沉澱二氧化矽;(c)以包含一為偶合劑之處理劑及選擇性之一與該處理劑不同之偶合劑及/或選擇性之一非偶合劑之一處理組成物形成該經乾燥之沉澱二氧化矽之一水性漿料,以形成一經處理的沉澱二氧化矽漿料;及(d)使該經處理的沉澱二氧化矽漿料乾燥以製造一經乾燥經處理的沉澱二氧化矽,其中,該處理劑包含下列之至少一者:(i)一不飽和脂肪酸,其包含一線性或分支的選擇性經取代之C4至C38烷基,其具有至少一個碳-碳雙鍵;及/或(ii)一(i)之該不飽和脂肪酸之衍生物,其中,至少一個碳-碳雙鍵係經反應而使其包含至少一官能基團;其中,該不飽和脂肪酸(i)及該衍生物(ii)之該不飽和脂肪酸於每一情況係相同或不同,且其中,該不飽和脂肪酸(i)及該衍生物(ii)之該不飽和脂肪酸每一者獨立地係選自由十一烯酸、α-亞麻油酸、花生四烯酸、二十二碳六烯烴、二十碳五烯酸、反油酸、芥酸、亞麻油酸、共軛亞麻油酸、反式亞麻油酸、十六碳烯酸、異油酸、肉荳蔻腦酸、棕櫚油酸、油酸、二十碳-9-烯酸、二十四碳烯酸,及其等之組合所組成之組群。
- 如請求項1之方法,其中,該不飽和脂肪酸係油酸及十一烯酸之至少一者。
- 如請求項1之方法,其中,該衍生物(ii)係存在於該處理劑中且該衍生物(ii)之每一官能基團係獨立地選自酮、硫醇、硫離子基、鹵基、胺基、烯基、炔基、羥基、酐,及環氧乙烷。
- 如請求項1之方法,其中,該處理組成物進一步包含一有機矽烷偶合劑,其係以下列化學式(I)表示:(R1)a(R2)bSiX4-a-b (I),其中,每一R1獨立地係包含1至36個碳原子及一官能基團之一烴基基團,其中,該烴基基團之該官能基團係乙烯基、烯丙基、己烯基、環氧基、環氧丙氧基、(甲基)丙烯醯氧基、硫化物、異氰酸基、多硫化物、巰基,或鹵素;每一R2獨立地係具有從1至36個碳原子或氫之一烴基基團,X獨立地係鹵素或具有1至36個碳原子之烷氧基;a係0、1、2,或3;b係0、1,或2;(a+b)係1、2,或3;但當b係1,(a+b)係2或3。
- 如請求項9之方法,其中,該處理組成物進一步包含不同於以化學式(I)表示之該有機矽烷的一有機矽烷。
- 如請求項1之方法,其中,該處理組成物進一步包含選自由(4-氯甲基-苯基)三甲氧基矽烷、(4-氯甲基-苯基)三乙氧基矽烷、[2-(4-氯甲基-苯基)-乙基]三甲氧基矽烷、[2-(4-氯甲基-苯基)-乙基]三乙氧基矽烷、(3-氯-丙烯基)-三甲氧基矽烷、(3-氯-丙烯基)-三乙氧基矽烷、(3-氯-丙基)-三乙氧基矽烷、(3-氯-丙基)-三甲氧基矽烷、三甲氧基-(2-對-甲苯基-乙基)矽烷,及三乙氧基-(2-對-甲苯基-乙基)矽烷,及此等之組合所組成族群之一有機矽烷。
- 如請求項1之方法,其中,該處理組成物進一步包含一非偶合劑,且其中,該非偶合劑係生物聚合物、脂肪酸、有機酸、聚合物乳化液、聚合物塗覆組成物,及其等之組合的一或多者,且其中,該非偶合劑係不同於該處理劑。
- 如請求項1之方法,其中,該處理組成物進一步包含一非偶合劑,其係選自一陰離子性界面活性劑、一非離子性界面活性劑、一兩性界面活性劑及其等之組合,且以未經處理的填料之重量為基準,該非偶合劑係以從大於1重量%至25重量%之量存在。
- 一種經處理的填料,其係藉由請求項1之方法製造。
- 一種經處理的沉澱二氧化矽,其係藉由請求項4之方法製備。
- 一種橡膠組成物,包含:(i)藉由如請求項1之方法製造之該經處理的填料;(ii)藉由如請求項4之方法製造之該經處理的沉澱二氧化矽;或(iii)藉由如請求項6之方法製造之該經處理的沉澱二氧化矽。
- 如請求項16之橡膠組成物,其中,該橡膠組成物包含(i)天然橡膠或是(ii)一橡膠混練母料。
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