TW202424067A - 以自由基起始劑及硫代胺基甲酸酯行聚合物之流變改性 - Google Patents
以自由基起始劑及硫代胺基甲酸酯行聚合物之流變改性 Download PDFInfo
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- TW202424067A TW202424067A TW112133755A TW112133755A TW202424067A TW 202424067 A TW202424067 A TW 202424067A TW 112133755 A TW112133755 A TW 112133755A TW 112133755 A TW112133755 A TW 112133755A TW 202424067 A TW202424067 A TW 202424067A
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- Prior art keywords
- bis
- free radical
- tert
- butyl
- diisocyanate
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- 150000003512 tertiary amines Chemical class 0.000 description 1
- LVEOKSIILWWVEO-UHFFFAOYSA-N tetradecyl 3-(3-oxo-3-tetradecoxypropyl)sulfanylpropanoate Chemical compound CCCCCCCCCCCCCCOC(=O)CCSCCC(=O)OCCCCCCCCCCCCCC LVEOKSIILWWVEO-UHFFFAOYSA-N 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
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- 238000003856 thermoforming Methods 0.000 description 1
- 150000003573 thiols Chemical class 0.000 description 1
- 150000003606 tin compounds Chemical class 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- YONPGGFAJWQGJC-UHFFFAOYSA-K titanium(iii) chloride Chemical compound Cl[Ti](Cl)Cl YONPGGFAJWQGJC-UHFFFAOYSA-K 0.000 description 1
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Abstract
本發明係關於一種用於對聚合材料之流變進行改性的方法,該方法包含在該聚合材料中併入改性劑摻合物之步驟,該改性劑摻合物包含:a)自由基起始劑,其係選自過氧化物、基於碳之自由基產生劑、雙偶氮化合物或穩定硝醯基化合物;及b)式(1)之硫代胺基甲酸酯。本發明亦係關於一種藉由在該聚合材料中併入該改性劑摻合物可獲得的經改性聚合材料;以及關於該改性劑摻合物。
Description
本發明係關於一種用於對聚合材料之流變進行改性的方法,該方法包含在該聚合材料中併入改性劑摻合物之步驟,該改性劑摻合物包含:a)自由基起始劑,其係選自過氧化物、基於碳之自由基產生劑、雙偶氮化合物或穩定硝醯基化合物;及b)式(1)之硫代胺基甲酸酯。本發明亦係關於一種藉由在該聚合材料中併入該改性劑摻合物可獲得的經改性聚合材料;且亦係關於該改性劑摻合物。
藉由習用混配方法(例如藉由擠出或注射成型)進行的聚合物類型(具有不同莫耳質量、熔體黏度、密度、莫耳質量分佈等之聚合物類型)之受控製備為聚合物製造商及聚合物加工商/混料商所採用之常規製程。藉助於此聚合物製程步驟設定例如熔體黏度之所需參數關鍵取決於所採用添加劑之受控反應性及作用模式。自由基形成劑,尤其過氧化物,常用於對聚合材料之熔體黏度及流變進行改性。
已知各種問題:需要高濃度的自由基起始劑才能提供預期性能;市場及監管趨勢總體上推動減少添加劑之量,例如以滿足安全及可持續要求;尤其過氧化物常常為危險的,相當不穩定,對熱、衝擊或摩擦敏感,容易發生反應,其中主要問題為火災及爆炸危險。
由於例如過氧化物之許多自由基形成劑之分解溫度較低,通常低於聚合物加工溫度之習用溫度,因此過氧化物之使用僅允許在受限的「加工溫度窗」內起作用。儘管業界已開發出可靠的製程來確保其安全使用,但仍需要最佳化其作為自由基起始劑之性能以促進聚合材料之流變改性。
該等目標藉由一種用於對聚合材料之流變進行改性的方法來解決,該方法包含在該聚合材料中併入改性劑摻合物之步驟,該改性劑摻合物包含
a) 自由基起始劑,其係選自過氧化物、基於碳之自由基產生劑、雙偶氮化合物或穩定硝醯基化合物,及
b)式(1)之硫代胺基甲酸酯
其中
R
a係基於有機異氰酸酯,
基團-S-R
a係藉由與異氰酸酯基之反應引入,
R
b為視情況經取代及/或經間雜之C
2-C
40烷基,且
n等於或大於1。
該等目標由藉由在該聚合材料中併入該改性劑摻合物可獲得的經改性聚合材料來解決,其中該改性劑摻合物包含
a) 自由基起始劑,其係選自過氧化物、基於碳之自由基產生劑、雙偶氮化合物或穩定硝醯基化合物,及
b)式(1)之硫代胺基甲酸酯
其中
R
a係基於有機異氰酸酯,
基團-S-R
a係藉由與異氰酸酯基之反應引入,
R
b為視情況經取代及/或經間雜之C
2-C
40烷基,且
n等於或大於1。
該等目標藉由一種改性劑摻合物來解決,其中該改性劑摻合物包含
a) 自由基起始劑,其係選自過氧化物、基於碳之自由基產生劑、雙偶氮化合物或穩定硝醯基化合物,及
b)式(1)之硫代胺基甲酸酯
其中
R
a係基於有機異氰酸酯,
基團-S-R
a係藉由與異氰酸酯基之反應引入,
R
b為視情況經取代及/或經間雜之C
2-C
40烷基,且
n等於或大於1。
硫代胺基甲酸酯具有式(1)
其中
R
a係基於有機異氰酸酯,
基團-S-R
a係藉由與異氰酸酯基之反應引入,
R
b為視情況經取代及/或經間雜之C
2-C
40烷基,且
n等於或大於1。
殘基 Ra較佳係基於有機異氰酸酯,該有機異氰酸酯為其中各者未經取代或經C
1-C
4烷基或二(C
1-C
4烷基)胺基取代之二異氰酸環己酯、二異氰酸亞甲基雙(環己基)酯、異佛酮二異氰酸酯(isophorone diisocyanate)、二異氰酸苯酯、二苯基甲烷二異氰酸酯或二異氰酸萘酯,或為二異氰酸C
4-C
20烷酯,或係基於藉由上述二異氰酸酯與其自身及/或與多元醇之反應獲得之寡聚或聚合產物。
更佳地,殘基R
a係基於有機異氰酸酯,該有機異氰酸酯為其中各者未經取代或經C
1-C
4烷基或二(C
1-C
4烷基)胺基取代之二異氰酸苯酯、二苯基甲烷二異氰酸酯或二異氰酸萘酯,或係基於藉由上述二異氰酸酯與其自身及/或與多元醇之反應獲得之寡聚或聚合產物。
高度較佳地,R
a係基於有機異氰酸酯,該有機異氰酸酯為未經取代或經C
1-C
4烷基取代之二異氰酸苯酯,或係基於藉由上述二異氰酸酯與其自身及/或與多元醇之反應獲得之寡聚或聚合產物。
最佳地,R
a係基於甲苯-2,4-二異氰酸酯或甲苯-2,6-二異氰酸酯,或藉由上述二異氰酸酯與其自身及/或與多元醇之反應獲得之寡聚或聚合產物。
藉由上述二異氰酸酯與其自身之反應獲得之產物的實例為三當量甲苯-2,4-二異氰酸酯或甲苯-2,6-二異氰酸酯之以下反應產物,其分別具有式(2)及(3):
。
藉由上述二異氰酸酯與多元醇之反應獲得之產物的實例為甲苯-2,4-二異氰酸酯或甲苯-2,6-二異氰酸酯與式HO-CH
2-C(CH
2-OH)
2-CH
2-CH
3之多元醇的以下反應產物,其分別具有式(4)及(5):
。
多元醇較佳為包含兩個或更多個羥基之C
1-C
10烷醇,或為聚C
2-C
10烷二醇。
作為多元醇之較佳C
1-C
10烷醇為經兩個至四個,尤其兩個或三個羥基取代之C
1-C
10烷醇。尤其較佳為對應地經羥基取代之C
2-C
10烷醇,尤其C
2-C
6烷醇。高度較佳為式HO-CH
2-C(CH
2-OH)
2-CH
2-CH
3之多元醇。
較佳聚C
2-C
10烷二醇為聚C
2-C
6烷二醇,尤其式(7)之聚C
2-C
6烷二醇
,
其中y為2至600,尤其2至200且最佳2至100之數目。高度較佳為2至50,尤其2至20之數目。關於式(7),較佳為對應聚乙二醇或聚丙二醇。較佳地,多元醇為經兩個至四個羥基取代之C
2-C
6烷醇,或聚C
2-C
6烷二醇,尤其式(7)之聚C
2-C
6烷二醇。
在二異氰酸酯與其自身反應,或不同類型之二異氰酸酯與其自身反應的情況下,可產生不同寡聚物或聚合物之混合物,且在與多元醇發生另外反應的情況下,甚至可獲得更複雜的混合物。對應有機異氰酸酯為已知的或可根據已知方法獲得,例如根據WO05/070987。
殘基 R
b 可例如間雜有-O-、-NH-、-S-及/或羰基。R
b之可能取代基為-SH。對應C
8-C
40烷基,尤其C
8-C
20烷基為較佳的。
Rb較佳為未經間雜或間雜有-O-、-NH-、-S-及/或羰基,尤其間雜有-O-及/或羰基之C
2-C
40烷基。
尤其較佳地,R
b為未經間雜或間雜有-O-及/或羰基之C
8-C
40烷基,尤其C
8-C
20烷基。
n等於或大於1,諸如1至10,較佳1至5,或尤其1至3。在另一形式中,n可為1、2、3、4或5。
硫代胺基甲酸酯可藉由有機異氰酸酯與式H-S-R
b之
硫醇之反應獲得,其中對於R
b,上述定義及偏好適用。
基團-S-R
b係藉由與有機異氰酸酯之異氰酸酯基
反應而引入,且在反應產物中作為式(8)之基團鍵結
,
其中R
b如上文所定義。
鑒於上文,術語「經硫代化合物官能化之異氰酸酯」係關於對應的硫代胺基甲酸酯。
用於製備硫代胺基甲酸酯之上述方法通常在
催化劑,如三級胺,例如三伸乙基二胺、二甲基哌𠯤、二甲基乙醇胺、1,4-二氮雜雙環[2.2.2]辛烷或1,8-二氮雜雙環[5,4,0]十一碳-7-烯存在下進行,或用錫化合物(例如,二月桂酸二丁基錫)作為催化劑進行。三乙胺為較佳的。按有機異氰酸酯之重量計,催化劑例如以0.1至10重量%之量使用。反應通常在如四氫呋喃或乙酸乙酯之有機溶劑存在下且在例如30至80℃之溫度下進行。
適合之硫代胺基甲酸酯具有式(9)、(10)或(11)
,
,
其中在式(9)及(10)中之各者中,R
b如上文所定義且上述偏好應適用,或
,
其中對於式(11),R
b為未經間雜或間雜有-O-及/或羰基之C
8-C
40烷基,且針對R
b給出之上述偏好應適用。較佳硫代胺基甲酸酯為式(9)及(10)之化合物,尤其式(10)之化合物。
在另一形式中,較佳硫代胺基甲酸酯具有式(12)
。
自由基起始劑可選自過氧化物、基於碳之自由基產生劑、雙偶氮化合物或穩定硝醯基化合物,其中過氧化物及基於碳之自由基產生劑為較佳的。在一個形式中,自由基起始劑為過氧化物。在另一形式中,自由基起始劑為基於碳之自由基產生劑。
適合之
過氧化物為有機或無機過氧化物,較佳為有機過氧化物。適合之有機過氧化物之典型實例包括2,5-二甲基-2,5-二(三級丁基過氧基)己烷、2,5-二甲基-2,5-二(三級丁基過氧基)己炔-3、3,6,6,9,9-五甲基-3-(乙酸乙酯)-1,2,4,5-四氧基環壬烷、氫過氧化三級丁基、過氧化氫、過氧化二異丙苯基、過氧化異丙基碳酸三級丁酯、過氧化二-三級丁基、過氧化對氯苯甲醯基、二過氧化二苯甲醯基、過氧化三級丁基異丙苯基;過氧化三級丁基羥乙基、過氧化二-三級戊基及2,5-二甲基己烯-2,5-二過氧化異壬酸酯、過氧化乙醯基環己烷磺醯基、過氧化二碳酸二異丙酯、過氧化新癸酸三級戊酯、過氧化新癸酸三級丁酯、過氧化新戊酸三級丁酯、過氧化新戊酸三級戊酯、過氧化雙(2,4-二氯苯甲醯基)、過氧化二異壬醯基、過氧化二癸醯基、過氧化二辛醯基、過氧化二月桂醯基、過氧化雙(2-甲基苯甲醯基)、過氧化二丁二醯基、過氧化二乙醯基、過氧化二苯甲醯基、過氧化2-乙基己酸三級丁酯、過氧化雙(4-氯苯甲醯基)、過氧化異丁酸三級丁酯、過氧化順丁烯二酸三級丁酯、1,1-雙(三級丁基過氧基)-3,5,5-三甲基環己烷、1,1-雙(三級丁基過氧基)環己烷、過氧化異丙基碳酸三級丁酯、過氧化異壬酸三級丁酯(tert-butyl perisononaoate)、2,5-二-甲基己烷2,5-二苯甲酸酯、過氧化乙酸三級丁酯、過氧化苯甲酸三級戊酯、過氧化苯甲酸三級丁酯、2,2-雙(三級丁基過氧基)丁烷、2,2-雙(三級丁基過氧基)丙烷、過氧化二異丙苯基、過氧化2,5-二甲基己烷2,5-二-三級丁基、3-三級丁基過氧基-3-苯基苯酞、過氧化二-三級戊基、α,α'-雙(三級丁基過氧異丙基)苯、3,5-雙(三級丁基過氧基)-3,5-二甲基-1,2-二氧戊環、過氧化二-三級丁基、過氧化2,5-二甲基己炔2,5-二-三級丁基、3,3,6,6,9,9-六甲基-1,2,4,5-四氧雜環壬烷、氫過氧化對薄荷烷、氫過氧化蒎烷、二異丙基苯單-α-氫過氧化物、氫過氧化異丙苯或氫過氧化三級丁基。
在另一形式中,適合之過氧化物為2,5-二甲基-2,5-雙(三級丁基過氧基)己烷(DHBP)、2,5-二甲基-2,5-雙(三級丁基過氧基)己炔-3 (DYBP)、過氧化二異丙苯基(DCUP)、過氧化二-三級丁基(DTBP)、過氧化三級丁基-異丙苯基(BCUP)、雙(三級丁基過氧異丙基)苯(DIPP)、3,6,9-三乙基-3,6,9-三甲基-1,4,7-三過氧壬烷、二(三級丁基過氧異丙基)苯、過氧化二碳酸二鯨蠟酯或單過氧化順丁烯二酸三級丁酯。
較佳過氧化物為2,5-二甲基-2,5-雙(三級丁基過氧基)己烷(DHBP)、過氧化三級丁基異丙苯基(BCUP)及3,6,9-三乙基-3,6,9-三甲基-1,4,7-三過氧壬烷,尤其2,5-二甲基-2,5-雙(三級丁基過氧基)己烷(DHBP)及3,6,9-三乙基-3,6,9-三甲基-1,4,7-三過氧壬烷。過氧化物尤其為2,5-二甲基-2,5-二(三級丁基過氧基)己烷。
適合之
雙偶氮化合物為2,2'-偶氮雙異丁腈、2,2'-偶氮雙(2-甲基丁腈)、2,2'-偶氮雙(2,4-二甲基戊腈)、2,2'-偶氮雙(4-甲氧基-2,4-二甲基戊腈)、1,1'-偶氮雙(1-環己烷甲腈)、2,2'-偶氮雙(異丁醯胺)二水合物、2-苯基偶氮-2,4-二甲基-4-甲氧基戊腈、2,2'-偶氮雙異丁酸二甲酯、2-(胺甲醯基偶氮)異丁腈、2,2'-偶氮雙(2,4,4-三甲基戊烷)、2,2'-偶氮雙(2-甲基-丙烷)、呈游離鹼或鹽酸鹽形式之2,2'-偶氮雙(N,N'-二亞甲基異丁脒)、呈游離鹼或鹽酸鹽形式之2,2'-偶氮雙(2-脒基丙烷)、2,2'-偶氮雙{2-甲基-N-[1,1-雙(羥甲基)乙基]丙醯胺}或2,2'-偶氮雙{2-甲基-N-[1,1-雙(羥甲基)-2-羥乙基]丙醯胺}。
適合之
穩定硝醯基化合物具有通式(13)
或為含有一或多個式(14)之基團之化合物
其中各R為烷基,且T為完成5員或6員環所需之基團。兩個或更多個硝醯基可藉由經由T部分連接而存在於同一分子中,如下文所例示,其中E為式(15)之連接基團:
適合之穩定硝醯基化合物包括癸二酸雙(1-氧基-2,2,6,6-四甲基哌啶-4-基)酯、4-羥基-1-氧基-2,2,6,6-四甲基哌啶、4-乙氧基-1-氧基-2,2,6,6-四甲基哌啶、4-丙氧基-1-氧基-2,2,6,6-四甲基哌啶、4-乙醯胺基-1-氧基-2,2,6,6-四甲基-哌啶、1-氧基-2,2,6,6-四甲基哌啶、1-氧基-2,2,6,6-四甲基哌啶-4-酮、乙酸1-氧基-2,2,6,6-四甲基哌啶-4-基酯、2-乙基-己酸1-氧基-2,2,6,6-四甲基哌啶-4-基酯、硬脂酸1-氧基-2,2,6,6-四甲基哌啶-4-基酯、苯甲酸1-氧基-2,2,6,6-四甲基-哌啶-4-基酯、4-三級丁基-苯甲酸1-氧基-2,2,6,6-四甲基哌啶-4-基酯、丁二酸雙(1-氧基-2,2,6,6-四甲基哌啶-4-基)酯、己二酸雙(1-氧基-2,2,6,6-四甲基哌啶-4-基)酯、正丁基丙二酸雙(1-氧基-2,2,6,6-四甲基哌啶-4-基)酯、鄰苯二甲酸雙(1-氧基-2,2,6,6-四甲基哌啶-4-基)酯、間苯二甲酸雙(1-氧基-2,2,6,6-四甲基哌啶-4-基)酯、對苯二甲酸雙(1-氧基-2,2,6,6-四甲基哌啶-4-基)酯、六氫對苯二甲酸雙(1-氧基-2,2,6,6-四甲基-哌啶-4-基)酯、N,N'-雙(1-氧基-2,2,6,6-四甲基哌啶-4-基)己二醯胺、N-(1-氧基-2,2,6,6-四甲基哌啶-4-基)己內醯胺、N-(1-氧基-2,2,6,6-四甲基哌啶基)十二烷基丁二醯亞胺、2,4,6-參-[N-丁基-N-(1-氧基-2,2,6,6-四甲基哌啶-4-基)]-均三𠯤、4,4'-伸乙基雙(1-氧基-2,2,6,6-四甲基哌𠯤-3-酮)、2-氧基-1,1,3,3-四甲基-2-異吲哚、1-氧基-2,2,5,5-四甲基吡咯啶及N,N-雙-(1,1,3,3-四甲基丁基)氮氧化物。
適合之
基於碳之自由基產生劑具有式(16)
其中R
1、R
3、R
4及R
6中之各者獨立地選自由以下組成之群:氫;具有1至12個碳原子之經取代及未經取代之直鏈、分支鏈及環狀烴;及具有6至12個碳原子之經取代及未經取代之芳族烴;且R2及R5中之各者獨立地選自由以下組成之群:具有1至12個碳原子之經取代及未經取代之直鏈、分支鏈及環狀烴;及具有6至12個碳原子之經取代及未經取代之芳族烴,且其中R
1、R
2、R
3、R
4、R
5及R
6中之至少一者為具有6至12個碳原子之經取代或未經取代之芳族烴。
式(16)之基於碳之自由基產生劑可具有對稱以及不對稱結構。R
2及R
5中之各者可獨立地選自具有6至12個碳原子之經取代或未經取代之芳基,且R
1、R
3、R
4及R
6中之各者獨立地選自由氫及C1-C6烷基組成之群。
在另一實施例中,基於碳之自由基產生劑具有式(17)
其中R
7、R
8、R
9及R
10中之各者獨立地選自由以下組成之群:氫原子、C1-6烷基、C1-2烷氧基、腈基及鹵素原子,且其中R
1、R
3、R
4及R
6中之各者獨立地選自由氫及C1-6烷基組成之群。
在又另一實施例中,基於碳之自由基產生劑係選自由以下組成之群:2,3-二甲基-2,3-二苯基丁烷、2,3-二丙基-2,3-二苯基丁烷、2,3-二丁基-2,3-二苯基丁烷、2,3-二己基-2,3-二苯基丁烷、2-甲基-3-乙基-2,3-二苯基丁烷、2-甲基-2,3-二苯基丁烷、2,3-二苯基丁烷、2,3-二甲基-2,3-二-(對甲氧基苯基)-丁烷、2,3-二甲基-2,3-二-(對甲基苯基)-丁烷、2,3-二甲基-2-甲基苯基-3-(對-2'3'-二甲基-3'-甲基苯基-丁基)-苯基-丁烷、3,4-二甲基-3,4-二苯基己烷、3,4-二乙基-3,4-二苯基己烷、3,4-二丙基-3,4-二苯基己烷、4,5-二丙基-4,5-二苯基辛烷、2,3-二異丁基-2,3-二苯基丁烷、3,4-二異丁基-3,4-二苯基己烷、2,3-二甲基-2,3-二-(對三級丁基苯基)丁烷、5,6-二甲基-5,6-二苯基癸烷、6,7-二甲基-6,7-二苯基十二烷、7,8-二甲基-7,8-二(甲氧基苯基)-十四烷、2,3-二乙基-2,3-二苯基丁烷、2,3-二甲基-2,3-二(對氯苯基)丁烷、2,3-二甲基-2,3-二(對碘苯基)丁烷及2,3-二甲基-2,3-二(對硝基苯基)丁烷。
在另一實施例中,基於碳之自由基產生劑係選自由以下組成之群:2,3-二甲基-2,3-二苯基丁烷及3,4-二甲基-3,4-二苯基己烷,較佳為2,3-二甲基-2,3-二苯基丁烷。
自由基起始劑可以0.0001至5重量%,尤其0.001至5重量%且更佳0.01至5重量%之量添加至聚合材料,諸如聚烯烴中。在另一形式中,自由基起始劑可以0.01至2重量%,尤其0.01至1重量%之量添加至聚合材料,諸如聚烯烴中。
硫代胺基甲酸酯可以0.0001至5重量%,尤其0.001至5重量%且更佳0.01至5重量%之量添加至聚合材料,諸如聚烯烴中。在另一形式中,自由基起始劑可以0.01至2重量%,尤其0.01至1重量%之量添加至聚合材料,諸如聚烯烴中。
自由基起始劑與硫代胺基甲酸酯之
重量比通常為1:2至30:1,較佳1:1至20:1,尤其1.2:1至15:1。在另一形式中,自由基起始劑與硫代胺基甲酸酯之重量比可為1:1至10:1,較佳1.5:1至5:1,尤其2:1至4:1。在另一形式中,自由基起始劑與硫代胺基甲酸酯之重量比為1:2至30:1,較佳1:1至20:1,尤其1.5:1至5:1。
在另一形式中,聚合材料為聚烯烴,自由基起始劑為過氧化物,且自由基起始劑與硫代胺基甲酸酯之重量比為1:1至20:1。
在另一形式中,聚合材料為聚烯烴,自由基起始劑為過氧化物,其中該過氧化物為2,5-二甲基-2,5-雙(三級丁基-過氧基)己烷(DHBP)、2,5-二甲基-2,5-雙(三級丁基-過氧基)己炔-3 (DYBP)、過氧化二異丙苯基(DCUP)、過氧化二-三級丁基(DTBP)、過氧化三級丁基-異丙苯基(BCUP)、雙(三級丁基過氧異丙基)苯(DIPP)、3,6,9-三乙基-3,6,9-三甲基-1,4,7-三過氧壬烷、二(三級丁基過氧異丙基)苯、過氧化二碳酸二鯨蠟酯或單過氧化順丁烯二酸三級丁酯,且自由基起始劑與硫代胺基甲酸酯之重量比為1:1至20:1。
在另一形式中,聚合材料為聚烯烴,自由基起始劑為基於碳之自由基產生劑,且自由基起始劑與硫代胺基甲酸酯之重量比為1:1至20:1。
在另一形式中,聚合材料為聚烯烴,自由基起始劑為基於碳之自由基產生劑,其中基於碳之自由基產生劑具有式(17),且自由基起始劑與硫代胺基甲酸酯之重量比為1:1至20:1。
在另一形式中,聚合材料為聚烯烴,自由基起始劑為過氧化物,且自由基起始劑與硫代胺基甲酸酯之重量比為1.5:1至5:1。
在另一形式中,聚合材料為聚烯烴,自由基起始劑為基於碳之自由基產生劑,且自由基起始劑與硫代胺基甲酸酯之重量比為1.5:1至5:1。
在另一形式中,聚合材料為聚烯烴,自由基起始劑為基於碳之自由基產生劑,其中基於碳之自由基產生劑具有式(17),且自由基起始劑與硫代胺基甲酸酯之重量比為1.5:1至5:1。
在另一形式中,聚合材料為聚烯烴,自由基起始劑為過氧化物,自由基起始劑與硫代胺基甲酸酯之重量比為1:1至20:1,且Ra係基於有機異氰酸酯,該有機異氰酸酯為其中各者未經取代或經C1-C4烷基或二(C1-C4烷基)胺基取代之二異氰酸環己酯、二異氰酸亞甲基雙(環己基)酯、異佛酮二異氰酸酯、二異氰酸苯酯、二苯基甲烷二異氰酸酯或二異氰酸萘酯,或為二異氰酸C4-C20烷酯,或係基於藉由上述二異氰酸酯與其自身及/或與多元醇之反應獲得之寡聚或聚合產物。
在另一形式中,聚合材料為聚烯烴,自由基起始劑為過氧化物,其中該過氧化物為2,5-二甲基-2,5-雙(三級丁基-過氧基)己烷(DHBP)、2,5-二甲基-2,5-雙(三級丁基-過氧基)己炔-3 (DYBP)、過氧化二異丙苯基(DCUP)、過氧化二-三級丁基(DTBP)、過氧化三級丁基-異丙苯基(BCUP)、雙(三級丁基過氧異丙基)苯(DIPP)、3,6,9-三乙基-3,6,9-三甲基-1,4,7-三過氧壬烷、二(三級丁基過氧異丙基)苯、過氧化二碳酸二鯨蠟酯或單過氧化順丁烯二酸三級丁酯,自由基起始劑與硫代胺基甲酸酯之重量比為1:1至20:1,且Ra係基於有機異氰酸酯,該有機異氰酸酯為其中各者未經取代或經C1-C4烷基或二(C1-C4烷基)胺基取代之二異氰酸環己酯、二異氰酸亞甲基雙(環己基)酯、異佛酮二異氰酸酯、二異氰酸苯酯、二苯基甲烷二異氰酸酯或二異氰酸萘酯,或為二異氰酸C4-C20烷酯,或係基於藉由上述二異氰酸酯與其自身及/或與多元醇之反應獲得之寡聚或聚合產物。
在另一形式中,聚合材料為聚烯烴,自由基起始劑為基於碳之自由基產生劑,自由基起始劑與硫代胺基甲酸酯之重量比為1:1至20:1,其R
a係基於有機異氰酸酯,該有機異氰酸酯為其中各者未經取代或經C
1-C
4烷基或二(C
1-C
4烷基)胺基取代之二異氰酸環己酯、二異氰酸亞甲基雙(環己基)酯、異佛酮二異氰酸酯、二異氰酸苯酯、二苯基甲烷二異氰酸酯或二異氰酸萘酯,或為二異氰酸C
4-C
20烷酯,或係基於藉由上述二異氰酸酯與其自身及/或與多元醇之反應獲得之寡聚或聚合產物。
在另一形式中,聚合材料為聚烯烴,自由基起始劑為基於碳之自由基產生劑,其中基於碳之自由基產生劑具有式(17),自由基起始劑與硫代胺基甲酸酯之重量比為1:1至20:1,且Ra係基於有機異氰酸酯,該有機異氰酸酯為其中各者未經取代或經C
1-C
4烷基或二(C
1-C
4烷基)胺基取代之二異氰酸環己酯、二異氰酸亞甲基雙(環己基)酯、異佛酮二異氰酸酯、二異氰酸苯酯、二苯基甲烷二異氰酸酯或二異氰酸萘酯,或為二異氰酸C
4-C
20烷酯,或係基於藉由上述二異氰酸酯與其自身及/或與多元醇之反應獲得之寡聚或聚合產物。
在另一形式中,聚合材料為聚烯烴,自由基起始劑為過氧化物,自由基起始劑與硫代胺基甲酸酯之重量比為1:1至20:1,且R
a係基於有機異氰酸酯,該有機異氰酸酯為未經取代或經C
1-C
4烷基取代之二異氰酸苯酯,或係基於藉由上述二異氰酸酯與其自身及/或與多元醇之反應獲得之寡聚或聚合產物。
在另一形式中,聚合材料為聚烯烴,自由基起始劑為基於碳之自由基產生劑,自由基起始劑與硫代胺基甲酸酯之重量比為1.5:1至5:1,且Ra係基於有機異氰酸酯,該有機異氰酸酯為未經取代或經C
1-C
4烷基取代之二異氰酸苯酯,或係基於藉由上述二異氰酸酯與其自身及/或與多元醇之反應獲得之寡聚或聚合產物。
在另一形式中,聚合材料為聚烯烴,自由基起始劑為過氧化物,自由基起始劑與硫代胺基甲酸酯之重量比為1.5:1至5:1,且R
a係基於有機異氰酸酯,該有機異氰酸酯為未經取代或經C
1-C
4烷基取代之二異氰酸苯酯,或係基於藉由上述二異氰酸酯與其自身及/或與多元醇之反應獲得之寡聚或聚合產物。
在另一形式中,聚合材料為聚烯烴,自由基起始劑為基於碳之自由基產生劑,自由基起始劑與硫代胺基甲酸酯之重量比為1:1至20:1,且R
a係基於有機異氰酸酯,該有機異氰酸酯為未經取代或經C
1-C
4烷基取代之二異氰酸苯酯,或係基於藉由上述二異氰酸酯與其自身及/或與多元醇之反應獲得之寡聚或聚合產物。
在另一形式中,聚合材料為聚烯烴,自由基起始劑為過氧化物,自由基起始劑與硫代胺基甲酸酯之重量比為1:1至20:1,且硫代胺基甲酸酯為式(9)及(10)之化合物。
在另一形式中,聚合材料為聚烯烴,自由基起始劑為過氧化物,其中該過氧化物為2,5-二甲基-2,5-雙(三級丁基-過氧基)己烷(DHBP)、2,5-二甲基-2,5-雙(三級丁基-過氧基)己炔-3 (DYBP)、過氧化二異丙苯基(DCUP)、過氧化二-三級丁基(DTBP)、過氧化三級丁基-異丙苯基(BCUP)、雙(三級丁基過氧異丙基)苯(DIPP)、3,6,9-三乙基-3,6,9-三甲基-1,4,7-三過氧壬烷、二(三級丁基過氧異丙基)苯、過氧化二碳酸二鯨蠟酯或單過氧化順丁烯二酸三級丁酯,自由基起始劑與硫代胺基甲酸酯之重量比為1:1至20:1,且硫代胺基甲酸酯為式(9)及(10)之化合物。
在另一形式中,聚合材料為聚烯烴,自由基起始劑為基於碳之自由基產生劑,自由基起始劑與硫代胺基甲酸酯之重量比為1:1至20:1,且硫代胺基甲酸酯為式(9)及(10)之化合物。
在另一形式中,聚合材料為聚烯烴,自由基起始劑為基於碳之自由基產生劑,其中基於碳之自由基產生劑具有式(17),自由基起始劑與硫代胺基甲酸酯之重量比為1:1至20:1,且硫代胺基甲酸酯為式(9)及(10)之化合物。
在另一形式中,改性劑摻合物包含:自由基起始劑,其係選自過氧化物;及硫代胺基甲酸酯,其中R
a係基於有機異氰酸酯,該有機異氰酸酯為未經取代或經C1-C4烷基取代之二異氰酸苯酯,或係基於藉由上述二異氰酸酯與其自身及/或與多元醇之反應獲得之寡聚或聚合產物,且自由基起始劑與硫代胺基甲酸酯之重量比為1:2至30:1,較佳1:1至20:1,尤其1.5:1至5:1。
在另一形式中,改性劑摻合物包含:自由基起始劑,其係選自過氧化物,其中該過氧化物為2,5-二甲基-2,5-雙(三級丁基-過氧基)己烷(DHBP)、2,5-二甲基-2,5-雙(三級丁基-過氧基)己炔-3 (DYBP)、過氧化二異丙苯基(DCUP)、過氧化二-三級丁基(DTBP)、過氧化三級丁基-異丙苯基(BCUP)、雙(三級丁基過氧異丙基)苯(DIPP)、3,6,9-三乙基-3,6,9-三甲基-1,4,7-三過氧壬烷、二(三級丁基過氧異丙基)苯、過氧化二碳酸二鯨蠟酯或單過氧化順丁烯二酸三級丁酯;及硫代胺基甲酸酯,且自由基起始劑與硫代胺基甲酸酯之重量比為1:2至30:1,較佳1:1至20:1,尤其1.5:1至5:1。
在另一形式中,改性劑摻合物包含:自由基起始劑,其係選自過氧化物,其中該過氧化物為2,5-二甲基-2,5-雙(三級丁基-過氧基)己烷(DHBP)、2,5-二甲基-2,5-雙(三級丁基-過氧基)己炔-3 (DYBP)、過氧化二異丙苯基(DCUP)、過氧化二-三級丁基(DTBP)、過氧化三級丁基-異丙苯基(BCUP)、雙(三級丁基過氧異丙基)苯(DIPP)、3,6,9-三乙基-3,6,9-三甲基-1,4,7-三過氧壬烷、二(三級丁基過氧異丙基)苯、過氧化二碳酸二鯨蠟酯或單過氧化順丁烯二酸三級丁酯;及硫代胺基甲酸酯,其中R
a係基於有機異氰酸酯,該有機異氰酸酯為未經取代或經C
1-C
4烷基取代之二異氰酸苯酯,或係基於藉由上述二異氰酸酯與其自身及/或與多元醇之反應獲得之寡聚或聚合產物,且自由基起始劑與硫代胺基甲酸酯之重量比為1:2至30:1,較佳1:1至20:1,尤其1.5:1至5:1。
在另一形式中,改性劑摻合物包含:自由基起始劑,其係選自過氧化物,其中該過氧化物為2,5-二甲基-2,5-雙(三級丁基-過氧基)己烷(DHBP)、2,5-二甲基-2,5-雙(三級丁基-過氧基)己炔-3 (DYBP)、過氧化二異丙苯基(DCUP)、過氧化二-三級丁基(DTBP)、過氧化三級丁基-異丙苯基(BCUP)、雙(三級丁基過氧異丙基)苯(DIPP)、3,6,9-三乙基-3,6,9-三甲基-1,4,7-三過氧壬烷、二(三級丁基過氧異丙基)苯、過氧化二碳酸二鯨蠟酯或單過氧化順丁烯二酸三級丁酯;及硫代胺基甲酸酯,其中該硫代胺基甲酸酯具有式(9)或(10),且自由基起始劑與硫代胺基甲酸酯之重量比為1:2至30:1,較佳1:1至20:1,尤其1.5:1至5:1。
在另一形式中,改性劑摻合物包含:自由基起始劑,其係選自基於碳之自由基產生劑;及硫代胺基甲酸酯,其中R
a係基於有機異氰酸酯,該有機異氰酸酯為未經取代或經C
1-C
4烷基取代之二異氰酸苯酯,或係基於藉由上述二異氰酸酯與其自身及/或與多元醇之反應獲得之寡聚或聚合產物,且自由基起始劑與硫代胺基甲酸酯之重量比為1:2至30:1,較佳1:1至20:1,尤其1.5:1至5:1。
在另一形式中,改性劑摻合物包含:自由基起始劑,其係選自基於碳之自由基產生劑,其中該等基於碳之自由基產生劑具有式(17);及硫代胺基甲酸酯,其中R
a係基於有機異氰酸酯,該有機異氰酸酯為未經取代或經C
1-C
4烷基取代之二異氰酸苯酯,或係基於藉由上述二異氰酸酯與其自身及/或與多元醇之反應獲得之寡聚或聚合產物,且自由基起始劑與硫代胺基甲酸酯之重量比為1:2至30:1,較佳1:1至20:1,尤其1.5:1至5:1。
在另一形式中,改性劑摻合物包含:自由基起始劑,其係選自基於碳之自由基產生劑,其中該等基於碳之自由基產生劑具有式(17);及硫代胺基甲酸酯,其中該硫代胺基甲酸酯具有式(9)或(10),且自由基起始劑與硫代胺基甲酸酯之重量比為1:2至30:1,較佳1:1至20:1,尤其1.5:1至5:1。
在較佳形式中,若自由基起始劑係選自過氧化物,則諸如聚烯烴之聚合材料不含式(18)或(19)之化合物
,
,
其中
G
1、G
2、G
3及G
4彼此獨立地為C
1-C
4烷基,或G
1及G
2一起或G
3及G
4一起為五亞甲基;
G
1'、G
2'、G
3'及G
4'彼此獨立地為C
1-C
4烷基,或G
1'及G
2'一起或G
3'及G
4'一起為五亞甲基;
G
5、G
6、G
5'及G
6'彼此獨立地為氫或C
1-C
4烷基;且
X及X'彼此獨立地為氫、C
1-C
18烷基、C
2-C
18烯基、-O-C
1-C
18烷基、-NH-C
1-C
18烷基、-N(C
1-C
6烷基)
2、苯基、苯氧基或-NH-苯基,
m為1或2,且
當m為1時,R
1為C
2-C
8伸烷基或C
2-C
8羥基伸烷基或C
4-C
36醯氧基伸烷基,或,
當m為2時,R
1為(-CH
2)
2C(CH
2-)
2,且
R1'為氫、C
1-C
8烷基、C
1-C
8羥烷基或式-(C=O)-C
1-C
40烷基之基團,或
-O-R
1'與連接其之-CH-基團一起為基團-(C=O)-。
聚合基質可為熱塑性聚合物,諸如聚烯烴、聚酯、聚醯胺、聚氯乙烯、聚醯亞胺、聚丙烯腈、聚碳酸酯或聚苯乙烯聚合物。較佳地,聚合基質為聚烯烴。
適合之
聚烯烴為單烯烴及二烯烴之聚合物,例如聚丙烯、聚異丁烯、聚丁-1-烯、聚-4-甲基戊-1-烯、聚乙烯基環己烷、聚異戊二烯或聚丁二烯;以及環烯烴之聚合物,例如環戊烯或降冰片烯之聚合物;聚乙烯(其視情況可交聯),例如高密度聚乙烯(HDPE)、高密度及高分子量聚乙烯(HDPE-HMW)、高密度及超高分子量聚乙烯(HDPE-UHMW)、中密度聚乙烯(MDPE)、低密度聚乙烯(LDPE)、直鏈低密度聚乙烯(LLDPE)、(VLDPE)及(ULDPE)。
聚烯烴,較佳聚乙烯及聚丙烯,可藉由以下方法製備:
a) 自由基聚合(通常在高壓及高溫下)。
b)使用通常含有一種或多於一種週期表第IVb、Vb、VIb或VIII族金屬之催化劑進行之催化聚合。此等金屬通常具有一個或多於一個配位體,通常為氧化物、鹵化物、醇化物、酯、醚、胺、烷基、烯基及/或芳基,其可經π-配位或σ-配位。此等金屬錯合物可呈游離形式或固定於基質上,通常固定於活性氯化鎂、氯化鈦(III)、氧化鋁或氧化矽上。此等催化劑可溶或不可溶於聚合介質中。催化劑可在聚合中單獨使用,或可使用其他活化劑,通常為金屬烷基化物、金屬氫化物、金屬烷基鹵化物、金屬烷基氧化物或金屬烷基㗁烷(alkyloxane),該等金屬為週期表第Ia、IIa及/或IIIa族元素。活化劑可便宜地經其他酯、醚、胺或矽基醚基團改性。此等催化劑系統通常稱為Phillips、Standard Oil Indiana、Ziegler (-Natta)、TNZ (DuPont)、茂金屬或單位點催化劑(SSC)。
聚烯烴之混合物之實例為聚丙烯與聚異丁烯之混合物、聚丙烯與聚乙烯之混合物(例如,PP/HDPE、PP/LDPE)及不同類型之聚乙烯之混合物(例如,LDPE/HDPE)。
單烯烴及二烯烴與彼此或與其他乙烯基單體之共聚物之實例為乙烯/丙烯共聚物、直鏈低密度聚乙烯(LLDPE)及其與低密度聚乙烯(LDPE)之混合物、丙烯/丁-1-烯共聚物、丙烯/異丁烯共聚物、乙烯/丁-1-烯共聚物、乙烯/己烯共聚物、乙烯/甲基戊烯共聚物、乙烯/庚烯共聚物、乙烯/辛烯共聚物、乙烯/乙烯基環己烷共聚物、乙烯/環烯烴共聚物(例如乙烯/降冰片烯,如COC)、乙烯/1-烯烴共聚物(其中1-烯烴原位生成);丙烯/丁二烯共聚物、異丁烯/異戊二烯共聚物、乙烯/乙烯基環己烯共聚物、乙烯/丙烯酸烷酯共聚物、乙烯/甲基丙烯酸烷酯共聚物、乙烯/乙酸乙烯酯共聚物或乙烯/丙烯酸共聚物及其鹽(離聚物),以及乙烯與丙烯及二烯(諸如己二烯、二環戊二烯或亞乙基-降冰片烯)之三元聚合物;及此類共聚物與彼此及與在上文提及之聚合物的混合物,例如聚丙烯/乙烯-丙烯共聚物、LDPE/乙烯-乙酸乙烯酯共聚物(EVA)、LDPE/乙烯-丙烯酸共聚物(EAA)、LLDPE/EVA、LLDPE/EAA及交替或無規聚烯烴(polyalkylene)/一氧化碳共聚物及其與其他聚合物(例如聚醯胺)之混合物。
更佳地,聚烯烴係選自由以下組成之群:聚乙烯(如直鏈低密度聚乙烯、低密度聚乙烯、中密度聚乙烯及高密度聚乙烯)、及聚乙烯共聚物、及聚丙烯均聚物、及聚丙烯共聚物。高度較佳為聚乙烯或聚丙烯,尤其聚丙烯。
再生塑膠亦適合作為聚合材料,其可自家庭、商業及工業廢物或自有用材料收集獲得。再生塑膠可來源於分離及分類,或來源於特定工業部門及返還義務,例如來源於汽車工業、電氣/電子工業、建築、農業及紡織工業或來源於家庭及商業(例如,超市)。再生塑膠可為單一材料再生塑膠,例如來自由聚烯烴(聚丙烯、高密度聚乙烯、低密度聚乙烯及聚丙烯摻合物)及共聚物(諸如PP/EPDM及PP/PE及聚苯乙烯)組成之聚合物類別,或為規定的再生塑膠混合物。
再生塑膠亦可含有聚對苯二甲酸乙二酯、聚醯胺、聚碳酸酯、乙酸纖維素及聚偏二氯乙烯。亦可存在次要量(至多約5%)之非熱塑性塑膠,例如聚胺基甲酸酯、甲醛樹脂及酚醛樹脂及典型胺基樹脂,以及彈性體,例如硫化或未硫化橡膠。在某些塑膠廢物中,亦可存在少量通常難以移除之異物,例如紙張、顏料及黏著劑。此等異物亦可來源於在使用或加工期間與各種物質之接觸,例如燃料殘餘物、塗料組分、痕量金屬、起始劑殘餘物或痕量水。
在諸如聚烯烴之
聚合材料中併入包含自由基起始劑及硫代胺基甲酸酯之改性劑摻合物的步驟可藉由習知方法達成,諸如將改性劑摻合物或其單一組分(亦即自由基起始劑及硫代胺基甲酸酯)添加至聚合材料中。改性劑摻合物或其單一組分(亦即自由基起始劑及硫代胺基甲酸酯)可以液體、粉末、顆粒或母料形式添加至聚合材料中。自由基起始劑及硫代胺基甲酸酯及視情況存在之其他添加劑可單獨或彼此混合地添加至聚合材料中。較佳的係自由基起始劑及硫代胺基甲酸酯一起添加,較佳以母料形式添加。
自由基起始劑及硫代胺基甲酸酯及
視情況存在之其他添加劑可在聚合之前、期間或之後或在交聯之前或之後添加至聚合材料中。自由基起始劑及硫代胺基甲酸酯及視情況存在之其他添加劑可藉由已知方法併入聚合材料中,例如在成形之前或期間,或藉由將經溶解或分散之各別化合物施加至聚合材料中,必要時隨後蒸發溶劑。
將化合物添加至聚合材料中可在所有習用混合
機器中進行,在該等混合機器中將聚合物熔融且與具有本發明組成及視情況存在之其他添加劑的化合物混合。適合之機器為混合機、捏合機及擠出機。該過程較佳藉由在擠出機中加工期間添加化合物來進行。尤其較佳之加工機器為單螺桿擠出機、同向旋轉及反向旋轉雙螺桿擠出機、行星齒輪擠出機、環擠出機或配備有至少一個可施加真空之氣體移除室的共捏合機。
將聚合物置於升高的
溫度下足夠的時間段以進行分子量改變。在本發明之方法的一較佳實施例中,採用約150℃至340℃之溫度範圍。在一較佳方法變化形式中,使用約200℃至320℃、或200℃至300℃、或170℃至290℃、尤其約180℃至280℃之溫度範圍。
改變分子量所需之時間段可隨溫度、待改性之材料的量及所採用之任何擠出機的類型而變化。其範圍可為例如約10秒至20分鐘,尤其20秒至10分鐘。
根據本發明之組合物之加工或轉化之實例為:注射吹塑、擠出、吹塑、滾塑、模內裝飾(背注塑(back injection))、搪塑、注射成型、共注射成型、成形、壓縮成型、壓製、薄膜擠出(流延薄膜;吹塑薄膜)、纖維紡絲、其他纖維加工(編織、非編織,尤其纖維熔噴、紡黏)、拉伸(單軸、雙軸)、退火、深拉伸、壓延、機械轉化、燒結、共擠出、塗佈、層壓、交聯(輻射、過氧化物、矽烷)、氣相沉積、焊接在一起、膠合、熱成形、管材擠出、型材擠出、片材擠出;片材鑄造、旋塗、捆紮、發泡、回收/返工、擠出塗佈。
根據本發明加工之材料可以廣泛多種
形式使用,例如作為薄膜、纖維(連續或非連續)、帶或模製品。包括雙組分纖維在內之纖維為較佳的。雙組分纖維意謂包含沿纖維長度緊密黏附之至少兩個不同聚合域a)及b)之纖維。此等纖維可具有任何形狀,且不限於特定形狀。此類形狀之實例為並列型、鞘芯型、桔瓣型及基質型及原纖維型。較佳為鞘芯型雙組分纖維及並列型雙組分纖維,尤其為鞘芯型雙組分纖維。
較佳
製品為非編織織物,其亦應包括網且應意謂定向或隨機定向且藉由摩擦及/或內聚力及/或黏附及/或機械過程黏合的個別纖維、長絲或線之紡織結構,如與以機械方式相互接合之纖維之規則圖案相反,亦即,其不為編織或針織織物。非編織織物之實例包括熔噴長絲、紡黏連續長絲網、梳理網、氣流成網網(air-laid web)及濕法成網網(wet-laid web)。適合之黏合方法包括熱黏合、化學或溶劑黏合、樹脂黏合、機械針刺、水力針刺、針腳式接合(stitch-bonding)。由聚合材料製成之適合製品為地工織物、屋頂、纜線、薄膜、過濾介質、過濾器、尿布、衛生棉、內褲內襯、成人用失禁產品、防護衣、手術單、手術衣或手術服。
諸如聚烯烴之聚合材料之
流變改性通常藉由長鏈支化、交聯或減黏裂煉來達成。流變改性允許改良
- 機械特性,如拉伸強度、伸長率、抗撕裂性;
- 障壁特性,尤其非編織物之障壁特性(例如,水頭(hydrohead)、透氣性、過濾特性);
- 加工特性(適合聚合物之更廣泛範疇、參數適應性,如非編織物之熱黏合溫度);
- 再生,因為調節再生聚合物之熔體黏度可提供具有更均勻分子量(更窄MWD)且因此具有更佳機械特性之再生物品。另外,可使用減黏裂煉聚合物作為加工助劑或增容劑,其亦有助於提高再生聚合物之機械特性。另外,由於再生聚合物之流變品質為可變的,因此本發明能夠調節聚合物之流變反應,從而可具有更穩定且可控的過程。
拉伸強度及伸長率方面之改良特性對於例如非編織織物之製造非常重要,因為其製備涉及多個步驟且改良之拉伸強度或伸長率有助於使其更好地經受此等步驟。重要地,更高的拉伸強度為非編織織物生產商提供了例如減輕重量同時保持產品之良好機械性能的選擇。
另一重要態樣為在製備非編織物過程中之加工安全性。期望在更低的加工溫度下在更溫和的條件下進行製備非編織織物之方法。為了能夠如此進行,必須在較低加工溫度下獲得仍良好的機械特性,如拉伸強度及伸長率。此允許降低加工溫度。此外,節能將為次要益處。
聚合材料之流變改性通常意謂降低分子量(例如,藉由使聚合材料降解)或增加分子量(例如,藉由使聚合材料交聯或支化)。經改性之流變通常藉由諸如根據EN ISO 133,例如在230℃下用2.16 kg分析熔體流動指數(MFI)來測定。
改性通常意謂包含具有一定量之自由基起始劑之改性劑摻合物的聚合材料(諸如聚烯烴)之流變(例如,用MFI測定)與僅具有該一定量之自由基起始劑(但不具有硫代胺基甲酸酯)的相同聚合材料之流變相比增加或減少(較佳MFI增加)至少1%、3%、5%、10%、20%、30%、40%或50%。
聚合材料亦可另外含有各種
習知添加劑,例如抗氧化劑、UV吸收劑及光穩定劑、金屬去活化劑、亞磷酸酯及亞膦酸酯、羥胺、硝酮、硫代增效劑、過氧化物清除劑、聚醯胺穩定劑、鹼性共穩定劑、成核劑、填充劑及增強劑、苯并呋喃酮及吲哚啉酮或其他添加劑,諸如塑化劑、潤滑劑、乳化劑、顏料、流變添加劑、催化劑、流動控制劑、光增白劑、防焰劑、抗靜電劑及發泡劑。
1. 抗氧化劑 1.1 . 烷基化單酚,例如2,6-二-三級丁基-4-甲基苯酚、2-三級丁基-4,6-二甲基苯酚、2,6-二-三級丁基-4-乙基苯酚、2,6-二-三級丁基-4-正丁基苯酚、2,6-二-三級丁基-4-異丁基苯酚、2,6-二環戊基-4-甲基苯酚、2-(α-甲基環己基)-4,6-二甲基苯酚、2,6-二(十八烷基)-4-甲基苯酚、2,4,6-三環己基苯酚、2,6-二-三級丁基-4-甲氧基甲基苯酚、側鏈為直鏈或分支鏈之壬基苯酚(例如2,6-二壬基-4-甲基苯酚)、2,4-二甲基-6-(1'-甲基十一烷-1'-基)苯酚、2,4-二甲基-6-(1'-甲基十七烷-1'-基)苯酚、2,4-二甲基-6-(1'-甲基十三烷-1'-基)苯酚及其混合物。
1.2. 烷基硫甲基苯酚,例如2,4-二辛基硫甲基-6-三級丁基苯酚、2,4-二辛基硫甲基-6-甲基苯酚、2,4-二辛基硫甲基-6-乙基苯酚、2,6-二-十二烷基硫甲基-4-壬基苯酚。
1.3. 氫醌 及烷基化 氫醌,例如2,6-二-三級丁基-4-甲氧基苯酚、2,5-二-三級丁基氫醌、2,5-二-三級戊基氫醌、2,6-二苯基-4-十八烷氧基苯酚、2,6-二-三級丁基氫醌、2,5-二-三級丁基-4-羥基大茴香醚、3,5-二-三級丁基-4-羥基大茴香醚、硬脂酸3,5-二-三級丁基-4-羥苯酯、己二酸雙(3,5-二-三級丁基-4-羥苯基)酯。
1.4. 生育酚,例如α-生育酚、β-生育酚、γ-生育酚、δ-生育酚及其混合物(維生素E)。
1.5. 羥基化硫代二苯醚,例如2,2'-硫代雙(6-三級丁基-4-甲基苯酚)、2,2'-硫代雙(4-辛基苯酚)、4,4'-硫代雙(6-三級丁基-3-甲基苯酚)、4,4'-硫代雙(6-三級丁基-2-甲基苯酚)、4,4'-硫代雙(3,6-二-二級戊基苯酚)、4,4'-雙(2,6-二甲基-4-羥苯基)二硫化物。
1.6. 亞烷基雙酚,例如2,2'-亞甲基雙(6-三級丁基-4-甲基苯酚)、2,2'-亞甲基雙(6-三級丁基-4-乙基苯酚)、2,2'-亞甲基雙[4-甲基-6-(α-甲基環己基)苯酚]、2,2'-亞甲基雙(4-甲基-6-環己基苯酚)、2,2'-亞甲基雙(6-壬基-4-甲基苯酚)、2,2'-亞甲基雙(4,6-二-三級丁基苯酚)、2,2'-亞乙基雙(4,6-二-三級丁基苯酚)、2,2'-亞乙基雙(6-三級丁基-4-異丁基苯酚)、2,2'-亞甲基雙[6-(α-甲基苯甲基)-4-壬基苯酚]、2,2'-亞甲基雙[6-(α,α-二甲基苯甲基)-4-壬基苯酚]、4,4'-亞甲基雙(2,6-二-三級丁基苯酚)、4,4'-亞甲基雙(6-三級丁基-2-甲基苯酚)、1,1-雙(5-三級丁基-4-羥基-2-甲基苯基)丁烷、2,6-雙(3-三級丁基-5-甲基-2-羥基苯甲基)-4-甲基苯酚、1,1,3-參(5-三級丁基-4-羥基-2-甲基苯基)丁烷、1,1-雙(5-三級丁基-4-羥基-2-甲基-苯基)-3-正十二烷基巰基丁烷、乙二醇雙[3,3-雙(3'-三級丁基-4'-羥苯基)丁酸酯]、雙(3-三級丁基-4-羥基-5-甲基-苯基)二環戊二烯、雙[2-(3'-三級丁基-2'-羥基-5'-甲基苯甲基)-6-三級丁基-4-甲基苯基]對苯二甲酸酯、1,1-雙-(3,5-二甲基-2-羥苯基)丁烷、2,2-雙(3,5-二-三級丁基-4-羥苯基)丙烷、2,2-雙(5-三級丁基-4-羥基-2-甲基苯基)-4-正十二烷基巰基丁烷、1,1,5,5-四-(5-三級丁基-4-羥基-2-甲基苯基)戊烷。
1.7. O- 苯甲基化合物 、 N- 苯甲基化合物及 S- 苯甲基化合物,例如3,5,3',5'-四-三級丁基-4,4'-二羥基二苯甲基醚、十八烷基-4-羥基-3,5-二甲基苯甲基巰基乙酸酯、十三烷基-4-羥基-3,5-二-三級丁基苯甲基巰基乙酸酯、參(3,5-二-三級丁基-4-羥基苯甲基)胺、雙(4-三級丁基-3-羥基-2,6-二甲基苯甲基)二硫代對苯二甲酸酯、雙(3,5-二-三級丁基-4-羥基苯甲基)硫化物、異辛基-3,5-二-三級丁基-4-羥基苯甲基巰基乙酸酯。
1.8. 羥基苯甲基化丙二酸酯,例如二(十八烷基)-2,2-雙(3,5-二-三級丁基-2-羥基苯甲基)丙二酸酯、二-十八烷基-2-(3-三級丁基-4-羥基-5-甲基苯甲基)丙二酸酯、二-十二烷基巰基乙基-2,2-雙(3,5-二-三級丁基-4-羥基苯甲基)丙二酸酯、雙[4-(1,1,3,3-四甲基丁基)苯基]-2,2-雙(3,5-二-三級丁基-4-羥基苯甲基)丙二酸酯。
1.9. 芳族羥基苯甲基化合物,例如1,3,5-參(3,5-二-三級丁基-4-羥基苯甲基)-2,4,6-三甲基苯、1,4-雙(3,5-二-三級丁基-4-羥基苯甲基)-2,3,5,6-四甲基苯、2,4,6-參(3,5-二-三級丁基-4-羥基苯甲基)苯酚。
1.10. 三 𠯤 化合物,例如2,4-雙(辛基巰基)-6-(3,5-二-三級丁基-4-羥基苯胺基)-1,3,5-三𠯤、2-辛基巰基-4,6-雙(3,5-二-三級丁基-4-羥基苯胺基)-1,3,5-三𠯤、2-辛基巰基-4,6-雙(3,5-二-三級丁基-4-羥基苯氧基)-1,3,5-三𠯤、2,4,6-參(3,5-二-三級丁基-4-羥基苯氧基)-1,2,3-三𠯤、1,3,5-參(3,5-二-三級丁基-4-羥基苯甲基)三聚異氰酸酯、1,3,5-參(4-三級丁基-3-羥基-2,6-二甲基苯甲基)三聚異氰酸酯、2,4,6-參(3,5-二-三級丁基-4-羥苯基乙基)-1,3,5-三𠯤、1,3,5-參(3,5-二-三級丁基-4-羥苯基丙醯基)-六氫-1,3,5-三𠯤、1,3,5-參(3,5-二環己基-4-羥基苯甲基)三聚異氰酸酯。
1.11. 苯甲基膦酸酯,例如二甲基-2,5-二-三級丁基-4-羥基苯甲基膦酸酯、二乙基-3,5-二-三級丁基-4-羥基苯甲基膦酸酯、二(十八烷基)-3,5-二-三級丁基-4-羥基苯甲基膦酸酯、二(十八烷基)-5-三級丁基-4-羥基-3-甲基苯甲基膦酸酯、3,5-二-三級丁基-4-羥基苯甲基膦酸單乙酯之鈣鹽。
1.12. 醯胺基苯酚,例如4-羥基月桂醯苯胺、4-羥基硬脂醯苯胺、N-(3,5-二-三級丁基-4-羥苯基)胺基甲酸辛酯。
1.13. β -(3,5- 二 - 三級丁基 -4- 羥苯基 ) 丙酸 與以下 之酯:一元醇或多元醇,例如甲醇、乙醇、正辛醇、異辛醇、十八醇、1,6-己二醇、1,9-壬二醇、乙二醇、1,2-丙二醇、新戊二醇、硫代二乙二醇、二乙二醇、三乙二醇、新戊四醇、參(羥乙基)三聚異氰酸酯、N,N'-雙(羥乙基)草醯胺、3-硫雜十一醇、3-硫雜十五醇、三甲基己二醇、三羥甲基丙烷、4-羥甲基-1-磷雜-2,6,7-三氧雜雙環[2.2.2]辛烷。
1.14. β-(5- 三級丁基 -4- 羥基 - 3- 甲基苯基 ) 丙酸與以下之酯:一元醇或多元醇,例如甲醇、乙醇、正辛醇、異辛醇、十八醇、1,6-己二醇、1,9-壬二醇、乙二醇、1,2-丙二醇、新戊二醇、硫代二乙二醇、二乙二醇、三乙二醇、新戊四醇、參(羥乙基)三聚異氰酸酯、N,N'-雙(羥乙基)草醯胺、3-硫雜十一醇、3-硫雜十五醇、三甲基己二醇、三羥甲基丙烷、4-羥甲基-1-磷雜-2,6,7-三氧雜雙環[2.2.2]辛烷;3,9-雙[2-{3-(3-三級丁基-4-羥基-5-甲基苯基)丙醯氧基}-1,1-二甲基乙基]-2,4,8,10-四氧雜螺[5.5]十一烷。
1.15. β -(3,5- 二環己基 -4- 羥苯基 ) 丙酸與以下之酯:一元醇或多元醇,例如甲醇、乙醇、辛醇、十八醇、1,6-己二醇、1,9-壬二醇、乙二醇、1,2-丙二醇、新戊二醇、硫代二乙二醇、二乙二醇、三乙二醇、新戊四醇、參(羥乙基)三聚異氰酸酯、N,N'-雙(羥乙基)草醯胺、3-硫雜十一醇、3-硫雜十五醇、三甲基己二醇、三羥甲基丙烷、4-羥甲基-1-磷雜-2,6,7-三氧雜雙環[2.2.2]辛烷。
1.16. 3,5- 二 - 三級丁基 -4- 羥苯基乙酸與以下之酯:一元醇或多元醇,例如甲醇、乙醇、辛醇、十八醇、1,6-己二醇、1,9-壬二醇、乙二醇、1,2-丙二醇、新戊二醇、硫代二乙二醇、二乙二醇、三乙二醇、新戊四醇、參(羥乙基)三聚異氰酸酯、N,N'-雙(羥乙基)草醯胺、3-硫雜十一醇、3-硫雜十五醇、三甲基己二醇、三羥甲基丙烷、4-羥甲基-1-磷雜-2,6,7-三氧雜雙環[2.2.2]辛烷。
1.17. β -(3,5- 二 - 三級丁基 -4- 羥苯基 ) 丙酸之醯胺,例如N,N'-雙(3,5-二-三級丁基-4-羥苯基丙醯基)六亞甲基二醯胺、N,N'-雙(3,5-二-三級丁基-4-羥苯基丙醯基)三亞甲基二醯胺、N,N'-雙(3,5-二-三級丁基-4-羥苯基丙醯基)醯肼、N,N'-雙[2-(3-[3,5-二-三級丁基-4-羥苯基]丙醯氧基)乙基]草醯胺(Naugard®XL-1,由Addivant供應)。
1.18. 抗壞血酸(維生素C)
1.19. 胺類抗氧化劑,例如N,N'-二-異丙基-對苯二胺、N,N'-二-二級丁基-對苯二胺、N,N'-雙(1,4-二甲基戊基)-對苯二胺、N,N'-雙(1-乙基-3-甲基戊基)-對苯二胺、N,N'-雙(1-甲基庚基)-對苯二胺、N,N'-二環己基-對苯二胺、N,N'-二苯基-對苯二胺、N,N'-雙(2-萘基)-對苯二胺、N-異丙基-N'-苯基-對苯二胺、N-(1,3-二甲基丁基)-N'-苯基-對苯二胺、N-(1-甲基庚基)-N'-苯基-對苯二胺、N-環己基-N'-苯基-對苯二胺、4-(對甲苯胺磺醯基)二苯胺、N,N'-二甲基-N,N'-二-二級丁基-對苯二胺、二苯胺、N-烯丙基二苯胺、4-異丙氧基二苯胺、N-苯基-1-萘胺、N-(4-三級辛基苯基)-1-萘胺、N-苯基-2-萘胺、辛基化二苯胺(例如p,p'-二-三級辛基二苯胺)、4-正丁基胺基苯酚、4-丁醯基胺基苯酚、4-壬醯基胺基苯酚、4-十二醯基胺基苯酚、4-十八醯基胺基苯酚、雙(4-甲氧基苯基)胺、2,6-二-三級丁基-4-二甲胺基甲基苯酚、2,4'-二胺基二苯基甲烷、4,4'-二胺基二苯基甲烷、N,N,N',N'-四甲基-4,4'-二胺基二苯基甲烷、1,2-雙[(2-甲基苯基)胺基]乙烷、1,2-雙(苯胺基)丙烷、(鄰甲苯基)二胍、雙[4-(1',3'-二甲基丁基)苯基]胺、三級辛基化N-苯基-1-萘胺、單烷基化及二烷基化三級丁基二苯胺/三級辛基二苯胺之混合物、單烷基化及二烷基化壬基二苯胺之混合物、單烷基化及二烷基化十二烷基二苯胺之混合物、單烷基化及二烷基化異丙基二苯胺/異己基二苯胺之混合物、單烷基化及二烷基化三級丁基二苯胺之混合物、2,3-二氫-3,3-二甲基-4H-1,4-苯并噻𠯤、啡噻𠯤、單烷基化及二烷基化三級丁基啡噻𠯤/三級辛基啡噻𠯤之混合物、單烷基化及二烷基化三級辛基-啡噻𠯤之混合物、N-烯丙基啡噻𠯤、N,N,N',N'-四苯基-1,4-二胺基丁-2-烯。
2. UV 吸收劑 及光穩定劑 2.1. 2-(2'- 羥苯基 ) 苯并三唑,例如2-(2'-羥基-5'-甲基苯基)-苯并三唑、2-(3',5'-二-三級丁基-2'-羥苯基)苯并三唑、2-(5'-三級丁基-2'-羥苯基)苯并三唑、2-(2'-羥基-5'-(1,1,3,3-四甲基丁基)苯基)苯并三唑、2-(3',5'-二-三級丁基-2'-羥苯基)-5-氯-苯并三唑、2-(3'-三級丁基-2'-羥基-5'-甲基苯基)-5-氯-苯并三唑、2-(3'-二級丁基-5'-三級丁基-2'-羥苯基)苯并三唑、2-(2'-羥基-4'-辛氧基苯基)苯并三唑、2-(3',5'-二-三級戊基-2'-羥苯基)苯并三唑、2-(3',5'-雙-(α,α-二甲基苯甲基)-2'-羥苯基)苯并三唑、2-(3'-三級丁基-2'-羥基-5'-(2-辛氧基羰基乙基)苯基)-5-氯-苯并三唑、2-(3'-三級丁基-5'-[2-(2-乙基己氧基)-羰基乙基]-2'-羥苯基)-5-氯-苯并三唑、2-(3'-三級丁基-2'-羥基-5'-(2-甲氧基羰基乙基)苯基)-5-氯-苯并三唑、2-(3'-三級丁基-2'-羥基-5'-(2-甲氧基羰基乙基)苯基)苯并三唑、2-(3'-三級丁基-2'-羥基-5'-(2-辛氧基羰基乙基)苯基)苯并三唑、2-(3'-三級丁基-5'-[2-(2-乙基己氧基)羰基乙基]-2'-羥苯基)苯并三唑、2-(3'-十二烷基-2'-羥基-5'-甲基苯基)苯并三唑、2-(3'-三級丁基-2'-羥基-5'-(2-異辛氧基羰基乙基)苯基苯并三唑、2,2'-亞甲基-雙[4-(1,1,3,3-四甲基丁基)-6-苯并三唑-2-基苯酚];2-[3'-三級丁基-5'-(2-甲氧基羰基乙基)-2'-羥苯基]-2H-苯并三唑與聚乙二醇300之轉酯化產物;
,
其中R = 3'-三級丁基-4'-羥基-5'-2H-苯并三唑-2-基苯基、2-[2'-羥基-3'-(α,α-二甲基苯甲基)-5'-(1,1,3,3-四甲基丁基)-苯基]苯并三唑;2-[2'-羥基-3'-(1,1,3,3-四甲基丁基)-5'-(α,α-二甲基苯甲基)-苯基]苯并三唑。
2.2. 2- 羥基二苯基酮,例如4-羥基、4-甲氧基、4-癸氧基、4-十二烷氧基、4-苯甲氧基、4,2',4'-三羥基及2'-羥基-4,4'-二甲氧基衍生物。
2.3. 經取代及未經取代之苯甲酸之酯,例如水楊酸4-三級丁基-苯酯、水楊酸苯酯、水楊酸辛基苯酯、二苯甲醯基間苯二酚、雙(4-三級丁基苯甲醯基)間苯二酚、苯甲醯基間苯二酚、3,5-二-三級丁基-4-羥基苯甲酸2,4-二-三級丁基苯酯、3,5-二-三級丁基-4-羥基苯甲酸十六烷酯、3,5-二-三級丁基-4-羥基苯甲酸十八烷酯、3,5-二-三級丁基-4-羥基苯甲酸2-甲基-4,6-二-三級丁基苯酯。
2.4. 丙烯酸酯 / 肉 桂酸酯,例如α-氰基-β,β-二苯基丙烯酸乙酯、α-氰基-β,β-二苯基丙烯酸異辛酯、α-甲氧羰基肉桂酸甲酯、α-氰基-β-甲基-對甲氧基肉桂酸甲酯、α-氰基-β-甲基-對甲氧基-肉桂酸丁酯、α-甲氧羰基-對甲氧基肉桂酸甲酯、N-(β-甲氧羰基-β-氰基乙烯基)-2-甲基吲哚啉、四(α-氰基-β,β-二苯基丙烯酸)新戊酯。氰基丙烯酸酯亦可用作EP 3587425中給出之此類化合物。
2.5. 鎳化合物,例如2,2'-硫代-雙[4-(1,1,3,3-四甲基丁基)苯酚]之鎳錯合物,諸如1:1或1:2錯合物,其具有或不具有額外配位體,諸如正丁胺、三乙醇胺或N-環己基二乙醇胺;二丁基二硫代胺基甲酸鎳;4-羥基-3,5-二-三級丁基苯甲基膦酸之單烷酯(例如甲酯或乙酯)之鎳鹽;酮肟,例如2-羥基-4-甲基苯基十一烷基酮肟之鎳錯合物;1-苯基-4-月桂醯基-5-羥基吡唑之鎳錯合物,其具有或不具有額外配位體。
2.6. 位阻胺,例如碳酸雙(1-十一烷氧基-2,2,6,6-四甲基-4-哌啶基)酯、雙(2,2,6,6-四甲基-4-哌啶基)癸二酸酯、雙(2,2,6,6-四甲基-4-哌啶基)丁二酸酯、雙(1,2,2,6,6-五甲基-4-哌啶基)癸二酸酯、雙(1-辛氧基-2,2,6,6-四甲基-4-哌啶基)癸二酸酯、正丁基-3,5-二-三級丁基-4-羥基苯甲基丙二酸雙(1,2,2,6,6-五甲基-4-哌啶基)酯、1-(2-羥乙基)-2,2,6,6-四甲基-4-羥基哌啶與丁二酸之縮合物、N,N'-雙(2,2,6,6-四甲基-4-哌啶基)六亞甲基二胺與4-三級辛基胺基-2,6-二氯-1,3,5-三𠯤之直鏈或環狀縮合物、參(2,2,6,6-四甲基-4-哌啶基)氮基三乙酸酯、肆(2,2,6,6-四甲基-4-哌啶基)-1,2,3,4-丁烷四甲酸酯、1,1'-(1,2-乙烷二基)-雙(3,3,5,5-四甲基哌𠯤酮)、4-苯甲醯基-2,2,6,6-四甲基哌啶、4-硬脂氧基-2,2,6,6-四甲基哌啶、雙(1,2,2,6,6-五甲基哌啶基)-2-正丁基-2-(2-羥基-3,5-二-三級丁基苯甲基)丙二酸酯、3-正辛基-7,7,9,9-四甲基-1,3,8-三氮雜螺[4.5]癸烷-2,4-二酮、雙(1-辛氧基-2,2,6,6-四甲基哌啶基)癸二酸酯、雙(1-辛氧基-2,2,6,6-四甲基哌啶基)丁二酸酯、N,N'-雙(2,2,6,6-四甲基-4-哌啶基)六亞甲基二胺與4-(N-𠰌啉基)-2,6-二氯-1,3,5-三𠯤之直鏈或環狀縮合物、2-氯-4,6-雙(4-正丁胺基-2,2,6,6-四甲基哌啶基)-1,3,5-三𠯤與1,2-雙(3-胺基丙胺基)乙烷之縮合物、2-氯-4,6-二-(4-正丁胺基-1,2,2,6,6-五甲基哌啶基)-1,3,5-三𠯤與1,2-雙(3-胺基丙胺基)乙烷之縮合物、8-乙醯基-3-十二烷基-7,7,9,9-四甲基-1,3,8-三氮雜螺[4.5]癸烷-2,4-二酮、3-十二烷基-1-(2,2,6,6-四甲基-4-哌啶基)吡咯啶-2,5-二酮、3-十二烷基-1-(1,2,2,6,6-五甲基-4-哌啶基)吡咯啶-2,5-二酮、4-十六烷氧基-2,2,6,6-四甲基哌啶及4-硬脂氧基-2,2,6,6-四甲基哌啶之混合物、N,N'-雙(2,2,6,6-四甲基-4-哌啶基)六亞甲基二胺與4-環己胺基-2,6-二氯-1,3,5-三𠯤之縮合物、1,2-雙(3-胺基丙胺基)乙烷與2,4,6-三氯-1,3,5-三𠯤以及4-丁胺基-2,2,6,6-四甲基哌啶之縮合物(CAS登記號[136504-96-6]);1,6-己二胺與2,4,6-三氯-1,3,5-三𠯤以及N,N-二丁胺及4-丁胺基-2,2,6,6-四甲基哌啶之縮合物(CAS登記號[192268-64-7]);N-(2,2,6,6-四甲基-4-哌啶基)-正十二烷基丁二醯亞胺、N-(1,2,2,6,6-五甲基-4-哌啶基)-正十二烷基丁二醯亞胺、2-十一烷基-7,7,9,9-四甲基-1-氧雜-3,8-二氮雜-4-側氧基-螺[4,5]癸烷、7,7,9,9-四甲基-2-環十一烷基-1-氧雜-3,8-二氮雜-4-側氧基-螺[4,5]癸烷與表氯醇之反應產物、1,1-雙(1,2,2,6,6-五甲基-4-哌啶基氧基羰基)-2-(4-甲氧基苯基)乙烯、N,N'-雙-甲醯基-N,N'-雙(2,2,6,6-四甲基-4-哌啶基)六亞甲基二胺、4-甲氧基亞甲基丙二酸與1,2,2,6,6-五甲基-4-羥基哌啶之二酯、聚[甲基丙基-3-氧基-4-(2,2,6,6-四甲基-4-哌啶基)]矽氧烷、順丁烯二酸酐-α-烯烴共聚物與2,2,6,6-四甲基-4-胺基哌啶或1,2,2,6,6-五甲基-4-胺基哌啶之反應產物、2,4-雙[N-(1-環己氧基-2,2,6,6-四甲基哌啶-4-基)-N-丁胺基]-6-(2-羥乙基)胺基-1,3,5-三𠯤、1-(2-羥基-2-甲基丙氧基)-4-十八醯氧基-2,2,6,6-四甲基哌啶、5-(2-乙基己醯基)氧基甲基-3,3,5-三甲基-2-𠰌啉酮、Sanduvor® 3058 (Clariant;CAS登記號106917-31-1]、5-(2-乙基己醯基)氧基甲基-3,3,5-三甲基-2-𠰌啉酮、2,4-雙[(1-環己氧基-2,2,6,6-哌啶-4-基)丁胺基]-6-氯-均三𠯤與N,N'-雙(3-胺基丙基)乙二胺)之反應產物、1,3,5-參(N-環己基-N-(2,2,6,6-四甲基哌𠯤-3-酮-4-基)胺基)-均三𠯤、1,3,5-參(N-環己基-N-(1,2,2,6,6-五甲基哌𠯤-3-酮-4-基)胺基)-均三𠯤。
2.7. 草醯胺,例如4,4'-二辛氧基草醯苯胺、2,2'-二乙氧基草醯苯胺、2,2'-二辛氧基-5,5'-二-三級丁草醯苯胺、2,2'-二(十二烷氧基)-5,5'-二-三級丁草醯苯胺、2-乙氧基-2'-乙基草醯苯胺、N,N'-雙(3-二甲胺基丙基)草醯胺、2-乙氧基-5-三級丁基-2'-乙草醯苯胺及其與2-乙氧基-2'-乙基-5,4'-二-三級丁草醯苯胺之混合物、鄰甲氧基二取代草醯苯胺與對甲氧基二取代草醯苯胺之混合物以及鄰乙氧基二取代草醯苯胺與對乙氧基二取代草醯苯胺之混合物。
2.8. 2-(2- 羥苯基 )-1,3,5- 三 𠯤,例如2,4,6-參(2-羥基-4-辛氧基苯基)-1,3,5-三𠯤、2-(2-羥基-4-辛氧基苯基)-4,6-雙(2,4-二甲基苯基)-1,3,5-三𠯤、2-(2,4-二羥苯基)-4,6-雙(2,4-二甲基苯基)-1,3,5-三𠯤、2,4-雙(2-羥基-4-丙氧基苯基)-6-(2,4-二甲基苯基)-1,3,5-三𠯤、2-(2-羥基-4-辛氧基苯基)-4,6-雙(4-甲基苯基)-1,3,5-三𠯤、2-(2-羥基-4-十二烷氧基苯基)-4,6-雙(2,4-二甲基苯基)-1,3,5-三𠯤、2-(2-羥基-4-十三烷氧基苯基)-4,6-雙(2,4-二甲基苯基)-1,3,5-三𠯤、2-[2-羥基-4-(2-羥基-3-丁氧基丙氧基)苯基]-4,6-雙(2,4-二甲基)-1,3,5-三𠯤、2-[2-羥基-4-(2-羥基-3-辛氧基丙氧基)苯基]-4,6-雙(2,4-二甲基)-1,3,5-三𠯤、2-[4-(十二烷氧基/十三烷氧基-2-羥基丙氧基)-2-羥苯基]-4,6-雙(2,4-二甲基苯基)-1,3,5-三𠯤、2-[2-羥基-4-(2-羥基-3-十二烷氧基丙氧基)苯基]-4,6-雙(2,4-二甲基苯基)-1,3,5-三𠯤、2-(2-羥基-4-己氧基)苯基-4,6-二苯基-1,3,5-三𠯤、2-(2-羥基-4-甲氧基苯基)-4,6-二苯基-1,3,5-三𠯤、2,4,6-參[2-羥基-4-(3-丁氧基-2-羥基丙氧基)苯基]-1,3,5-三𠯤、2-(2-羥苯基)-4-(4-甲氧基苯基)-6-苯基-1,3,5-三𠯤、2-{2-羥基-4-[3-(2-乙基己基-1-氧基)-2-羥基丙氧基]苯基}-4,6-雙(2,4-二甲基苯基)-1,3,5-三𠯤、2,4-雙(4-[2-乙基己氧基]-2-羥苯基)-6-(4-甲氧基苯基)-1,3,5-三𠯤、2,4-雙(4-聯苯基)-6-[2-羥基-4-(2-乙基己氧基)苯基]-1,3,5-三𠯤。
3. 金屬去活化劑,例如N,N'-二苯基草醯胺、N-水楊醛-N'-水楊醯肼、N,N'-雙(水楊醯基)肼、N,N'-雙(3,5-二-三級丁基-4-羥苯基丙醯基)肼、3-水楊醯胺基-1,2,4-三唑、雙(苯亞甲基)草醯基二肼、草醯苯胺、間苯二甲醯基二肼、癸二醯基雙苯基肼、N,N'-二乙醯基己二醯基二肼、N,N'-雙(水楊醯基)草醯基二肼、N,N'-雙(水楊醯基)硫代丙醯基二肼。
4. 亞磷酸酯及亞膦酸酯,例如亞磷酸三苯酯、亞磷酸二苯基烷酯、亞磷酸苯基二烷酯、亞磷酸參(壬基苯基)酯、亞磷酸三月桂酯、亞磷酸三(十八烷基)酯、二硬脂基新戊四醇二亞磷酸酯、亞磷酸參(2,4-二-三級丁基苯基)酯、新戊四醇二亞磷酸二異癸酯、雙(2,4-二-三級丁基苯基)新戊四醇二亞磷酸酯、雙(2,4-二-異丙苯基苯基)新戊四醇二亞磷酸酯、雙(2,6-二-三級丁基-4-甲基苯基)新戊四醇二亞磷酸酯、二異癸氧基新戊四醇二亞磷酸酯、雙(2,4-二-三級丁基-6-甲基苯基)新戊四醇二亞磷酸酯、雙(2,4,6-參(三級丁基苯基)新戊四醇二亞磷酸酯、山梨糖醇三亞磷酸三硬脂酯、4,4'-伸聯苯二亞膦酸肆(2,4-二-三級丁基苯基)酯、6-異辛氧基-2,4,8,10-四-三級丁基-12H-二苯并[d,g]-1,3,2-二氧磷雜八環、亞磷酸雙(2,4-二-三級丁基-6-甲基苯基)甲酯、亞磷酸雙(2,4-二-三級丁基-6-甲基苯基)乙酯、6-氟-2,4,8,10-四-三級丁基-12-甲基-二苯并[d,g]-1,3,2-二氧磷雜八環、2,2',2''-氮基[三乙基參(3,3',5,5'-四-三級丁基-1,1'-聯苯-2,2'-二基)亞磷酸酯]、2-乙基己基(3,3',5,5'-四-三級丁基-1,1'-聯苯-2,2'-二基)亞磷酸酯、5-丁基-5-乙基-2-(2,4,6-三-三級丁基苯氧基)-1,3,2-二氧雜磷雜環丙烷、亞磷酸混合2,4-雙(1,1-二甲基丙基)苯基三酯及4-(1,1-二甲基丙基)苯基三酯(CAS:939402-02-5)、與α-氫-ω-羥基聚[氧基(甲基-1,2-乙烷二基)] C10-16烷基酯之亞磷酸三苯酯聚合物(CAS:1227937-46-3)、Doverphos LGP-12 (CAS:116265-68-1)。
以下亞磷酸酯為尤其較佳的:亞磷酸參(2,4-二-三級丁基苯基)酯、亞磷酸參(壬基苯基)酯、雙(2,4-二-異丙苯基苯基)新戊四醇二亞磷酸酯,
。
5. 羥胺,例如N,N-二苯甲基羥胺、N,N-二乙基羥胺、N,N-二辛基羥胺、N,N-二月桂基羥胺、N,N-二(十四烷基)羥胺、N,N-二(十六烷基)羥胺、N,N-二(十八烷基)羥胺、N-十六烷基-N-十八烷基羥胺、N-十七烷基-N-十八烷基羥胺、來源於氫化動物脂胺或來源於植物來源之N,N-二烷基羥胺。
6. 硝酮,例如N-苯甲基-α-苯基硝酮、N-乙基-α-甲基硝酮、N-辛基-α-庚基硝酮、N-月桂基-α-十一烷基硝酮、N-十四烷基-α-十三烷基硝酮、N-十六烷基-α-十五烷基硝酮、N-十八烷基-α-十七烷基硝酮、N-十六烷基-α-十七烷基硝酮、N-十八烷基-α-十五烷基硝酮、N-十七烷基-α-十七烷基硝酮、N-十八烷基-α-十六烷基硝酮、由來源於氫化動物脂胺之N,N-二烷基羥胺衍生之硝酮。
7. 硫代增效劑,例如硫代二丙酸二月桂酯、硫代二丙酸二肉豆蔻酯、硫代二丙酸二硬脂酯或新戊四醇肆[3-(十二烷基硫基)丙酸酯]或二硬脂基二硫化物。
8. 過氧化物清除劑,例如β-硫代二丙酸之酯,例如月桂酯、硬脂酯、肉豆蔻酯或十三烷酯、巰基苯并咪唑、或2-巰基苯并咪唑之鋅鹽、二丁基二硫代胺基甲酸鋅、二(十八烷基)二硫化物、新戊四醇肆(β-十二烷基巰基)丙酸酯。
9. 聚醯胺穩定劑,例如與碘化物及/或磷化合物組合之銅鹽及二價錳鹽。
10. 鹼性共穩定劑,例如三聚氰胺、聚乙烯吡咯啶酮、二氰二胺、三聚氰酸三烯丙酯、脲衍生物、肼衍生物、胺、聚醯胺、聚胺基甲酸酯、沸石、水滑石、水合鈣鋁酸鹽(hydrocaluminate)、氧化鋅、高級脂肪酸之鹼金屬鹽及鹼土金屬鹽(例如硬脂酸鈣、硬脂酸鋅、山崳酸鎂、硬脂酸鎂、蓖麻油酸鈉及棕櫚酸鉀)、鄰苯二酚銻或鄰苯二酚鋅。
11. 成核劑,例如無機物質,諸如滑石;金屬氧化物,諸如二氧化鈦或氧化鎂;磷酸鹽,包括諸如2,2'-亞甲基-雙(4,6-二-三級丁基苯酚)磷酸鈉鹽、2,2'-亞甲基-雙(4,6-二-三級丁基苯酚)磷酸鋁鹽或2,2'-亞甲基-雙(4,6-二-三級丁基苯酚)磷酸鋰鹽之磷酸鹽;較佳鹼土金屬之碳酸鹽或硫酸鹽;有機化合物,諸如單羧酸或聚羧酸及其鹽,例如4-三級丁基苯甲酸、己二酸、二苯基乙酸、丁二酸鈉或苯甲酸鈉、1,2-環己烷二羧酸鈣鹽、雙環[2.2.1]庚烷-2,3-二羧酸二鈉鹽;聚合化合物,諸如離子共聚物(離聚物)、三胺基苯衍生物(諸如1,3,5-參[2,2-二甲基丙醯基胺]苯)、甘油酸鋅及壬醇衍生物。尤其較佳為1,3:2,4-雙(3',4'-二甲基苯亞甲基)山梨糖醇、1,3:2,4-二(對甲基二苯亞甲基)山梨糖醇及1,3:2,4-二(苯亞甲基)山梨糖醇。
12. 填充劑及增強劑,例如碳酸鈣、矽酸鹽、表面經處理之矽石(如例如US-A-2007/60,697及US-A-2009/111,918中所描述)、玻璃纖維、玻璃珠粒、石棉、滑石、高嶺土、雲母、硫酸鋇、金屬氧化物及氫氧化物、碳黑、石墨、木粉及其他天然產物之粉或纖維、合成纖維。
13. 其他添加劑,例如塑化劑、潤滑劑、乳化劑、顏料、流變添加劑、催化劑、流動控制劑、光增白劑、防焰劑、抗靜電劑及發泡劑。其他添加劑亦可包括抗黏連添加劑,其用於薄膜中以減少兩個聚乙烯表面彼此之間的負黏附力,否則該負黏附力將導致薄膜分離困難。其他添加劑包括助滑添加劑,其用於幫助薄膜表面相互滑動。亦可添加防霧劑。
14. 苯并呋喃酮及吲哚啉酮,例如揭示於U.S. 4,325,863、U.S. 4,338,244、U.S. 5,175,312、U.S. 5,216,052、U.S. 5,252,643、DE-A-4316611、DE-A-4316622、DE-A-4316876、EP-A-0589839、EP-A-0591102、EP-A-1291384中之彼等者,或3-[4-(2-乙醯氧基乙氧基)苯基]-5,7-二-三級丁基苯并呋喃-2-酮、5,7-二-三級丁基-3-[4-(2-硬脂醯氧基乙氧基)苯基]苯并呋喃-2-酮、3,3'-雙[5,7-二-三級丁基-3-(4-[2-羥基乙氧基]苯基)苯并呋喃-2-酮]、5,7-二-三級丁基-3-(4-乙氧基苯基)苯并呋喃-2-酮、3-(4-乙醯氧基-3,5-二甲基苯基)-5,7-二-三級丁基苯并呋喃-2-酮、3-(3,5-二甲基-4-特戊醯氧基苯基)-5,7-二-三級丁基苯并呋喃-2-酮、3-(3,4-二甲基苯基)-5,7-二-三級丁基苯并呋喃-2-酮、3-(2,3-二甲基苯基)-5,7-二-三級丁基苯并呋喃-2-酮、3-(2-乙醯基-5-異辛基苯基)-5-異辛基苯并呋喃-2-酮、5,7-二-三級丁基-3-[3,5-二甲基-4-[(1,3,7,9-四-三級丁基-5-甲基-5H-苯并[d][1,3,2]苯并二氧磷雜八環-11-基)氧基]苯基]-3H-苯并呋喃-2-酮。適合之苯并呋喃酮亦包括WO2015/121445及WO2017/025431中鑑別之化合物。
較佳為另外含有選自由以下組成之群的另一添加劑之組合物:抗氧化劑、加工穩定劑、光穩定劑、UV吸收劑、填充劑、增強劑、顏料、金屬去活化劑、塑化劑、潤滑劑、乳化劑、流變添加劑、催化劑、流動控制劑、光增白劑、防焰劑、抗靜電劑及發泡劑。
實例ThioU:式(12)之硫代胺基甲酸酯。
PER:2,5-二甲基-2,5-二(三級丁基過氧基)己烷,以Enox 101商購自Vesta Chemicals
DIC:2,3-二甲基-2,3-二苯基丁烷,商購自Acros Organics。
實例 1 至 8
使用高速混合機(Mixaco Lab CM 12,Mixaco Maschinenbau,德國)將鹼穩定劑(0.1% Irganox® B 225及0.05%硬脂酸鈣)及表1中所列之添加劑添加至市售聚丙烯粉末(來自法國Polychim Industrie之HA10XT,熔體流動指數3 g/10min ASTM D1238)中。在Tmax = 230℃之溫度下,以4 kg/h之生產量及100 rpm在N2下在雙螺桿擠出機(Berstorff ZE25A x 47D,KraussMaffei Berstorff GmbH,德國)上擠出該混合物。所得聚合物股在水浴中粒化。
熔體流動指數(MFI)係根據EN ISO 1133在Göttfert MI Robo (Göttfert Werkstoff Prüfmaschinen GmbH,德國)中在230℃下以2.16 kg測定。
MFI之增加指示減黏裂煉活性,分別指示受控的聚丙烯鏈降解。MFI之差值(「∆MFI」,亦即加添加劑之調配物之MFI相對於未加添加劑之參考調配物之MFI)為添加劑之不同活性的衡量標準。結果概述於表1a至1d中。
表1a
添加劑 | MFI | ∆MFI | |
參考物 | – | 4.6 | 0.0 |
比較實例1 | 0.006% PER | 7.5 | 2.9 |
比較實例2 | 0.04% PER | 23.7 | 19.1 |
比較實例3 | 0.06% PER | 37.1 | 32.5 |
比較實例4 | 0.006% ThioU | 4.8 | 0.2 |
實例1 | 0.003% PER 0.003% ThioU | 7.6 | 3.0 |
比較實例1至3顯示當增加過氧化物濃度時MFI之已知增加。比較實例4顯示當不使用過氧化物時,ThioU對MFI幾乎無影響。實例1顯示,當與ThioU組合時,僅用0.003%過氧化物就可達成約3之∆MFI,而在比較實例1中,需要雙倍的量,亦即0.006%過氧化物。
表1b
表1c
添加劑 | MFI | ∆MFI | |
參考物 | --- | 4.6 | 0.0 |
比較實例2 | 0.04% PER | 23.7 | 19.1 |
比較實例4 | 0.006% ThioU | 4.8 | 0.2 |
實例2 | 0.03% PER 0.01% ThioU | 31.6 | 27.0 |
實例4 | 0.034% PER 0.006% ThioU | 33.0 | 28.4 |
實例5 | 0.04% PER 0.006% ThioU | 40.3 | 35.7 |
添加劑 | MFI | ∆MFI | |
參考物 | --- | 4.6 | 0.0 |
比較實例3 | 0.06% PER | 37.1 | 32.5 |
比較實例4 | 0.006% ThioU | 4.8 | 0.2 |
實例3 | 0.054% PER 0.006% ThioU | 49.2 | 44.6 |
實例2、3、4及5顯示,當過氧化物與ThioU組合時,∆MFI甚至可進一步增加。
表1d
添加劑 | MFI | ∆MFI | |
參考物 | --- | 4.6 | 0.0 |
比較實例4 | 0.006% ThioU | 4.8 | 0.2 |
比較實例5 | 0.04% DIC | 4.9 | 0.3 |
實例6 | 0.03% DIC 0.01% ThioU | 6.2 | 1.6 |
實例7 | 0.034% DIC 0.006% ThioU | 5.7 | 1.1 |
實例8 | 0.04% DIC 0.006% ThioU | 5.9 | 1.3 |
比較實例4及5顯示在DIC的情況下MFI之已知較少增加。實例6至8顯示,當與ThioU組合時,∆MFI可明顯增加。
實例 9 至 10
實例9至10如實例1中所描述進行,但使用270℃之溫度而非230℃之擠出溫度。結果概述於表2中。
表2
添加劑 | MFI | ∆MFI | |
參考物 | --- | 6.6 | 0.0 |
比較實例6 | 0.04% PER | 29.5 | 22.9 |
實例9 | 0.03% PER 0.01% ThioU | 40.2 | 33.6 |
實例10 | 0.034% PER 0.006% ThioU | 41.1 | 34.5 |
實例9及10顯示,當過氧化物與ThioU組合時,∆MFI可增加。
實例 11 至 12
實例11至12如實例1中所描述進行,但使用250℃之溫度而非230℃之擠出溫度,且使用不同市售聚丙烯(來自lyondellbasell之Moplen HP561R研磨物,MFI 25 g/10 min ISO 1133-1)。結果概述於表3a及3b中。
表3a
添加劑 | MFI | ∆MFI | |
參考物 | --- | 28.6 | 0 |
比較實例7 | 0.006% PER | 33.7 | 5.1 |
比較實例8 | 0.006% ThioU | 31.2 | 2.6 |
實例11 | 0.003% PER 0.003% ThioU | 34.8 | 6.1 |
實例11顯示,當過氧化物與ThioU組合時,即使與比較實例7相比以較低濃度使用過氧化物時,∆MFI亦可增加。
表3b
添加劑 | MFI | ∆MFI | |
參考物 | --- | 28.6 | 0 |
比較實例9 | 0.006% DIC | 28.2 | -0.3 |
比較實例8 | 0.006% ThioU | 31.2 | 2.6 |
實例12 | 0.003% DIC 0.003% ThioU | 30.8 | 2.1 |
實例12顯示,當DIC與ThioU組合時,即使與比較實例9相比以一半濃度使用DIC時,∆MFI亦可增加。
實例 13 至 14
A)
製備母料經由浸泡將0.15% PER添加至市售聚丙烯(來自Lyondell Basell之Moplen HP 561R研磨物,MFI 25)中,產生過氧化物母料。出於此目的,將聚合物顆粒放入圓形陽模中。將陽模預加熱至60℃且隨後藉助於滴管添加PER。將陽模封閉且用PTFE密封。將陽模置放於旋轉蒸發器上且將混合物連續旋轉處理3小時。
藉助於高速混合機將0.15% ThioU混合至相同聚丙烯粉末(Moplen HP 561R)中,產生活化劑母料。在接下來的步驟中,在200℃下在雙螺桿擠出機(Berstorff ZE 25AX47D)中混配混合物。
B)
製備雙組分非編織物紡黏型非編織物係用聚丙烯製成:芯部為聚丙烯Total 7059 (MFI 11,來自TotalEnergies)且鞘部為聚丙烯PP 511A (MFI 25,來自Sabic),芯部含有或不含有添加劑,該等非編織物係在具有每公尺長度具有約6800個孔之單經軸的1 m寬Reicofil 4生產線上製造。該等孔具有0.62 mm之直徑。每孔之生產量設定為0.55 g/min。該生產線具有鞘芯型組態,其中鞘部含有20重量%之聚合物,且芯部含有80重量%之聚合物。製備比較纖維,其中兩個域均不含添加劑。
生產的非編織物之織物重量為70 g/m2 (生產線速度:52 m/min)。目標長絲細度為1.7分特(dtex) (分特為纖維之線性質量密度之量測單位,且定義為每10000公尺之質量,以公克為單位)。使用設定為165℃之軋花輥及設定為90 N/mm之夾持壓對非編織物進行熱黏合。
下表中給出之添加劑經由如上文所描述之其對應母料添加,其中重量%指示存在於母料中之添加劑之總量。
下文給出其他加工條件 :- 擠出機溫度為在Reicofil 4生產線上擠出聚丙烯或聚丙烯/添加劑摻合物時使用之溫度,在所有實例中,芯部設定為270℃且鞘部設定為250℃。
- 機艙壓力為模具後面及下面的機艙中之壓力,在所有實例中均設定為4500 Pa。
C)
對 機械特性之評估非編織織物之機械特性根據DIN EN 29073-3進行測定,其中樣品夾持長度為100 mm,樣品寬度為50 mm,前進(變形速度)為200 mm/min。拉伸強度TD及伸長率TD為在垂直於機器方向之方向上量測之對應最大值。伸長率MD為在機器方向上量測之對應最大值。結果概述於表4a及4b中。
表4a
添加劑 | 拉伸強度TD N/5 cm | |
參考物 | --- | 116.8 |
比較實例10 | 0.006% ThioU | 125.1 |
比較實例11 | 0.006% PER | 131.4 |
實例13 | 0.003% ThioU 0.003% PER | 133.0 |
實例13顯示,即使當使用較低量或一半量之PER時,與比較實例10至11相比,拉伸強度亦有所增加。
表4b
添加劑 | 伸長率MD % | 伸長率TD % | |
參考物 | --- | 125.3 | 119.4 |
比較實例12 | 0.006% ThioU | 133.0 | 129.4 |
比較實例13 | 0.006% PER | 147.5 | 129.1 |
實例14 | 0.003% ThioU 0.003% PER | 149.3 | 130.2 |
實例14顯示,即使當使用較低量或一半量之PER時,與比較實例12至13相比,伸長率亦有所增加。
Claims (15)
- 一種用於對聚合材料之流變進行改性的方法,其包含在該聚合材料中併入改性劑摻合物之步驟,該改性劑摻合物包含 a) 自由基起始劑,其係選自過氧化物、基於碳之自由基產生劑、雙偶氮化合物或穩定硝醯基化合物,及 b)式(1)之硫代胺基甲酸酯 其中 R a係基於有機異氰酸酯, 基團-S-R a係藉由與異氰酸酯基之反應引入, R b為視情況經取代及/或經間雜之C 2-C 40烷基,且 n等於或大於1。
- 如請求項1之方法,其中該自由基起始劑與該硫代胺基甲酸酯之重量比為1:2至30:1,較佳1:1至20:1,尤其1.5:1至5:1。
- 如請求項1或2之方法,其中該自由基起始劑係選自過氧化物或基於碳之自由基產生劑。
- 如請求項1至3中任一項之方法,其中該等基於碳之自由基產生劑具有式(17) 其中R 7、R 8、R 9及R 10中之各者獨立地選自由以下組成之群:氫原子、C1-6烷基、C1-2烷氧基、腈基及鹵素原子,且其中R 1、R 3、R 4及R 6中之各者獨立地選自由氫及C1-6烷基組成之群。
- 如請求項1至4中任一項之方法,其中該過氧化物為2,5-二甲基-2,5-雙(三級丁基-過氧基)己烷(DHBP)、2,5-二甲基-2,5-雙(三級丁基-過氧基)己炔-3 (DYBP)、過氧化二異丙苯基(DCUP)、過氧化二-三級丁基(DTBP)、過氧化三級丁基-異丙苯基(BCUP)、雙(三級丁基過氧異丙基)苯(DIPP)、3,6,9-三乙基-3,6,9-三甲基-1,4,7-三過氧壬烷、二(三級丁基過氧異丙基)苯、過氧化二碳酸二鯨蠟酯或單過氧化順丁烯二酸三級丁酯。
- 如請求項1至5中任一項之方法,其中該自由基起始劑以0.0001至5重量%之量添加至該聚合材料中。
- 如請求項1至6中任一項之方法,其中該硫代胺基甲酸酯以0.0001至5重量%之量添加至該聚合材料中。
- 如請求項1至7中任一項之方法,其中R a係基於有機異氰酸酯,該有機異氰酸酯為其中各者未經取代或經C 1-C 4烷基或二(C 1-C 4烷基)胺基取代之二異氰酸環己酯、二異氰酸亞甲基雙(環己基)酯、異佛酮二異氰酸酯(isophorone diisocyanate)、二異氰酸苯酯、二苯基甲烷二異氰酸酯或二異氰酸萘酯,或為二異氰酸C 4-C 20烷酯,或係基於藉由上述二異氰酸酯與其自身及/或與多元醇之反應獲得之寡聚或聚合產物。
- 如請求項1至8中任一項之方法,其中R a係基於有機異氰酸酯,該有機異氰酸酯為未經取代或經C 1-C 4烷基取代之二異氰酸苯酯,或係基於藉由上述二異氰酸酯與其自身及/或與多元醇之反應獲得之寡聚或聚合產物。
- 如請求項8或9之方法,其中該多元醇為包含兩個或更多個羥基之C 1-C 10烷醇,或為聚C 2-C 10烷二醇。
- 如請求項1至10中任一項之方法,其中R b為未經間雜或間雜有-O-及/或羰基之C 8-C 40烷基。
- 如請求項1至11中任一項之方法,其中該硫代胺基甲酸酯具有式(9)或(10) , 其中R b為視情況經取代及/或經間雜之C 2-C 40烷基。
- 如請求項1至12中任一項之方法,其中該聚合材料為熱塑性聚合物,較佳聚烯烴,且尤其為直鏈低密度聚乙烯、低密度聚乙烯、中密度聚乙烯、高密度聚乙烯、聚乙烯共聚物、聚丙烯均聚物或聚丙烯共聚物。
- 一種經改性聚合材料,其可藉由在如前述請求項中任一項中所定義之聚合材料中併入如前述請求項中任一項中所定義之改性劑摻合物來獲得,其中該改性劑摻合物包含 a) 自由基起始劑,其係選自過氧化物、基於碳之自由基產生劑、雙偶氮化合物或穩定硝醯基化合物,及 b)式(1)之硫代胺基甲酸酯 其中 R a係基於有機異氰酸酯, 基團-S-R a係藉由與異氰酸酯基之反應引入, R b為視情況經取代及/或經間雜之C 2-C 40烷基,且 n等於或大於1。
- 一種如前述請求項中任一項之改性劑摻合物,其中該改性劑摻合物包含 a) 自由基起始劑,其係選自過氧化物、基於碳之自由基產生劑、雙偶氮化合物或穩定硝醯基化合物,及 b)式(1)之硫代胺基甲酸酯 其中 R a係基於有機異氰酸酯, 基團-S-R a係藉由與異氰酸酯基之反應引入, R b為視情況經取代及/或經間雜之C 2-C 40烷基,且 n等於或大於1。
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