CN101191018A - 液体硅橡胶 - Google Patents
液体硅橡胶 Download PDFInfo
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- CN101191018A CN101191018A CNA2007101960234A CN200710196023A CN101191018A CN 101191018 A CN101191018 A CN 101191018A CN A2007101960234 A CNA2007101960234 A CN A2007101960234A CN 200710196023 A CN200710196023 A CN 200710196023A CN 101191018 A CN101191018 A CN 101191018A
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Abstract
一种制备可固化的有机聚硅氧烷组合物的方法,该组合物包括(A)具有含脂肪族碳碳多重键的基团的化合物,(B)具有硅键接的氢原子的有机聚硅氧烷,(D)催化剂,所述方法包括首先将100重量份的(A)和(B)或(A)和(D)加到容器中,然后进料至塑料加工机器的混合器中,或将以催化剂配方计为0.3至5重量份的(D)添加至(A)和(B)中,或将0.3至5重量份的(B)添加至(A)和(D)中。
Description
技术领域
本发明涉及一种制备可固化的有机聚硅氧烷(organopolysiloxane)组合物的方法。
背景技术
迄今为止,LRS(液体硅橡胶)或LTM(液体注射成型)典型地包括两种组分(A和B),该两种组分以1∶1或9∶1比例泵加至静态混合器中。然后利用注压机或其它设备进一步加工该混合物,进而得到模制品、挤出物或涂料。
该两种组分至少由具有乙烯基的聚二甲基硅氧烷(也可以是甲基之外的其它取代基,粘度在0.65至10,000,000mPas之间)组成。为了获得最终性质,绝大多数情况还添加填料和添加剂。
填料可以是活性(增强)或惰性填料,这依赖于LSR所设的要求。活性填料的例子有疏水或亲水的高度分散二氧化硅、疏水或亲水的沉淀二氧化硅、疏水或亲水的氧化铝等等。使用的惰性填料的例子有石英粉、滑石、硅灰石等等。
将铂催化剂(例如六氯铂酸或乙烯基硅氧烷配合物)添加至A组分中。将每个分子至少含2或3个氢原子的Si-H化合物添加至B组分中。将阻聚剂添加至A组分或B组分中以控制交联速度。
一组分或两组分还可以接受添加的助粘剂或与基体不相容的油,例如苯基硅油,或者热稳定剂(金属氧化物、金属辛酸盐、炭黑)。
对于180℃的硫化温度,在利用注射量为5克的1∶1至9∶1的混合物制备奶嘴(pacifier)的生产过程中,该A组分和B组分所需的交联时间一般不超过25秒。在室温下,该A-B混合物在至少3天内保持为液体,这样在任意停止生产后,可允许重新开始生产。
图1显示了现有技术LSR的加工过程:
在该图中,两种组分(组分A和组分B)以1∶1或9∶1的混合比泵加至静态或动态混合器(3)中。经另一管线(2)添加色料,然后在塑模(4)和(5)中进一步加工得到的组合物。
发明内容
本发明的目的在于提供一种制备可固化的有机聚硅氧烷组合物的方法,该组合物包括
(A)具有含脂肪族碳碳多重键的基团的化合物,
(B)具有硅键接的氢原子的有机聚硅氧烷,
(D)催化剂,
该方法包括首先将100重量份的(A)和(B)或(A)和(D)加到容器中,然后进料至塑料加工机器的混合器中,例如优选注压机、刮刀装置、挤出机、压延机系统等等,优选注压机,优选通过泵的装置,或优选将以催化剂配方计为0.3至5重量份,优选0.3至4重量份,更优选0.3至3重量份,尤其优选0.3至2重量份,尤其非常优选0.3至1重量份,更优选1重量份的(D)添加至(A)和(B)中,或优选将0.3至5重量份,优选0.3至4重量份,更优选0.3至3重量份,尤其优选0.3至2重量份,尤其非常优选0.3至1重量份,更优选1重量份的(B)添加至(A)和(D)中。
(D)催化剂(D)用作二有机聚硅氧烷(A)(diorganopolysiloxanes(A))的脂肪族不饱和烃基与有机氢化聚硅氧烷(B)(organohydropoly-siloxanes(B))的硅键接氢原子间氢化硅烷化作用加成反应的氢化硅烷化催化剂。文献描述了多种适合的氢化硅烷化催化剂。原则上可以使用加成交联硅橡胶组合物中采用的任何现有技术的氢化硅烷化催化剂。
使用的氢化硅烷化催化剂(D)可包括金属及其化合物,例如铂、铑、钯、钌和铱,优选铂。如果合适,金属可以连接在细颗粒载体材料上,例如活性炭,或金属氧化物、例如氧化铝,或二氧化硅。
优选使用铂和铂化合物。尤其优选在聚有机硅氧烷中可溶的铂化合物。可以使用的可溶铂化合物的例子为式(PtCl2·烯烃)2和H(PtCl3·烯烃)的铂-烯烃配合物,这里优选使用具有2至8个碳原子的烯烃,例如乙烯、丙烯、丁烯和辛烯的异构体、或具有5至7个碳原子的环烷烃,例如环戊烯、环己烯和环庚烯。其它可溶的铂催化剂为式(PtCl2C3H6)2的铂-环丙烷配合物、六氯铂酸与醇、醚、醛及其混合物的反应产物、或在乙醇溶液中六氯铂酸与甲基乙烯基环四硅氧烷在碳酸氢钠存在条件下的反应产物。也可以使用具有磷配体、硫配体和胺配体的铂催化剂,例如(Ph3P)2PtCl2。尤其优选铂与乙烯基硅氧烷的配合物,例如对称二乙烯基四甲基二硅氧烷,这里尤其优选1,3-二乙烯基-1,1,3,3-四甲基二硅氧烷铂配合物。
氢化硅烷化催化剂(D)的使用量依赖于所需要的交联速度和经济上的因素。每100重量份的二有机聚硅氧烷(A)通常使用的量优选为1×10-8至5×10-2重量份,尤其为1×10-6至1×10-2重量份的铂催化剂,以铂金属的含量计算。(本发明的组合物包含铂催化剂(D),其使用量使结果得到的铂含量每次以组合物总重量计优选为0.05至500重量ppm之间(ppm=每100万重量份之一重量份),尤其优选为0.5至100重量ppm之间,特别是为1至50重量ppm之间)。
铂催化剂为选自下式的化合物
和/或下述通式的结构单元
和(如果适合)下述通式的结构单元
R9 rSiO(4-r)/2 (VI),
构成的低聚物或聚合物,
其中
R2为任选取代的二烯,其通过至少一个π键连接到铂上,且其为具有4至18个碳原子的未支化或支化链,或为具有6至28个碳原子的环,
R3可以相同或不同,其为氢原子、卤原子、-SiR4 3、-OR6或具有1至24个碳原子的一价的任意取代的烃基,条件是在式(III)的化合物中至少一个R3基为-SiR4 3,
R4可以相同或不同,其为氢原子、卤原子、-OR6或具有1至24个碳原子的一价的任选取代的烃基,
R6可以相同或不同,其为氢原子、-SiR4 3、或具有1至20个碳原子的一价的任选取代的烃基,
R7可以相同或不同,其为氢原子、卤原子、-SiR4 3、-SiR4 (3-t)[R8SiR9 sO(3-s)/2]t、-OR6或具有1至24个碳原子的一价的任意取代的烃基,条件是在式(V)中至少一个R7基为-SiR4 (3-t)[R8SiR9 sO(3-s)/2]t,
R8可以相同或不同,其为氧或具有1至24个碳原子的二价的任选取代的烃基,其可以通过氧原子键接到硅上,
R9可以相同或不同,其为氢或有机基,
r为0、1、2或3,
s为0、1、2或3,及
t为1、2或3。
如果R2是取代的二烯或如果R3、R4、R5、R6、R7和R8基团是取代的烃基,优选的取代基为卤原子、例如F、Cl、Br和I,氰基,-NR6 2,杂原子、例如O、S、N和P,以及-OR6基团,其中R6定义如上。
本发明使用的铂催化剂(D)优选为二(炔基)(1,5-环辛二烯)铂配合物、二(炔基)(二环[2.2.1]庚-2,5-二烯)铂配合物、二(炔基)(1,5-二甲基-1,5-环辛二烯)铂配合物和二(炔基)(1,6-二甲基-1,5-环辛二烯)铂配合物。
尤其优选铂与乙烯基硅氧烷的配合物,例如对称二乙烯基四甲基二硅氧烷,以及尤其非常优选1,3-二乙烯基-1,1,3,3-四甲基二硅氧烷铂配合物。
本发明使用的铂催化剂(D)的量依赖于所需要的交联速度和各自的使用情况,以及经济上的因素。本发明的组合物包含铂催化剂(D),其使用量使结果得到的铂含量每次以组合物总重量计优选为0.05至500重量ppm之间(ppm=每100万重量份之一重量份),尤其优选为0.5至100重量ppm之间,特别是为1至50ppm重量之间。
为了达到本发明的目的,术语“有机聚硅氧烷”的意思不仅包括聚合和低聚硅氧烷,还包括二聚硅氧烷。
本发明方法中使用的组合物可以包括单组分有机聚硅氧烷组合物或者两组分有机聚硅氧烷组合物。在后一种情况中,本发明组合物的两种组分可以包含在任何所需要的结合中的任意组分,一般条件是一组分不能同时包含具有脂肪族多重键的硅氧烷、具有硅键接的氢原子的硅氧烷和催化剂,也就是,本质上不能同时包含组分(A)、(B)和(D)或、分别地(C)和(D)。本发明的组合物也优选称作单组分组合物。
以已知的方式选择本发明组合物中使用的化合物(A)和(B),以致允许交联。例如,因此,化合物(A)至少包含两个脂肪族不饱和基团,及硅氧烷(B)包含至少三个硅键接的氢原子,或化合物(A)至少包含三个脂肪族不饱和基团,及硅氧烷(B)包含至少两个硅键接的氢原子,或者不使用化合物(A)和(B),使用硅氧烷(C),其具有上述比例的脂肪族不饱和基团和硅键接的氢原子。
本发明使用的化合物(A)还可以是优选具有至少两个脂肪族不饱和基团的不含硅的有机化合物,或优选具有至少两个脂肪族不饱和基团的有机硅化合物。本发明组合物中作为化合物(A)使用的有机化合物的例子是1,3,5-三乙烯基环己烷、2,3-二甲基-1,3-丁二烯、7-甲基-3-亚甲基-1,6-辛二烯、2-甲基-1,3-丁二烯、1,5-己二烯、1,7-辛二烯、4,7-亚甲基-4,7,8,9-四氢茚、甲基环戊二烯、5-乙烯基-2-降冰片烯、二环[2.2.1]庚-2,5-二烯、1,3-二异丙烯基苯、含乙烯基的聚丁二烯、1,4-二乙烯基环己烷、1,3,5-三烯丙基苯、1,3,5-三乙烯基苯、1,2,4-三乙烯基环己烷、1,3,5-三异丙烯基苯、1,4-二乙烯基苯、3-甲基-1,5-庚二烯、3-苯基-1,5-己二烯、3-乙烯基-1,5-己二烯和4,5-二甲基-4,5-二乙基-1,7-辛二烯、N,N′-亚甲基二(丙烯酰胺)、1,1,1-三(羟甲基)丙烷三丙烯酸酯、1,1,1-三(羟甲基)丙烷三甲基丙烯酸酯、三丙二醇二丙烯酸酯、二烯丙基醚、二烯丙基胺、二烯丙基碳酸酯、N,N′-二烯丙基脲、三烯丙基胺、三(2-甲基烯丙基)胺、2,4,6-三烯丙氧基-1,3,5-三嗪、三烯丙基-s-三嗪-2,4,6-(1H,3H,5H)三酮、二烯丙基丙二酸、聚乙二醇二丙烯酸酯、聚乙二醇二甲基丙烯酸酯及聚丙二醇甲基丙烯酸酯。
然而,该新的硅氧烷组合物优选包括作为组分(A)的脂肪族不饱和有机硅化合物,并可以使用迄今为止在加成-交联组合物中使用的任何脂肪族不饱和有机硅化合物,或者,例如,具有脲嵌段的硅氧烷嵌段共聚物,具有酰胺嵌段和/或具有酰亚胺嵌段和/或具有酯-酰胺嵌段和/或具有聚苯乙烯嵌段和/或具有硅杂亚芳基(silarylene)嵌段和/或具有碳硼烷嵌段的硅氧烷嵌段聚合物以及与醚基团的硅氧烷接枝共聚物。
有机硅化合物(A),其具有含脂肪族碳碳多重键的SiC键接的基团,优选包含由下式单元构成的线性或支化有机聚硅氧烷
RaR1 bSiO(4-a-b)/2 (I)
其中,
R可以相同或不同,其为不含脂肪族碳碳多重键的有机基,
R1可以相同或不同,其为具有脂肪族碳碳多重键的一价的未取代或取代的、SiC键接的烃基,
a为0、1、2或3,及
b为0、1或2,
条件是a和b的和小于或等于3,及每个分子中平均至少含2个R1基团。
R基可以是一价基团或具有两个或多个化合价的基团,其中具有两个或多个化合价的基团,例如二价、三价和四价基团,然后使式(I)的一定数目的甲硅烷氧基单元相互键接,例如,两个、三个或四个甲硅烷氧基单元。
R包括一价基团-F、-Cl、-Br、-OR6、-CN、-SCN、-NCO基和SiC键接的未取代或取代的烃基,其可以由氧原子或-C(O)-基团隔开,或者如在式(I)中在两边硅键接的二价基团。
如果R基为SiC键接的取代烃基、优选的取代基为卤原子、含磷的基团、氰基、-OR6、-NR6-、-NR6 2、-NR6-C(O)-NR6 2、-C(O)-NR6 2、-C(O)-R6、-C(O)OR6、-SO2-Ph和C6F5,其中R6定义如上,Ph为苯基。
R基的例子是烷基、例如甲基、乙基、正丙基、异丙基、正丁基、异丁基、叔丁基、正戊基、异戊基、新戊基和叔戊基,己基、例如正己基,庚基、例如正庚基,辛基、例如正辛基,和异辛基、例如2,2,4-三甲基-戊基,壬基、例如正壬基,癸基、例如正癸基,十二烷基、例如正十二烷基,十八烷基、例如正十八烷基,环烷基、例如环戊基、环己基、环庚基和甲基环己基,芳基、例如苯基、萘基、蒽基和菲基,烷芳基、例如邻、间和对甲苯基、二甲苯基和乙基苯基,及芳烷基、例如苄基和α-及β-苯乙基。
取代的R基的例子是卤烷基、例如3,3,3-三氟-n-丙基、2,2,2,2′,2′,2′-六氟异丙基、七氟异丙基,卤芳基、例如邻、间和对氯苯基,-(CH2)n-N(R6)C(O)NR6 2,-(CH2)n-C(O)NR6 2,-(CH2)n-C(O)R6,-(CH2)n-C(O)OR6,-(CH2)n-C(O)NR6 2,-(CH2)n-C(O)-(CH2)m-C(O)CH3,-(CH2)n-NR6-(CH2)m-NR6 2,-(CH2)n-O-CO-R6,-(CH2)n-O-(CH2)m-CH2)m-CH(OH)-CH2OH,-(CH2)n-(OCH2CH2)m-OR6,-(CH2)n-SO2-Ph和-(CH2)n-O-C6F5,其中R6具有一种上述所给的意思,n和m为0至10之间的相同或不同的整数,Ph为苯基。
如式(I)中在两边都硅键接的二价R基的例子为由上述所给出的R一价基团例子衍生得到的基团,其中另一个键取代氢原子。该类型的基团的例子是-(CH2)n-、-CH(CH3)-、-C(CH3)2-、-CH(CH3)-CH2-、-C6H4-、-CH(Ph)-CH2-、-C(CF3)2-、-(CH2)n-C6H4-(CH2)n-、-(CH2)n-C6H4-C6H4-(CH2)n-、-(CH2O)m-、-(CH2CH2O)m-和-(CH2)n-Ox-C6H4-SO2-C6H4-Ox-(CH2)n-,其中x为0或1,m和n定义如上,Ph为苯基。
R基优选为一价的、SiC键接的未取代或取代的具有1至18个碳原子及不含脂肪族碳碳多重键的烃基,尤其优选一价的、SiC键接的、具有1至6个碳原子及不含脂肪族碳碳多重键的烃基,尤其是甲基或苯基。
R1基可以是用于与SiH官能团化合物加成反应(氢化硅烷化)的任何所需基团。
如果R1基为SiC键接的取代的烃基,优选的取代基为卤原子、氰基和-OR6,其中R6定义如上。
R1优选为具有2至16个碳原子的烯基或炔基,例如乙烯基、烯丙基、甲代烯丙基、1-丙烯基、5-己烯基、乙炔基、丁二烯基、己二烯基、环戊烯基、环戊二烯基、环己烯基、乙烯基环己基乙基、二乙烯基环己基乙基、降冰片烯基、乙烯基苯基或苯乙烯基,尤其优选乙烯基、烯丙基和己烯基。
组分(A)的摩尔质量可以在很宽的范围内变化,例如在102至106g/mol之间。因此,组分(A)可以是,例如相对低分子量烯基官能的低聚硅氧烷,如1,2-二乙烯基-四甲基二硅氧烷,但也可以是在链上或链端具有硅键接的乙烯基的高度聚合的聚二甲基硅氧烷,例如具有105g/mol的摩尔质量(由核磁共振测得的数均分子量)。还没有限定形成组分(A)的分子结构。特别是,较高分子量的结构,也就是低聚或聚合硅氧烷的结构可以是线性的、环状的、支化的甚或类似树脂或网状的结构。线性和环状聚硅氧烷优选由式R3SiO1/2、R1R2SiO1/2、R1RSiO2/2和R2SiO2/2的单元构成,其中R和R1定义如上。支化或网状聚硅氧烷还包含三官能和/或四官能的单元,其中优选具有式RSiO3/2、R1SiO3/2和SiO4/2的那些单元。当然也可能使用满足组分(A)标准的不同硅氧烷的混合物。
使用的组分(A)优选包含乙烯基官能的基本上线性的每种情况下25℃时具有0.01至500,000Pa·s粘度的、尤其优选25℃时具有0.1至100,000Pa·s粘度的聚二有机硅氧烷。
使用的有机硅化合物(B)可以是迄今为止在加成-交联组合物中使用的任何氢官能的有机硅化合物。
使用的具有硅键接的氢原子的有机聚硅氧烷(B)优选包括线性、环状或支化的由下式单元构成的有机聚硅氧烷
RcHdSiO(4-c-d)/2 (II)
其中
R可以相同或不同,其定义如上,
c为0、1、2或3,及
d为0、1或2,
条件是c和d的和小于或等于3,及每个分子中平均至少含2个硅键接的氢原子。
本发明使用的有机聚硅氧烷(B)优选包含以有机聚硅氧烷(B)的总重量计为0.04至1.7重量%的硅键接的氢原子。
组分(B)的摩尔质量同样可以在宽的范围内变化,例如在102至106g/mol之间变化。因此,组分(B)可以是,例如相对低分子量SiH-官能的低聚硅氧烷,如四甲基二硅氧烷,但也可以是在链上或链端具有SiH基团的高度聚合的聚二甲基硅氧烷,或具有SiH基团的有机硅树脂。构成组分(B)的分子结构也可以自由选择。特别是,较高分子量的结构,也就是含有SiH基团的低聚或聚合硅氧烷的结构可以是线性的、环状的、支化的甚或类似树脂或网状的结构。线性和环状聚硅氧烷优选由式R3SiO1/2、HR2SiO1/2、HRSiO2/2和R2SiO2/2的单元构成,其中R定义如上。支化或网状聚硅氧烷还包含三官能和/或四官能的单元,其中优选具有式RSiO3/2、HSiO3/2和SiO4/2的那些单元。当然也可能使用满足组分(B)标准的不同硅氧烷的混合物。特别是,构成组分(B)的分子除包含必须的SiH基团外,如果需要同时还可以包含脂肪族不饱和基团。尤其优选使用低分子量的SiH官能的化合物,例如四(二甲基甲硅烷氧基)硅烷和四甲基环四硅氧烷,以及相对高分子量的含SiH的硅氧烷,例如聚(羟甲基)硅氧烷和在25℃时具有10至10,000mPa·s粘度的聚(二甲基羟甲基)硅氧烷,或一些甲基基团被3,3,3-三氟丙基或苯基基团所取代的类似的含SiH化合物。
优选组分(B)在新的可交联硅氧烷组合物中的使用量使得SiH基团对脂肪族不饱和基团的摩尔比在0.1至20之间,优选在1.0至5.0之间。
本发明中使用的组分(A)和(B)为商业上可获得的产品或由常见的化学方法制备。
几种二(炔基)(η-烯烃)铂化合物及其制备方法是本领域技术人员已知的。例如可以参考J.Chem.Soc.,Dalton Trans.(1986)1987-92和Organometallics(1992)11 2873-2883。可以采用类似的合成和提纯步骤制备本发明的铂催化剂(D)。
本发明使用的铂催化剂(D)优选为二(炔基)(1,5-环辛二烯)铂配合物、二(炔基)(二环[2.2.1]庚-2,5-二烯)铂配合物、二(炔基)(1,5-二甲基-1,5-环辛二烯)铂配合物和二(炔基)(1,6-二甲基-1,5-环辛二烯)铂配合物。
本发明使用的铂催化剂(D)也可以是铂与乙烯基硅氧烷的配合物,例如对称二乙烯基四甲基二硅氧烷,尤其优选1,3-二乙烯基-1,1,3,3-四甲基二硅氧烷铂配合物。
本发明使用的铂催化剂(D)的量依赖于所需要的交联速度和各自的应用,以及经济因素。本发明的组合物包含铂催化剂(D),其使用量使结果得到的铂含量每次以组合物总重量计优选为0.05至500重量ppm之间(ppm=每100万重量份之一重量份),尤其优选为0.5至100重量ppm之间,特别是为1至50ppm重量之间。
除组分(A)至(D)外,本发明可固化的组合物也可以包括迄今为止用来制备加成-可交联组合物使用的任何其它物质。
本发明组合物中用作组分(E)的增强填料的例子是BET表面积至少50m2/g的热解或沉淀二氧化硅,也可以是炭黑和活性炭,例如炉法炭黑和乙炔黑,优选BET表面积至少50m2/g的热解和沉淀二氧化硅。
上述的二氧化硅填料可以具有亲水特征或已经由已知的方法疏水化。在混合引入亲水填料时需要疏水剂。
本发明的可交联组合物的活性增强填料(E)的含量在0至70重量%之间,优选在0至50重量%之间。
本发明的硅橡胶组合物可以任选包含比例至多70重量%,优选在0.0001至40重量%之间的作为组分(F)的进一步填料。这些添加剂,例如可以是惰性填料、不同于硅氧烷(A)、(B)和(C)的类树脂的聚有机聚硅氧烷、分散剂、溶剂、助粘剂、颜料、染料、增塑剂、有机聚合物、热稳定剂等等。其中的添加剂如石英粉、硅藻土、粘土、白垩、锌钡白、炭黑、石墨、金属氧化物、金属碳酸盐、金属硫酸盐、羧酸的金属盐、金属灰尘(metal dusts)、纤维如玻璃纤维、合成纤维、塑料粉、染料、颜料等等。
还可以使用添加剂(G),其用于控制调节本发明的组合物加工时间、初始温度和交联速度。这些抑制剂(inhibitor)和稳定剂在加成-交联组合物领域已非常熟悉。常用抑制剂的例子为炔醇、例如1-乙炔基-1-环己醇、2-甲基-3-丁炔-2-醇和3,5-二甲基-1-己炔-3-醇、3-甲基-1-十二炔-3-醇,聚甲基乙烯基环硅氧烷、如1,3,5,7-四乙烯基四甲基四环硅氧烷,具有甲基乙烯基SiO2/2基团和/或R2乙烯基SiO1/2端基的低分子量硅氧烷油、例如二乙烯基四甲基二硅氧烷、四乙烯基二甲基二硅氧烷,三烷基氰尿酸酯,顺丁烯二酸烷基酯、如顺丁烯二酸二烯丙酯、顺丁烯二酸二甲酯和顺丁烯二酸二乙酯,反丁烯二酸烷基酯、如反丁烯二酸二烯丙酯和反丁烯二酸二乙酯,有机氢过氧化物、如异丙基苯氢过氧化物、叔丁基氢过氧化物和蒎烷氢过氧化物,有机过氧化物,有机亚砜,有机胺、二胺,及酰胺、磷酸盐(phosphane),及亚磷酸盐,腈,三唑,二氮丙啶,及肟。这些抑制剂添加剂(inhibitoradditives)(G)的作用依赖于其化学结构,因此必须分别确定。
本发明组合物的抑制剂含量优选在0至50,000ppm之间,尤其优选在20至2000ppm之间,特别在100至1000ppm之间。
如果需要,本发明的有机聚硅氧烷组合物可以溶解、分散、悬浮或乳化在液体中。尤其依赖于组分的粘度和填料的含量,本发明的组合物可以是低粘度和可流动的,具有类似浆状物的稠度,可以是粉状的,或高粘度的均匀组合物,被本领域技术人员经常称作RTV-1、RTV-2、LSR和HTV的组合物的例子已为人所熟知。特别是,如果本发明的组合物具有高的粘度,可以将其制成粒丸(pellet)形式。这里每个单独的粒丸可以包含所有的组分,或本发明使用的组分D和B可以单独包含在不同的粒丸中。同样,本发明交联的硅氧烷组合物包含了所有的弹性性质,由极其软的硅氧烷凝胶开始,到橡胶似的材料,至形成高度交联的具有类似玻璃性质的硅氧烷。
可以通过已知的方法制备本发明的有机聚硅氧烷组合物,例如通过不同组分的均匀混合。这里的顺序是所需的,但是优选均匀混合由(A)和(B),如果适合,(E)、(F)和(G)构成的混合物,形成组合物,添加至容器中。接下来可以固体物质、分散体、或溶液(溶解在合适的溶剂中)、或已知的母料的形式添加本发明使用的铂催化剂(D)。在加工之前使用静态或动态混合器立即混合,参见下面。优选通过附加泵添加催化剂(D)。
本发明使用的组分(A)至(G)中的每种组分可以是单一类型该组分,或是由至少两种不同类型的该组分组成的混合物。
本发明的组合物可以通过硅键接的氢对脂肪族多重键的加成反应交联,其可以在与迄今为止已知组合物使用的相同条件下交联,及通过氢化硅烷化作用反应交联。这里温度优选为100至220℃之间,尤其优选在130至190℃之间,这里压力优选在900至1100hPa之间。然而,也可以使用较高或较低的温度和压力。
附图说明
图2描述的本发明的方法:
将100份的主要组分由计量装置(1)和1至2份的铂催化剂由计量装置(2)泵加至混合器(3)中。然后混合的反应料向前进行加工。此时优选采用注压机的注射装置方式。然后优选将其注射进加热的冷流道模(4,5),并硫化得到模制品。
本发明的一个惊奇发现是,单元重5克的奶嘴的循环时间现在只是混合比为1∶1或9∶1的传统液体硅氧烷循环时间的一半。
由该事实获得了另外的好处,主要组分现在可以包含与铂催化剂不相容的组分。由于铂催化剂与不相容物质间短的接触时间,于是在进行加工之前其活性不受影响。
而且,根据不同的加工要求,可以熟练的改变铂催化剂的量来调节硫化速度。这样获得了利用9∶1或1∶1体系所不能获得的节约的可能性,因为在后一种情况中,必须精确保证混合比。
而且,为了修理的目的在装置关闭前,减少催化剂的量延长了生产重新开始前消耗的时间。
在一种本发明优选的制备可固化有机聚硅氧烷组合物的方法中,以任意所需要的混合比,由一个鼓将软组合物(低粘度)和由另一个鼓将硬组合物(高粘度)泵加至静态混合器中,且(D)和/或(B)通过泵装置进料。
具体实施方式
母体组合物:均匀混合70%的粘度为20,000mPas(室温下)、带有乙烯基端基的聚二甲基硅氧烷(PDMS)和30%的比表面积为300m2/g的硅氮烷疏水化的二氧化硅。
实施例1:
将0.3份的三甲基硅烷醇、1.75份的Si-H交联剂(具有0.46%的H官能团和100mPas的粘度)和0.08份的乙炔基环己醇添加至100份的母体组合物中。
将该混合物进料至20升(20l)鼓中。
这些鼓夹在ENGEL LSR机器的泵装置上。将制备的铂催化剂(粘度为500mPas的硅油中的1,3-二乙烯基-,1,3,3-四甲基二硅氧烷铂配合物;铂含量为0.1%)进料至机器的色料管线(一般只用于进料色料母料)中,以每100%的混合物1.5%的水平泵加至静态混合器中。
在静态混合器中,100份的混合物与1.5份的铂催化剂相互混合并均化,然后压入注压机的注射圆筒中。然后接下来进行注射循环。利用EMDE模生产的注射成型物为吸水螺纹接口(drinking nipple)。循环时间为10s。
实施例2:
将0.3份的三甲基硅烷醇、1.5份制备的铂催化剂(实施例1)和0.08份的乙炔基环己醇添加至100份的母体组合物中。
将该混合物进料至20升(20l)鼓中。
这些鼓夹在ENGEL LSR机器的泵装置上。将Si-H交联剂(具有0.46%的H官能团和100mPas的粘度)进料至机器的色料管线(一般只用于进料色料母料)中,以每100%的混合物1.75%的水平泵加至静态混合器中。
在静态混合器中,100份的混合物与1.75份的Si-H交联剂混合并均化,然后压入注压机的注射圆筒中。然后接下来进行注射循环。利用EMDE模生产的注射成型物为吸水螺纹接口。循环时间为20s。
机械性质可以根据交联剂量在±10%范围内的改变而变化。
循环时间也可以由具有高Si-H含量的交联剂的添加而变化。
对比实施例:
A组分包含100份的母体组合物、3份的铂催化剂和0.3份的三甲基硅烷醇。
B组分包含100份的母体组合物、3.5份的Si-H交联剂和0.16份的乙炔基环己醇。
同一LSR的A组分和B组分在同一装置上以1∶1的混合比按照传统的方法加工。循环时间是20秒。循环时间和/或机械性质不变。
Claims (4)
1.一种制备可固化的有机聚硅氧烷组合物的方法,其包括
(A)具有含脂肪族碳碳多重键的基团的化合物,
(B)具有硅键接的氢原子的有机聚硅氧烷,
(D)催化剂,
其包括首先将100重量份的(A)和(B)或(A)和(D)加到容器中,然后进料至塑料加工机器的混合器中,或将以催化剂配方计为0.3至5重量份的(D)添加至(A)和(B)中,或将0.3至5重量份的(B)添加至(A)和(D)中。
2.根据权利要求1所述的制备可固化的有机聚硅氧烷组合物的方法,其中,使用的催化剂包括1,3-二乙烯基-1,1,3,3-四甲基-二硅氧烷铂配合物、二(炔基)(1,5-环辛二烯)铂配合物、二(炔基)(二环[2.2.1]庚-2,5-二烯)铂配合物、二(炔基)(1,5-二甲基-1,5-环辛二烯)铂配合物和二(炔基)(1,6-二甲基-1,5-环辛二烯)铂配合物。
3.根据权利要求1或2所述的制备可固化的有机聚硅氧烷组合物的方法,其中,(D)和(B)通过泵装置进料。
4.根据权利要求1所述的制备可固化的有机聚硅氧烷组合物的方法,其中,塑料加工机器是注压机。
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DE102006056378A DE102006056378A1 (de) | 2006-11-29 | 2006-11-29 | Flüssigsiliconkautschuk |
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CN101798391A (zh) * | 2010-03-29 | 2010-08-11 | 东莞市良展有机硅科技有限公司 | 一种改性纺织品硅胶的制备工艺及其制品 |
CN105694047A (zh) * | 2016-04-26 | 2016-06-22 | 烟台德邦先进硅材料有限公司 | 主链含环状结构改性有机硅聚合物及其制备方法 |
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DE102010062139A1 (de) * | 2010-11-29 | 2012-05-31 | Wacker Chemie Ag | Einkomponentige Organopolysiloxanmassen mit hoher relativer Permittivität |
US20120252924A1 (en) * | 2011-03-29 | 2012-10-04 | Cassandra Ann Mahoney | Flavored silicone products |
WO2019023841A1 (en) | 2017-07-31 | 2019-02-07 | Dow Silicones Corporation | METHOD AND APPARATUS FOR MANUFACTURING LIQUID SILICONE RUBBER COMPOSITIONS |
BE1025602B1 (nl) * | 2017-09-29 | 2019-04-29 | Exypnos Bvba | Verbeterd product uit twee componenten siliconen rubber |
TWM588049U (zh) * | 2019-05-03 | 2019-12-21 | 美商埃肯矽樹脂美國股份有限公司 | 用於經由射出成型產生模製矽膠產品的裝置總成 |
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JPS58171442A (ja) * | 1981-12-07 | 1983-10-08 | Toray Silicone Co Ltd | シリコ−ンゴム成形体とその製造方法 |
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US4803244A (en) * | 1987-11-16 | 1989-02-07 | Union Carbide Corporation | Process for the preparation of thermoplastic elastomers |
US4929669A (en) * | 1988-12-27 | 1990-05-29 | Dow Corning Corporation | Organosiloxane compositions yielding elastomers with improved recovery following prolonged compression |
JPH0899332A (ja) * | 1994-09-29 | 1996-04-16 | Toray Dow Corning Silicone Co Ltd | 複合体の成形方法 |
TW296401B (zh) * | 1994-12-26 | 1997-01-21 | Shinetsu Chem Ind Co | |
US5698654A (en) * | 1996-07-30 | 1997-12-16 | General Electric Company | Process for preparing hydrogen siloxane copolymers |
US5753751A (en) * | 1996-10-24 | 1998-05-19 | General Electric Company | Process for preparing self-curable alkenyl hydride siloxane copolymers and coating composition |
DE19701393A1 (de) * | 1997-01-16 | 1998-07-23 | Wacker Chemie Gmbh | Polymere Organosiliciumverbindungen, deren Herstellung und Verwendung |
JP4565478B2 (ja) * | 2000-02-22 | 2010-10-20 | 東レ・ダウコーニング株式会社 | シリコーンゴム成形品の製造方法 |
JP4947858B2 (ja) * | 2001-08-21 | 2012-06-06 | 東レ・ダウコーニング株式会社 | 導電性液状シリコーンゴム組成物、導電性シリコーンゴム成形物およびその製造方法 |
DE10214137A1 (de) * | 2002-03-28 | 2003-10-16 | Wacker Chemie Gmbh | Siliconmassen mit verbesserter Hitzestabilität |
DE10359705A1 (de) * | 2003-12-18 | 2005-07-14 | Wacker-Chemie Gmbh | Additionsvernetzende Siliconharzzusammensetzungen |
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CN101798391A (zh) * | 2010-03-29 | 2010-08-11 | 东莞市良展有机硅科技有限公司 | 一种改性纺织品硅胶的制备工艺及其制品 |
CN105694047A (zh) * | 2016-04-26 | 2016-06-22 | 烟台德邦先进硅材料有限公司 | 主链含环状结构改性有机硅聚合物及其制备方法 |
CN105694047B (zh) * | 2016-04-26 | 2018-09-25 | 烟台德邦先进硅材料有限公司 | 主链含环状结构改性有机硅聚合物及其制备方法 |
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