CN107532040A - 用含有烷氧基聚硅氧烷的组合物浸渍纺织品的方法 - Google Patents
用含有烷氧基聚硅氧烷的组合物浸渍纺织品的方法 Download PDFInfo
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- CN107532040A CN107532040A CN201680022933.8A CN201680022933A CN107532040A CN 107532040 A CN107532040 A CN 107532040A CN 201680022933 A CN201680022933 A CN 201680022933A CN 107532040 A CN107532040 A CN 107532040A
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Classifications
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- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/643—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
- D06M15/647—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain containing polyether sequences
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/14—Polysiloxanes containing silicon bound to oxygen-containing groups
- C08G77/18—Polysiloxanes containing silicon bound to oxygen-containing groups to alkoxy or aryloxy groups
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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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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
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- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/04—Polysiloxanes
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- D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
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- D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
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- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/263—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acids; Salts or esters thereof
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Abstract
本发明涉及一种用包含下式(I)的烷氧基聚硅氧烷(A)的组合物浸渍纺织品的方法:R1 3SiO[SiR1(OR2)O]x[SiR1 2O]y[SiR1R3O]zSiR1 3(I);其中:R1相同或不同,并且代表任选取代的C1‑C7烃基,R2相同或不同,并且代表氢原子或C1‑C6烃基,R3相同或不同,并且代表C8‑C30烃基,x是具有至少1的值的整数,优选至少5,至多1000,优选至多100,y是具有至少0至多1000,优选至多100,前提条件是:x单元[SiR1(OR2)O]的量至少10mol%,优选至少30mol%,并且至多100mol%,优选至多70mol%,y单元[SiR1 2O]的量至少0mol%且至多90mol%,优选至多50mol%,并且z单元[SiR1R3O]的量至少0mol%,优选至少20mol%,并且至多90mol%,优选至多70mol%,所有的量均基于硅氧烷单元的x+y+z的总和。
Description
本发明涉及用包含烷氧基聚硅氧烷的组合物浸渍纺织品的方法以及具有较长烷基部分的烷氧基聚硅氧烷。
纺织品在诸如工业纺织品、帐篷和遮阳篷、特别是服装的不同行业中使用。暴露于天气的纺织品,例如雨衣,需要不渗透且不吸收水分。对于服装,特别需要的是纺织品-尽管是防水的-仍然应该保持足够的透气性,即不被聚合物的不间断膜密封。
耐水处理可以利用石蜡与锆皂的混合物。这些确实引起了非常高的接触角,但是洗衣或干洗后该影响明显更差(Odvarka,J.,Dembicky,J.,Wiener,J.,Kovacic,V.,Textile Faculty,Technical University of Liberec,Liberec,捷克共和国,Vlakna aTextil,9(2),58-69,2002)。具有Si-H基团的硅氧烷乳液在这方面则是有利的(Ramaszeder,K.,Textilveredlung 1995,30(11/12),256-62)。然而,这些硅氧烷在使用中具有产生氢气并因而具有安全风险的缺点。
因此,近几十年来,氟碳化合物用于防水处理(例如US 4,070,152A,EP 1 687 359B1)。但由于环保的原因,这些产品由于某些原料和分解产品而可能会保留在环境中。
由于这些环境问题及其高成本,含氟硅烷和硅氧烷的配制物也不具有吸引力(例如EP 1 217 119 B1和WO 04/018758 A2)。
可水解硅烷的应用在技术上过于复杂,以致于不能广泛应用(例如US 2009/0206296 A1)。
因此,本发明解决的问题是提供一种用包含有机聚硅氧烷的组合物浸渍纺织品的方法,其能够以优异和持久的防水方式浸渍不同的纺织品,同时保持它们的透气性,这在应用中不会产生氢气,并且环保。
该问题通过本发明得到解决。
本发明提供了一种用包含下式烷氧基聚硅氧烷(A)的组合物浸渍纺织品的方法:
R1 3SiO[SiR1(OR2)O]x[SiR1 2O]y[SiR1R3O]zSiR1 3 (I)
其中:
R1在每种情况下相同或不同,并且代表任选取代的C1-C7烃基,
R2在每种情况下相同或不同,并且代表氢原子或C1-C6烃基,
R3在每种情况下相同或不同,并且代表C8-C30烃基,
x代表不小于1,优选不小于5,更优选不小于10且不大于1000,优选不大于100,更优选不大于50的整数,
y代表不小于0且不大于100,优选不大于50,更优选不大于10的整数,
z代表不小于0,优选不小于5,更优选不小于10,并且不大于1000,优选不大于100,更优选不大于50的整数,
前提条件是:
x单元[SiR1(OR2)O]的量不小于10mol%,优选不小于30mol%,并且不大于100mol%,优选不大于70mol%,
y单元[SiR1 2O]的量不小于0mol%且不大于90mol%,优选不大于50mol%,并且
z单元[SiR1R3O]的量不小于0mol%,优选不小于20mol%,并且不大于90mol%,优选不大于70mol%,所有均基于硅氧烷单元的x+y+z的总和。
作为烷氧基聚硅氧烷(A)优选使用式(I)中y代表0且z代表不小于1的整数的那些。
因此,作为烷氧基聚硅氧烷(A)优选使用式(II)中的那些:
R1 3SiO[SiR1(OR2)O]x’[SiR1R3O]z’SiR1 3 (II)
其中:
R1、R2和R3各自如上所限定,
x’代表不小于1,优选不小于5,更优选不小于10且不大于1000,优选不大于100,更优选不大于50的整数,
z’代表不小于1,优选不小于5,更优选不小于10,并且不大于1000,优选不大于100,更优选不大于50的整数,
前提条件是:
X’单元[SiR1(OR2)O]的量不小于10mol%,优选不小于20mol%,更优选不小于30mol%,并且不大于95mol%,优选不大于80mol%,更优选不大于70mol%,
Z’单元[SiR1R3O]的量不小于5mol%,优选不小于20mol%,更优选不小于30mol%,并且不大于90mol%,优选不大于80mol%,更优选不大于70mol%,所有均基于硅氧烷单元的x’+z’的总和。
本发明因而提供包含下式的烷氧基聚硅氧烷(A)的组合物:
R1 3SiO[SiR1(OR2)O]x’[SiR1R3O]z’SiR1 3 (II)
其中:
R1、R2和R3各自如上所限定,
x’代表不小于1的整数,优选不小于5,更优选不小于10且不大于1000,优选不大于100,更优选不大于50,
z’代表不小于1的整数,优选不小于5,更优选不小于10,并且不大于1000,优选不大于100,更优选不大于50,
前提条件是:
X’单元[SiR1(OR2)O]的量不小于10mol%,优选不小于20mol%,更优选不小于30mol%,并且不大于95mol%,优选不大于80mol%,更优选不大于70mol%,
Z’单元[SiR1R3O]的量不小于5mol%,优选不小于20mol%,更优选不小于30mol%,并且不大于90mol%,优选不大于80mol%,更优选不大于70mol%,所有量均基于硅氧烷单元的x’+z’的总和。
式(I)和(II)的烷氧基聚硅氧烷(A)可包含至多10mol%,优选至多5mol%的式R1SiO3/2的单元和至多10mol%,优选至多5mol%的具有式-O-R2的Si键合基团的末端硅氧烷单元,其中R1和R2各自如上所限定。这些硅氧烷单元在烷氧基聚硅氧烷(A)的合成过程中通过副反应形成,其中所述副反应是不希望的但很大程度上是不可避免的。
用作烷氧基聚硅氧烷(A)的烷氧基聚硅氧烷可以是一种烷氧基聚硅氧烷或两种或更多种烷氧基聚硅氧烷的混合物。
烷氧基聚硅氧烷或烷氧基聚硅氧烷(A)的混合物优选在25℃下为液体,优选粘度为10至100000mPa·s(25℃),更优选100至10000mPa·s(25℃)或者(a)熔点优选为30-100℃,更优选30-70℃的固体物质。
具有1至7个碳原子的烃基R1的实例为烷基,例如甲基、乙基、正丙基、异丙基、1-正丁基、2-正丁基、异丁基、叔丁基、正戊基、异戊基、新戊基、叔戊基;己基,例如正己基;庚基,例如正庚基;环烷基,例如环戊基、环己基、环庚基和甲基环己基;烯基,例如乙烯基、1-丙烯基和2-丙烯基;芳基,例如苯基;烷芳基,例如邻-、间-、对-甲苯基;和芳烷基,例如苄基。
取代基R1的实例是由卤素、氰基、缩水甘油氧基、聚亚烷基二醇或氨基而取代的基团,例如三氟丙基、氰基乙基、缩水甘油氧基丙基、聚亚烷基二醇丙基和含氨基的烃基。
R1基团优选具有1至4个碳原子的烃基或苯基,优选C1-C4烷基或苯基,更优选甲基。
R2基团的实例是氢原子和1-6个碳原子,优选2-4个碳原子的烷基。
优选用作R3基团的是具有10至20个碳原子的烃基。
R3基团的实例是具有12至18个碳原子的烷基,例如异十二烷基、正十二烷基、正十四烷基、正十六烷基和正十八烷基。
烷氧基聚硅氧烷(A)通过已知方法而制备,例如如US 2003/0180624A、JP2004067561A、WO 2014/099497A2或Titvinidze等人,Oxidation Communications 37(2014),372中所述。
除了所述烷氧基聚硅氧烷(A)之外,本发明的组合物可以包含其它成分。其他成分的实例是乳化剂(B)、水(C)、催化剂(D)、有机溶剂(E)和其它组分(F)。
可用的催化剂(D)包括促进烷氧基硅氧烷水解和/或缩合的任何已知催化剂,优选碱金属氢氧化物、胺、胍,以及锡、锌、锆或钛的化合物。
催化剂(D)的优选用量对于每100份烷氧基聚硅氧烷(A)为0.01至1份。所述催化剂优选仅在施用时而加入。
在本发明的一个实施方案中,本发明的烷氧基聚硅氧烷(A)是有机溶剂(E)中的溶质。该溶液可以包含催化剂(D)。
本发明使用的烷氧基聚硅氧烷(A)的有机溶剂(E)的典型实例为烃,例如戊烷、正己烷、己烷异构体混合物、庚烷、辛烷、石脑油、石油醚、苯、甲苯和二甲苯;卤代烃,例如二氯甲烷、三氯甲烷、四氯甲烷、1,2-二氯乙烷和三氯乙烯;醇类,例如甲醇、乙醇、正丙醇、异丙醇、正戊醇和异戊醇;酮类,例如丙酮、甲基乙基酮、二异丙基酮和甲基异丁基酮(MIBK);酯类,例如乙酸乙酯、乙酸丁酯、丙酸丙酯、丁酸乙酯和异丁酸乙酯;醚类,例如四氢呋喃、乙醚、二异丙醚和二甘醇二甲醚;或其混合物。
当使用有机溶剂(E)时,对于每100重量份的烷氧基聚硅氧烷(A),优选用量为100至10000重量份。
在本发明的另一个实施方案中,本发明的组合物为包含本发明烷氧基聚硅氧烷(A)、乳化剂(B)和水(C)的水性乳液。
基于100重量份的烷氧基聚硅氧烷(A),乳化剂(B)的用量优选1至60重量份,更优选2至30重量份。
所有已知类型的乳化剂可用于本发明方法。它们例如包括阴离子型、阳离子型、非离子型和两性乳化剂、稳定乳液的保护胶体以及颗粒。
对于乳液的成分(B),优选可市购的乳化剂,例如具有10至22个碳原子的脂肪酸的脱水山梨糖醇酯;具有10至22个碳原子并且环氧乙烷含量高至35%的脂肪酸的聚氧化乙烯脱水山梨糖醇酯;具有10-22个碳原子的脂肪酸的聚氧化乙烯山梨糖醇酯;在芳族化合物上具有6-20个碳原子且环氧乙烷含量至多95%的酚的聚氧化乙烯衍生物;具有10至22个碳原子的氨基甜菜碱和脂肪氨基甜菜碱;具有8至22个碳原子且环氧乙烷含量至多95%的脂肪酸或脂肪醇的聚氧化乙烯缩合物;离子型乳化剂,例如烷基中具有6至20个碳原子的烷基芳基磺酸盐;具有8至22个碳原子的脂肪酸皂;具有8至22个碳原子的脂肪硫酸盐;具有10-22个碳原子的烷基磺酸盐;二烷基磺基琥珀酸盐的碱金属盐;具有10-22个碳原子的脂肪胺氧化物;具有6至20个碳原子的脂肪咪唑啉;具有10-22个碳原子的脂肪酰氨基磺基甜菜碱;季铵乳化剂,例如具有10-22个碳原子的脂肪铵化合物;具有10-22个碳原子的脂肪吗啉氧化物;具有10-22个碳原子且至多95%的环氧乙烷的羧基化的、乙氧基化的醇的碱金属盐;具有10至22个碳原子且至多95%的环氧乙烷的甘油的脂肪酸单酯的环氧乙烷缩合物;具有10至22个碳原子的脂肪酸的单-或二乙醇酰胺;具有环氧乙烷单元和/或环氧丙烷单元的烷氧基化的硅氧烷乳化剂;磷酸烷基酯及其盐。
如在乳化剂领域中所熟知,在阴离子乳化剂的情况下,反离子可以是碱金属离子、氨或取代胺的铵离子,诸如三甲胺或三乙醇胺的铵离子。通常优选铵、钠和钾离子。在阳离子乳化剂的情况下,反离子为卤化物、硫酸盐或甲基硫酸盐。氯化物通常是工业上可获得的化合物。
乳化剂的实例为癸基氨基甜菜碱、椰油酰胺基磺基甜菜碱、油烯酰胺基甜菜碱、椰油咪唑啉、椰油磺基咪唑啉、十六烷基咪唑啉、1-羟乙基-2-十七碳烯基咪唑啉、正椰油基吗啉氧化物、癸基二甲基胺氧化物、椰油酰氨基二甲基胺氧化物、具有环氧乙烷缩合基团的脱水山梨醇三硬脂酸酯、具有环氧乙烷缩合基团的脱水山梨醇三油酸酯、十二烷基硫酸钠或钾、硬脂基硫酸钠或钾、十二烷基苯磺酸钠或钾、硬脂基磺酸钠或钾、十二烷基硫酸三乙醇胺盐、三甲基十二烷基氯化铵、三甲基硬脂基甲基硫酸铵、月桂酸钠、肉豆蔻酸钠或钾、磷酸二正丁酯、磷酸二正己基酯、磷酸单正辛酯、磷酸二正辛酯、磷酸单-2-乙基己酯、磷酸二-2-乙基己酯、磷酸单-异壬酯、磷酸二-异壬酯、磷酸单-正癸酯、磷酸正辛正癸酯、磷酸二正癸酯、磷酸单异十三酯、苯基磷酸二正壬酯、磷酸单油酯、磷酸二硬脂酸酯、磷酸单正辛酯、磷酸二正辛酯、磷酸单-正癸酯、磷酸正辛正癸酯、磷酸二正癸酯、具有200个乙二醇单元的乙氧基化蓖麻油、具有40个乙二醇单元的乙氧基化蓖麻油、和具有200个乙二醇单元的乙氧基化的氢化蓖麻油、聚氧化乙烯(20)脱水山梨糖醇硬脂酸酯(Polysorbate 60)、聚氧化乙烯(20)脱水山梨醇三硬脂酸酯(Polysorbate 65)、聚氧化乙烯(20)脱水山梨醇油酸酯(Polysorbate 80)和聚氧化乙烯(20)脱水山梨醇月桂酸酯(Polysorbate 20)、式i-C13H27-O-(CH2CH2O)10-H、C16H33-O-(CH2CH2O)4-H、C16H33-O-(CH2CH2O)20-H、C16H33-O-(CH2CH2O)25-H、C18H37-O-(CH2CH2O)4-H、C18H37-O-(CH2CH2O)20-H、C18H37-O-(CH2CH2O)25-H、C18H35-O-(CH2CH2O)20-H、C12H23-O-(CH2CH2O)4-H、C12H23-O-(CH2CH2O)23-H、C16H33-CH2-C(O)-O-(CH2CH2O)20-H、C16H33-CH2-C(O)-O-(CH2CH2O)30-H、C16H33-CH2-C(O)-O-(CH2CH2O)40-H和C16H33-CH2-C(O)-O-(CH2CH2O)100-H的化合物。
组分(B)可以由一种乳化剂或两种或更多种乳化剂的混合物组成。
在一个优选的实施方案中,组分(B)包含大于50重量%的非离子型乳化剂,更优选包含大于75重量%的非离子型乳化剂。
所述包含在本发明乳液中的非离子型乳化剂(B)优选平均HLB值为10至17,优选11至15。
HLB值表示乳化剂的亲水性基团和疏水性基团之间的平衡。HLB值的限定以及其量化方法为本领域技术人员所熟知,并且例如描述于Journal of Colloid and InterfaceScience,298(2006),441-450中以及其引用的文献,特别是引用[23]中。
有用的乳化保护胶体例如包括聚乙烯醇和纤维素醚,例如甲基纤维素,羟乙基纤维素和羧甲基纤维素。
用于稳定乳液的有用颗粒例如包括部分疏水的胶体二氧化硅。
除了组分(A)、(B)、(C)、(D)和(E)之外,可以使用常添加到硅氧烷乳液中的任何其它物质(F),实例是除了烷氧基聚硅氧烷(A)以外的其它硅氧烷,例如聚醚硅氧烷,硅烷,特别是烷氧基硅烷,增稠剂和/或保护胶体,填料和添加剂,例如防腐剂、消毒剂、润湿剂、腐蚀抑制剂、染料和香料。
除了乳化剂(B)以之外,当本发明方法还使用增稠剂和/或保护胶体作为组分(F)时,优选使用丙烯酸共聚物、纤维素醚和多糖,诸如黄原胶。
当使用增稠剂和/或保护胶体(F)时,基于100重量份的烷氧基聚硅氧烷(A),用量优选0.01至2重量份。
本发明可用的添加剂(F)的实例例如包括常规防腐剂、染料/香料,特别是防腐剂,例如甲基异噻唑啉酮、氯甲基异噻唑啉酮、苄基异噻唑啉酮、苯氧基乙醇、对羟基苯甲酸甲酯,对羟基苯甲酸乙酯,对羟基苯甲酸丙酯、对羟基苯甲酸丁酯,对羟基苯甲酸异丁酯、碱金属苯甲酸盐、碱金属山梨酸盐、碘代丙炔基丁基氨基甲酸酯、苄醇和2-溴-2-硝基丙烷-1,3-二醇。
当使用添加剂(F)时,基于100重量份的烷氧基聚硅氧烷(A),用量优选为0.0005至2重量份。本发明方法优选使用添加剂(F),特别是防腐剂。
根据DIN EN ISO 3251所测量的本发明乳液优选具有1至80重量%,更优选30至70重量%的不挥发物含量。
本发明乳液的pH优选3至10,更优选6至8。
作为水(C),可以使用迄今为止用于制备乳液的任何类型的水。
作为水(C),优选使用部分或完全去离子的水、蒸馏或(重复)重蒸的水、用于医用或制药目的的水,例如纯净水(Aqua purificata,Pharm.Eur.)。
本发明使用的水(C)优选在25℃和1010hPa下的电导率小于50μS/cm,优选小于10μS/cm,更优选小于1.3μS/cm。
用于制备呈水乳液形式的本发明组合物的可用的混合和均化工具包括任何常规的乳化装置,例如高速搅拌器、溶解盘、转子-定子均化器、各种设计的超声波均化器和高压均化器。当需要大颗粒时,慢速搅拌器也合适。
制备呈水乳液形式的本发明组合物的方法可以基于连续、基于半连续或基于分批而进行操作。
为了制备呈水乳液形式的本发明的组合物,所有组分可以通过例如以任何所需顺序的搅拌和/或均化而混合在一起,此时,搅拌器和/或转子-定子均化器的圆周速度优选大于5m/s,更优选大于10m/s,特别是5至50m/s。
包含组分(A)、(B)、(C)和任选(F)的呈水乳液形式的本发明组合物优选通过首先将某些组分(C)与其它组分进行混合以形成高粘度的非流动糊(nonfluent paste)。特别优选该糊状预混合物的屈服极限(相应DIN 53019-1及其引用标准)大于100Pa(25℃),特别是大于1000Pa(25℃)。然后优选通过剪切能量的作用将该糊状预混合物进行均化,直至达到所需的粒径,并且在搅拌和/或均化下用水(C)进行稀释以形成流动的乳液。
本发明的乳液优选包含大于50重量份,更优选包含50至1000重量份,还更优选包含80至500重量份的水(C),均基于100重量份的组分(A)。
纺织品的实例为天然或合成制备的纤维、纱线、维网、无光表面(matts)、绞纱、织物、打结或针织的纺织品。所述纺织品可以作为单独的纤维、纤维束、纤维填充纤维、纱线、地毯、织物网或服装或服装部件而存在。
所述纺织品可以由棉、羊毛、乙酸乙烯酯共聚物、人造丝、大麻、天然丝、聚丙烯、聚乙烯、聚酯、聚氨酯、聚酰胺、芳族聚酰胺、聚酰亚胺、聚丙烯酸酯、聚丙烯腈、聚乳酸、聚氯乙烯、玻璃纤维、陶瓷纤维、纤维素或其混合物而组成。
对待处理的纺织品的施用可以以任何适合且广泛用于处理纺织品的期望方式而进行,例如通过浸渍、铺展、浇铸、喷涂、轧制、填充、印刷或泡沫施用。
处理过的纺织品优选在10℃至250℃,优选25至200℃,更优选80℃至180℃的温度下进行干燥。
在所述干燥步骤的过程中,本发明的烷氧基聚硅氧烷经受固化,并且处理过的纺织品进行浸渍,从而使其具有防水性。
本发明的烷氧基聚硅氧烷的优点在于它们在不同的纺织品上提供了非常好的防水性。
本发明的烷氧基聚硅氧烷的优点在于所述防水处理对洗涤具有非常高的耐久性。
本发明的烷氧基聚硅氧烷的优点在于它们加工简单且安全。
本发明的烷氧基聚硅氧烷的优点在于它们没有持久的环境污染物而即可获得。
除非另有说明,以下实施例中的份数和百分比均以重量计。类似地,除非另有说明,以下实施例在约1010hPa环境气氛的压力和约25℃的温度下,或者在室温下将反应物一起加热而无需额外的加热或冷却下建立的温度下而进行。实施例中报导的粘度均基于25℃的温度。
为了确定其结构,在含有0.1mol/l Cr(acac)3的CDCl3中记录烷氧基聚硅氧烷的29Si NMR光谱(来自Bruker的AVANCE 400,10mm选择性29Si NMR探针,脉冲角90°,延迟时间15s,400次扫描)。
对以下实施例中所得到的乳液进行如下测试:
使用Malvern Mastersizer 2000(Malvern Instruments GmbH D-Herrenberg;测量原理:依据ISO 13320的Fraunhofer衍射)进行粒度测试。作为测量的参数,使用球形模型,连续相的折射率为1.33,分散相的折射率为1.39,且吸收为0.01。
pH在20℃下依据US Pharmacopeia USP 33测量。
按照AATCC试验方法No.22-2005,经由喷雾试验而对经处理的纺织品的疏水性进行测试。在该测试中,用去离子水的纺织品具有斑点。通过将斑点纺织品表面与方法描述中的评级图像进行比较,报告结果表明大约一定比例的面积没有得到润湿。
制备实施例1
将20g式(CH3)3-Si-O-[SiH(CH3)-O]50-Si(CH3)3的聚有机硅氧烷与20g甲苯和15.2g乙醇一起加热至70℃,并与0.174g全氟三苯基硼烷B(C6F5)3的甲苯溶液混合5分钟。在3小时的过程中将温度升到100℃,从90℃开始所形成氢气开始增加。然后搅拌30分钟。将该混合物在1-2毫巴下加热至锅的温度为140℃,得到70克式(CH3)3-Si-O-[Si(CH3)OEt-O]50-Si(CH3)3(NMR分析)的无色液体。
制备实施例2
重复实施例1,不同之处在于所用原料为下式的聚有机硅氧烷。
(CH3)3-Si-O-[SiH(CH3)-O]47-[Si(CH3)2-O]13-Si(CH3)3
NMR显示所得产物具有式
(CH3)3-Si-O-[Si(CH3)OEt-O]47-[Si(CH3)2-O]13-Si(CH3)3。
制备实施例3
将50g式(CH3)3-Si-O-[Si(CH3)H-O]54-Si(CH3)3的硅氧烷和0.18g的Karstedt催化剂(1%Pt)加热至80℃。在1小时过程中,逐渐混入101g十八碳烯,在此过程中温度升至120℃。冷却至80℃后,在75分钟的过程中混入30g乙醇,在此期间观察到显著释放气体和泡沫。然后在80℃下搅拌2小时。此后,在旋转蒸发仪上在100℃和10mbar下除去挥发物。在冷却时,产物变得坚固并在47℃下将产物重新熔化。
NMR分析显示产物由以下比例的不同硅氧烷单元组成;
制备实施例4
将50g式(CH3)3-Si-O-[Si(CH3)H-O]54-Si(CH3)3的硅氧烷和0.18g Karstedt催化剂(1%Pt)加热至40℃。
在60分钟内混入14g甲醇,将反应混合物在80℃再搅拌2小时。然后,在1小时的过程中逐渐混入101g十八碳烯,期间温度升至115℃。然后在80℃下搅拌2小时。将0.18g催化剂和14g甲醇混合后,将反应混合物在80℃再搅拌2小时,然后再与0.18g催化剂和20g十八碳烯进行混合,并在80℃下再搅拌2小时。
然后,在旋转蒸发仪上在100℃和10mbar下除去挥发物。冷却时,产品变得坚固并在58℃下重新熔化。
NMR分析显示产物由以下比例的不同硅氧烷单元组成:
制备实施例5
将106g式(CH3)3-Si-O-[SiH(CH3)-O]47-[Si(CH3)2-O]13-Si(CH3)3的硅氧烷和0.18g的Karstedt催化剂(1%Pt)加热至80℃。在1小时的过程中逐渐混入67.3g十二碳烯,期间温度升至120℃。冷却至75℃后,在30分钟的过程中混入20g乙醇,期间观察到显著释放气体和泡沫。然后在80℃下搅拌2小时。随后进一步混合0.18g催化剂和40g辛烯,并在80℃再搅拌2小时。然后,在旋转蒸发仪上在100℃和10mbar下除去挥发物,得到粘度为2370mPas的棕色油状物。
NMR分析显示产物由以下比例的不同硅氧烷单元组成:
制备实施例6
将50g式(CH3)3-Si-O-[Si(CH3)H-O]54-Si(CH3)3的硅氧烷和0.18g的Karstedt催化剂(1%Pt)加热到80℃。在80分钟的过程中逐渐混入50.53g十二碳烯,期间升至110℃。然后在80℃下搅拌2小时。加热至90℃后,在30分钟的过程中混入32g正丙醇,期间观察到显著释放气体和泡沫。然后在100℃下搅拌2小时。随后进一步混合0.18g催化剂和40g辛烯,并在80℃再搅拌2小时。然后,在旋转蒸发仪上在100℃和10mbar下除去挥发物,得到粘度为1320mPas的棕色油状物。
NMR分析显示产物由以下比例的不同硅氧烷单元组成:
制备实施例7
将HLB值为13.7的乙氧基化异十三烷醇(来自BASF SE D-Ludwigshafen的"TO 109")和15g水使用ULTRA-T50在4000/min下进行混合。将如实施例3所述而得到的250g产物在70℃下进行熔融,在6000/min下逐步混合并均化,得到屈服极限为4220Pa的坚固凝胶型相,将该相用218g含有0.45g ACTICIDE TM MV防腐剂(可从Thor GmbH Speyer获得)的水逐渐稀释。乳液的粒径为432nm(体积分布D(50)值),并且在50℃下保存28天而没有任何分离的迹象。
使用实施例1-7
制备实施例1-3中的产物用于制备4%异丙醇溶液。使用NaOH将这些溶液的pH调节至9.0。制备实施例4-6的产物用于制备4%甲苯溶液。将这些溶液与0.02%的钛酸丁酯进行混合。
将流浆灰(popeline gray)65/35PES/Co的条浸入这些溶液中2小时,在实验室张布架中在通风橱中,室温下进行预干燥,然后在150℃下固化10分钟。
将10份制备实施例7的产物用990份完全不含铁的水进行稀释以形成液体。使用NaOH将该液体的pH调节至9.0。将A4尺寸的流浆灰65/35PES/CO浸入该液体中。将饱和的织物用双辊垫角度挤压至70%的湿涂层量,拉伸并在实验室张布架上在150℃下干燥10分钟。
在3天、20天后和在40℃洗涤(Miele Softtronic W 1935洗衣机;Express 20程序;1kg棉和聚酯压舱物)后对疏水性进行测试。结果总结在表1中。
表1:测试结果
表1中的值越高,疏水性越高,即织物上的防水涂层越好。用本发明实施例1-7的烷氧基聚硅氧烷处理的纺织品显示具有良好至非常好的防水涂层,并且还具有良好至非常好的耐洗涤性。使用实施例3-7的烷氧基聚硅氧烷,即式(II)除了具有烷氧基的硅氧烷单元外还含有具有较长烷基的硅氧烷单元的烷氧基聚硅氧烷,还实现了特别好的防水涂层和耐洗涤性。
Claims (12)
1.一种用包含下式的烷氧基聚硅氧烷(A)的组合物浸渍纺织品的方法:
R1 3SiO[SiR1(OR2)O]x[SiR1 2O]y[SiR1R3O]zSiR1 3 (I)
其中:
R1在每种情况下相同或不同,并且代表任选取代的C1-C7烃基,
R2在每种情况下相同或不同,并且代表氢原子或C1-C6烃基,
R3在每种情况下相同或不同,并且代表C8-C30烃基,
x代表不小于1的整数,优选不小于5,更优选不小于10且不大于1000,优选不大于100,更优选不大于50,
y代表不小于0且不大于100的整数,优选不大于50,更优选不大于10,
z代表不小于0的整数,优选不小于5,更优选不小于10,并且不大于1000,优选不大于100,更优选不大于50,
前提条件是:
x单元[SiR1(OR2)O]的量不小于10mol%,优选不小于30mol%,并且不大于100mol%,优选不大于70mol%,
y单元[SiR1 2O]的量不小于0mol%且不大于90mol%,优选不大于50mol%,并且
z单元[SiR1R3O]的量不小于0mol%,优选不小于20mol%,并且不大于90mol%,优选不大于70mol%,
所有的量均基于硅氧烷单元的x+y+z的总和。
2.如权利要求1所述的方法,其特征在于y代表0且z代表不小于1的整数。
3.如权利要求1或2所述的方法,其特征在于所存在的烷氧基聚硅氧烷具有下式:
R1 3SiO[SiR1(OR2)O]x’[SiR1R3O]z’SiR1 3 (II)
R1、R2和R3各自如上所限定,
x’代表不小于1的整数,优选不小于5,更优选不小于10且不大于1000,优选不大于100,更优选不大于50,
z’代表不小于1的整数,优选不小于5,更优选不小于10,并且不大于1000,优选不大于100,更优选不大于50,
前提条件是:
X’单元[SiR1(OR2)O]的量不小于10mol%,优选不小于20mol%,更优选不小于30mol%,并且不大于95mol%,优选不大于80mol%,更优选不大于70mol%,
z’单元[SiR1R3O]的量不小于5mol%,优选不小于20mol%,更优选不小于30mol%,并且不大于90mol%,优选不大于80mol%,更优选不大于70mol%,
所有的量均基于硅氧烷单元的x’+z’的总和。
4.如权利要求1、2或3所述的方法,其特征在于R1代表C1-C4烷基或苯基。
5.如权利要求1至4中任一项所述的方法,其特征在于所使用的组合物为如权利要求1至4中任一项所限定的烷氧基聚硅氧烷(A)在有机溶剂中的溶液。
6.如权利要求1至5中任一项所述的方法,其特征在于所使用的组合物为包含如下组分的水性乳液:
如权利要求1至4中任一项所限定的烷氧基聚硅氧烷(A),
乳化剂(B),和
水(C)。
7.如权利要求1至6中任一项所述的方法,其特征在于将所述组合物施加于织物,并且将由此处理的织物在25至200℃的温度下进行干燥。
8.根据如权利要求1至7任一项所限定的方法处理的织物。
9.一种包含下式的烷氧基聚硅氧烷(A)的组合物:
R1 3SiO[SiR1(OR2)O]x’[SiR1R3O]z’SiR1 3 (II)
R1、R2和R3各自如上所限定,
x’代表不小于1的整数,优选不小于5,更优选不小于10且不大于1000,优选不大于100,更优选不大于50,
z’代表不小于1的整数,优选不小于5,更优选不小于10,并且不大于1000,优选不大于100,更优选不大于50,
前提条件是:
X’单元[SiR1(OR2)O]的量不小于10mol%,优选不小于20mol%,更优选不小于30mol%,并且不大于95mol%,优选不大于80mol%,更优选不大于70mol%,
Z’单元[SiR1R3O]的量不小于5mol%,优选不小于20mol%,更优选不小于30mol%,并且不大于90mol%,优选不大于80mol%,更优选不大于70mol%,
所有均基于硅氧烷单元的x’+z’的总和。
10.如权利要求9所述的组合物,其特征在于R1代表C1-C4烷基或苯基。
11.如权利要求9或10所述的组合物,其特征在于所述组合物为如权利要求9或10所限定的烷氧基聚硅氧烷(A)在有机溶剂中的溶液。
12.如权利要求9、10或11所述的组合物,其特征在于所述组合物为包含如下组分的水性乳液:
如权利要求9、10或11所限定的烷氧基聚硅氧烷(A),
乳化剂(B),和
水(C)。
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2015
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2016
- 2016-11-03 US US15/568,153 patent/US10577742B2/en not_active Expired - Fee Related
- 2016-11-03 CN CN201680022933.8A patent/CN107532040B/zh not_active Expired - Fee Related
- 2016-11-03 EP EP16790611.4A patent/EP3250653B1/de not_active Not-in-force
- 2016-11-03 KR KR1020177030429A patent/KR102052674B1/ko active IP Right Grant
- 2016-11-03 WO PCT/EP2016/076483 patent/WO2017080894A1/de active Application Filing
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CN1422305A (zh) * | 2000-04-04 | 2003-06-04 | 西巴特殊化学品普法希股份有限公司 | 用于处理羊毛材料的聚硅氧烷组合物 |
CN101522758A (zh) * | 2006-10-10 | 2009-09-02 | 陶氏康宁公司 | 聚硅氧烷聚合物乳液 |
CN102549046A (zh) * | 2009-09-15 | 2012-07-04 | 赢创高施米特有限公司 | 具有季铵基团的新型聚硅氧烷及其用途 |
WO2014099497A2 (en) * | 2012-12-19 | 2014-06-26 | 3M Innovative Properties Company | Alkoxy polysiloxanes and methods of making alkoxy silanes and siloxanes |
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KR20170129256A (ko) | 2017-11-24 |
KR102052674B1 (ko) | 2020-01-07 |
JP2018510948A (ja) | 2018-04-19 |
EP3250653B1 (de) | 2018-10-24 |
EP3250653A1 (de) | 2017-12-06 |
CN107532040B (zh) | 2020-01-31 |
US20180148889A1 (en) | 2018-05-31 |
US10577742B2 (en) | 2020-03-03 |
DE102015222139A1 (de) | 2017-05-11 |
JP6577050B2 (ja) | 2019-09-18 |
WO2017080894A1 (de) | 2017-05-18 |
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