CN105051072B - 碱可溶胀性乳液聚合物 - Google Patents
碱可溶胀性乳液聚合物 Download PDFInfo
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- CN105051072B CN105051072B CN201480017710.3A CN201480017710A CN105051072B CN 105051072 B CN105051072 B CN 105051072B CN 201480017710 A CN201480017710 A CN 201480017710A CN 105051072 B CN105051072 B CN 105051072B
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- monomer
- monomer mixture
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- methyl
- crosslinking agent
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- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
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- 238000000518 rheometry Methods 0.000 description 1
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- 239000011734 sodium Substances 0.000 description 1
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- TUNFSRHWOTWDNC-HKGQFRNVSA-N tetradecanoic acid Chemical compound CCCCCCCCCCCCC[14C](O)=O TUNFSRHWOTWDNC-HKGQFRNVSA-N 0.000 description 1
- UEUXEKPTXMALOB-UHFFFAOYSA-J tetrasodium;2-[2-[bis(carboxylatomethyl)amino]ethyl-(carboxylatomethyl)amino]acetate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]C(=O)CN(CC([O-])=O)CCN(CC([O-])=O)CC([O-])=O UEUXEKPTXMALOB-UHFFFAOYSA-J 0.000 description 1
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Abstract
本发明涉及一种乳液聚合物粒子，所述乳液聚合物粒子包含25wt％到45wt％的至少一种C3‑C6羧酸单体的聚合残基和0.1wt％到3wt％的至少一种交联剂的聚合残基，其中交联剂百分比从粒子中心向粒子表面连续增加。
Description
背景技术
本发明大体上涉及使用单体动力进料来制得的碱可溶胀性乳液聚合物。
使用单体动力进料制得的聚合物是已知的。举例来说，美国专利3,804,881公开使用此方法制得的聚合物。然而，本申请中所公开的适用作流变改性剂的碱可溶胀性聚合物不是已知的。
由本发明解决的问题是提供用作流变改性剂的其它碱可溶胀性聚合物。
发明内容
本发明是针对乳液聚合物粒子，所述乳液聚合物粒子包含25wt％到45wt％的至少一种C3-C6羧酸单体的聚合残基和0.1wt％到3wt％的至少一种交联剂的聚合残基，其中交联剂百分比从粒子中心向粒子表面连续增加。
本发明进一步是针对一种用于产生乳液聚合物粒子的方法，所述方法通过以下步骤来进行：(a)提供第一单体混合物，所述第一单体混合物包含25wt％到45wt％的至少一种C3-C6羧酸单体；(b)提供第二单体混合物，所述第二单体混合物包含0.1wt％到3wt％的至少一种交联剂；以及(c)在向所述第一单体混合物中添加所述第二单体混合物的同时，向聚合反应器中添加所述第一单体混合物；其中重量百分比是按所述第一和第二单体混合物的总重量计。
具体实施方式
除非另外指明，否则所有百分比都是重量百分比(wt％)，所有级分都是按重量计并且所有温度都是以℃为单位。聚合物中聚合单体残基的百分比是按固体聚合物的全部重量计，并且单体百分比是按总单体重量计。在“室温(room temperature)”(room temp.)下进行的测量都是在20℃-25℃下进行。含有圆括号的任何术语替代性地是指如同圆括号不存在的整个术语和没有其内容的术语以及每一替代方案的组合。因此，术语“(甲基)丙烯酸类”是指丙烯酸类、甲基丙烯酸类以及其混合物中的任一种。“C3-C6羧酸单体”是具有一个或两个羧酸基的单烯系不饱和化合物，例如(甲基)丙烯酸、顺丁烯二酸、反丁烯二酸、衣康酸、顺丁烯二酸酐、丁烯酸等。优选地，酸单体具有三个或四个碳原子，优选地具有一个羧酸基，优选地是(甲基)丙烯酸，优选地是甲基丙烯酸(MAA)。烷基是可以为直链或分支链的饱和烃基。
交联剂是具有两个或更多个非共轭烯系不饱和基团的单体。优选的交联剂包括例如二醇或多元醇的二烯丙基醚或三烯丙基醚以及二(甲基)丙烯酰酯或三(甲基)丙烯酰酯(例如，三羟甲基丙烷二烯丙基醚(TMPDAE)和三羟甲基丙烷三甲基丙烯酸酯(TMPTMA))、二酸或三酸的二烯丙酯或三烯丙酯、(甲基)丙烯酸烯丙酯、二乙烯基砜、磷酸三烯丙酯、二乙烯基芳香族化合物(例如，二乙烯基苯)。优选地，交联剂的分子量不超过800，优选地不超过700，优选地不超过600，优选地不超过500，优选地不超过400。优选地，交联剂除以烯系不饱和基团数目后的分子量不超过150，优选地不超过140，优选地不超过130；优选地是至少50，优选地是至少65。
优选地，聚合物粒子是丙烯酸类聚合物，即，具有至少70wt％、优选地至少80wt％、优选地至少90wt％、优选地至少95wt％、优选地至少98wt％、优选地至少99wt％丙烯酸类单体聚合残基的丙烯酸类聚合物。丙烯酸类单体包括(甲基)丙烯酸和其C1-C22烷酯或羟烷酯；丁烯酸、衣康酸、反丁烯二酸、顺丁烯二酸、顺丁烯二酸酐、(甲基)丙烯酰胺、(甲基)丙烯腈以及丁烯酸、衣康酸、反丁烯二酸或顺丁烯二酸的烷酯或羟烷酯。丙烯酸类聚合物也可以包含其它聚合单体残基，包括例如非离子型(甲基)丙烯酸酯、阳离子型单体、单不饱和二羧酸酯、C1-C22烷基羧酸的乙烯酯、乙烯基酰胺(包括例如N-乙烯基吡咯烷酮)、磺化的丙烯酸类单体、乙烯基磺酸、乙烯基卤化物、含磷单体、杂环单体、苯乙烯以及经取代的苯乙烯。优选地，聚合物含有不超过3wt％、优选地不超过2wt％、优选地不超过1wt％、优选地不超过0.5wt％、优选地不超过0.2wt％的含硫或含磷单体。
优选地，聚合物粒子还包含54wt％到74wt％；优选地至少56wt％、优选地至少58wt％、优选地至少60wt％、优选地至少62wt％；优选地不超过72wt％、优选地不超过70wt％、优选地不超过68wt％的至少一种(甲基)丙烯酸C1-C12烷酯的聚合残基。优选地，(甲基)丙烯酸C1-C12烷酯限于(甲基)丙烯酸C1-C8烷酯，优选地(甲基)丙烯酸C2-C8烷酯；优选地，(甲基)丙烯酸C1-C12烷酯限于丙烯酸C1-C12烷酯，优选地丙烯酸C1-C8烷酯，优选地丙烯酸C2-C8烷酯。优选地，聚合物粒子包含至少27wt％、优选地至少29wt％、优选地至少31wt％、优选地至少33wt％；优选地不超过43wt％、优选地不超过41wt％、优选地不超过39wt％、优选地不超过37wt％的至少一种C3-C6羧酸单体的聚合残基。优选地，聚合物粒子包含至少0.2wt％、优选地至少0.3wt％、优选地至少0.4wt％、优选地至少0.5wt％；优选地不超过2.5wt％、优选地不超过2wt％、优选地不超过1.5wt％、优选地不超过1.2wt％、优选地不超过1wt％、优选地不超过0.9wt％、优选地不超过0.8wt％的至少一种交联剂的聚合残基。
优选地，聚合物粒子包含具有结构H2C＝C(R)C(O)X(CH2CH2O)n(CH(R′)CH2O)mR″的亲脂性单体的聚合残基，其中X是O或NH，R是氢或甲基，R′是甲基或乙基；R″是C8-C22烷基、C8-C16烷基苯基或C13-C36芳烷基苯基；n是6-100的平均数并且m是0-50的平均数，其条件是n≥m并且m+n是6-100。优选地，X是O。优选地，聚合物粒子包含0.2wt％到10wt％、优选地0.3wt％到8wt％、优选地0.5wt％到5wt％、优选地0.5wt％到4wt％、优选地1wt％到4wt％的结构H2C＝C(R)C(O)X(CH2CH2O)n(CH(R′)CH2O)mR″的单体的聚合残基。优选地，R″是C8-C22烷基，优选地C10-C22烷基，优选地C12-C20烷基。优选地，n是15-30并且m是0-5；优选地n是18-25并且m是0-3；优选地n是18-25并且m是0-2；优选地R′是甲基。优选地，R是甲基。优选地，R″是C10-C22烷基，n是15-30并且m是0-5；优选地，R″是C12-C22烷基，n是18-25，m是0-3并且R是甲基。
优选地，以含有聚合物作为分散于水性介质中的不连续粒子的水性组合物(即，聚合物胶乳)的形式提供聚合物粒子。在此水性分散液中，聚合物粒子的平均粒径优选地在50到2000nm、优选地100到1000nm、优选地150到800nm的范围内。水性分散液中聚合物粒子的含量通常在按水性分散液重量计15wt％到60wt％、优选地25wt％到50wt％的范围内。
在描述本发明方法中，单体的百分比是按总单体重量计。优选地，第一单体混合物进一步包含54wt％到74wt％；优选地至少56wt％、优选地至少58wt％、优选地至少60wt％、优选地至少62wt％；优选地不超过72wt％、优选地不超过70wt％、优选地不超过68wt％的至少一种(甲基)丙烯酸C1-C12烷酯的聚合残基。优选地，(甲基)丙烯酸C1-C12烷酯限于(甲基)丙烯酸C1-C8烷酯，优选地(甲基)丙烯酸C2-C8烷酯；优选地，(甲基)丙烯酸C1-C12烷酯限于丙烯酸C1-C12烷酯，优选地丙烯酸C1-C8烷酯，优选地丙烯酸C2-C8烷酯。优选地，第一单体混合物包含至少27wt％、优选地至少29wt％、优选地至少31wt％、优选地至少33wt％；优选地不超过43wt％、优选地不超过41wt％、优选地不超过39wt％、优选地不超过37wt％的至少一种C3-C6羧酸单体。优选地，第一单体混合物包含至少27wt％、优选地至少29wt％、优选地至少31wt％、优选地至少33wt％；优选地不超过43wt％、优选地不超过41wt％、优选地不超过39wt％、优选地不超过37wt％的至少一种C3-C6羧酸单体。优选地，第二单体混合物包含至少0.3wt％、优选地至少0.4wt％、优选地至少0.5wt％；优选地不超过2.5wt％、优选地不超过2wt％、优选地不超过1.5wt％、优选地不超过1.2wt％、优选地不超过1wt％、优选地不超过0.9wt％、优选地不超过0.8wt％的至少一种交联剂。优选地，第二单体混合物进一步包含至多15wt％、优选地至多10wt％、优选地至多8wt％的并非交联剂的单体。优选地，第二单体混合物中并非交联剂的单体包含存在于第一单体混合物中的相同(甲基)丙烯酸C1-C12烷酯；优选地，这些单体包含不超过5wt％、优选地不超过3wt％、优选地不超过2wt％、优选地不超过1wt％、优选地不超过0.5wt％、优选地不超过0.2wt％的(甲基)丙烯酸C3-C6烷酯。
优选地，第一单体混合物包含具有结构H2C＝C(R)C(O)X(CH2CH2O)n(CH(R′)CH2O)mR″的亲脂性单体，其中X是O或NH，R是氢或甲基，R′是甲基或乙基；R″是C8-C22烷基、C8-C16烷基苯基或C13-C36芳烷基苯基；n是6-100的平均数并且m是0-50的平均数，其条件是n≥m并且m+n是6-100。优选地，X是O。优选地，第一单体混合物包含0.2wt％到10wt％、优选地0.3wt％到8wt％、优选地0.5wt％到5wt％、优选地0.5wt％到4wt％、优选地1wt％到4wt％的结构H2C＝C(R)C(O)X(CH2CH2O)n(CH(R′)CH2O)mR″的单体。优选地，R″是C8-C22烷基，优选地C10-C22烷基，优选地C12-C20烷基。优选地，n是15-30并且m是0-5；优选地n是18-25并且m是0-3；优选地n是18-25并且m是0-2；优选地R′是甲基。优选地，R是甲基。优选地，R″是C10-C22烷基，n是15-30并且m是0-5；优选地，R″是C12-C22烷基，n是18-25，m是0-3并且R是甲基。
优选地，第一单体混合物包含优选地具有结构H2C＝C(R)C(O)X(CH2CH2O)n(CH(R′)CH2O)mR″的非离子型水溶性单体，其中X是O或NH，R是氢或甲基，R′是甲基或乙基；R″是甲基或乙基；n是6-100的平均数并且m是0-50的平均数，其条件是n≥m并且m+n是6-100。优选地，X是O。优选地，第一单体混合物包含0.2wt％到10wt％、优选地0.5wt％到8wt％、优选地1wt％到7wt％、优选地2wt％到7wt％、优选地3wt％到7wt％的结构H2C＝C(R)C(O)X(CH2CH2O)n(CH(R′)CH2O)mR″的单体。优选地，R″是甲基。优选地，n是15-30并且m是0-5；优选地n是18-25并且m是0-3；优选地n是18-25并且m是0-2；优选地R′是甲基。优选地，R是甲基。优选地，R″是甲基，n是15-30并且m是0-5；优选地，R″是甲基，n是18-25，m是0-3并且R是甲基。其它优选的非离子型水溶性单体包括丙烯酰胺、N-甲基或N-乙基丙烯酰胺、N，N-二甲基或N，N-二乙基丙烯酰胺、聚乙二醇(甲基)丙烯酸酯、N-乙烯基乙酰胺、N-甲基-N-乙烯基乙酰胺、N-乙烯基甲酰胺、N-甲基-N-乙烯基甲酰胺、N-乙烯基内酰胺、丙烯酸羟乙酯、丙烯酸羟丙酯、甲基丙烯酸羟乙酯、甲基丙烯酸羟丙酯以及其混合物。尤其优选的非离子型水溶性单体是甲氧基-聚(乙二醇)单甲基丙烯酸酯。
在添加第一单体混合物之前，优选地小于10wt％、优选地小于7wt％、优选地小于5wt％、优选地小于3wt％、优选地小于2wt％、优选地小于1wt％的单体处于聚合反应器中。优选地，经60到240分钟、优选地80到160分钟、优选地90到150分钟的时间段向反应器中添加单体。优选地，向第一单体混合物中添加第二单体混合物的时间是向聚合反应器中添加所述第一单体混合物的时间的50％到120％、优选地75％到100％、优选地90％到100％。优选地，向第一单体混合物中添加第二单体混合物不迟于向聚合反应器中添加所述第一单体混合物开始，优选地同时开始。
典型水乳液聚合技术适用于本发明方法中。水乳液聚合方法通常在水性反应混合物中进行，所述水性反应混合物含有至少一种单体和各种合成佐剂，如水性反应介质中的自由基来源、缓冲液以及还原剂。可以使用链转移剂来限制分子量，所述链转移剂优选地是硫醇、优选地C8-C12烷基硫醇。水性反应介质是水性反应混合物的连续流体相，并且含有按水性反应介质的重量计大于50wt％的水以及任选地一种或多种水可混溶性溶剂。合适的水可混溶性溶剂包括甲醇、乙醇、丙醇、丙酮、乙二醇乙基醚、丙二醇丙基醚以及二丙酮醇。优选地，水性反应介质含有按水性反应介质的重量计至少90wt％水、优选地至少95wt％水、优选地至少98wt％水。
本发明的乳液聚合物粒子适用于如上文所描述的多种增稠的水性调配物，包括沐浴露、洗发精、个人护理清洁剂；液体肥皂(例如，液体洗手皂)、用于织物(例如，衣物洗涤剂)、餐具和硬质表面的清洁调配物；液体自动餐具洗涤剂、手动餐具洗涤剂、斑点预处理剂、烘箱清洁剂、以及玻璃/窗户清洁剂、护理剂(例如，头发和皮肤)、双组分染发剂、发胶；头发定型乳膏、糊剂或胶；摩丝(mousse)、永久卷发调配物、助黑洗液(lotion)、防晒剂以及皮肤洗液。聚合物也适用作例如无表面活性剂系统(例如，乳膏或洗液)中的乳化剂。用聚合物粒子增稠的调配物可以用于悬浮珠粒、硅酮、二氧化硅、润肤油、有机和无机uv过滤剂以及磨料。聚合物粒子可以与其它流变改性剂组合使用。当粒子经由与碱金属接触而溶胀时，常常不可能区分所形成的凝胶类系统中的个别粒子。
增稠的水性调配物含有基于相对于水性调配物全部重量的聚合物固体所计算的0.1wt％到5wt％的聚合物粒子。优选地，增稠的水性调配物含有至少0.3wt％、优选地至少0.5wt％、优选地至少0.7wt％、优选地至少0.9wt％、优选地至少1.1wt％、优选地至少1.3wt％、优选地至少1.5wt％的聚合物粒子。优选地，增稠的水性调配物含有不超过4wt％、优选地不超过3wt％、优选地不超过2.5wt％、优选地不超过2wt％的聚合物粒子。优选地，增稠的水性组合物还含有至少一种表面活性剂、优选地至少两种表面活性剂。用于实践本发明的优选的阴离子型表面活性剂可以选自C8到C18脂肪酸或其水溶性盐；C8到C18醇的水溶性硫酸盐或醚硫酸盐；磺化的烷基芳基化合物，如例如十二烷基苯磺酸盐；烷基苯氧基聚乙氧基乙醇，例如具有C7到C18烷基和9到40个或更多个氧亚乙基(oxyethylene)单元；长链羧酸的环氧乙烷衍生物，例如月桂酸、肉豆蔻酸、棕榈酸或油酸的环氧乙烷衍生物；长链醇的环氧乙烷衍生物，例如月桂基醇或鲸蜡基醇的环氧乙烷衍生物；烷醇酰胺和多糖苷，例如烷基多糖苷；以及衍生自氨基酸的表面活性剂，例如谷氨酸盐。尤其优选的表面活性剂包括例如月桂醇醚硫酸钠(sodium laureth sulfate，SLES)和椰油酰胺基丙基甜菜碱(cocamidopropyl betaine，CAPB)。优选地，水性组合物中表面活性剂的总量是5wt％到30wt％；优选地至少8wt％，优选地至少10wt％，优选地至少12wt％；优选地不超过25wt％，优选地不超过22wt％，优选地不超过20wt％。优选地，增稠的水性组合物的pH是3到12，优选地3.5到10，优选地3.5到8，优选地4到7。
优选地，本发明中所描述的聚合物粒子为增稠的水性组合物提供透明度和悬浮特性，即，使用美国环境保护局(U.S.Environmental Protection Agency)方法180.1(浊度方法(Nephelometric Method))的样品浊度(turbidity)小于50NTU。悬浮是指颗粒性或固体材料、液体材料或空气在整个调配物连续相中的均匀分散。悬浮失败的特点在于所分散的材料在一系列储存温度条件下与连续相的相分离。
本发明聚合物适用的特定水性组合物是沐浴露。沐浴露的典型组分除先前提及的聚合物增稠剂和表面活性剂之外还包括足以达到pH为4-7、优选地4.5-6.8、优选地4.5到5.5、优选地5-6.6的碱或酸；和任选的成分，包括硅酮、珠光剂(pearlizing agent)、维生素、油、芳香剂、染料、杀生物剂以及由多种材料制成的不溶性珠粒，所述材料包括聚烯烃(例如聚乙烯和聚苯乙烯)、明胶、云母、封装油或维生素珠以及荷荷芭蜡珠。优选地，珠粒的量是0.1％到2％，更优选地0.2％到1％。优选地，珠粒的平均半径是0.1mm到10mm。通常，所用表面活性剂是阴离子型表面活性剂和两性表面活性剂的混合物，优选地是8％到16％阴离子型表面活性剂和1％到5％两性表面活性剂的混合物。
本发明聚合物适用的第二特定水性组合物是洗发精。护理洗发精的典型组分除先前提及的聚合物增稠剂和表面活性剂之外还包括足以达到pH为4-7、优选地4-6、优选地4.7-7.0的碱。本发明的一个特定实施例是含有分散的硅酮和任选的成分(包括珠光剂和吡啶硫酮锌或其它去屑剂)的护理洗发精。
本发明聚合物适用的第三水性组合物是硬质表面清洁剂。硬质表面清洁剂的典型组分除先前提及的聚合物增稠剂和表面活性剂之外还包括足以实现pH为9-12的碱和任选的成分(包括溶剂、盐、芳香剂以及染料)。
优选地，增稠的水性组合物通过将乳液聚合物中和到pH在6.5到8、优选地7到7.5、优选地7到7.5的范围内；并且随后酸化到pH在4到6、优选地4.5到5.5、优选地4.8到5.3的范围内来产生。中和调配物的合适的碱包括无机碱，如氢氧化钠和氢氧化钾；氢氧化铵以及有机碱，如单乙醇胺、二乙醇胺或三乙醇胺；优选地碱金属氢氧化物；优选地氢氧化钠或氢氧化钾；优选地氢氧化钠。可以使用碱的混合物。酸化调配物的合适的酸包括无机酸，如盐酸、磷酸和硫酸以及有机酸，如乙酸；优选地羧酸；优选地柠檬酸。可以使用酸的混合物。
本发明的组合物任选地可以包括其它成分，例如盐、共流变改性剂(例如LAPONITE粘土、纤维素制品、角叉菜胶、黄原胶、PEG-150二硬脂酸酯(ACULYN 60流变改性剂)PEG-150季戊四醇基四硬脂酸酯、其它缔合或非缔合丙烯酸类流变改性剂(如丙烯酸酯共聚物、丙烯酸酯共聚物的衍生物、ACULYN 33流变改性剂、ACULYN 22流变改性剂、ACULYN 28流变改性剂、丙烯酸酯/山嵛醇聚醚-25甲基丙烯酸酯共聚物、丙烯酸酯/山嵛醇聚醚-25甲基丙烯酸酯共聚物的衍生物以及ACULYN 88流变改性剂)、CARBOPOL Aqua-SF1、CARBOPOL Aqua 30和CARBOPOL Ultrez-21、其它丙烯酸类或氨基甲酸酯聚合物(如ACULYN 44流变改性剂或ACULYN 46流变改性剂)、有机或无机粒子(包括例如磨料、珠粒、云母、封装油珠)、硅酮、珠光剂、分散的液体、分散剂、可溶性或分散的杀生物剂、维生素、保湿剂、酶、漂白剂、润肤剂、芳香剂、染料、硫代乙醇酸、UVA和UVB吸收剂、红外吸收剂等。可以悬浮于水性组合物中的不溶性材料包括粘土、珠粒、蜡、明胶以及其它颗粒性材料。
实例
在以下实例中，使用以下术语和测试程序：
οBA＝丙烯酸丁酯
οMAA＝甲基丙烯酸
οEHA＝丙烯酸2-乙基己酯
οEA＝丙烯酸乙酯
οLipo1是具有经由18到26个氧亚乙基残基连接到甲基丙烯酰基上的直链饱和C16-18烷基的经亲脂性改性的单体。
οLipo2是具有经由20-28个氧亚乙基残基连接到甲基丙烯酰基上的直链饱和C10-14烷基的经亲脂性改性的单体。
οTMPDE：三羟甲基丙烷二烯丙基醚
οSR399：二季戊四醇五丙烯酸酯
οTMPTMA＝三羟甲基丙烷三甲基丙烯酸酯
οTMPDAE＝(三羟甲基丙烷二烯丙基醚)
οSLES＝月桂醇醚硫酸钠
οCAPB＝椰油酰胺基丙基甜菜碱
实例1
向配备有机械搅拌器、热电偶、冷凝器以及氮气鼓泡装置的3升4颈圆底烧瓶中添加350克去离子水和2克月桂基硫酸钠。用氮气吹扫反应器并且使之升温到90℃。单独地，1)由935克去离子水、25克月桂基硫酸钠、419克EA、242克MAA制备单体乳液(A)。2)通过混合5.3克TMPTA和38克EA来制备单体乳液添加剂(B)。3)通过将0.4克过硫酸铵溶解在19克去离子水中来制备引发剂溶液C1。4)通过将0.7克过硫酸铵溶解在42克去离子水中来制备引发剂溶液C2。在约90℃反应器温度下，将引发剂溶液C1装入反应器中。随后在将单体乳液添加剂(B)装入单体乳液(A)中的同时，将所述单体乳液(A)装入反应器中。控制速率以使得两个进料都在120分钟内结束。单独地，在120分钟内将引发剂溶液C2进料到反应器中。在这些添加都完成之后，用去离子水冲洗单体乳液和引发剂进料线，接着用单体冲洗，追加自由基催化剂和活化剂。过滤所得胶乳并且分析其固体％、pH、残余单体、粒度、凝胶含量以及粘度。
比较实例1
向配备有机械搅拌器、热电偶、冷凝器以及氮气鼓泡装置的3升4颈圆底烧瓶中添加350克去离子水和2克月桂基硫酸钠。用氮气吹扫反应器并且使之升温到90℃。单独地，1)由935克去离子水、25克月桂基硫酸钠、457克EA、242克MAA以及5.3克TMPTA制备单体乳液(A)。3)通过将0.4克过硫酸铵溶解在19克去离子水中来制备引发剂溶液C1。4)通过将0.7克过硫酸铵溶解在42克去离子水中来制备引发剂溶液C2。在约90℃反应器温度下，将引发剂溶液C1装入反应器中。随后将单体乳液(A)装入反应器中。控制速率以使得进料在120分钟内结束。单独地，在120分钟内将引发剂溶液C2进料到反应器中。在这些添加都完成之后，用去离子水冲洗单体乳液和引发剂进料线，接着用单体冲洗，追加自由基催化剂和活化剂。过滤所得胶乳并且分析其固体％、pH、残余单体、粒度、凝胶含量以及粘度。
实例2-7
除了组成如表1中所描述而变化之外，根据如实例1中所描述的程序来制备聚合物样品2-7。
比较实例2-5
除了组成如表1中所描述而变化之外，根据如实例1中所描述的程序来制备比较实例2-5。
表1：来自实例(E)的用交联剂动力进料来制得的聚合物和来自比较实例(CE)的通过常规聚合来制得的聚合物
| 聚合物 | 聚合物组成 |
| E1 | 65EA/35MAA//0.75％TMPTA |
| E2 | 65EA/35MAA//0.60％TMPTA |
| E3 | 60EA/5EHA/35MAA//0.75％TMPTA |
| E4 | 60EA/5EHA/35MAA//0.6％TMPTA |
| E5 | 60EA/40MAA/0.75％TMPTA |
| CE1 | 65EA/35MAA//0.75％TMPTA |
| CE2 | 65EA/35MAA//0.6％TMPTA |
| CE3 | 60EA/5EHA/35MAA//0.75％TMPTA |
| CE4 | 60EA/5EHA/35MAA//0.6％TMPTA |
| CE5 | 60EA/40MAA/0.75％TMPTA |
| E6 | 65EA/35MAA//1.5％SR399 |
| E7 | 65EA/35MAA/1 Lipo 1//0.75％TMPTA |
实例11-12：
如表2中所概括的用于测量经中和水溶液特性(粘度和浊度)的程序
对1％活性聚合物的溶解粘度程序：
1.称出足以在最终调配物中具有1.0％聚合物的聚合物实例。
2.用去离子水预稀释以制得500g溶液。
3.添加4.2g的20％w/w氢氧化钠水溶液并且用顶置式搅拌器有效地搅拌直到均质。
4.pH测量值应处于7.2到7.5范围内。必要时用20％NaOH调节
5.使用具有对应轴的布洛克菲尔德粘度计(Brookfield viscometer)以30rpm测量粘度以至少在10％尺度下获得测量值。
6.将样品转移到1oz小瓶中以用于浊度测量
对2.5％活性聚合物的溶解粘度程序：
1.称出足以在最终调配物中具有2.5％聚合物的聚合物实例。
2.用去离子水预稀释以制得500g溶液。
3.添加3.5g的20％w/w氢氧化钠水溶液并且用顶置式搅拌器有效地搅拌直到完全均质。
4.pH测量值应处于6.4到6.8范围内。必要时用20％NaOH调节
5.使用具有对应轴的布洛克菲尔德粘度计以30rpm测量粘度以至少在10％尺度下获得测量值
6.将样品转移到1oz小瓶中以用于浊度测量
浊度测量：
1.将具有样品的1oz小瓶在离心机上以3500rpm旋转30分钟。
2.在浊度计上测量浊度。
表2.聚合物样品1-7和比较实例1-5的经中和水溶液特性(粘度和浊度)
总体而言，聚合物实例1-5得到比对应比较实例1-5好得多的水溶液浊度。
调配物实例23-45(表3)
A.用于制备个人护理调配物的程序：
1.称出足以在最终调配物中具有1.8％-2.2％聚合物的聚合物实例样品。用去离子水预稀释。
2.添加乙二胺四乙酸四钠盐(VERSENE 100XL，可购自陶氏化学公司(The DowChemical Company))以在最终调配物中具有0.1％活性成分。
3.添加月桂醇醚硫酸钠(EMPICOL ESB-70，可购自亨斯曼公司(Hunstman))以在最终调配物中具有12.5％活性成分。
4.添加椰油酰胺基丙基甜菜碱(EMPIGEN BS/FA，可购自亨斯曼公司)以在最终调配物中具有2.5％活性成分。
5.用30％NaOH溶液将调配物的pH调节到高于pH 7。
6.用柠檬酸将pH调节回到指定值。
7.添加甲基异噻唑啉酮(和)苯氧基乙醇(NEOLONE PE，可购自陶氏化学公司)
8.添加去离子水以达到总体积。
B.调配物可变参数：
-月桂醇醚硫酸钠(SLES)和椰油酰胺基丙基甜菜碱(CAPB)比率和含量范围如下：
| SL-2EO-S | SL-1EO-S | CAPB | 比率 | |
| 调配物5 | 12.5 | 2.5 | 5/1 | |
| 调配物13 | 6.25 | 6.25 | 2.5 | 5/1 |
| 调配物9 | 8.3 | 1.7 | 4.9/1 | |
| 调配物10 | 11 | 4 | 2.75/1 | |
| 调配物12 | 16.5 | 3.5 | 4.7/1 |
-聚合物浓度在1.4％到2.2％活性成分范围内
-pH在4.5到7.0范围内
C.粘度测量
通过两种不同方法来进行流变分析：
1.在20℃下使用具有40mm 4°丙烯酸类锥体的TA仪器公司(TA Instrument)AR1000流变仪。在剪切应力从0.006Pa到1000Pa缓慢变化的情况下使用从低到高剪切应力的标准稳定状态流动方法来分析。对至少老化24小时并且存储在室温或40℃下的样品进行流变性概况分析。使用埃利斯模型(Ellis model)来提供零应力粘度(ZSV)。
2.在23℃下使用具有轴4的LV布洛克菲尔德流变仪。粘度在12或60rpm下以cP为单位进行报告，并且对应于存储在室温下的老化介于2与7天之间的样品的粘度。
D.透明度评估
使用两种不同技术来评估透明度：
1.使用HACH 18900-00浊度计和1cm圆柱形玻璃样品单元。透明度以NTU值形式进行报告。
2.使用HACH DR2000分光光度计和2.2cm正方形玻璃单元。透明度以320nm或400nm下的Abs值形式进行报告。
E.悬浮特性评估
以不同方式评估悬浮液：
1.查看珠粒和/或气泡悬浮液，并且在测试温度下超过至少4周的稳定性报告为“通过”测试结果。使用荷荷芭酯珠(来自Florabeads的青金石(Lapis)28/60)。在样品中手动引入气泡(预期气泡大小随机分布)。
2.上文零应力值(埃利斯模型)
F.杂项：
使用SCHOTT CG-837pH计在室温下进行pH调节和测值。
使用温度控制在40+/-2℃下的RA 6015型PROLABO EB烘箱来进行对具有悬浮珠粒或气泡的纯净聚合物或调配物样品的热老化测试。
表3：在pH为5和6.5下的各种聚合物实例的个人护理调配物特性(零应力粘度、浊度)
| 聚合物 | pH | 零应力粘度 | NTU | Abs(320nm) | Abs(400nm) |
| E1 | 5 | 85650 | 29.3 | 0.243 | 0.136 |
| 6.5 | 28030 | 11.5 | 0.144 | 0.076 | |
| E2 | 5 | 141600 | 37.0 | 0.281 | 0.166 |
| 6.5 | 15380 | 5.6 | 0.128 | 0.058 | |
| E3 | 5 | 78140 | 23.3 | 0.340 | 0.179 |
| 6.5 | 5900 | 4.6 | 0.163 | 0.065 | |
| E4 | 5 | 51240 | 19.6 | 0.318 | 0.160 |
| 6.5 | 7995 | 5.0 | 0.173 | 0.073 | |
| CE1 | 5 | 56840 | 115.6 | N/M | N/M |
| 6.5 | 5083 | 5.8 | N/M | N/M | |
| CE2 | 5 | 20790 | 103.4 | N/M | N/M |
| 6.5 | 5724 | 6.5 | N/M | N/M | |
| CE3 | 5 | 35250 | 66.2 | 0.637 | 0.414 |
| 6.5 | 14990 | 9.1 | 0.231 | 0.118 | |
| CE4 | 5 | 10350 | 57.6 | 0.632 | 0.412 |
| 6.5 | 466 | 14.8 | 0.268 | 0.151 | |
| E6 | 5 | 119500 | 43.0 | 0.362 | 0.234 |
| 6.5 | 23460 | 9.8 | 0.152 | 0.097 | |
| E7 | 5 | 131.4 | 0.869 | 0.577 | |
| 6.5 | 116.0 | 0.640 | 0.418 |
与个人护理调配物中的比较实例1-5相比，聚合物实例1-5在两个pH下都产生较高的零应力粘度并且在pH 5下产生低得多的浊度。
Claims (8)
1.一种乳液聚合物粒子，所述乳液聚合物粒子包含25wt％到45wt％的至少一种C3-C6羧酸单体的聚合残基和0.1wt％到3wt％的至少一种交联剂的聚合残基，其中交联剂的聚合残基百分比从粒子中心向粒子表面连续增加；其中，所述聚合物粒子进一步包含54wt％到74wt％至少一种(甲基)丙烯酸C1-C12烷基酯的聚合残基。
2.根据权利要求1所述的聚合物粒子，其包含29wt％到41wt％的至少一种C3-C6羧酸单体的聚合残基、0.4wt％到1.5wt％的至少一种交联剂的聚合残基以及58wt％到70wt％的至少一种(甲基)丙烯酸C1-C12烷基酯的聚合残基。
3.根据权利要求2所述的聚合物粒子，其中所述聚合物粒子的平均粒径在100到1000nm范围内。
4.根据权利要求3所述的聚合物粒子，其中所述交联剂的分子量除以所述交联剂中烯系不饱和基团数目后不超过150。
5.一种用于产生乳液聚合物粒子的方法，所述方法通过以下步骤来进行：(a)提供第一单体混合物，所述第一单体混合物包含25wt％到45wt％的至少一种C3-C6羧酸单体；(b)提供第二单体混合物，所述第二单体混合物包含0.1wt％到3wt％的至少一种交联剂；以及(c)在向所述第一单体混合物中添加所述第二单体混合物的同时，向聚合反应器中添加所述第一单体混合物；其中重量百分比是按所述第一和第二单体混合物的总重量计；其中，所述第一单体混合物进一步包含54wt％到74wt％的至少一种(甲基)丙烯酸C1-C12烷基酯。
6.根据权利要求5所述的方法，其中在添加所述第一单体混合物之前，小于5wt％的所述单体处于所述聚合反应器中。
7.根据权利要求6所述的方法，其中所述第一单体混合物包含29wt％到41wt％的至少一种C3-C6羧酸单体和58wt％到70wt％的至少一种(甲基)丙烯酸C1-C12烷基酯并且所述第二单体混合物包含0.4wt％到1.5wt％的至少一种交联剂。
8.根据权利要求7所述的方法，其中向所述第一单体混合物中添加所述第二单体混合物的时间是向所述聚合反应器中添加所述第一单体混合物的时间的50％到100％。
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- 2014-04-04 BR BR112015025137-4A patent/BR112015025137B1/pt active IP Right Grant
- 2014-04-04 JP JP2016506648A patent/JP6506253B2/ja active Active
- 2014-04-04 CN CN201480017710.3A patent/CN105051072B/zh active Active
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| BR112015025137B1 (pt) | 2020-12-22 |
| US9587057B2 (en) | 2017-03-07 |
| CN105051072A (zh) | 2015-11-11 |
| JP2016525582A (ja) | 2016-08-25 |
| JP6506253B2 (ja) | 2019-04-24 |
| EP2953979B1 (en) | 2017-03-15 |
| WO2014165767A1 (en) | 2014-10-09 |
| US20160046747A1 (en) | 2016-02-18 |
| BR112015025137A2 (pt) | 2017-07-18 |
| EP2953979A1 (en) | 2015-12-16 |
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