CN106795458A - 稳定的消泡组合物 - Google Patents

稳定的消泡组合物 Download PDF

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CN106795458A
CN106795458A CN201580054802.3A CN201580054802A CN106795458A CN 106795458 A CN106795458 A CN 106795458A CN 201580054802 A CN201580054802 A CN 201580054802A CN 106795458 A CN106795458 A CN 106795458A
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methyl
ethene
defoamer
composition according
defoaming composition
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P·E·布鲁托
A·S·卡里卡利
W·C·迈尔斯
C·J·图克
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Dow Global Technologies LLC
Rohm and Haas Co
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Rohm and Haas Co
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Abstract

一种稳定化的消泡组合物，其具有至少三种组分。第一组分是消泡剂。第二组分是乙烯‑(甲基)丙烯酸共聚物。第三组分是盐。

Description

稳定的消泡组合物
本发明涉及消泡组合物，其在分散于水性介质中时稳定。
美国专利第6,569,924号描述了用于消泡组合物的增溶剂。这些增溶剂是烷氧基化的化合物。但是，此参考文献未描述如何形成稳定的消泡组合物。
发明内容
本发明提供了一种稳定化的消泡组合物，所述组合物包含：(a)消泡剂；(b)乙烯-(甲基)丙烯酸共聚物；以及(c)盐。
具体实施方式
除非另外规定，否则百分比是重量百分比(wt％)并且温度以℃为单位。除非另外规定，否则操作在室温(20-25℃)下进行。组分的重量百分比是以活性成分的重量(例如不具有可能在商业表面活性剂产品中的任何水的表面活性剂分子的重量)计以及以包括水在内的整个消泡组合物的重量计。共聚物中乙烯、(甲基)丙烯酸或交联剂单元的百分比是以聚合物链的总重量计。术语“(甲基)丙烯酸”意味着甲基丙烯酸或丙烯酸。
优选地，消泡剂是有机改性的硅氧烷聚合物、环氧乙烷-环氧丙烷共聚物或有机磷化合物。优选地，有机改性的硅氧烷聚合物是二甲基聚硅氧烷、二乙基聚硅氧烷、二丙基聚硅氧烷、甲基乙基聚硅氧烷、二辛基聚硅氧烷、二乙基聚硅氧烷、甲基丙基聚硅氧烷、二丁基聚硅氧烷或十二烷基聚硅氧烷；优选二甲基聚硅氧烷。有机改性的硅氧烷聚合物可含有不同烷基的混合物。优选地，有机改性的硅氧烷聚合物具有30到1000个硅氧烷单元，优选40到500个。优选地，有机磷化合物是具有三个烷基或芳基取代基的磷酸酯或亚磷酸酯，各取代基具有三到十个碳原子；优选磷酸正三丁酯、磷酸正三丁氧基乙酯、亚磷酸三苯酯或其混合物。优选地，环氧乙烷-环氧丙烷共聚物是嵌段共聚物，优选具有1,000到10,000的Mn的嵌段共聚物。
优选地，乙烯-(甲基)丙烯酸共聚物包含50wt％到90wt％乙烯和10wt％到50wt％(甲基)丙烯酸；优选至少55wt％乙烯、优选至少60wt％、优选至少65wt％、优选至少70wt％、优选至少75wt％；优选不超过85wt％乙烯、优选不超过82wt％、优选不超过79wt％、优选不超过76wt％；优选至少15wt％(甲基)丙烯酸，优选至少18wt％、优选至少21wt％；优选不超过45wt％(甲基)丙烯酸、优选不超过40wt％、优选不超过35wt％、优选不超过30wt％、优选不超过25wt％。优选地，乙烯-(甲基)丙烯酸共聚物是乙烯-丙烯酸共聚物。
优选地，乙烯-(甲基)丙烯酸共聚物的数均分子量(number-average molecularweight，Mn)是2,000到20,000；优选2,500到15,000；优选3,000到10,000。优选地，乙烯-(甲基)丙烯酸共聚物的重均分子量(weight-average molecular weight，Mw)是8,000到150,000；优选10,000到100,000；优选12,000到60,000；优选14,000到30,000。优选地，乙烯-(甲基)丙烯酸共聚物部分被中和，即，通过加入碱，中和50摩尔％到100摩尔％(甲基)丙烯酸羧酸基(即，呈盐形式)，优选至少70％、优选至少80％、优选至少85％、优选至少88％；优选不超过96％、优选不超过94％。优选地，碱是碱金属氢氧化物，优选氢氧化钠或氢氧化钾，优选氢氧化钾。优选地，乙烯-(甲基)丙烯酸共聚物中交联剂的量不大于0.15wt％、优选不大于0.1wt％、优选不大于0.05wt％、优选不大于0.02wt％；所有百分比都以干聚合物计。交联剂是多烯键式不饱和单体的聚合单元或金属离子。
优选地，消泡组合物包含0.05wt％到3wt％消泡剂；优选至少0.3wt％、优选至少0.6wt％、优选至少0.9wt％、优选至少1.2wt％、优选至少1.5wt％；优选不超过2.5wt％、优选不超过2.3wt％、优选不超过2.1wt％。优选地，消泡组合物包含0.2wt％到12wt％乙烯-(甲基)丙烯酸共聚物；优选至少1.2wt％、优选至少2.4wt％、优选至少3.6wt％、优选至少4.8wt％、优选至少6wt％；优选不超过10wt％、优选不超过9wt％、优选不超过8.5wt％。优选地，乙烯-(甲基)丙烯酸共聚物与消泡剂的重量比是0.5:1到6:1，优选1:1到5:1，优选2:1到5:1。优选地，消泡组合物包含至少79wt％水、优选至少81wt％、优选至少83wt％、优选至少85wt％、优选至少87wt％；优选不超过95wt％、优选不超过92wt％、优选不超过89wt％。
优选地，消泡组合物包含1到6wt％盐；优选至少2wt％、优选至少2.5wt％、优选至少3wt％；优选不超过5wt％、优选不超过4.5wt％、优选不超过4wt％、优选不超过3.5wt％。优选地，盐所具有的阳离子是碱金属或碱土金属离子或质子化胺；优选钠离子、钾离子、镁离子、钙离子或铵离子或质子化氨基醇，优选C2-C8氨基醇。优选地，阴离子是乙酸根、氯离子、C1-C12羧酸根、硫酸根、磷酸根或C1-C12磺酸根和膦酸根；优选乙酸根或氯离子；优选乙酸根。优选地，盐是碱金属乙酸盐；优选乙酸钠或乙酸钾。优选地，组合物中的盐浓度是0.1-2M，优选0.2到1.5M，优选0.3到1M。组合物可含有盐混合物。
优选地，消泡组合物包含0.5wt％到6wt％表面活性剂；优选至少1wt％、优选至少1.5wt％、优选至少2wt％、优选至少2.5wt％、优选至少3wt％；优选不超过5wt％、优选不超过4.5wt％。优选地，表面活性剂为非离子型表面活性剂或阴离子型表面活性剂，优选非离子型表面活性剂。优选地，非离子型表面活性剂具有一个含至少八个碳原子的烷基和至少五个聚合环氧乙烷或环氧丙烷残基。优选地，非离子型表面活性剂具有至少六个聚合环氧乙烷单元，优选至少七个、优选至少八个、优选至少九个；优选不超过十二个、优选不超过十一个、优选不超过十个。任选地，非离子型表面活性剂优选在烷基与环氧乙烷单元之间具有聚合环氧丙烷单元。优选地，非离子型表面活性剂具有C10-C18烷基，优选C12-C16。优选地，表面活性剂浓度与乙烯-(甲基)丙烯酸共聚物浓度的比率是0.05:1到2:1，优选0.1:1到1.5:1，优选0.2:1到1:1。
优选地，首先将消泡剂与乙烯-(甲基)丙烯酸共聚物组合，接着组合盐。如果表面活性剂是消泡组合物的一部分，那么其在盐后加入。
优选地，消泡组合物的pH值是7到11。调节调配物pH值的适合碱包括无机碱，例如氢氧化钠和氢氧化钾；氢氧化铵；以及有机碱，例如单乙醇胺、二乙醇胺或三乙醇胺；或2-二甲氨基-2-甲基-1-丙醇(DMAMP)。可以使用碱混合物。调节水性介质pH值的适合酸包括无机酸，例如盐酸、磷酸和硫酸；以及有机酸，例如乙酸。可以使用酸混合物。可以用碱将调配物调到较高pH值，接着用酸反向滴定到上文所描述的范围。
在本发明的一个优选实施例中，将消泡组合物加入金属加工流体浓缩物中。当去除浓缩物的部分并进一步稀释以供用作金属加工流体时，消泡剂针对相分离的稳定性是重要的。优选地，金属加工流体浓缩物中消泡组合物的浓度是1wt％到10wt％、优选2wt％到9wt％。相信金属加工流体中消泡组合物稀释成较低离子强度可将消泡剂从经共聚物封装中释放出，并使其可用作活性消泡剂。金属加工流体通常是至少40w％水。优选地，金属加工流体中消泡剂的浓度是0.01wt％到0.2wt％。
实例
通过首先将消泡剂与聚合物混合，接着加入3.2wt％NaCl溶液，来制成2wt％消泡剂(ALDRICH消泡剂B：水、α-甲基-ω-甲氧基聚二甲基硅氧烷、纤维素甲基醚和氢化牛脂甘油酯)、8wt％PRIMACOR(Ecosmooth Satin：Mn＝4,780，Mw＝31,380，80％乙烯，约85％经NaOH中和)、3.2wt％NaCl、4wt％GENAPOL C-100(C16-C18，具有10摩尔环氧乙烷)和82.8wt％水的调配物。最后，GENAPOL C-100溶解于3.2wt％NaCl溶液并加入。这些步骤中添加次序是关键的。此调配物被称为消泡剂浓缩物。
将消泡剂浓缩物加入低油半合成金属加工流体(MWF)，其由2％CORFREE M1、47％去离子水、7％CORRGUARD EXT、4％CORRGUARD 95、10％HYDROCAL 100、14％PETRONATE HL、8％L5、2.4％Actrafos 110、3％DOWANOL PnB和2.2％GENAPOL C-100(都是wt％)组成。MWF浓缩物中最终消泡剂浓度是0.05wt％。制成另一MWF，其含有0.05wt％消泡剂B，无任何其它物质。随时间的推移，进行泡沫测试，以确定在MWF浓缩物中PRIMACOR聚合物是否能够稳定化消泡剂。
通过在制备浓缩物后的指示时间，量出MWF浓缩物的5g样品并将其加入95g去离子水中来进行泡沫测试。将容器盖上盖子并轻缓地混合溶液，直到其均匀。此刻，将溶液轻缓地倾入掺合器中并高速运行15秒。接着将溶液倾入250mL刻度量筒中，并在打开掺合器后195秒时测量剩余的泡沫体积。
样品的粒径通过动态光散射(dynamic light scattering，DLS)测量来测定，所述测量是用Malvern ZETASIZER NanoZS粒子分析器(Malvern Instruments Ltd.,Malvern,U.K.)，在来自4.0mW固态He-Ne激光器的633nm波长下，在173°散射角度和25+/-0.1℃下进行。使稳定化的粒子悬浮于3.2wt％氢氧化钠溶液中，消泡剂浓度大约是0.1mg/mL。接着样品用移液管移取到干净的聚苯乙烯比色皿中。三次分开测量的平均值用于产生粒径柱状图。对于长时间实验，相同样品的粒径每5分钟测量一次。结果列表于下方。
在两种情况下(消泡剂1和2，消泡剂1是由Sigma Aldrich供应的消泡剂B，并且消泡剂2是Munzing FOAMBAN HP710)，在稳定化后消泡剂的粒径显著地减小。此表明聚合物正稳定化比并入消泡剂产物中的乳化剂更小的粒子。
下表含有检查粒径随时间的推移如何改变的实验的结果。出于两个原因，对于仅消泡剂，只作一次测量。首先，如先前图表中所示，其明显大于稳定化的消泡剂。其次，对于发生凝聚的系统，随时间的推移由光散射来测量尺寸是不可靠的。在粒径计算中进行的许多假设在凝聚系统中都被打破。因此，重要的是证实在任何种类的光散射测量后小瓶底部是否有沉降，以及针对沉降的标志，检查实际原始数据。在此情况下，对于稳定化的消泡剂，在小瓶底部或从软件，未看到沉降标志，但对于对照消泡剂，都观测到沉降标志。

Claims (9)

1.一种稳定化的消泡组合物，所述组合物包含∶(a)消泡剂；(b)乙烯-(甲基)丙烯酸共聚物；以及(c)盐。
2.根据权利要求1所述的组合物，其中乙烯-(甲基)丙烯酸共聚物与消泡剂的重量比是0.5:1到6:1。
3.根据权利要求2所述的组合物，其中所述消泡剂是硅氧烷或环氧乙烷与环氧丙烷的共聚物。
4.根据权利要求3所述的组合物，其中所述乙烯-(甲基)丙烯酸共聚物包含50wt％到90wt％乙烯和10wt％到50wt％(甲基)丙烯酸。
5.根据权利要求4所述的组合物，其中50摩尔％到100摩尔％所述(甲基)丙烯酸被中和。
6.根据权利要求5所述的组合物，其包含0.5wt％到6wt％表面活性剂。
7.根据权利要求6所述的组合物，其包含0.05wt％到3wt％消泡剂和0.2wt％到12wt％乙烯-(甲基)丙烯酸共聚物。
8.根据权利要求7所述的组合物，其包含79wt％到95wt％水和1wt％到6wt％盐。
9.根据权利要求8所述的组合物，其中所述共聚物包含乙烯和丙烯酸。
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WO1993001269A1 (en) * 1991-07-01 1993-01-21 Unilever Plc Antifoam ingredient
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