CN105722574B - 用于造纸工业的基于水包油乳液的消泡剂 - Google Patents
用于造纸工业的基于水包油乳液的消泡剂 Download PDFInfo
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- CN105722574B CN105722574B CN201480062753.3A CN201480062753A CN105722574B CN 105722574 B CN105722574 B CN 105722574B CN 201480062753 A CN201480062753 A CN 201480062753A CN 105722574 B CN105722574 B CN 105722574B
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Abstract
本发明提供了用于造纸工业的基于水包油乳液的消泡剂,其中如果所述乳液的油相包含如下成分,则油相占所述乳液的5‑50重量%:(a)不少于12个碳原子的醇、不少于22个碳原子的醇与C1‑C36羧酸的脂肪酯、可在通过羰基合成法或Ziegler法制备具有较高碳原子数的醇中获得且可此外被烷氧基化的蒸馏残留物、所述化合物的混合物,和(b)任选地,C12‑C22羧酸与一元至三元C1‑C18醇的脂肪酯,和(c)任选地,沸点高于200℃的烃或12‑22个碳原子的脂肪酸,且组合有1‑80重量%的组分(d),其包含:(d1)可通过用一种或多种12‑36个碳原子的脂肪酸不少于20%地酯化如下聚甘油混合物而获得的聚甘油酯:0‑10重量%的单甘油,15‑40重量%的二甘油,30‑55重量%的三甘油,10‑25重量%的四甘油,0‑15重量%的五甘油,0‑10重量%的六甘油和0‑5重量%的具有更高缩合度的聚甘油,和(d2)山萮酸C18‑C30烷基酯。所述消泡剂可用于在浆料蒸煮、纸浆打浆、造纸和分散造纸用颜料中防止起泡。此外,所述消泡剂可用于在纸浆中防止起泡。
Description
本发明涉及用于造纸工业的基于水包油乳液的消泡剂,其中油相占所述乳液的5-50重量%,且包含已知消泡剂的组合,例如长链醇或不少于22个碳原子的醇与C1-C36羧酸的脂肪酯。
美国专利4,950,420公开了用于造纸工业的消泡剂,其包含10-90重量%的表面活性剂聚醚,例如聚氧烷基化的甘油或聚烷氧基化的山梨糖醇,和10-90重量%的多元醇的脂肪酯,例如聚乙二醇或聚丙二醇的单酯或二酯。这些消泡剂不含任何油、酰胺或斥水性二氧化硅或硅油。
EP-A-0 140 812公开了基于水包油乳液的消泡剂,其中所述乳液的油相包含:
(a)C12-C26醇、在通过羰基合成法或Ziegler法制备具有较高碳原子数的醇中获得且可此外被烷氧基化的蒸馏残留物,和/或
(b)C12-C22羧酸与一元至三元C1-C18醇的脂肪酯,和需要的话
(c)沸点高于200℃的烃或12-22个碳原子的脂肪酸,
且占所述乳液的15-60重量%且具有0.5-15μm的平均粒径,所述消泡剂可通过添加0.05-0.5重量%高分子量的丙烯酸、甲基丙烯酸、丙烯酰胺或甲基丙烯酰胺的水溶性均聚物或共聚物而稳定化,从而提高粘度和储存期间的乳状液分层。
JP-A-60/083559和JP-A-61/227756公开了聚甘油基脂肪酯在食品如豆腐生产中作为消泡剂的用途。这些配制剂不含脂肪醇;然而必须存在碱土金属盐。已知消泡剂配制剂仅对它们所开发的应用范围有效,例如纺织工业、食品工业、造纸工业、表面涂料工业和皮革工业。由于该特定的效力,消泡剂不能成功地转用于或者用于其他领域中。
由于在造纸厂中使用封闭水循环的趋势日益增强,其结果是造纸中的循环水温度提高,因此迄今为止所用的消泡剂的效力显著降低。
EP-A-0 322 830公开了基于水包油乳液的消泡剂,其中所述乳液的油相包含:
(a)C12-C26醇、可在通过羰基合成法或Ziegler法制备具有较高碳原子数的醇中获得且可此外被烷氧基化的蒸馏残留物,和/或
(b)C12-C22羧酸与一元至三元C1-C18醇的脂肪酯,和需要的话
(c)沸点高于200℃的烃或12-22个碳原子的脂肪酸,
其占所述乳液的5-50重量%且具有<25μm的平均粒径,且其中所述水包油乳液的油相的组分(a)和(b)的5-50重量%被(d)代替:
(d)一种或多种在高于70℃下熔融且选自不少于28个碳原子的脂肪醇、C1-C22羧酸与不少于28个碳原子的醇的酯、C2-C4氧化烯与不少于28个碳原子的醇的加合物、具有不小于2,000的分子量的聚乙烯蜡、巴西棕榈蜡、褐煤酸酯蜡、褐煤酸蜡及其盐的化合物。所述水包油乳液是造纸中的有效消泡剂。
EP-A-531713公开了用于造纸工业的基于水包油乳液的消泡剂,其中如果所述乳液的油相包含如下成分,则油相占所述乳液的5-50重量%:
(a)不少于12个碳原子的醇、不少于22个碳原子的醇与C1-C36羧酸的脂肪酯、可在通过羰基合成法或Ziegler法制备具有较高碳原子数的醇中获得且可此外被烷氧基化的蒸馏残留物,所述化合物的混合物,和/或
(b)C12-C22羧酸与一元至三元C1-C18醇的脂肪酯,和需要的话,
(c)沸点高于200℃的烃或12-22个碳原子的脂肪酸,
且组合有:
(d)1-80重量%的可通过用一种或多种12-36个碳原子的脂肪酸不少于20%地酯化如下聚甘油混合物而获得的聚甘油酯:
0-10重量%的单甘油,
15-40重量%的二甘油,
30-55重量%的三甘油,
10-25重量%的四甘油,
0-15重量%的五甘油,
0-10重量%的六甘油,和
0-5重量%的具有更高缩合度的聚甘油。
发现EP-A-531713的消泡剂至少在造纸工业中有效。
本发明的目的是提供一种更有效的用于造纸工业的消泡剂。
该目的通过本发明实现,其提供了用于造纸工业的基于水包油乳液的消泡剂,其中如果所述乳液的油相包含如下成分,则油相占所述乳液的5-50重量%:
(a)不少于12个碳原子的醇、不少于22个碳原子的醇与C1-C36羧酸的脂肪酯、可在通过羰基合成法或Ziegler法制备具有较高碳原子数的醇中获得且可此外被烷氧基化的蒸馏残留物、所述化合物的混合物,和
(b)任选地,C12-C22羧酸与一元至三元C1-C18醇的脂肪酯,和
(c)任选地,沸点高于200℃的烃或12-22个碳原子的脂肪酸,
且组合有1-80重量%的组分(d),其包含:
(d1)可通过用一种或多种12-36个碳原子的脂肪酸不少于20%地酯化如下
聚甘油混合物而获得的聚甘油酯:
0-10重量%的单甘油,
15-40重量%的二甘油,
30-55重量%的三甘油,
10-25重量%的四甘油,
0-15重量%的五甘油,
0-10重量%的六甘油,和
0-5重量%的具有更高缩合度的聚甘油,
和
(d2)山萮酸C18-C30烷基酯。
一般而言,具有更高缩合度的聚甘油可具有至少为7(即,至少7个甘油重复单元)的缩合度。所述具有更高缩合度的聚甘油可具有至少为10的缩合度。这可为至少14或至少15或者可为至少20。缩合度可高达25,或者甚至高达30,且可高达40或50。
组分(d2)的烷基结构部分可为直链或支化的,但优选为直链的。优选地,组分(d2)为山萮酸C18-C24烷基酯,例如山萮酸C18-C22烷基酯。更优选地,组分(d2)为山萮酸C22烷基酯,特别为山萮酸山萮基酯。
这些消泡剂以0.02-0.5重量份/100重量份消泡介质的量使用以防止在浆料蒸煮、纸浆打浆、造纸和分散造纸用颜料中起泡。在所述的量下,它们还在纸浆中起除气剂的作用。
特别地,将不少于12个碳原子的醇或醇混合物用作所述水包油乳液的组分(a)。这些通常为在分子中包含至多48个碳原子的一元醇。该产品可商购获得。然而,也可使用在分子中包含显著更大碳原子数的脂肪醇作为组分(a)。组分(a)为天然或合成醇。例如,月桂醇、肉豆蔻醇、鲸蜡醇、棕榈醇、硬脂醇、山萮醇、油醇、蓖麻油醇、亚麻醇和瓢儿菜醇是合适的。
也可将醇的混合物,例如(1)12-26个碳原子的醇和(2)28-48个碳原子的醇的混合物作为组分(a)。
可例如借助Ziegler法通过氧化烷基铝而获得的合成醇是饱和的直链、非支化醇。合成醇也可通过羰基合成法获得。此时通常获得醇混合物。在通过羰基合成法或Ziegler法制备上述醇中获得的蒸馏残留物也可用作所述消泡剂乳液油相的组分(a)。在上述通过羰基合成法或Ziegler法制备高级醇的方法中获得的烷氧基化蒸馏残留物也适于作为所述消泡剂乳液油相的组分(a)。氧烷基化的蒸馏残留物借助已知方法通过用氧化乙烯或氧化丙烯或氧化乙烯与氧化丙烯的混合物对所述蒸馏残留物进行烷氧基化而获得。所述蒸馏残留物中的醇的每个OH基团加成至多5个氧化乙烯或氧化丙烯基团。优选地,所述蒸馏残留物中的醇的每个OH基团加成1或2个氧化乙烯基团。
其他合适的组分(a)为不少于22个碳原子醇与C1-C36羧酸的脂肪酯,例如褐煤蜡或巴西棕榈蜡。
组分(a)的上述化合物(单独或者作为任意比例的组分(a)的一部分彼此的混合物)可形成所述水包油乳液的油相。
所述消泡剂乳液油相的任选组分(b)为C12-C22羧酸与一元至三元C1-C18醇的脂肪酯的任意化合物。形成所述酯的基础的脂肪酸例如为月桂酸、肉豆蔻酸、棕榈酸、硬脂酸、花生酸和山萮酸。优选使用棕榈酸或硬脂酸来制备所述酯。可使用一元C1-C18醇如甲醇、乙醇、丙醇、丁醇、己醇、癸醇和硬脂醇,以及二元醇如乙二醇,或三元醇如甘油来酯化所述羧酸。多元醇可完全或部分酯化。
所述乳液的油相可额外由另一类水不溶性化合物(下文称为组分(c))形成。组分(c)的化合物可占至多50重量%,基于所述消泡剂乳液油相的组分(a)和存在的话(b)。它们可添加至在组分(a)下所述的化合物中,或者如果存在组分(b)的化合物,则添加至组分(a)和(b)的混合物中。合适的组分(c)为具有在1013毫巴下超过200℃的沸点和低于0℃的倾点的烃,或者为12-22个碳原子的脂肪酸。优选的烃为液体石蜡,例如市售石蜡混合物,其也称为白油。
一般而言,本发明的消泡剂组合物仅包含组分(a)和(d)。然而,当所述组合物还包含组分(b)时,组分(a)和(b)可以以任意比例用于制备所述消泡剂乳液。这两种组分各自可单独或作为彼此的混合物存在于所述消泡剂中。例如,可使用包含40-60重量%组分(a)和60-40重量%组分(b)的(a)和(b)的混合物。代替组分(b)或者除组分(c)之外,所述水包油乳液的油相可包含一种或多种化合物(c)。优选地,本发明的组合物不含组分(b)或组分(c)。然而,必要的是,上述组分(a)的至少一种化合物与下述组(d)的一种或多种化合物组合地形成所述水包油乳液的油相。化合物(d)占所述水包油乳液油相的1-80重量%,优选5-20重量%。在油相组成的所有三种上述组合的情况下,组分(c)的化合物可以以基于所述水包油乳液的油相为至多40重量%的量使用。
所述油相的合适组分(d1)为可通过用一种或多种在分子中具有12-36个碳原子的脂肪酸不少于20%地酯化如下聚甘油混合物而获得的聚甘油酯:
0-10重量%的甘油,
15-40重量%的二甘油,
30-55重量%的三甘油,
10-25重量%的四甘油,
0-15重量%的五甘油,
0-10重量%的六甘油,和
0-10重量%,优选0-5重量%的具有更高缩合度的聚甘油。
上述聚甘油混合物优选被16-30个碳原子的脂肪酸酯化。酯化度为20-100%,优选为60-100%。适于酯化所述聚甘油混合物的脂肪酸可为饱和脂肪酸以及不饱和脂肪酸,例如月桂酸、肉豆蔻酸、棕榈酸、硬脂酸、花生酸、山萮酸和褐煤酸。烯属不饱和脂肪酸,例如油酸、十六碳烯酸、反油酸、二十碳烯酸和二十二碳烯酸,例如芥酸或巴西烯酸,以及多不饱和酸,例如十八碳二烯酸和辛三烯酸,例如亚油酸和亚麻酸,以及所述饱和和不饱和羧酸的混合物也适于酯化所述聚甘油混合物。优选地,所述脂肪酸为山萮酸。优选的聚甘油酯为聚甘油基山萮酸酯。
所述具有更高缩合度的聚甘油可如本说明书前文所定义。
所述聚甘油混合物可例如通过在升高的温度下碱催化缩合甘油而获得(例如参见Fette,Seifen,Anstrichmittel,第88年,第3期,第101-106页(1986)或DE-A 3 842 692),通过使甘油与表氯醇在酸性催化剂存在下在升高的温度下反应而获得。然而,所述混合物也可通过将纯聚甘油组分如二甘油、三甘油和四甘油彼此混合而获得。被不少于20%酯化的聚甘油混合物通过用所需的脂肪酸或脂肪酸混合物借助已知方法酯化聚甘油混合物而制备。所述反应通常在酸性酯化催化剂如硫酸、对甲苯磺酸、柠檬酸、亚磷酸、磷酸或次磷酸,或碱性催化剂如甲醇钠或叔丁醇钾存在下进行。
组分(d2)可通过酯化相应醇和山萮酸而获得。山萮酸是市售的羧酸,例如由BASF市售。
根据本发明,可使用任意重量比的组分(d1)和组分(d2)。组分(d1)与组分(d2)的比例可合适地为99:1-1:99(重量),例如60:40-5:95,例如40:60-5:95,例如25:75-10:90。
特别优选的配制剂使用聚甘油基山萮酸酯作为组分(d1),且使用山萮酸山萮基酯作为组分(d2)。
组分(d)(即组分(d1)和(d2)总体)的化合物优选以0.5-20重量%,优选1-15重量%,更优选5-10重量%的量存在于油相中。油相可占所述水包油乳液的5-50重量%,而所述乳液中的水相含量为95-50重量%,所述重量百分比总和为100。
油相应乳化在水相中。为此,需要其中所述乳液的组分可经历强剪切梯度的装置,例如分散混合器。为了获得特别稳定的水包油乳液,油相在水相中的乳化例如在具有大于6的HLB值(HLB值的定义参见W.C.Griffin,Journal of the Society of CosmeticChemists,5(1954),249-246)的表面活性剂存在下进行。所述表面活性剂为水包油乳化剂或者通常的润湿剂。在表面活性剂中,可使用阴离子、阳离子或非离子化合物或者彼此相容的这些化合物的混合物,例如阴离子和非离子的混合物,或者阳离子和非离子润湿剂的混合物。所述类型的物质例如为高级脂肪酸的钠盐或铵盐如油酸铵或硬脂酸铵,氧烷基化的酚如以1:2-1:50的摩尔比与氧化乙烯反应的壬基酚或异辛基酚,氧乙基化的不饱和油如1摩尔蓖麻油与30-40摩尔氧化乙烯的反应产物或1摩尔精醇与60-80摩尔氧化乙烯的反应产物。还优选使用壬基酚或辛基酚的硫酸化氧乙基化产物作为乳化剂,所述产物作为相应硫酸半酯的钠或铵盐存在。100重量份水包油乳液通常包含0.1-5重量份乳化剂或乳化剂混合物。除上述乳化剂之外,还可将保护性胶体或增稠剂如高分子量多糖和皂,或其他常规添加剂如稳定剂用于制备所述水包油乳液。例如,已证明添加基于全部乳液为0.05-1.0重量%丙烯酸、甲基丙烯酸、丙烯酰胺或甲基丙烯酰胺的高分子量水溶性均聚物和共聚物以作为稳定剂是有用的。例如EP-A 0 149 812涉及使用该类稳定剂。合适的增稠剂包括黄原酸胶。
将油相乳化于水相中获得了在紧邻制备之后(例如制备后0-30分钟或者制备后0-15分钟或者制备后0-10分钟或者制备后0-5分钟)具有300-3,000mPa.s粘度和小于25μm,优选0.5-10μm,更优选3-5μm油相平均粒度的水包油乳液。
尽管组分(d)(即组分(d1)和(d2)的组合)的化合物单独或者作为与组分(c)的混合物基本上不具有作为水包油乳液消泡剂的活性,然而将组分(d)的化合物与至少一种组分(a)的化合物组合令人惊讶地产生了协同增效效果。将组分(d)添加至包含组分(a)和需要的话呈乳化形式的其他组分的消泡剂油相中对所得消泡剂在较低温度下,例如在室温下的功效具有很小或者不具有不利影响,然而将消泡剂在温度例如为30-50℃的含水体系中的功效提高至预料不到的程度。所述新型水包油乳液用于其中必须防止在较高温度下形成泡沫的造纸工业的含水体系中,例如用于浆料蒸煮中、纸浆打浆中、在造纸机中使用封闭水循环的造纸中和分散造纸用颜料中。基于每100份处于起泡性介质中的纸浆,使用0.02-0.5重量份,优选0.05-0.3重量份所述水包油消泡剂乳液。当添加至纸浆悬浮液中时,所述消泡剂此外导致除气,因此还在造纸中用作除气剂(添加剂至纸浆中)。它们还适于作为纸涂料中的消泡剂,其中将它们添加至纸涂料液中。所述消泡剂也可用于食品工业、淀粉工业以及用于废水处理中以用于防止起泡。如果将它们作为除气剂添加至纸浆中,则用于该目的的量为0.02-0.5重量份/100重量份纸浆。
实施例
根据本发明,如下所述制备产物A:
制备水相:
在烧杯中装入713,8g去离子水。在搅拌下,小心添加2,5g Xanthan TG粉末(获自德国Jungbunzlauer)以避免成团。然后添加6,8g Emulan TO4070(获自BASF)。将所述混合物加热至95℃并在该温度下保持15分钟。
制备油相:
在烧杯中混合如下组分:
202g NafolTM 20+BA(脂肪醇混合物(C18-C24)),获自Sasol
3,4g 聚甘油基山萮酸酯(包含27重量%二甘油基山萮酸酯、44重量%三甘油基山萮酸酯、19重量%四甘油基山萮酸酯和10重量%具有更高缩合度(即,至少5个缩合的甘油单元)的聚甘油的山萮酸酯,获自BASF)
2,5g 山萮酸山萮基酯(法国Stéarinerie Dubois)
45g Paraffin 52/54(获自H&R Wax Company或Sasol WaxgmbH,德国)将所述混合物加热至98℃并轻柔搅拌熔体。
均化步骤:
将两种混合物混合并用Ultra Turrax T 50(IKA)乳化,直至达到所选粒度。使用Beckmann Coulter粒度检测仪,型号LS 13320测定粒度。在将混合物冷却至室温后,使用4gActicide MBS(Thor Chemie)使所述分散体微生物学稳定。
实施例1
在实验中,在强韧箱纸板厂中在短期实验中相对于竞争性消泡剂Nalco74192(28%固体)测试消泡剂产物A(根据本发明,29%固体)。所述纸厂使用回收纸(旧瓦楞纸板)作为原料。湿部温度为31℃。将所述两种消泡剂直接投料至白水盘中的白水中(操作面)。
在实验期间,相对于随时间变化的消泡剂剂量监控流浆箱(HB)和白水(WW)(在网部之后)中的空气含量。空气含量使用EGT-Tester(GB Machining Inc,4415 102nd Ave E,Edgewood,Wa 98371,USA)测定。
结果在下表中给出:
为了避免启动工艺的初始工艺复杂性,通常仅在初始阶段提高各新型消泡剂产物的剂量。在这种情况下,在改变之前,新型消泡剂产物A相对于所用的Nalco 74192提高16.3%。
因此观察到与使用Nalco 74192的其初始水平相比,由纸厂在线测得的空气含量在白水中降至48.6%,在流浆箱中降至39.1%。
实施例2
在纸厂实验中,在新闻纸厂中,在实验中相对于Afranil MG(29%固体,BASF的广为市场认可的消泡剂)测试产物A(29%固体)。所述纸厂使用破碎的研磨木浆,主要是脱墨纸浆作为原料。湿部温度为44℃。将所述两种消泡剂直接投料至白水盘中的循环白水中(操作面)。
在该纸厂中,将Afranil MG作为标准产品投料。在实验启动时,停止Afranil MG投料。同时,以精确相同的投料体积在相同的投料位置开始产物A的投料。使用SONARtrac VF/GVF—100(CiDRA,50 Barnes Park North,Wallingford,CT 06492,USA)在线测定空气含量。
结果示于图1中。
因此观察到在稀浆料中空气含量由约1%显著降至约0.3%。由产物A切换回至Afranil MG(以恒定的投料水平),空气含量缓慢升至其原先的空气含量水平。
实施例3
在新闻纸厂中使用产物A(29%固体)的更长实验中,将除气剂投料切换至AfranilMG(29%固体),并切换回,从而对比这两种产品的功效。所述纸厂使用破碎的研磨木浆,主要是脱墨纸浆作为原料。湿部温度为43℃。将所述两种消泡剂直接投料至白水盘中的白水中(操作面)。
连续投料产物A。在实验启动时,将消泡剂由产物A切换至Afranil MG,随后切换回至产物A。在使用0.122L/分钟产物A下,稀浆料的空气含量令人惊讶地保持在低水平下。在使用相同投料量的Afranil MG下,稀浆料的空气含量显著增大。为了获得1.22L/分钟产物A的除气水平,Afranil MG的投料体积必须提高至0.177L/分钟。因此,Afranil MG的投料速率必须提高45%以匹配相同的稀浆料空气含量。
空气含量使用SONARtrac VF/GVF—100(CiDRA,50 Barnes Park North,Wallingford,CT 06492,USA)在线测定。
结果示于图2中。
Claims (5)
1.一种用于造纸工业的基于水包油乳液的消泡剂,其中油相占所述乳液的5-50重量%,并且所述乳液的油相包含如下成分:
(a)不少于12个碳原子的醇、不少于22个碳原子的醇与C1-C36羧酸的脂肪酯、可在通过羰基合成法或Ziegler法制备具有较高碳原子数的醇中获得的且任选地被烷氧基化的蒸馏残留物、前述组分的混合物,和
(b)任选地,C12-C22羧酸与一元至三元C1-C18醇的脂肪酯,和
(c)任选地,沸点高于200℃的烃或12-22个碳原子的脂肪酸,
且组合有1-80重量%的组分(d),其包含:
(d1)可通过用一种或多种12-36个碳原子的脂肪酸不少于20%地酯化如下聚甘油混合物而获得的聚甘油酯:
0-10重量%的单甘油,
15-40重量%的二甘油,
30-55重量%的三甘油,
10-25重量%的四甘油,
0-15重量%的五甘油,
0-10重量%的六甘油,和
0-5重量%的具有更高缩合度的聚甘油,
和
(d2)山酸C18-C30烷基酯。
2.根据权利要求1的消泡剂,其中组分(d1)的聚甘油酯为聚甘油基山酸酯。
3.根据权利要求1或2的消泡剂,其中所述山酸C18-C30烷基酯为山酸山基酯。
4.一种用于在浆料蒸煮中、在纸浆精磨中制备浆料中、在造纸中和在分散造纸用颜料中防止起泡的方法,其包括添加有效量的如权利要求1-3中任一项所述的消泡剂。
5.一种用于在纸浆中防止起泡的方法,其包括添加其量为0.02-0.5重量份如权利要求1-3中任一项所述的消泡剂/100重量份纸浆。
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