CN110691584A - 制备浅色二盐的方法 - Google Patents
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Abstract
本发明涉及一种制备浅色含水表面活性剂组合物的方法,所述组合物包含:相对于整个组合物为10‑60重量%的一种或多种通式(I)的α‑磺基脂肪酸二盐(A),R1CH(SO3M1)COOM2(I),其中基团R1为具有6‑18个碳原子的直链或支化烷基或烯基,基团M1和M2彼此独立地选自H、Li、Na、K、Ca/2、Mg/2、铵和链烷醇胺;和水,其中所述方法的特征在于将通式(Ia)的脂肪酸R2CH2COOH(Ia),其中基团R2表示具有6‑18个碳原子的直链或支化烷基或烯基,(i)用气态三氧化硫进行磺化,(ii)将所得的酸性磺化产物—任选在陈化后—中和,然后(iii)用过氧化氢对其进行漂白,其中漂白在高于7的pH下在80‑95℃的温度范围内在相对于整个组合物为50‑500ppm的稳定剂存在下进行,所述稳定剂选自氧化镁、镁盐、水玻璃、次氮基三乙酸、乙二胺四乙酸、葡糖酸及其盐。
Description
发明领域
本发明涉及一种制备具有α-磺基脂肪酸二盐含量的浅色含水表面活性剂组合物的方法。
现有技术
阴离子表面活性剂是一些最普遍的界面活性化合物,除用于洗涤剂和清洁剂之外,还用于化妆品领域中的各种目的。尤其用于化妆品中的常规阴离子表面活性剂是烷基醚硫酸盐(烷基聚醚硫酸盐、脂肪醇聚乙二醇醚硫酸盐,简称为醚硫酸盐)。它们的特征在于起泡能力强,清洁能力强,对硬度和油脂的敏感度低,广泛用于制备化妆品如洗发剂、泡沫浴或淋浴,以及手洗餐具洗涤剂中。
对于许多现行应用,除良好的界面活性效果以外,对阴离子表面活性剂还有其他要求。特别地,在化妆品中需要高的皮肤病相容性。此外,通常希望良好的起泡能力和令人愉悦的感觉。此外,需要可至少部分地由生物来源,特别是还有可再生原料制备的阴离子表面活性剂。满足该要求的表面活性剂优选为α-磺基脂肪酸二盐,其例如可通过用气态三氧化硫磺化脂肪酸且随后进行中和而获得。
从文献中长期已知将饱和脂肪酸磺化来制备α-磺基脂肪酸。磺化通常通过使脂肪酸与气态三氧化硫反应而进行。然而,在这种情况下可获得的产物是深色的,该形式仅具有有限的应用。
各种专利文献涉及磺化条件的优化,以便从一开始就尽可能减少初始颜色载体的形成,例如将DE 4224735与其中引用的文献相比。然而,仅初始颜色的改善不能产生可接受的产物颜色。以此方式,只能提供更多的可漂白的产物。然而,总是需要漂白剂形式的后处理。
已知脂肪酸酯的磺化产物的漂白可用过氧化氢进行,其中漂白完全或部分用尚未中和的酸性粗磺酸进行(例如与DE1179931、DE1234709、DE3319591相比)。然而,申请人的研究表明,这无法容易地转用到脂肪酸磺化产物的漂白中,因为当漂白脂肪酸的未中和的酸性磺化产物时,会发生胶凝。
申请人的研究还表明,使用过氧化氢在7或更低的pH值下进行的脂肪酸磺化产物的中和含水浆料的漂白不能达到可接受的产物颜色。可接受的产物颜色需要使用非常大量的过氧化氢,长处理时间,并且还需要复杂的过程监控和控制,尤其是为了避免形成不可控制的泡沫,以及还导致不希望的稀释,即水进入。
发明描述
本发明的目的在于提供一种简单,可靠,可重现且经济上可行的,但解决了上述过氧化氢漂白的技术问题的制备包含α-磺基脂肪酸二盐的浅色含水表面活性剂组合物的方法,其基于用气态三氧化硫来磺化脂肪酸且随后中和及漂白。
在本发明的上下文中,术语“浅色”应理解为意指含水表面活性剂组合物在稀释成基于稀释溶液总含量为4重量%的干残留物之后,具有200哈森或更低,优选为100哈森或更低的哈森色值。在这种情况下,用去离子水(95重量%)和异丙醇(5重量%)的混合物稀释以进行颜色测量。颜色测量在市售颜色测量仪器(例如获自Hach Lange GmbH的Lico 500)中的11mm圆形比色杯中进行。
本发明涉及一种制备浅色含水表面活性剂组合物的方法,所述组合物包含:
·基于整个组合物为10-60重量%的一种或多种通式(I)的α-磺基脂肪酸二盐(A),
R1CH(SO3M1)COOM2 (I)
其中基团R1为具有6-18个碳原子的直链或支化烷基或烯基,基团M1和M2彼此独立地选自H、Li、Na、K、Ca/2、Mg/2、铵和链烷醇胺,
·水,
其中所述方法的特征在于将通式(Ia)的脂肪酸,
R2CH2COOH (Ia)
其中基团R2为具有6-18个碳原子的直链或支化烷基或烯基,
(i)用气态三氧化硫进行磺化,
(ii)将酸性的磺化产物—任选在陈化后—中和,然后
(iii)用过氧化氢进行漂白,其中漂白在高于7的pH下在80-95℃的温度范围内在基于整个组合物为50-500ppm的稳定剂存在下进行,所述稳定剂选自氧化镁、镁盐、水玻璃、次氮基三乙酸、乙二胺四乙酸、葡糖酸及其盐。
如上所述,通过本发明方法获得的组合物包含基于整个组合物为10-60重量%的一种或多种通式(I)的α-磺基脂肪酸二盐(A)。在优选实施方案中,所述组合物包含基于整个组合物为30-40重量%的一种或多种通式(I)的α-磺基脂肪酸二盐(A)。
在式(I)中,基团M1和M2优选为钠(Na)。
如上文所详述的那样,本发明的方法需要首先使脂肪酸与气态三氧化硫反应。在这种情况下,三氧化硫优选以1.0:1.0至1.5:1.0的SO3:脂肪酸摩尔比使用。在这种情况下,在70-95℃的储存温度下将脂肪酸引入反应器中。优选地,将磺化后获得的液态硫化产物在温度控制的后反应盘管中在该温度下保持并陈化5-20分钟。
然后将以这种方式获得的粗产物(即酸性磺化产物)部分或完全中和,优选用NaOH水溶液完全中和。
对于随后使用过氧化氢的漂白,适用上文所述的条件,即
1.pH值高于7,
2.温度为80-95℃,
3.漂白在基于整个组合物为50-500ppm的选自氧化镁、镁盐、水玻璃、次氮基三乙酸、乙二胺四乙酸、葡糖酸及其盐的稳定剂存在下进行。
优选地,首先将待漂白的含水表面活性剂组合物装入反应器中,搅拌并控制温度,并调节至所需的pH。然后,首先向含水表面活性剂组合物中添加稳定剂,该稳定剂在所选的漂白条件下防止过氧化氢突然分解,从而防止不可控制的泡沫形成和热量散发。稳定剂优选以基于整个组合物为200-400ppm的量使用。
将如此制备的初始装料用过氧化氢(H2O2)处理。此处,过氧化氢优选以市售浓度为30-70重量%,优选30-45重量%的水溶液形式使用。将过氧化氢计量加入到初始装入的表面活性剂组合物中是连续进行的,优选通过浸没在液位下方的管连续进行。特别地,对计量速率加以选择,以设定<3000ppm,优选100-1000ppm的稳态过氧化物浓度,从而确保恒定的漂白进程。
漂白优选在85-92℃的温度下进行。在漂白期间,特别地将水溶液的pH值调节为10-11.5,尤其是10.2-10.7的值。如果在漂白期间pH降低,则将其重新调节。用NaOH水溶液调节pH。在这种情况下,所用的NaOH溶液的浓度为至多50重量%,优选为至多20重量%。
组合物的用途
本发明的另一主题是可通过本发明方法获得的表面活性剂组合物在化妆品组合物以及洗涤剂和清洁剂中的用途。
就化妆品而言,此处特别优选地尤其为以洗发剂、淋浴凝胶、肥皂、合成清净剂、洗涤膏、洗液、洗擦制剂、泡沫浴,油浴、淋浴、剃须泡沫、剃须液、剃须霜和牙科护理产品(例如牙膏,漱口水等)形式存在的那些。
就清洁剂而言,此处特别优选具有低pH的用于清洁硬表面的产品,例如洗浴和WC清洁剂等,以及用于卫生设施的清洁和/或香气凝胶。
实施例
所用的物质
所用的起始物质:
未漂白的含水组合物,其包含基于天然C12/14脂肪酸(C12/14重量比为70:30)的工业级质量的α-磺基脂肪酸二钠盐;组成:水含量为46.5%,干残留物为53.5%,由α-磺基脂肪酸或(二)钠盐,C12/14脂肪酸或钠盐和硫酸钠组成,比例大约为8:1:1,pH值为5.1。
该组合物的颜色只有在进一步稀释10倍(对应于0.4重量%干残留物)后才可使用下文所述的方法进行测量,然后为330哈森。
所用的测量方法
pH:使用标准的市售pH计,直接在配制剂(即含水表面活性剂组合物)中测量pH。
颜色:将含水表面活性剂组合物用去离子水(95重量%)和异丙醇(5重量%)的混合物稀释至4%的干残留物(基于稀释溶液的总含量)。在获自Hach Lange GmbH的市售颜色测量仪(Lico 500)的11mm圆形比色杯中测定该溶液的颜色值。颜色值以哈森单位表示。
过氧化物浓度:通过半定量测试条(获自Merck的MQuant)测定过氧化物的浓度,将水稀释液调节至试纸条的测量范围内。
漂白实验的结果
表1和表2中的数据在每种情况下基于100kg的初始装料量。
表1:
在本发明的实施例1中,选择工艺条件以确保良好的受控漂白进展(参见产物颜色随处理时间而减轻,与表2对比)。在18小时后,获得了颜色非常浅的产物(88哈森)。
在对比实施例1中,选择本领域技术人员由现有技术显而易见的条件。其表明,在低于7的pH范围内,即在酸性pH范围内,即使在较高的稳态过氧化物浓度下,也无法实现可接受的漂白进展(参见产物颜色随处理时间而减轻,与表2对比)。在30小时后,产物颜色仍然太深。由于处理时间长,随后终止该实验。此外,证明所导致的泡沫形成是有问题的。
对比实施例2表明,如果不添加稳定剂,则根本无法在碱性pH范围内启动漂白。计量加入的过氧化物立即分解,从而形成极其严重的泡沫。
下表2显示了在漂白过程中作为时间函数而测得的产物颜色。在实施例1和对比实施例1中,在每种情况下首次提及的哈森值是在可测量范围内的值。
表2
Claims (16)
1.一种制备浅色含水表面活性剂组合物的方法,所述组合物包含:
·基于整个组合物为10-60重量%的一种或多种通式(I)的α-磺基脂肪酸二盐(A),
R1CH(SO3M1)COOM2 (I)
其中基团R1为具有6-18个碳原子的直链或支化烷基或烯基,基团M1和M2彼此独立地选自H、Li、Na、K、Ca/2、Mg/2、铵和链烷醇胺,
·水,
其中将通式(Ia)的脂肪酸,
R2CH2COOH (Ia)
其中基团R2为具有6-18个碳原子的直链或支化烷基或烯基,
(i)用气态三氧化硫进行磺化,
(ii)将酸性的磺化产物—任选在陈化后—中和,然后,
(iii)用过氧化氢进行漂白,其中漂白在高于7的pH下在80-95℃的温度范围内在基于整个组合物为50-500ppm的稳定剂存在下进行,所述稳定剂选自氧化镁、镁盐、水玻璃、次氮基三乙酸、乙二胺四乙酸、葡糖酸及其盐。
2.根据权利要求1的方法,其中式(I)中的基团R1为具有10-16个碳原子的饱和的直链烷基,其中对于化合物(A),情况是基于化合物(A)的总量,其中基团R1为癸基或十二烷基的化合物(A)的比例为90重量%或更高。
3.根据权利要求1或2的方法,其中基团M1和M2为钠。
4.根据权利要求1-3中任一项的方法,其中在漂白步骤(iii)中,使用氧化镁作为稳定剂。
5.根据权利要求1-4中任一项的方法,其中在漂白步骤(iii)中,稳定剂以200-400ppm的量使用。
6.根据权利要求1-5中任一项的方法,其中在漂白步骤(iii)中,将漂白步骤(iii)中的温度调节至85-92℃。
7.根据权利要求1-6中任一项的方法,其中在漂白步骤(iii)中,将pH调节至10-11.5,尤其是10.2-10.7的值。
8.根据权利要求1-6中任一项的方法,其中在漂白步骤(iii)中,将pH调节至10.2-10.7的值。
9.根据权利要求1-8中任一项的方法,其中在漂白步骤(iii)中,过氧化氢以市售浓度为30-70重量%,尤其是30-40重量%的水溶液形式使用。
10.根据权利要求1-9中任一项的方法,其中在漂白步骤(iii)中,将过氧化氢在液位下方连续计量加入到初始装入的表面活性剂组合物中。
11.根据权利要求10的方法,其中在漂白步骤(iii)中,选择过氧化氢的计量加入速率,以使得固定的过氧化物浓度设定为低于3000ppm。
12.根据权利要求10的方法,其中在漂白步骤(iii)中,选择过氧化氢的计量加入速率,以使得固定的过氧化物浓度设定为100-1000ppm。
13.可通过权利要求1-12中任一项的方法获得的表面活性剂组合物在化妆品组合物中的用途。
14.根据权利要求13的用途,其中所述化妆品组合物呈洗发剂、淋浴凝胶、肥皂、合成清净剂、洗涤膏、洗液、洗擦制剂、泡沫浴,油浴、淋浴、剃须泡沫、剃须液、剃须霜和牙科护理产品的式。
15.可通过权利要求1-12中任一项的方法获得的表面活性剂组合物在洗涤剂和清洁组合物中的用途。
16.根据权利要求15的用途,其中所述洗涤剂和清洁组合物是具有低pH值的组合物,其用于清洁硬质表面,例如洗浴和WC清洁剂等,以及用于卫生设施的清洁和/或香气凝胶。
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