CN114727933B - 多孔可溶性固体结构体 - Google Patents
多孔可溶性固体结构体 Download PDFInfo
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- CN114727933B CN114727933B CN201980102332.1A CN201980102332A CN114727933B CN 114727933 B CN114727933 B CN 114727933B CN 201980102332 A CN201980102332 A CN 201980102332A CN 114727933 B CN114727933 B CN 114727933B
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Classifications
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/88—Ampholytes; Electroneutral compounds
- C11D1/94—Mixtures with anionic, cationic or non-ionic compounds
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
- A61K8/0216—Solid or semisolid forms
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
- A61Q19/10—Washing or bathing preparations
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
- C11D17/0047—Detergents in the form of bars or tablets
- C11D17/0065—Solid detergents containing builders
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/20—Organic compounds containing oxygen
- C11D3/2003—Alcohols; Phenols
- C11D3/2065—Polyhydric alcohols
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
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- C11D3/3746—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C11D3/3753—Polyvinylalcohol; Ethers or esters thereof
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/02—Anionic compounds
- C11D1/04—Carboxylic acids or salts thereof
- C11D1/10—Amino carboxylic acids; Imino carboxylic acids; Fatty acid condensates thereof
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/02—Anionic compounds
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- C11D1/126—Acylisethionates
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/02—Anionic compounds
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- C11D1/28—Sulfonation products derived from fatty acids or their derivatives, e.g. esters, amides
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/88—Ampholytes; Electroneutral compounds
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/88—Ampholytes; Electroneutral compounds
- C11D1/90—Betaines
Abstract
本发明提供了一种多孔可溶性固体,该多孔可溶性固体可包含:羟乙磺酸盐表面活性剂;非硫酸盐阴离子表面活性剂;以及两性表面活性剂、两性离子表面活性剂或者它们的组合。
Description
技术领域
本申请涉及含有非硫酸盐表面活性剂的多孔可溶性固体结构体。
背景技术
在水溶性聚合物载体或基质中包含表面活性剂和/或其他活性成分的多孔可溶性固体结构体可用于清洁。此类片材特别用于在溶于水中时递送表面活性剂和/或其他活性成分。相比于相同产品类别的传统颗粒或液体形式,此类结构体具有较好的结构完整性,更为浓缩,并且易于储存、运送/运输、搬运和处理。最近推动不含硫酸盐的清洁剂。然而,基于硫酸盐的清洁剂传统上用于可溶性固体结构体中,并且去除它们可产生难以加工的结构体。因此,需要一种可加工的不含硫酸盐的可溶性固体结构体。
发明内容
在一个方面,本申请涉及一种多孔可溶性固体结构体,该多孔可溶性固体结构体包含:a)按所述多孔可溶性固体的重量计约20%至约50%,优选地约20%至约50%,更优选地约28%至约45%,甚至更优选地约34%至约41%的羟乙磺酸盐表面活性剂,优选地椰油酰羟乙磺酸钠、月桂酰羟甲基乙磺酸钠、或者它们的组合;b)按所述多孔可溶性固体的重量计约4%至约20%,优选地约6%至约18%,更优选地约8%至约16%,甚至更优选地约10%至约16%的非硫酸盐阴离子表面活性剂,优选地椰油酰谷氨酸钠、月桂酰谷氨酸钠、月桂醇聚氧乙烯醚磺基琥珀酸酯二钠、或者它们的组合;c)按所述固体结构体的重量计约5%至约28%,优选地约7%至约26%,更优选地约9%至约24%,甚至更优选地约11%至约22%的两性表面活性剂、两性离子表面活性剂、或者它们的组合,优选地月桂酰胺基丙基甜菜碱、椰油酰胺基丙基甜菜碱、月桂酰两性基乙酸钠、或者它们的组合;d)按所述多孔可溶性固体结构体的重量计约18%至约38%,优选地约20%至约36%,更优选地约22%至约34%,甚至更优选地约24%至约32%的聚乙烯醇;以及e)约4.5%至约20%,优选地约5.5%至约17%,更优选地约6.5%至约14%,甚至更优选地约7.5%至约11%的甘油;其中所述多孔可溶性固体结构体的密度为:约0.05g/cm3至约0.20g/cm3,优选地约0.07g/cm3至约0.18g/cm3,更优选地约0.09g/cm3至约0.16g/cm3,或甚至更优选地约0.11g/cm3至约0.14g/cm3。
在阅读以下具体实施方式时,这些和其他方面将变得更明显。
具体实施方式
定义
如本文所用,术语“柔性”是指当制品沿垂直于其纵向的中心线弯曲90°时制品承受应力而不破损或显著破裂的能力。优选地,此类制品可经历显著的弹性变形并且特征在于不大于5GPa,优选地不大于1GPa,更优选地不大于0.5GPa,最优选地不大于0.2GPa的杨氏模量。
如本文所用,术语“固体”是指当制品不受限制时并且当没有向其施加外部力时制品在20℃和大气压下基本上保持其形状(即,其形状没有任何可见变化)的能力。
可以通过如下方式来制备多孔可溶性固体结构体:首先制备包含各种材料的预混物,然后通过向其中引入气体对预混物进行充气,接着使充过气的预混物形成为片材,最终在升高的温度下对片材进行干燥。在如下同时发生的机制下,在干燥步骤期间形成多孔可溶性固体结构体:水蒸发、气泡塌陷、间隙液体从薄膜泡面层排出进入气泡间的普拉托边界(其在气泡间产生开口并形成开孔),以及预混物的固化。各种加工条件可能影响这些机理,例如湿预混物中的固体含量、湿预混物的粘度、重力和干燥温度、以及平衡此类加工条件以便实现受控排水并形成期望的多孔可溶性固体结构体的需要。
此处是多孔可溶性固体结构体的制造过程的示例。用充过气的湿预混物填充进料槽。将加热的可旋转圆筒(也称为滚筒干燥器)置于所述进料槽上方。所述加热的滚筒干燥器具有圆柱形加热的外表面,其特征在于受控的表面温度为约130℃,并且其沿顺时针方向(如带有箭头的细曲线所示)旋转以从进料槽拾取充过气的湿预混物。充过气的湿预混物在滚筒干燥器的圆柱形加热的外表面上形成薄片材,其在大约10-15分钟内旋转并干燥充过气的湿预混物的此类片材以形成多孔固体结构体。可在预混物拾取位置附近放置调平刀片以确保如此形成的片材的一致厚度,尽管可简单地通过调节充过气的湿预混物的粘度以及滚筒干燥器的旋转速度和表面温度来控制片材的厚度。一旦干燥,则可在滚筒旋转结束时手动或通过刮刀拾取多孔固体结构体。可以将多孔固体结构体的片材卷成卷子等待进一步加工。
湿预混物在变成多孔固体结构体的过程中通过非常严格的过程,并且完成的多孔固体结构体可以经受另外的加工以形成为消费者友好的产品。因此,加工预混物以形成多孔固体结构体以及加工所形成的多孔固体结构体的能力都是重要的。当从预混物配制物中去除基于硫酸盐的表面活性剂时,将这些配制物加工成多孔固体结构体以及在形成多孔固体结构体之后的加工期间存在问题。这些问题可包括例如在卷子退绕和切割期间的剥离能力、滚动能力和强度。
在评估初始非硫酸盐配制物时,发现存在一些与可加工性相关的问题。据信非硫酸盐配制物可能易于具有不良的拉伸特性,这使得预混物和/或所得的多孔固体结构体难以加工和商业化。已经发现断裂应变的拉伸特性与配制物的可加工性和扩大相关,并且特别是与在卷子退绕和纵切/切割期间的剥离能力、滚动能力和强度相关。特别地,20mm或更大的断裂应变倾向于预测将为可充分加工的产品。因此,多孔可溶性结构体的断裂应变可为例如20mm或更大、30mm或更大、或35mm或更大。
令人惊讶的是,本发明人已经发现,包含高水平的基于羟乙磺酸盐的表面活性剂(按多孔可溶性固体的重量计20%或更多)(作为主要表面活性剂)与次要阴离子辅助表面活性剂和两性/两性离子表面活性剂组合的多孔可溶性固体结构体提供了阶跃变化的拉伸强度以解决迄今为止提及的加工挑战,同时在消费者相关条件下仍然提供快速溶解特性。尽管不受理论束缚,但是假设了通过将羟乙磺酸盐表面活性剂调节到足够程度(以实现孔在充气之后干燥过程期间开口以及高弹性和拉伸强度)而平衡羟乙磺酸盐表面活性剂与次要阴离子助表面活性剂和两性/两性离子表面活性剂的结晶度允许形成可接受的多孔可溶性固体结构体。
然而,表面活性剂混合物的平衡需要一些工作。如下表1中可以看出,含有变化水平的类似表面活性剂的若干多孔固体结构体(确切的配制物在下文实施例部分中)具有大不相同的断裂应变。据信,20mm或更大的断裂应变值意味着将为可充分加工的多孔可溶性固体结构体。因此,编号为14和20-24的实施例具有不可接受的断裂应变。
表1
预混物
如上所述,多孔可溶性固体结构体开始于预混物。通常通过将所需成分混合来制备预混物。多孔可溶性固体结构体的成分可包括例如表面活性剂、水溶性聚合物、增塑剂、水等。这些将更充分地论述于下文。可使用机械混合器来形成预混物。可用于本文的机械混合器包括但不限于斜叶桨混合器或MAXBLENDTM混合器(Sumitomo Heavy Industries)。
可以调节预混物的粘度以获得最佳的可加工性。当在40℃和1s-1下测量时,它可以例如在约1,000cps至约25,000cps的范围内。在随后的干燥步骤中,预混物的粘度可对充过气的预混物的孔膨胀和孔开口具有显著影响,并且具有不同粘度的预混物可形成非常不同的泡沫结构体的柔性多孔可溶性固体片材制品。一方面,当预混物具有高于约25,000cps的粘度时,此类湿预混物的充气可能变得更加困难。更重要的是,在随后的干燥步骤期间从薄膜气泡面层到三维泡沫的平台边界的间隙液体排出可能受到不利影响或显著限制。干燥期间的间隙液体排出影响在随后的干燥步骤期间在充过气的湿预混物中的孔膨胀和孔开口。因此,如此形成的柔性多孔可溶性固体片材制品从而可具有显著较小的孔和较小的孔间互连度(即,比开孔更“闭合的”孔),这使水难以进入和溢出此类片材制品。另一方面,当预混物具有低于约1,000cps的粘度时,充过气的预混物可能不够稳定,即在充气之后并且在干燥之前,湿预混物中的气泡可能过快地破裂、塌陷或聚结。因此,所得的固体片材制品可比预期孔隙少得多且更为致密。
因此,如在40℃和1秒-1下测量的,预混物的粘度可在例如以下范围内:约1,000cps至约25,000cps、约3,000cps至约24,000cps、约5,000cps至约23,000cps、或约10,000cps至约20,000cps。可使用具有锥板几何形状(CP1/50SR3468 SS)的Malvern Kinexus Lab+流变仪、0.054mm的间隙宽度、40℃的温度和1.0倒秒的剪切速率持续360秒的时间段来测量预混物粘度值。
预混物中固体的水平也可影响可加工性。预混物中固体的水平可为例如按所述湿预混物的总重量计约15%至约70%、约20%至约50%、或约25%至约45%。固体百分含量是所有固体组分、半固体组分以及除了水和任何明显挥发性物质诸如低沸点醇之外的液体组分按总加工混合物的重量计的重量百分比之和。
在充气过程之前和/或期间在高于环境温度但低于将导致其中的组分降解的任何温度下,可将湿预混物立即预热。例如,湿预混物可保持在处于以下范围内的升高的温度下:约40℃至约100℃、约50℃至约95℃、约60℃至约90℃、或约75℃至约85℃。此外,在充气过程期间可施加附加的热以试图将预混物保持在此类升高的温度下,正如充气之前所获得的那样。这可例如经由从一个或多个表面的传导加热、注入蒸汽或其他加工装置来实现。
据信在充气步骤之前和/或期间预热湿预混物的行为可提供用于降低包括较高固体百分含量的预混物的粘度,以用于改善气泡向混合物中的引入和所期望的固体片材制品的形成。期望实现较高的固体百分含量,因为这可降低干燥所需的总体能量。因此,固体百分比的增加可能相反地导致水含量降低和粘度增加。如上所述,粘度太高的预混物是不期望的。预热可有效地抵消此类粘度增大,因此允许甚至在使用高固含量预混物时制造出快速溶解的片材制品。
还可对预混物进行充气。进行湿预混物的充气,以便将足够量的气泡引入湿预混物中,随后在干燥时在其中形成多孔可溶性固体结构体。一旦充分充气,预混物的特征在于密度低于未充过气的预混物(其可能包含一些无意中滞留的气泡)或未充分充过气的湿预混物(其中可能包含一些气泡但体积百分比低得多且气泡尺寸显著更大)的密度。充过气的湿预混物具有在例如以下范围内的密度:约0.05g/ml至约0.5g/ml、约0.08g/ml至约0.4g/ml、约0.1g/ml至约0.35g/ml、约0.15g/ml至约0.3g/ml、或约0.2g/ml至约0.25g/ml。
充气可通过物理或化学方法来实现。例如,它可通过机械搅拌将气体引入预混物中来实现,例如,通过使用任何合适的机械加工装置,包括但不限于:转子定子混合器、行星式混合器、加压混合器、非加压混合器、间歇混合器、连续混合器、半连续混合器、高剪切混合器、低剪切混合器、浸没式分布器、或者它们的任何组合。它可经由化学方法来实现,例如,通过使用化学发泡剂经由一种或多种成分的化学反应提供原位气体形成,包括通过泡腾体系形成二氧化碳(CO2气体)。
充过气的预混物的气泡尺寸有助于实现所得固体片材制品的多孔可溶性固体结构体中的均匀层。充过气的预混物的气泡尺寸可为例如约5至约100微米或约20微米至约80微米。气泡尺寸的均匀性导致所得多孔可溶性固体结构体具有一致密度。
片材形成
在充分充气之后,充过气的预混物可形成具有相对的第一侧和第二侧的一个或多个片材。片材形成步骤可以任何合适的方式进行,例如通过挤出、浇铸、模塑、真空形成、压制、印刷、涂覆等。更具体地,充过气的预混物可通过以下而形成为片材:(i)将其浇铸到浅腔或托盘或特殊设计的片材模具中;(ii)将其挤出到干燥器的连续带或筛网上;(iii)将其涂覆到旋转滚筒干燥器的外表面上。其上形成有片材的支撑表面可由以下材料形成或涂覆有以下材料:抗腐蚀材料、不相互作用和/或不粘附的材料,诸如金属(例如,钢、铬等)、聚碳酸酯、/>HDPE、LDPE、橡胶、玻璃等。合适的制造方法的示例可见于例如CN2019/071751;WO2012138820;和WO2010077627中,这些专利均以引用方式并入本文。
充过气的湿预混物的形成片材(即,多孔固体可溶性结构体)可具有在例如以下范围内的厚度:0.5mm至4mm、0.6mm至3.5mm、0.7mm至3mm、0.8mm至2mm、或0.9mm至1.5mm。控制充过气的预混物的此类形成片材的厚度对于确保所得固体片材制品具有期望的开孔结构体可能是重要的。如果形成的片材太薄(例如,厚度小于0.5mm),则滞留于充过气的预混物中的许多气泡将在后续干燥步骤期间膨胀,以形成延伸穿过所得固体片材制品的整个厚度的通孔。此类通孔如果过多则可能显著损害片材制品的总体结构完整性和美学外观。如果形成的片材太厚,则不仅将花费更长时间来干燥,而且还会使固体片材制品在不同区域(例如,顶部、中间和底部区域)之间沿其厚度具有更大的孔尺寸变化。干燥时间越长,可以通过气泡破裂/塌陷/聚结、液体排出、孔膨胀、孔开口、水蒸发等发生更多不平衡的力。此外,相对较薄片材的多个层可组装成较大厚度的三维结构,以递送期望的清洁有益效果或其他有益效果,同时仍然提供令人满意的快速溶解的孔结构并且确保在相对较短的干燥时间内有效的干燥。
干燥
多孔可溶性固体结构体可以在本领域中任何合适的方式干燥。在干燥期间,所述方法可包括在整个干燥时间或至少一半干燥时间中使用反重力加热方向。不受任何理论的束缚,据信此类反重力加热方向可在干燥步骤期间减少或抵消朝向形成的片材的底部区域的过量间隙液体排出。此外,因为顶部表面最后被干燥,所以允许更长的时间使形成的片材的顶表面附近的空气气泡膨胀并在顶部表面上形成孔开口(因为一旦湿基质干燥,空气气泡就不再能够膨胀或形成表面开口)。因此,通过用此类反重力加热干燥形成的多孔可溶性固体结构体的特征在于改善的开孔结构体,其可实现更快的溶解以及其他意料之外的有益效果。反重力加热可以例如由旋转滚筒、基于传导的加热装置等提供。
干燥过程还可包括使用加热的可旋转圆筒。常用于滚筒干燥中的加热的可旋转圆筒可在内部例如通过蒸汽或电加热,并且可例如通过安装在底座支架上的电动驱动器以预定的旋转速度旋转。加热的可旋转圆筒或滚筒可具有在例如以下范围内的外径:约0.5米至约10米、约1米至约5米、或约1.5米至约2米。其可具有例如约80℃至约170℃、约90℃至约150℃、或约100℃至约140℃的受控表面温度。此外,此类加热的可旋转圆筒可以例如约0.005rpm至约0.25rpm、约0.05rpm至约0.2rpm、或约0.1rpm至约0.18rpm的速度旋转。
所述加热的可旋转圆筒可在其外表面上涂覆有不粘涂层。不粘涂层可覆盖在加热的可旋转滚筒的外表面上,或者它可固定到加热的可旋转滚筒的外表面的介质。介质包括但不限于耐热非织造织物、耐热碳纤维、耐热金属或非金属网等。不粘涂层可有效地保持片状制品的结构完整性在片材形成过程期间免受损坏。
还可设置进料机构,用于将如上所述的充过气的原材料预混物加入到加热的可旋转滚筒上,从而在加热的可旋转滚筒的外表面上形成粘性预混物的薄层。因此,预混物的此类薄层经由接触加热/干燥由加热的可旋转滚筒干燥。进料机构包括例如进料槽,而所述进料槽具有安装在其上的至少一个或多个进料料斗、用于动态观察进料的成像装置、以及用于调节进料料斗的位置和倾斜角度的调节装置。通过使用所述调节装置来调节所述进料料斗和加热的可旋转滚筒的外表面之间的距离,可满足对形成的片状制品的不同厚度的需要。调节装置还可用于将进料料斗调节到不同的倾斜角度以便满足速度和质量的材料要求。
还可以存在静态刮擦机构,用于刮擦或铲起已经由加热的可旋转滚筒形成的多孔可溶性固体结构体。静态刮擦机构可安装在例如底座支架上或其一侧上,用于将已经形成的多孔可溶性固体结构体向下游输送以用于进一步加工。静态刮擦机构可自动或手动地移动靠近并远离加热的可旋转滚筒。
多孔可溶性固体结构体制品的制备方法如下。首先,在底座支架上具有不粘涂层的加热的可旋转滚筒由电动驱动器驱动。接下来,调节装置调节进料机构,使得进料料斗和加热的可旋转滚筒的外表面之间的距离达到预设值。同时,进料料斗将包含用于制备多孔可溶性固体结构体的全部或一些原材料的充过气的预混物加入到加热的可旋转滚筒的外表面上,以在其上形成具有期望厚度的所述充过气的预混物的薄层。任选地,加热罩的抽吸装置抽吸由加热的可旋转滚筒产生的热蒸汽。接着,静态刮擦装置刮擦/铲起充过气的湿预混物的薄层由加热可旋转圆筒以相对较低温度(例如130℃)干燥之后所形成的经干燥/固化片材制品。经干燥/固化片材制品也可手动或自动地剥离而无需此类静态刮擦机构,然后通过滚棒卷起。
总干燥时间取决于预混物中的配制物和固体含量、干燥温度、热能流入量和待干燥的多孔可溶性固体结构体的厚度。干燥时间可为例如约1分钟至约60分钟、约2分钟至约30分钟、约2至约15分钟、约2至约10分钟、或约2至约5分钟。
在此类干燥时间期间,加热方向可被布置成使得其基本上与重力方向相反持续大于一半的干燥时间,持续大于55%或60%的干燥时间(例如,如在上文所述的基于旋转滚筒的加热/干燥装置中),或持续大于75%或甚至100%的干燥时间(例如,如在基于底部传导的加热/干燥装置中)。此外,充过气的湿预混物的片材可在第一加热方向下干燥第一持续时间,并且然后在第二持续时间下在第二相反加热方向下干燥,而第一加热方向基本上与重力方向相反。加热方向的此类变化可通过本文未示出的各种其它装置容易地实现,例如,通过蛇形形状的细长加热带,其可沿纵向中心轴线旋转。
多孔可溶性固体片材制品的特征还可在于以下中的一个或多个:
·约85%至100%或约90%至100%的开孔百分含量;
·约150μm至约1000μm、或约200μm至约600μm的总体平均孔尺寸;
·约5μm至约200μm、约10μm至约100μm、或约10μm至约80μm的平均孔壁厚度;
·按所述多孔可溶性固体结构体的重量计约0.5%至约25%、约1%
至约20%、或约3%至约10%的最终含水量;
·在以下范围内的厚度:约0.6mm至约3.5mm、约0.7mm至约3mm、约0.8mm至约2mm、或约1mm至约1.5mm;
·约50克/m2至约250克/m2、约80克/m2至约220克/m2、或约100克/m2至约200克/m2的基重;
·约0.05克/cm3至约0.5克/cm3、约0.06克/cm3至约0.4克/cm3、约0.07克/cm3至约0.2克/cm3、或约0.08克/cm3至约0.15克/cm3的密度;以及
·约0.03m2/g至约0.25m2/g、约0.04m2/g至0.22m2/g、约0.05
m2/g至约0.2m2/g、或约0.1m2/g至约0.18m2/g的比表面积。
配制物
如本文所述的多孔可溶性固体结构体可以含有例如表面活性剂、水溶性聚合物、增塑剂、添加剂等。多孔可溶性固体结构体可包含例如按多孔可溶性固体结构体的重量计约25%至约80%、约40%至约70%的总表面活性剂。它还可包含按多孔可溶性固体结构体的重量计约10%至约40%的水溶性聚合物。多孔可溶性结构体还可包含多个层。这些层可以由例如多孔可溶性固体结构体的单层组成。例如,单层多孔可溶性结构体可以呈任何适用的形式,例如片材。多孔可溶性结构体也可为柔性的。多孔可溶性固体结构体可例如用作皮肤清洁剂。多孔可溶性固体结构体可为开孔泡沫。
表面活性剂
表面活性剂可在充气过程期间用作乳化剂,以产生足以形成期望的开孔结构体的量的稳定气泡。表面活性剂也可用作递送期望的清洁有益效果的活性成分。多孔可溶性固体结构体可包含例如羟乙磺酸盐表面活性剂、非硫酸盐阴离子表面活性剂、两性表面活性剂、两性离子表面活性剂、或两性和两性离子表面活性剂的组合。
羟乙磺酸盐表面活性剂可以按多孔可溶性固体的重量计约20%至约50%、约22%至约50%、约28%至约45%、约31%至约41%、约34%至约41%、约38%至约41%、约20%至约30%、约21%至约25%的水平存在。羟乙磺酸盐表面活性剂可包括例如椰油酰羟乙磺酸钠、月桂酰羟甲基乙磺酸钠、或者它们的组合。在一个示例中,多孔可溶性固体结构体包含按重量计约15%至约32%的月桂酰羟甲基乙磺酸钠;和按重量计约7%至约25%的椰油酰羟乙磺酸钠。在另一个示例中,多孔可溶性固体结构体包含按重量计约21%至约25%的椰油酰羟乙磺酸钠。
非硫酸盐阴离子表面活性剂包括不含硫酸盐的阴离子表面活性剂。非硫酸盐阴离子表面活性剂可以按多孔可溶性固体结构体的重量计约4%至约25%、约6%至约18%、约7%至约18%、约7%至约17%、约8%至约16%、约10%至约16%、约14%至约17%、约15%至约25%、或约22%至约25%的水平存在。非硫酸盐阴离子表面活性剂可包括月桂酰肌氨酸钠、月桂基肌氨酸、椰油酰肌氨酸、月桂酰谷氨酸钠、椰油酰谷氨酸钠、月桂基磺基琥珀酸二钠、月桂醇聚氧乙烯醚磺基琥珀酸酯二钠、椰油酰牛磺酸钠、月桂酰牛磺酸钠、月桂酰乳酸钠、椰油酰乳酸钠、月桂酰甘氨酸钠、椰油酰甘氨酸钠、以及它们的组合。非硫酸盐阴离子表面活性剂的子集可包括例如椰油酰谷氨酸钠、月桂酰谷氨酸钠、月桂醇聚氧乙烯醚磺基琥珀酸酯二钠、或者它们的组合。
两性和/或两性离子表面活性剂可以按多孔固体结构体的重量计约5%至约28%、约7%至约26%、约9%至约24%、约11%至约22%、约7%至约18%、约7%至约17%、约14%至约17%、约15%至约25%、或约22%至约25%的水平存在。适于在本文中使用的两性辅助表面活性剂包括被描述为脂族仲胺和叔胺的衍生物的那些表面活性剂,其中脂族基团可为直链或支链,并且其中脂族取代基中的一个含有约8至约18个碳原子,并且一个脂族取代基含有阴离子基团,诸如羧基、磺酸根、硫酸根、磷酸根或膦酸根。合适的两性表面活性剂包括但不限于选自以下的那些:椰油基氨基丙酸钠、椰油基氨基二丙酸钠、椰油酰两性基乙酸钠、椰油酰两性基羟丙基磺酸钠、椰油酰两性基丙酸钠、玉米油酰两性基丙酸钠、月桂氨基丙酸钠、月桂酰两性基乙酸钠、月桂酰两性基羟丙基磺酸钠、月桂酰两性基丙酸钠、玉米油酰两性基丙酸钠、月桂亚氨基二丙酸钠、椰油基氨基丙酸铵、椰油基氨基二丙酸铵、椰油酰两性基乙酸铵、椰油酰两性基羟丙基磺酸铵、椰油酰两性基丙酸铵、玉米油酰两性基丙酸铵、月桂氨基丙酸铵、月桂酰两性基乙酸铵、月桂酰两性基羟丙基磺酸铵、月桂酰两性基丙酸铵、玉米油酰两性基丙酸铵、月桂亚氨基二丙酸铵、椰油基氨基丙酸三乙醇胺、椰油基氨基二丙酸三乙醇胺、椰油酰两性基乙酸三乙醇胺、椰油酰两性基羟丙基磺酸三乙醇胺、椰油酰两性基丙酸三乙醇胺、玉米油酰两性基丙酸三乙醇胺、月桂氨基丙酸三乙醇胺、月桂酰两性基乙酸三乙醇胺、月桂酰两性基羟丙基磺酸三乙醇胺、月桂酰两性基丙酸三乙醇胺、玉米油酰两性基丙酸三乙醇胺、月桂亚氨基二丙酸三乙醇胺、椰油酰两性基二丙酸、癸酰两性基二乙酸二钠、癸酰两性基二丙酸二钠、辛酰两性基二乙酸二钠、辛酰两性基二丙酸二钠、椰油酰两性基羧乙基羟丙基磺酸二钠、椰油酰两性基二乙酸二钠、椰油酰两性基二丙酸二钠、二羧乙基椰油基丙二胺二钠、月桂基聚氧乙烯醚-5羧基两性基二乙酸二钠、月桂亚氨基二丙酸二钠、月桂酰两性基二乙酸二钠、月桂酰两性基二丙酸二钠、油基两性基二丙酸二钠、PPG-2-异癸醇聚醚-7羧基两性基二乙酸二钠、月桂基氨基丙酸、月桂酰两性基二丙酸、月桂基氨丙基甘氨酸、月桂基二亚乙基二氨基甘氨酸、以及它们的混合物
两性辅助表面活性剂可为符合以下结构的表面活性剂:
其中R12为选自以下的C-连接的一价取代基:包含9至15个碳原子的取代的烷基体系、包含9至15个碳原子的未取代的烷基体系、包含9至15个碳原子的直链烷基体系、包含9至15个碳原子的支链烷基体系、以及包含9至15个碳原子的不饱和烷基体系;R13、R14和R15各自独立地选自:包含1至3个碳原子的C-连接的二价直链烷基体系和包含1至3个碳原子的C-连接的二价支链烷基体系;并且M+为一价抗衡离子,该一价抗衡离子选自钠、铵和质子化三乙醇胺。合适的两性表面活性剂的一个子集包括椰油酰两性基乙酸钠、椰油酰两性基二乙酸钠、月桂酰两性基乙酸钠、月桂酰两性基二乙酸钠、月桂酰两性基乙酸铵、椰油酰两性基乙酸铵、月桂酰两性基乙酸三乙醇胺、椰油酰两性基乙酸三乙醇胺、以及它们的混合物。
多孔可溶性固体结构体可包含两性离子表面活性剂,其中两性离子表面活性剂为脂族季铵、磷和硫化合物的衍生物,其中脂族基团可为直链或支链,并且其中脂族取代基中的一个含有约8至约18个碳原子,并且一个脂族取代基含有阴离子基团,诸如羧基、磺酸根、硫酸根、磷酸根或膦酸根。两性离子表面活性剂可选自由以下组成的组:椰油酰胺基乙基甜菜碱、椰油酰胺基丙基氧化胺、椰油酰胺基丙基甜菜碱、椰油酰胺基丙基二甲基氨基羟丙基水解胶原、椰油酰胺基丙基二甲基铵羟丙基水解胶原、椰油酰胺基丙基羟基磺基甜菜碱、椰油甜菜碱酰胺基两性基丙酸盐、椰油基甜菜碱、椰油基羟基磺基甜菜碱、椰油基/油基酰胺基丙基甜菜碱、椰油基磺基甜菜碱、月桂酰胺基丙基甜菜碱、月桂基甜菜碱、月桂基羟基磺基甜菜碱、月桂基磺基甜菜碱、以及它们的混合物。合适的两性离子表面活性剂为月桂基羟基磺基甜菜碱。两性离子表面活性剂可选自:月桂基羟基磺基甜菜碱、椰油酰胺基丙基羟基磺基甜菜碱、椰油基甜菜碱、椰油基羟基磺基甜菜碱、椰油基磺基甜菜碱、月桂基甜菜碱、月桂基磺基甜菜碱、以及它们的混合物。
两性和/或两性离子表面活性剂的子集可包括例如月桂酰胺基丙基甜菜碱、椰油酰胺基丙基甜菜碱、月桂酰两性基乙酸钠、椰油酰两性基乙酸钠、或者它们的组合。
水溶性聚合物
多孔可溶性固体结构体可包含例如按多孔可溶性固体结构体的重量计约18%至约38%、约22%至约34%、或约24%至约32%的量的水溶性聚合物。
本文中合适的水溶性聚合物可选自例如重均分子量在以下范围内的那些:约50,000至约400,000道尔顿、约60,000至约300,000道尔顿、约70,000至约200,000道尔顿、或约80,000至约150,000道尔顿。通过计算每种聚合物原材料的重均分子量与它们相应的按多孔可溶性固体结构体内存在的聚合物总重量计的相对重量百分比的乘积的和来计算重均分子量。本文所用水溶性聚合物的重均分子量可影响湿预混物的粘度,其可继而影响充气步骤期间的气泡数量和尺寸以及干燥步骤期间的孔扩张/打开结果。此外,水溶性聚合物的重均分子量可影响湿预混物的总体成膜特性以及其与特定表面活性剂的相容性/不相容性。
可用于本文的水溶性聚合物可包括但不限于合成聚合物,包括聚乙烯醇、聚乙烯吡咯烷酮、聚环氧烷、聚丙烯酸酯、己内酰胺、聚甲基丙烯酸酯、聚甲基丙烯酸甲酯、聚丙烯酰胺、聚甲基丙烯酰胺、聚二甲基丙烯酰胺、聚乙二醇一甲基丙烯酸酯、丙烯酸和丙烯酸甲酯的共聚物、聚氨酯、聚羧酸、聚乙酸乙烯酯、聚酯、聚酰胺、聚胺、聚乙烯亚胺、马来酸/(丙烯酸酯或甲基丙烯酸酯)共聚物、甲基乙烯基醚与马来酸酐的共聚物、乙酸乙烯酯与巴豆酸的共聚物、乙烯吡咯烷酮与乙酸乙烯酯的共聚物、乙烯吡咯烷酮与己内酰胺的共聚物、乙烯吡咯烷酮/乙酸乙烯酯共聚物、阴离子、阳离子和两性单体的共聚物、以及它们的组合。
水溶性聚合物还可选自源自天然的聚合物,包括植物源的那些,其示例包括刺梧桐树胶、黄蓍胶、阿拉伯树胶、乙酰吗喃、魔芋葡苷聚糖、金合欢胶、达瓦树胶、乳清分离蛋白、和大豆分离蛋白;种子提取物,包括瓜尔胶、刺槐豆胶、温柏树籽和车前籽;海藻提取物诸如角叉菜胶、海藻酸盐和琼脂;果实提取物(果胶);微生物源的那些,包括黄原胶、结冷胶、普鲁兰、透明质酸、硫酸软骨素和葡聚糖;和动物源的那些,包括酪蛋白、胶质、角蛋白、角蛋白水解产物、磺基角蛋白、白蛋白、胶原、谷蛋白、高血糖素、谷胶、玉米蛋白和紫胶。
改性的天然聚合物也可用作水溶性聚合物。适宜的改性天然聚合物包括但不限于,纤维素衍生物如羟丙基甲基纤维素、羟甲基纤维素、羟乙基纤维素、甲基纤维素、羟丙基纤维素、乙基纤维素、羧甲基纤维素、乙酸邻苯二甲酸纤维素、硝化纤维以及其他纤维素醚/酯;和瓜尔胶衍生物诸如羟丙基瓜尔胶。
水溶性聚合物还可包括淀粉。如本文所用,术语“淀粉”包括天然存在和改性的淀粉。淀粉的典型天然来源可包括谷物、块茎、根、豆类和水果。更具体的天然来源可包括玉米、豌豆、马铃薯、香蕉、大麦、小麦、稻米、西米、苋属植物、木薯、竹芋、美人蕉、高粱、以及它们的蜡质或高淀粉酶品种。天然淀粉可通过本领域已知的任何改性方法进行改性,以形成改性的淀粉,包括物理改性的淀粉,诸如剪切淀粉或热抑制淀粉;化学改性的淀粉,诸如已被交联、乙酰化和有机酯化、羟乙基化和羟丙基化、磷酸化、以及无机酯化的那些,其阳离子、阴离子、非离子、两性和两性离子衍生物,以及其琥珀酸盐和取代的琥珀酸盐衍生物;由淀粉中的任一种衍生的转化产品,包括通过氧化、酶转化、酸性水解、加热或酸性糊精化制备的流体淀粉或稀糊淀粉,经热处理和/或剪切的产品也可用于本文;以及本领域已知的预胶凝淀粉。
水溶性聚合物的可用子集可包括聚乙烯醇、聚乙烯吡咯烷酮、聚环氧烷、淀粉和淀粉衍生物、普鲁兰、胶质、羟丙基甲基纤维素、甲基纤维素、羧甲基纤维素、或者它们的组合。甚至另外的子集包括聚乙烯醇、羟丙基甲基纤维素、或者它们的组合。
可用于本文的聚乙烯醇可包括特征在于水解度在以下范围内的那些:约40%至约100%、约50%至约95%、约70%至约92%、或约80%至约90%。可商购获得的聚乙烯醇可包括以SELVOLTM商品名得自Celanese Corporation(Texas,USA)的那些,包括但不限于SELVOLTM 523、SELVOLTM 530、SELVOLTM 540、SELVOLTM 518、SELVOLTM 513、SELVOLTM 508、SELVOLTM 504;以和POVALTM商标名得自Kuraray Europe GmbH(Frankfurt,Germany)的那些;和PVA 1788(也称为PVA BP17),可从包括Lubon Vinylon Co.(Nanjing,China)的各种供应商商购获得;以及它们的组合。多孔可溶性固体结构体可包含例如按此类制品的总重量计约10%至约25%、或约15%至约23%的聚乙烯醇,该聚乙烯醇具有在80,000至约150,000道尔顿范围内的重均分子量和在约80%至约90%范围内的水解度。
单一淀粉或淀粉组合能够以降低所需的水溶性聚合物总体水平的量用作填充材料,只要这有助于提供具有所需结构体和如本文所述物理/化学特性的多孔可溶性固体结构体。然而,过多的淀粉可包括片材制品的溶解度和结构完整性。淀粉可以例如按所述多孔可溶性固体结构体的重量计不超过20%、0%至约10%、0%至5%、或0%至1%的水平存在。
增塑剂
增塑剂可以按所述多孔可溶性固体结构体的总重量计在约4.5%至约20%、约5.5%至约17%、约6.5%至约14%、7.5%至11%范围内的量存在于多孔可溶性固体结构体中。用于本文中的合适的增塑剂包括例如多元醇、共聚多元醇、多元羧酸、聚酯、聚二甲基硅氧烷共聚多元醇、以及它们的组合。
可用的多元醇的示例包括但不限于:甘油、双甘油、乙二醇、聚乙二醇(尤其是200-600)、丙二醇、丁二醇、戊二醇、甘油衍生物(诸如丙氧基化甘油)、缩水甘油、环己烷二甲醇、己二醇、2,2,4-三甲基戊烷-1,3-二醇、季戊四醇、脲、糖醇(诸如山梨糖醇、甘露糖醇、乳糖醇、木糖醇、麦芽糖醇和其他一元醇和多元醇)、单聚糖、二聚糖和低聚糖(诸如果糖、葡萄糖、蔗糖、麦芽糖、乳糖、高果糖玉米糖浆固体和糊精)、抗坏血酸、山梨酸盐、乙烯双甲酰胺、氨基酸、以及它们的组合。
多元羧酸的示例包括但不限于柠檬酸、马来酸、琥珀酸、聚丙烯酸、聚马来酸、以及它们的组合。
合适的聚酯的示例包括但不限于三乙酸甘油酯、乙酰化甘油一酯、邻苯二甲酸二乙酯、柠檬酸三乙酯、柠檬酸三丁酯、柠檬酸乙酰基三乙酯、柠檬酸乙酰基三丁酯、以及它们的组合。
合适的聚二甲基硅氧烷共聚多元醇的示例包括但不限于PEG-12聚二甲基硅氧烷、PEG/PPG-18/18聚二甲基硅氧烷、PPG-12聚二甲基硅氧烷、以及它们的组合。
其它合适的增塑剂包括但不限于邻苯二甲酸烷基酯和邻苯二甲酸烯丙基酯;萘酯;乳酸盐(例如钠盐、铵盐和钾盐);脱水山梨糖醇聚氧乙烯醚-30;脲;乳酸;吡咯烷酮羧酸钠(PCA);透明质酸钠或透明质酸;可溶的胶原;改性蛋白;L-谷氨酸单钠;α和β-羟基酸,诸如乙醇酸、乳酸、柠檬酸、马来酸和水杨酸;聚甲基丙烯酸甘油酯;聚合物增塑剂,诸如聚季铵盐;蛋白质和氨基酸,诸如谷氨酸、天冬氨酸和赖氨酸;氢淀粉水解产物;其它低分子量酯(例如C2-C10醇和酸的酯);以及食品和塑料工业领域技术人员已知的任何其它水可溶的增塑剂;以及它们的混合物。
增塑剂的可用子集包括甘油、乙二醇、聚乙二醇、丙二醇、以及它们的混合物。在本文中,甘油是最常用的增塑剂。
附加成分
除上述成分例如水溶性聚合物、表面活性剂和增塑剂之外,多孔可溶性固体结构体可根椐其预期应用而包含一种或多种附加成分。此类一种或多种附加成分可包括例如个人清洁活性物质。此类成分还可用于帮助多孔可溶性固体结构体的配制和/或美观性,例如pH调节剂、着色剂、香料等。
多孔可溶性固体结构体还可包含已知用于或可用于多孔可溶性固体结构体中的其他任选成分,前提条件是此类任选物质与本文描述的所选择的基本物质相容,或不会不适当地削弱产品的性能。
多层多孔可溶性固体结构体
一旦形成多孔可溶性固体结构体,就可以进一步组合和/或处理两个或更多个此类片材以形成任何期望三维形状(包括但不限于:球形、立方形、矩形、椭圆形、圆柱形、杆、片材、花形、扇形、星形、圆盘形等)的多层多孔可溶性固体结构体。可通过本领域已知的任何方法将片材组合和/或处理,该方法的示例包括但不限于化学方法、机械方法、以及它们的组合。此类组合和/或处理步骤在此统称为“转化”过程,即,其用于将两个或更多个多孔可溶性固体结构体转化为具有期望三维形状的多层多孔可溶性固体结构体。
常规的可溶性固体制品具有相对较高的长度/宽度与厚度比率,即它们相对较薄,从而确保此类制品在水中较快溶解。因此,此类可溶性固体制品通常以相对较大但较薄的片材产品形式提供,这可能难以处理(例如,太软且易于粘在一起并且难以在使用时分开)并且对于消费者不美观。然而,由于溶解需求所赋予的约束,存在很少或不存在此类产品形式的变化或改善空间。
然而,通过将多孔可溶性固体结构体的多个层堆叠在一起而形成的多层多孔固体结构体可以比具有相同纵横比的单层固体结构体更可溶。这允许此类多层固体结构体沿厚度方向显著延伸,以产生易于处理且对于消费者更美观的三维产品形状(例如,厚垫或甚至立方体形式的产品)。
通过将多孔可溶性固体结构体的多个层堆叠而形成的多层多孔可溶性固体结构体的特征可在于最大尺寸D和最小尺寸z(该最小尺寸垂直于最大尺寸),而D/z的比率(下文也称为“纵横比”)在1至约10、约1.4至约9、约1.5至约8、或约2至约7的范围内。需注意,当纵横比为1时,可溶性固体制品具有球形形状。当纵横比为约1.4时,可溶性固体制品具有立方体形状。
多层多孔可溶性固体结构体可具有例如约3mm至约20cm、约4mm至约10cm、或约5mm至约30mm的最小尺寸z。
上述多层多孔可溶性固体结构体可包含例如约2个至约60个、约4个至约50个、约5个至约40个、或约6个至约30个单层多孔可溶性结构体。
多层可溶性固体结构体可包含不同颜色的多孔可溶性固体结构体,其可从此类多层多孔可溶性固体结构体的外表面(例如,一个或多个侧表面)可见。此类不同颜色的可见片材可在美学上令消费者愉悦。此外,不同颜色可提供指示包含在单独片材中的不同有益剂的视觉提示。例如,多层多孔可溶性固体结构体可包含具有第一颜色并包含第一有益剂的第一片材和具有第二颜色并包含第二有益剂的第二片材,而第一颜色提供指示第一有益剂的视觉提示,并且第二颜色提供指示第二有益剂的视觉提示。
此外,一种或多种功能性成分可“夹在”如上所述的多层多孔可溶性固体结构体的单独片材之间,例如通过喷雾、喷洒、撒粉、涂覆、散布、浸渍、注射或甚至气相沉积。为了避免此类功能性成分与单独片材周边附近的切割密封或边缘密封的干扰,功能性成分可位于两个相邻片材之间的中心区域内,该区域被限定为与此类相邻片材的周边间隔开的距离是最大尺寸D的至少10%。
测试方法
A)平均孔径的确定
使用Hitachi TM3000台式显微镜(S/N:123104-04)获取样品的SEM显微照片。多孔可溶性固体结构体的样品的面积为大约1cm×1cm,并从较大的片材上切下。以50倍的放大率收集图像,并且在15kV下操作该单元。从每个样品上的随机选择的位置收集最少5个显微照片图像,从而得到大约43.0mm2的总分析面积,估计每个样品上的平均孔径。
然后首先使用Matlab中的图像分析工具箱处理SEM显微照片。如果需要,图像将转换为灰度。对于给定图像,使用“imhist”Matlab函数生成每个单一像素的强度值的直方图。通常,从此类直方图中,两个独立分布是明显的,对应于较亮的片材表面的像素和孔内的较暗区域的像素。选择阈值,对应于这两个分布的峰值之间的强度值。然后将具有低于该阈值的强度值的所有像素设定为强度值0,而将具有更高强度值的像素设定为1,从而产生二进制黑白图像。然后使用ImageJ(https://imagej.nih.gov,版本1.52a)分析二元图像,以检查孔面积分数和孔尺寸分布两者。每个图像的比例尺用于提供像素/mm比例因子。对于分析,使用自动阈值处理和分析粒子函数来隔离每个孔。分析函数的输出包括总体图像的面积分数以及检测到的每个单独孔的孔面积和孔周长。
平均孔径被定义为DA50:50%的总孔面积由具有与DA50平均直径相等或更小的水力直径的孔组成。
水力直径=“4*孔面积(m2)/孔周长(m)”。
它是一个等效直径,计算出的孔并非都是圆形的。
B)区域平均孔尺寸和平均孔壁厚度的确定
孔隙率是空隙空间与由多孔可溶性固体结构体占据的总空间之间的比率。经由阈值来分割空隙空间并确定空隙体素与总体素的比率,可从μCT扫描计算孔隙率。类似地,固体体积分数(SVF)是固体空间与总空间之间的比率,并且SVF可被计算为所占据的体素与总体素的比率。孔隙率和SVF两者为平均标量值,其不提供结构信息,诸如多孔可溶性固体结构体高度方向上的孔尺寸分布或多孔可溶性固体结构体撑条的平均孔壁厚度。
为了表征多孔可溶性固体结构体的3D结构,使用能够以高各向同性空间分辨率获取数据集的μCT X射线扫描仪器对样品成像。合适的仪器的一个示例是SCANCO系统模型50μCT扫描仪(Scanco Medical AG,Brüttisellen,Switzerland),其以以下设定操作:在133μA下45kVp的能量水平;3000个投影;15mm视野;750ms积分时间;平均为5;以及每像素3μm的体素大小。在扫描和随后的数据重建完成之后,扫描仪系统创建一个16位数据集,称为ISQ文件,其中灰度级反映x射线衰减的变化,而x射线衰减继而与材料密度有关。然后使用比例因子将ISQ文件转换为8位。
扫描的样品通常通过冲压直径为大约14mm的芯来制备。将冲头平放在低衰减泡沫上,并且然后安装在15mm直径的塑料圆柱形管中进行扫描。获取样本的扫描,使得所有安装的切割样本的整个体积包括在数据集中。从这个较大的数据集中,从扫描的样品的总横截面中提取样品数据集的较小子体积,创建3D数据板,其中可定性评估孔而没有边缘/边界效应。
为了表征高度方向上的孔径分布和撑条尺寸,在子体积数据集上实施局部厚度图算法或LTM。LTM方法以欧几里德距离映射(EDM)开始,该映射指定灰度级值等于每个空体素距其最近边界的距离。基于EDM数据,表示孔的3D空隙空间(或表示撑条的3D实体空间)被镶嵌成尺寸与EDM值匹配的球体。由球体包围的体素被指定为最大球体的半径值。换句话说,每个空体素(或撑条的实体素)被指定最大球体的径向值,其既适合空隙空间边界(或撑条的实体空间边界)并且包括指定的体素。
来自LTM数据扫描的3D标记球体分布输出可被视为高度方向(或Z方向)上的二维图像的堆叠,并且用于估计作为样品深度的函数的从切片到切片的球体直径的变化。将撑条厚度视为3D数据集,并且可评估子体积的全部或部分的平均值。可使用来自ThermoFisher Scientific的AVIZO Lite(9.2.0)和来自Mathworks的MATLAB(R2017a)进行计算和测量。
C)开孔百分含量
经由气体测比重法测量开孔百分含量。气体测比重法是使用气体置换方法精确测定体积的常见分析技术。使用惰性气体如氦气或氮气作为置换介质。将多孔可溶性固体结构体的样品密封于已知体积的仪器隔室中,导入适当的惰性气体,然后膨胀至另一个精确的内部体积。测量膨胀前后的压力,并且用于计算样品的体积。
ASTM标准测试方法D2856使用较老的空气对比比重计模型,提供了测定开孔百分比的程序。该装置已不再制造。然而,通过执行使用Micromeritics的AccuPyc比重计的测试能够方便且精确地测定开孔百分比。ASTM程序D2856描述了用于测定泡沫材料开孔百分比的5种方法(A、B、C、D和E)。就这些实验而言,可使用氮气与ASTM foampyc软件,采用Accupyc1340来分析样品。ASTM程序中的方法C用于计算开孔百分比。该方法简单地将如使用厚度和标准体积计算测得的几何体积与如由Accupyc测得的开孔体积进行比较,根据以下等式:
开孔百分比=样品的开孔体积/样品的几何体积*100
推荐由Micromeritics Analytical Services,Inc.(One Micromeritics Dr,Suite 200,Norcross,GA 30093)进行这些测量。与该技术相关的更多信息可见于Micromeritics Analytical Services网站(www.particletesting.com或www.micromeritics.com),或公布于Clyde Orr和Paul Webb的“Analytical Methods inFine particle Technology”中。
D)最终含水量
通过使用Mettler Toledo HX204水分分析仪(S/N B706673091)获得多孔可溶性固体结构体的最终含水量。将最少1g的样品放在测量托盘上。然后执行标准程序,其中附加的程序设定为10分钟分析时间和110℃的温度。
E)厚度
通过使用测微器或厚度计诸如Mitutoyo Corporation型号IDS-1012E的盘座式数字测微器(Mitutoyo Corporation,965Corporate Blvd,Aurora,IL,USA 60504)来获得多孔可溶性固体结构体的厚度。测微器具有直径1英寸、重约32克的台板,其测量约0.09psi(6.32gm/cm2)施压下的厚度。
通过将台板升起,将样品的一部分置于台板下的底座上,小心地降低台板以接触样品,释放台板,并且根据数字读出,测出以毫米计的样品的厚度,来测量多孔可溶性固体结构体的厚度。样品应完全延伸至台板的整个边缘,以确保在最低的可能表面压力下测量厚度,除非是在不扁平的更刚性基底情况下。
F)片材制品的基重
多孔可溶性固体结构体的基重可以计算为样品每单位面积的重量(克/m2)。面积计算为投影到垂直于样品的外边缘的扁平表面上的面积。将样品切成10cm×10cm的正方形,因此该面积是已知的。然后称重此类正方形中的每一个,并且然后将所得重量除以100cm2的已知面积以确定对应的基重。
对于不规则形状的多孔可溶性固体结构体,如果它是扁平物体,则该面积基于此类物体的外周边内包围的面积计算。由此就球形物体而言,所述面积根据平均直径计算,为3.14×(直径/2)2。由此就圆柱形物体而言,所述面积根据平均直径和平均长度计算,为直径×长度。就不规则形状的三维物体而言,该面积基于投影到与具有最大外部尺寸的侧面垂直取向的扁平表面上的该侧面计算。这可通过用铅笔仔细将物体的外部尺寸描绘到一张图纸上,然后通过大致点算正方形数,并且乘以已知的正方形面积,或通过拍摄包括标尺在内的所描绘面积的照片(被阴影化以供对比)并且使用图像分析技术,计算出所述面积来实现。
G)密度
多孔可溶性固体结构体的密度可由下式确定:计算出的密度=多孔固体的基重/(多孔固体厚度×1,000)。多孔可溶性固体结构体的基重和厚度可根据上文所述的方法测定。
H)比表面积
经由气体吸附技术测量多孔可溶性固体结构体的比表面积。表面积是分子级的固体样品暴露表面的量度。BET(Brunauer,Emmet,和Teller)理论是用于测定表面积的最流行模型,并且它基于气体吸附等温线。气体吸附使用物理吸附和毛细管冷凝来测量气体吸附等温线。该技术由以下步骤概述;将样品置于样品管中,并且在真空或流动的气体下加热以去除样品表面上的污物。通过从脱气样品和样品管总重量中减去空样品管的重量,获得样品重量。然后将样品管置于分析端口并且开始分析。分析方法中的第一步是将样品管排空,然后在液氮温度下使用氦气来测量样品管的自由空间体积。然后将样品第二次排空以去除氦气。然后仪器通过以使用者指定的间隔定量投入氪气,直到实现所需的压力量度,开始收集吸附等温线。然后可使用ASAP 2420和氪气吸附来分析样品。推荐由MicromeriticsAnalytical Services,Inc.(One Micromeritics Dr,Suite 200,Norcross,GA 30093)进行这些测量。与该技术相关的更多信息可见于Micromeritics Analytical Service网站(www.particletesting.com或www.micromeritics.com),或公布于Clyde Orr和Paul Webb的书籍“Analytical Methods in Fine Particle Technology”中。
实施例
以下实施例进一步例示了本文描述的内容。所给出的实施例仅是例证的目的,并且不应被理解为限制,因为在不脱离本发明的实质和范围的情况下可能有许多变型。除非另外指明,否则所有例示的量均为按总预混物重量计的浓度,即,重量/重量百分比。
下列表面活性剂/聚合物液体预混物以标明的重量百分比制备,如下文所述。液体配制物在以下物质的量和类型的水平上不同:羟乙磺酸盐主要表面活性剂(椰油酰羟乙磺酸钠和月桂酰羟甲基乙磺酸钠)、阴离子辅助表面活性剂(椰油酰谷氨酸钠、月桂醇聚氧乙烯醚磺基琥珀酸酯二钠)、以及两性表面活性剂(椰油酰胺基丙基甜菜碱、月桂酰胺基丙基甜菜碱、月桂酰两性基乙酸钠)
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1 Superol K,USP FCC EP甘油,CAS:56-81-5,供应商:Procter&GambleChemicals
2 BP-17,粘度为21-26cps并且%水解为86-89%,CAS:9002-89-5,供应商:LiweiChemical Company LTD,China。
3 JORDAPON SCI,CAS:61789-32-0,供应商:BASF。
4 ISELUX,CAS:928663-45-0,供应商:Innospec Active Chemicals
5 MIRANOL ULTRA L-32,CAS:68608-66-2,供应商:McIntyre Group Ltd,University Park,IL。
6 AMPHOSOL HCA-B,供应商:Stepan Company,Northfield,IL。
7 MACKAM DAB-ULS,CAS:4292-10-8,供应商:McIntyre Group Ltd,UniversityPark,IL。
8 EVERSOFT UCS-50SG,CAS:68187-30-4,供应商:Sino Lion,New Jersey。
9 MACKANATE EL P,CAS:68815-56-5,供应商:Solvay,
10无水柠檬酸细粒51N,供应商:S.A.Citrique Belge N.V.Pastorijstraat 249,B-3300Tienen,Belgium
通过使用常规的塔顶搅拌器(RW20DZM Stirrer,可获自/>Works,Inc.,Wilmington,DE)和热板(Corning Incorporated Life Sciences,Lowell,MA)来制备以上液体预混物组合物。向适宜大小的洁净容器中加入蒸馏水和甘油,同时以100-150rpm速率搅拌直到均匀。称量聚乙烯醇至适宜的容器中,并且使用药匙以小增量缓慢加入到主混合物中,同时持续搅拌以避免形成明显的团块。调节混合速度以使泡沫的形成最小化。将混合物缓慢加热到75℃至80℃,然后加入表面活性剂。然后将混合物加热到85℃,同时持续搅拌,然后使其冷却到室温。添加附加的蒸馏水以补偿由于蒸发而损失的水(基于容器的初始皮重)。
实施例13、14、15、16、17、18、19、20、21、22、23和24中表示的多孔可溶性固体结构体分别由来自实施例1、2、3、4、5、6、7、8、9、10、11和12的表面活性剂/聚合物液体加工溶液制备。
注意:为简单起见,假设极干燥条件(0%相对湿度)显示配制物。然而,多孔固体是吸湿且吸收水分,这取决于空气中的%相对湿度。例如,在50%相对湿度下,多孔固体将包含大约7至10%水分。
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如下由预混物液体加工溶液制备多孔可溶性固体结构体。将10ml预混物在室温下转移到80ml有刻度的塑料烧杯中。使用IKA ULTRA-T 25高速混合器(可例如获自Hobart Corporation,Troy,OH)在6,500RPM下对混合物进行充气,直到夹带的空气将浆料膨胀到有刻度的烧杯上的40ml标记(处于0.25g/cm3的密度)。然后将所得的充过气的混合物用刮刀摊开在矩形40mm×175mm的铝模具中,所述模具具有1.0mm深度,以45度角拿着金属刮刀,用其直边缓慢均匀地拖过模具表面将过量的润湿泡沫移除。然后将铝模具放置在预热表面温度为100℃的热板上,然后保持干燥达30分钟,直到表面触摸起来干燥。使模具冷却到室温,在薄刮刀和镊子的帮助下,将大体上干燥的多孔固体从模具中移除。
本文所公开的量纲和值不应理解为严格限于所引用的精确数值。相反,除非另外指明,否则每个此类量纲旨在表示所述值以及围绕该值功能上等同的范围。例如,公开为“40mm”的量纲旨在表示“约40mm”。
除非明确排除或以其它方式限制,本文中引用的每一篇文献,包括任何交叉引用或相关专利或专利申请以及本申请对其要求优先权或其有益效果的任何专利申请或专利,均据此全文以引用方式并入本文。对任何文献的引用不是对其作为与本发明的任何所公开或本文受权利要求书保护的现有技术的认可,或不是对其自身或与任何一个或多个参考文献的组合提出、建议或公开任何此类发明的认可。此外,当本发明中术语的任何含义或定义与以引用方式并入的文献中相同术语的任何含义或定义矛盾时,应当服从在本发明中赋予该术语的含义或定义。
虽然已举例说明和描述了本发明的具体实施方案,但是对于本领域技术人员来说显而易见的是,在不脱离本发明的实质和范围的情况下可作出各种其他变化和修改。因此,本文旨在于所附权利要求中涵盖属于本发明范围内的所有此类变化和修改。
Claims (14)
1.一种多孔可溶性固体结构体,包含:
a.按所述多孔可溶性固体结构体的重量计22%至41%的羟乙磺酸盐表面活性剂,所述羟乙磺酸盐表面活性剂选自下组:椰油酰羟乙磺酸钠、月桂酰羟甲基乙磺酸钠或者它们的组合;
b.按所述多孔可溶性固体结构体的重量计7%至25%的非硫酸盐阴离子表面活性剂,所述非硫酸盐阴离子表面活性剂包含椰油酰谷氨酸钠、月桂醇聚氧乙烯醚磺基琥珀酸酯二钠或者它们的组合;
c.按所述多孔可溶性固体结构体的重量计5%至25%的两性表面活性剂、两性离子表面活性剂或其组合,所述两性表面活性剂、两性离子表面活性剂或其组合选自:月桂酰胺基丙基甜菜碱、月桂酰两性基乙酸钠或者它们的组合;
d.按所述多孔可溶性固体结构体的重量计18%至38%的聚乙烯醇;
e.按所述多孔可溶性固体结构体的重量计4.5%至20%的甘油;
其中所述多孔可溶性固体结构体的密度为:0.05g/cm3至0.20g/cm3。
2.根据权利要求1所述的多孔可溶性固体结构体,其中所述多孔可溶性固体结构体的断裂应变为20mm或更大。
3.根据权利要求1或2中任一项所述的多孔可溶性固体结构体,其中所述羟乙磺酸盐表面活性剂的水平为按所述多孔可溶性固体结构体的重量计20%至30%,并且所述非硫酸盐阴离子表面活性剂的水平为按所述多孔可溶性固体结构体的重量计15%至25%。
4.根据权利要求1或2中任一项所述的多孔可溶性固体结构体,其中所述羟乙磺酸盐表面活性剂的水平为按所述多孔可溶性固体结构体的重量计31%至41%,并且所述非硫酸盐阴离子表面活性剂的水平为按所述多孔可溶性固体结构体的重量计7%至18%。
5.根据权利要求1或2中任一项所述的多孔可溶性固体结构体,其中所述羟乙磺酸盐表面活性剂的水平为按所述多孔可溶性固体结构体的重量计38%至41%,并且所述非硫酸盐阴离子表面活性剂的水平为按所述多孔可溶性固体结构体的重量计7%至17%。
6.根据权利要求5所述的多孔可溶性固体结构体,其中所述羟乙磺酸盐表面活性剂包括椰油酰羟乙磺酸钠,并且所述非硫酸盐阴离子表面活性剂包括椰油酰谷氨酸钠。
7.根据权利要求5所述的多孔可溶性固体结构体,其中所述羟乙磺酸盐表面活性剂包括月桂酰羟甲基乙磺酸钠和椰油酰羟乙磺酸钠,并且所述非硫酸盐阴离子表面活性剂包括椰油酰谷氨酸钠。
8.根据权利要求1所述的多孔可溶性固体结构体,其中所述羟乙磺酸盐表面活性剂的水平为按所述多孔可溶性固体结构体的重量计22%至25%,并且所述非硫酸盐阴离子表面活性剂的水平为按所述多孔可溶性固体结构体的重量计14%至17%。
9.根据权利要求1所述的多孔可溶性固体结构体,其中所述羟乙磺酸盐表面活性剂的水平为按所述多孔可溶性固体结构体的重量计22%至25%,并且所述非硫酸盐阴离子表面活性剂的水平为按所述多孔可溶性固体结构体的重量计22%至25%。
10.根据权利要求8或9中任一项所述的多孔可溶性固体结构体,其中所述羟乙磺酸盐表面活性剂包括椰油酰羟乙磺酸钠,并且所述非硫酸盐阴离子表面活性剂包括椰油酰谷氨酸钠和月桂醇聚氧乙烯醚磺基琥珀酸酯二钠。
11.根据权利要求8或9中任一项所述的多孔可溶性固体结构体,其中所述羟乙磺酸盐表面活性剂包括椰油酰羟乙磺酸钠,并且所述非硫酸盐阴离子表面活性剂包括椰油酰谷氨酸钠。
12.根据权利要求1所述的多孔可溶性固体结构体,其中所述多孔可溶性固体结构体具有多个层。
13.根据权利要求1所述的多孔可溶性固体结构体,其中总表面活性剂的量为按所述多孔可溶性固体结构体的重量计40%至70%。
14.根据权利要求1所述的多孔可溶性固体结构体,其中所述多孔可溶性固体结构体为开孔泡沫。
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MX2022003979A (es) | 2022-04-26 |
EP4061320A1 (en) | 2022-09-28 |
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