CN1930177A - 液体纺织品预处理剂 - Google Patents
液体纺织品预处理剂 Download PDFInfo
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Abstract
本发明涉及适用于所有连续和间歇预处理操作的液体纺织品预处理剂，其为基于烷氧化Guerbet醇的磷酸酯并且不但制剂形式/而且液体形式均对碱非常稳定。所述纺织品预处理剂通常以具有40－70％重量的活性内含物、有或无0.1－3.5％重量的其他辅助物质(例如表面活性剂、杀生物剂、消泡剂或抑泡剂)的含水组合物形式使用。
Description
本发明涉及适用于所有连续和间歇预处理操作的液体纺织品预处理剂，其为基于烷氧化Guerbet醇的磷酸酯并且不但制剂形式而且液体形式均对碱非常稳定。
在坯布转化中，对天然或合成纤维材料的预处理构成进一步加工的重要基础。各种操作(例如退浆、煮练、漂白或丝光)使用各种各样的纺织化学品，所述纺织品化学品的实例有表面活性剂、分散剂、乳化剂、漂白剂、抑泡剂或消泡剂。在各种必要条件中，已知这些助剂必须满足对碱高度稳定，特别在机织棉织物的碱洗过程中。因此，仍需要具有合适的性能概况的新活性化合物。
现在已令人惊奇地发现，特定的烷氧基化Guerbet醇的磷酸酯非常适用于连续和间歇预处理纺织材料。这样的烷氧基化Guerbet醇例如自WO 03/091192 A1已知。虽然该专利已公开将各种制剂用于纺织工业，但是并没有给出各种磷酸酯的优异且令人惊奇的性质。
因此，本发明提供了式(I)化合物：
其中：
m为1到3；
n为2到4；
x为4到12；且
R为式(II)基团：
其中：
r为0到8；
s为0到8；
(r+s)的总和为4到8；且
各烷基链可独立为线形或支化的烷基链。
本发明的化合物为非常稳定的表面活性剂，其可以高浓度(例如60％溶液)而无需任何添加剂在水中存在。所述化合物结合了良好可润湿性和低成泡性，从而具有独特的性能。特别是这些化合物不但制剂形式而且液体形式均对碱具有极高的稳定性，从而注定这些化合物在碱煮练过程中不但可用作分散剂，还可能用作乳化剂或消泡剂组分。
以下化合物也非常适合，其中
m为1到3；
n为2或3；
x为6到8；
r为2到6；
s为0到4；且
(r+s)的总和为5到7。
以下化合物显示特别好的性质，其中
m为1到2；
n为2；
x为7；
r为4；
s为2；且
(r+s)的总和为6。
指数m为平均值，特别优选的m值为1.2到1.3。
本发明的化合物通过如WO 03/091192 A1所述将适当的Guerbet醇烷氧基化，随后优选用五氧化二磷磷酸化来制备。所使用的Guerbet醇的环氧烷单元主要为环氧乙烷或环氧丙烷单元，但主要为与低分数环氧丙烷组合的环氧乙烷单元，或者仅为环氧乙烷单元。
磷酸化在90-120℃下在空气存在下通过分批加入磷化剂4-24小时完成在期间。
本发明的化合物可以本身或以水性组合物形式用于预处理纺织品。
因此，本发明还提供了包含一种或多种式(I)化合物和其他助剂的水溶液的组合物。
所述水性组合物优选包含40-70％重量的化合物(I)，尽管约2-4％重量的化合物(I)还可以钠盐形式存在。所述组合物还可包含0.1-3.5％重量的其他助剂物质，例如表面活性剂、杀生物剂、消泡剂或抑泡剂。
本发明的组合物可由简单混合其组分而得到。
式(I)化合物或上述水性组合物的优选用途为在碱性条件下连续或批操作地预处理纺织品。
下列实施例说明本发明。
实施例
现如下描述所使用的烷氧基化Guerbet醇、通过磷酸化由其得到的产物、由其制备的水性制剂和统计表格中的所得的应用结果。
使用下列试验方法：
碱稳定性
在各情况下用总共100ml液体试验5g/l表面活性剂的碱稳定性。所述试验在室温20-25℃下进行。将所需量的氢氧化钠水溶液称量入玻璃烧杯中且用去离子水制成95ml。在搅拌下向所述碱批料中加入5ml 10％表面活性剂溶液。在不搅拌的情况下将玻璃烧杯在室温下静置24小时。
24小时之后试验溶液的稳定性。尤其注意形成乳状液及沉淀物，容许无明显沉淀物的混浊。确定在多高浓度下该表面活性剂仍稳定。记录碱稳定性X°Bé-NaOH。
Ross-Miles泡沫试验
在自一定高度倾入一定量的液体之后立即及一分钟之后测量泡沫体积。
使用内径为60mm且内部高度为430mm的1000ml量筒。允许所述试验液体从21分液漏斗中经长度为70mm、内径为2mm的毛细管从600mm的高度(从毛细管的出口到量筒底部测量)流出。
将待试验的500ml溶液填充到分液漏斗中且使其经毛细管以受控的流出速率约0.171/min流到量筒中。一旦所有溶液都流出，则开动秒表计时，读出量筒刻度的整个体积(泡沫体积加溶液体积)。一分钟后重复读数。
使用浓度为2g/l的表面活性剂的2°BéNaOH去离子水溶液测试碱性泡沫性能，其中2°BéNaOH相当于12g/l NaOH固体或30ml/lNaOH 36°Bé。试验温度为20-25℃。
碱润湿性
该试验方法测定织物样品下沉到装有表面活性剂溶液的容量为1升、高度为14cm、直径为10cm的玻璃烧杯底部的所需的秒数。所使用的织物样品是得自St.Gallen，Switzerland的EMPA TestmaterialienAG的试验棉布。将该布模切成直径为3.5cm的圆盘形且与特定的夹具一起浸入表面活性剂溶液中。在25℃、2°BéNaOH下测试润湿作用。
表1
使用烷氧基化Guerbet醇和其他醇
| 序号 | 醇 | EO | PO | 剩余醇 |
| 1 | 不少于70％2-丙基-1-庚醇、不多于30％2-丙基异庚醇 | 7 | 0 | 6 |
| 2 | 不少于70％2-丙基-1-庚醇、不多于30％2-丙基异庚醇 | 10 | 0 | 2 |
| 3 | 不少于70％2-丙基-1-庚醇、不多于30％2-丙基异庚醇 | 7 | 1 | ≤1 |
| V1 | 异十一醇(标准) | 7 | 0 | 低 |
| V2 | Exxal-C11(得自Exxon的i-C11) | 7 | 0 | 低 |
| V3 | i-C12/C14 | 7 | 0 | 低 |
EO、PO＝环氧乙烷、环氧丙烷；V1-V3为比较用醇。
表2
磷酸化
| 醇序号 | 1/4P4O10 | 磷酸化温度 | 磷酸酯序号 | ||
| 摩尔比 | 摩尔比 | ℃ | |||
| 1 | 1 | 1.25 | 6小时100℃ | I | |
| 1 | 1 | 1.25 | 24小时115℃ | II | |
| 2 | 1 | 1.25 | 6小时100℃ | III | |
| 3 | 1 | 1.25 | 6小时100℃ | IV | |
| 3a | 0.9醇3+0.1异癸醇 | 1.25 | 6小时100℃ | V | |
| 比较测试 | |||||
| V1 | 1 | 1.25 | 6小时100℃ | VI | |
| V2 | 1 | 1.25 | 6小时100℃ | VII | |
| V3 | 1 | 1.25 | 6小时100℃ | VIII | |
表3
含水制剂
| 制剂序号 | 次编号 | 组分名称 | 浓度(％重量) | 备注 |
| I | a | 磷酸酯I | 60.00％ | -无问题制剂-无增溶剂-无抑泡剂 |
| 苛性钠 | 12.80％ | -无消泡剂 | ||
| 杀生物剂(Acticid MBS) | 0.10％ | |||
| 水 | 27.10％ | |||
| 100.00％ | ||||
| I | b | 磷酸酯I | 60.00％ | -无问题制剂 |
| SagTex DSA | 0.50％ | -无增溶剂 |
| 苛性钠 | 12.80％ | |||
| 杀生物剂(ActicidMBS) | 0.10％ | |||
| 水 | 26.60％ | |||
| 100.00％ | ||||
| I | c | 磷酸酯I | 60.00％ | -无问题制剂-无增溶剂 |
| ZJ 834(异壬酰胺) | 3.00％ | -无消泡剂 | ||
| 苛性钠 | 12.80％ | -仅抑泡剂(不含Si) | ||
| 杀生物剂(Acticid MBS) | 0.10％ | |||
| 水 | 24.10％ | |||
| 100.00％ | ||||
| I | d | 磷酸酯I | 60.00％ | -无问题制剂 |
| SagTex DSA | 0.20％ | -无增溶剂 | ||
| ZJ 834(异壬酰胺) | 1.00％ | |||
| 苛性钠 | 12.80％ | |||
| 杀生物剂(Acticid MBS) | 0.10％ | |||
| 水 | 25.90％ | |||
| 100.00％ | ||||
| II | a | 磷酸酯II(24小时115℃) | 60.00％ | -除24小时外，类似于Ib |
| SagTex DSA | 0.50％ | -在115℃下进行磷酸化-粘度稍高 | ||
| 苛性钠 | 12.80％ | -与Ib相同 | ||
| 杀生物剂(Acticid MBS) | 0.10％ | |||
| 水 | 26.60％ | |||
| 100.00％ | ||||
| III | a | 磷酸酯III | 60.00％ | -粘稠液体 |
| SagTex DSA | 0.50％ |
| 苛性钠 | 12.20％ | |||
| 杀生物剂(Acticid MBS) | 0.10％ | |||
| 水 | 27.20％ | |||
| 100.00％ | ||||
| III | b | 磷酸酯III | 60.00％ | -粘稠液体 |
| ZJ 834(异壬酰胺) | 3.00％ | |||
| 苛性钠 | 12.20％ | |||
| 杀生物剂(Acticid MBS) | 0.10％ | |||
| 水 | 24.70％ | |||
| 100.00％ | ||||
| IV | a | 磷酸酯IV | 60.00％ | -无色到黄色液体 |
| SagTex DSA | 1.00％ | -取决于磷酸化有时还可为糊膏状 | ||
| 苛性钠 | 7.50％ | -增加的消泡剂含量 | ||
| 杀生物剂(Acticid MBS) | 0.00％ | |||
| 水 | 31.50％ | |||
| 100.00％ | ||||
| V | a | 磷酸酯V | 60.00％ | -无色液体 |
| SagTex DSA | 1.00％ | -除在磷酸化醇中还有10％异癸醇外，类似于IV | ||
| 苛性钠 | 7.50％ | -与IV相比较具有降低的碱稳定性，因此不再进行任何另外试验 | ||
| 杀生物剂(Acticid MBS) | 0.00％ | |||
| 水 | 31.50％ | |||
| 100.00％ | ||||
| 比较制剂 | ||||
| VI | a | 磷酸酯VI | 60.00％ | -褐色糊膏 |
| SagTex DSA | 0.50％ | |||
| 苛性钠 | 12.20％ | |||
| 杀生物剂(ActicidMBS) | 0.10％ | |||
| 水 | 27.20％ | |||
| 100.00％ | ||||
| VI | b | 磷酸酯VI | 60.00％ | -褐色糊膏 |
| ZJ 834(异壬酰胺) | 3.00％ | |||
| 苛性钠 | 12.20％ | |||
| 杀生物剂(ActicidMBS) | 0.10％ | |||
| 水 | 24.70％ | |||
| 100.00％ | ||||
| VII | a | 磷酸酯VII | 60.00％ | -褐色糊膏 |
| SagTex DSA | 0.50％ | |||
| 苛性钠 | 12.20％ | |||
| 杀生物剂(ActicidMBS) | 0.10％ | |||
| 水 | 27.20％ | |||
| 100.00％ | ||||
| VII | b | 磷酸酯VII | 60.00％ | -褐色糊膏 |
| ZJ834(异壬酰胺) | 3.00％ | |||
| 苛性钠 | 12.20％ | |||
| 杀生物剂(ActicidMBS) | 0.10％ | |||
| 水 | 24.70％ | |||
| 100.00％ | ||||
| VIII | a | 磷酸酯VIII | 30.00％ | -褐色糊膏 |
| SagTex DSA | 0.25％ | -在60％形式下不可搅拌，因此不可配制 | ||
| 苛性钠 | 6.10％ | -一半浓度 | ||
| 杀生物剂(ActicidMBS) | 0.05％ | |||
| 水 | 63.60％ | |||
| 100.00％ | ||||
| VIII | b | 磷酸酯VIII | 30.00％ | -褐色糊膏 |
| -在60％形式下不可搅拌，因此不可配制 | ||||
| ZJ 834(异壬酰胺) | 1.50％ | |||
| 苛性钠 | 6.10％ | -一半浓度 | ||
| 杀生物剂(ActicidMBS) | 0.05％ | |||
| 水 | 62.35％ | |||
| 100.00％ |
表4
应用结果
| 磷酸酯序号 | 制剂* | 外观 | 粘度 | 碱稳定性 | Ross-Miles泡沫，碱(2°Bé) | 润湿性，碱 | |||
| 直接 | 保持1分钟 | 2g/l | |||||||
| cPs | °Bé | ml | ml | s | |||||
| Ia | 澄清、无色 | 225 | 16 | 175 | 90 | 46 | |||
| Ib | 稍微混浊、无色 | 225 | 16 | 0 | 0 | 42 | |||
| Ic | 澄清、无色 | 215 | 16 | 65 | 10 | 40 | |||
| Id | 稍微混浊、无色 | 220 | 16 | 40 | 0 | 41 | |||
| IIa | 适度粘稠 | 470 | 16 | 0 | 0 | 50 | |||
| IIIa | 稳定、粘稠 | 960 | ＞17 | 20 | 0 | 78 | |||
| IIIb | 稳定、粘稠 | 800 | ＞17 | 60 | 10 | 78 | |||
| IVa | 1％消泡剂 | 稳定、液体 | n.b. | 15 | 50 | 10 | 50 | ||
| Va | 1％消泡剂 | 稳定、液体 | n.b. | 10 | n.b. | n.b. | n.b. | ||
| 比较试验 | |||||||||
| VIa | 褐色糊膏 | 1700 | 17 | 10 | 0 | 85 | |||
| VIb | 褐色糊膏 | 1700 | 17 | 40 | 20 | 79 | |||
| VIIa | 褐色糊膏 | 1500 | 15 | 50 | 5 | 60 | |||
| VIIb | 褐色糊膏 | 1400 | 17 | 20 | 0 | 59 | |||
| VIIIa | 30％AS，所应用量的两倍 | 褐色糊膏 | 高度粘稠 | ＞17 | 20 | 0 | 约200 | ||
| VIIIb | 30％AS，所应用量的两倍 | 褐色糊膏 | 高度粘稠 | ＞17 | 80 | 50 | 约200 | ||
*除非明确提到，否则所有制剂均含有60％活性物和0％增溶剂，且所有的浊点均大于80℃(应用优势)；
n.b.未确定；
AS 活性物质
所述实施例清楚地显示某些Guerbet醇的新型磷酸酯的本发明制剂具有非常好的性能概况，即对碱的高度稳定性、极微的起泡性和良好的润湿性。
Claims (9)
1.一种式(I)化合物
其中：
m为1到3；
n为2或3；
x为6到8；且
R为式(II)基团
其中：
r为2到6；
s为0到4；
(r+s)的总和为5到7；且
各烷基链可独立为线形或支化的烷基链。
2.权利要求1的化合物，其中
m为1到2；
n为2；
x为7；
r为4；
s为2；且
(r+s)的总和为6。
3.一种制备权利要求1或2的式(I)化合物的方法，其特征在于将Guerbet醇R-OH烷氧基化且随后磷酸化，其中R具有式(II)的含义。
4.权利要求3的方法，其特征在于使C10-Guerbet醇与环氧乙烷反应，接着与五氧化二磷反应。
5.一种组合物，所述组合物包含一种或多种权利要求1或2的式(I)化合物和其他助剂的水溶液。
6.权利要求5的组合物，所述组合物包含40-70％重量的化合物(I)，2-4％重量的化合物(I)呈钠盐形式，和0.1-3.5％重量的表面活性剂、杀生物剂、消泡剂或抑泡剂。
7.一种制备权利要求5或6的组合物的方法，其特征在于将所述式(I)化合物与其他组分在含水介质中混合。
8.权利要求1或2的式(I)化合物或权利要求5或6的组合物用于预处理纺织品的用途。
9.权利要求8的用途，其特征在于所述预处理包括在碱性条件下的连续或间歇预处理操作。
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| EP (1) | EP1737873A1 (zh) |
| KR (1) | KR20070005627A (zh) |
| CN (1) | CN1930177A (zh) |
| BR (1) | BRPI0508910A (zh) |
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| CN116143828A (zh) * | 2023-04-23 | 2023-05-23 | 四川科宏达集团有限责任公司 | 一种高双酯含量磷酸酯表面活性剂的合成方法 |
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| CN101495593B (zh) | 2006-07-24 | 2013-12-25 | 巴斯夫欧洲公司 | 用于在石油或天然气提取过程中改善发泡的组合物 |
| EP2176349A2 (de) | 2007-08-02 | 2010-04-21 | Clariant Finance (BVI) Limited | Phosphorsäureester enthaltend über diol-einheiten verbrückte phosphoratome |
| DE102007036188A1 (de) | 2007-08-02 | 2008-06-19 | Clariant International Limited | Verfahren zur Herstellung alkoxylierter Phosphorsäuretriester |
| US20100260696A1 (en) * | 2007-08-02 | 2010-10-14 | Clariant Finance (Bvi) Limited | Aqueous Compositions Containing Alkoxylated Phosphoric Acid Triesters |
| CA2795104C (en) * | 2010-04-23 | 2018-05-15 | Basf Se | Process for producing mineral oil using surfactants based on a mixture of c32 guerbet-, c34 guerbet-, c36 guerbet-containing alkyl alkoxylates |
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| US4453946A (en) * | 1981-04-29 | 1984-06-12 | Ciba-Geigy Corporation | Dyeing assistant and use thereof in dyeing synthetic fibre material |
| JPH05140174A (ja) * | 1991-11-20 | 1993-06-08 | Sakai Chem Ind Co Ltd | りん酸トリエステルの製造方法 |
| DE10035617A1 (de) * | 2000-07-21 | 2002-01-31 | Basf Ag | Sekundäre C¶1¶¶0¶-C¶1¶¶8¶-Tensidalkohole |
| CA2483472C (en) * | 2002-04-26 | 2010-09-21 | Basf Aktiengesellschaft | C10-alkanol alkoxylate mixtures and their use |
| DE20303420U1 (de) * | 2003-03-03 | 2003-09-25 | Sasol Germany GmbH, 22297 Hamburg | Alkoholmischungen und deren Derivate |
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- 2005-03-02 WO PCT/IB2005/000569 patent/WO2005090366A1/en not_active Application Discontinuation
- 2005-03-02 EP EP05708677A patent/EP1737873A1/en not_active Withdrawn
- 2005-03-02 CN CNA2005800079277A patent/CN1930177A/zh active Pending
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2006
- 2006-09-05 MX MXPA06010103 patent/MXPA06010103A/es not_active Application Discontinuation
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116143828A (zh) * | 2023-04-23 | 2023-05-23 | 四川科宏达集团有限责任公司 | 一种高双酯含量磷酸酯表面活性剂的合成方法 |
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|---|---|
| EP1737873A1 (en) | 2007-01-03 |
| IN2006CH03368A (zh) | 2007-06-22 |
| MXPA06010103A (es) | 2006-11-01 |
| BRPI0508910A (pt) | 2007-08-14 |
| WO2005090366A1 (en) | 2005-09-29 |
| US20080254695A1 (en) | 2008-10-16 |
| KR20070005627A (ko) | 2007-01-10 |
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