CN1372609A - 萤光增白剂混合物 - Google Patents
萤光增白剂混合物 Download PDFInfo
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- C—CHEMISTRY; METALLURGY
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- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
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- C07C255/49—Carboxylic acid nitriles having cyano groups bound to carbon atoms of six-membered aromatic rings of a carbon skeleton
- C07C255/50—Carboxylic acid nitriles having cyano groups bound to carbon atoms of six-membered aromatic rings of a carbon skeleton to carbon atoms of non-condensed six-membered aromatic rings
- C07C255/51—Carboxylic acid nitriles having cyano groups bound to carbon atoms of six-membered aromatic rings of a carbon skeleton to carbon atoms of non-condensed six-membered aromatic rings containing at least two cyano groups bound to the carbon skeleton
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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
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
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- C11D3/42—Brightening agents ; Blueing agents
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- D06L—DRY-CLEANING, WASHING OR BLEACHING FIBRES, FILAMENTS, THREADS, YARNS, FABRICS, FEATHERS OR MADE-UP FIBROUS GOODS; BLEACHING LEATHER OR FURS
- D06L4/00—Bleaching fibres, filaments, threads, yarns, fabrics, feathers or made-up fibrous goods; Bleaching leather or furs
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- D06L4/636—Optical bleaching or brightening in aqueous solvents with disperse brighteners
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- D06L4/00—Bleaching fibres, filaments, threads, yarns, fabrics, feathers or made-up fibrous goods; Bleaching leather or furs
- D06L4/60—Optical bleaching or brightening
- D06L4/65—Optical bleaching or brightening with mixtures of optical brighteners
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- D06L—DRY-CLEANING, WASHING OR BLEACHING FIBRES, FILAMENTS, THREADS, YARNS, FABRICS, FEATHERS OR MADE-UP FIBROUS GOODS; BLEACHING LEATHER OR FURS
- D06L4/00—Bleaching fibres, filaments, threads, yarns, fabrics, feathers or made-up fibrous goods; Bleaching leather or furs
- D06L4/60—Optical bleaching or brightening
- D06L4/664—Preparations of optical brighteners; Optical brighteners in aerosol form; Physical treatment of optical brighteners
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y10S8/92—Synthetic fiber dyeing
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Abstract
本发明涉及萤光增白剂的一种混合物,其中包括20-70重量%的化学式(1)的一种化合物的,30-80%的化学式(2)的一种化合物及0.5-5%的化学式(3)的一种化合物,涉及含该混合物的组合物及该组合物在增白合成纤维尤其聚酯中的应用。
Description
本发明涉及基于氰基取代1,4-双苯乙烯基苯的各种异构体的萤光增白剂的混合物。
由于这些混合物可呈现白度比由单独各组分总和的白度更高,所以对萤光增白剂常常采用两种或更多种组分的混合物形式。
因此,例如,GB 2200660描述了这些混合物,不过该组合物受到制备方法的限制,而US 5695686描述了类似还含非对称异构体的混合物,也由于制备方法而受限制。此外,DE 19609956描述了一些极复杂的混合物,其内含最多五个不同异构体的双氰基-取代联苯乙烯苯。
双氰基取代联苯乙烯苯的这些混合物的结构不仅对增白效果重要,而且对色泽也重要,它可以是或多或少微红或浅绿色的,这种需要对直接用户是极为重要的事。
此外,特别有兴趣的混合物是包括50-70重量%化学式(1)的化合物、30-50%化学式(2)的化合物及0.5-5%化学式(3)的化合物,而特别适宜的混合物是包括55-70重量%化学式(1)的化合物、30-45%化学式(2)的化合物及0.5-3%化学式(3)的化合物,而优选应该采用混合物包括58-62重量%化学式(1)的化合物、38-42%化学式(2)的化合物及0.5-3%化学式(3)的化合物。
本发明的混合物通过使对苯二亚甲基醛与4-二烷基膦酰甲基苄腈的缩合,然后进一步使作为中间产物获得的4-氰基-4’-甲酰基二苯乙烯与2-或3-二烷基膦酰甲基苄腈缩合来制取,其缩合路径如下:在此R代表甲基、乙基、丙基或丁基,优选甲基或乙基。
对苯二亚甲基醛与4-二烷基膦酰甲基苄腈的初始缩合是在低级醇例如甲醇、乙醇、正或异丙醇或正、仲或叔丁醇,优选甲醇作为溶剂及在碱金属氢氧化物如氢氧化锂、氢氧化钾或氢氧化钠,优选氢氧化钾的存在下进行的。缩合过程产生了少量即最多5%的一种副产物4,4’-双氰基-(1,4-双苯乙烯基)苯,这时最终混合物中因它存在而有利。反应之后,4-氰基4’-甲酰二苯乙烯从反应混合物中沉淀出来,并经过滤使之分出。
第二缩合步骤是在偶极非质子传递溶剂中,诸如在二甲基甲酰胺、二甲基亚砜、N-甲基吡咯烷酮或四甲脲中,优选在二甲基甲酰胺中,和在强碱存在下诸如C1-C5醇化钠或钾的一种强碱存在下,特别在甲醇钠存在下进行。
30-80%化学式(2)的一种化合物,和
此外,特别有兴趣的混合物是包括50-70%化学式(1)的化合物、30-50%的化学式(2)的化合物及0.5-5%化学式(3)的化合物,而尤其适宜的是混合物包括55-70重量%化学式(1)的化合物、30-45%化学式(2)的化合物及0.5-3%化学式(3)的化合物,而且优选地是,应该使用包括58-62重量%化学式(1)的化合物、38-42%化学式(2)的化合物及0.5-3%化学式(3)化合物的混合物。
按照利用萤光增白剂混合物的惯例,采用将各单组分分散在液体介质中的方法,优选分散在水中,可将各单组分加工为商用形式。这一点可采用先分散各单组分后将所得分散相合并一起的方法做到。但是也可能将各单组分大体混合一起然后使之共同分散。可在球磨机、胶体磨、玻珠研磨机等中,以常规方式完成这种分散操作。
因此本发明还提供内含水和各例中按配方重量计3-25重量%,优选5-15重量%上述定义的荧光增白剂混合物以及0-60%,优选5-50重量%的助剂的各种增白剂组合物。
适宜助剂包括例如阴离子或非离子的分散剂,选自与脂肪醇、高级脂肪酸或烷基酚的环氧乙烷加成物类,或乙二胺环氧乙烷-环氧丙烷加成物类,N-乙烯基吡咯烷酮与3-乙烯基丙酸的共聚物类,保水性助剂如乙二醇、甘油或山梨糖醇,或杀菌剂。
本发明混合物及含该混合物的组合物适用于增白由合成纤维制成的纺织品,尤其增白由那些直链聚酯制成的纺织品。但是,这些混合物及组合物也可用于增白含直链聚酯的混合物。
通常按萤光增白剂的用法来使用本发明混合物,例如,采用染色机(dying machine)的浸染法(exhaust dying process)或采用浸轧热固化染色法(pad-thermofixation)。这种处理在水介质中进行方便,其中这些化合物可以极细微粒形式存在,如悬浮液、微分散体或可能的溶液。在处理过程中,只要适宜,也可加入分散剂、稳定剂、润湿剂及其它助剂。这种处理通常在约20-140℃温度完成,优选110-130℃的范围,例如在该浴沸点温度或接近沸点的温度下完成。对于使用混合物进行浸轧热固化场合,该热固化优选在170-200℃间温度下完成。
以下实施例用于说明本发明;除非另有说明,所有份数及百分率均按重量计。
A、制备实施例
实施例1:4-氰基4-甲酰基二苯乙烯
在氮气氛下将480毫升甲醇装入1.5升烧瓶中,并搅拌加入43.4克的85%氢氧化钾粉末。氢氧化钾溶解,温度升至43℃。将该溶液冷却至2℃,加入82.1克的98%对苯二亚甲基醛。向所得清液中搅拌滴加120毫升甲醇中溶有144.8克4-二甲基膦酰甲基苄腈的溶液,并于2℃下对起冷却2小时。在2℃下搅拌2小时之后,将温度升至25℃,再搅拌该混合物另外2小时。随后将温度升至40℃,并在此温度下持续搅拌另外2小时。然后用180毫升的甲醇稀释该混合物,并在室温下搅拌该悬浮液过夜。然后抽吸过滤该沉淀物,用250毫升甲醇洗涤并吸干。这样获得260克的湿滤饼,相当于干燥产物123克,内含98.7%的4-氰基-4’-甲酰基二苯乙烯及1.3%的化学式(3)的4,4’-双氰基-(1,4-双苯乙烯基)苯。
在氮气氛下,将380毫升的N,N-二甲基甲酰胺装入1.5升烧瓶中,然后依次加入131.8克的3-二甲基膦酰甲基苄腈及259.0克实施例1中所得的湿滤饼。将此黄色悬浮液加热至40℃,并滴加99.0克的30%甲醇钠的甲醇溶液,于40-44℃下使之冷却40分。接着在40-42℃下搅拌所得悬浮液另外4小时,接着于室温下过夜。在用400毫升甲醇稀释之后,添加8.0克的蚁酸,使混合物用酚酞显示呈中性,然后将其冷却至0℃并加以过滤。用250毫升2份甲醇洗涤该滤饼。于70℃下真空干燥后,获得137.8克的产物,内含94.8%的化学式(1)的化合物及1.9%的化学式(3)的化合物。
在氮气氛下,将170毫升的N,N-二甲基甲酰胺装入1.5升烧瓶中,依次加入331.2克的34%的2-二甲基膦酰甲基苄腈及272.0克实施例1中获得的湿滤饼。将此悬浮液加热至40℃,滴加99.0克的30%甲醇钠的甲醇溶液,于40-44℃下将其冷却40分钟。接着在40-42℃下搅拌所得悬浮液另外4小时。在用400毫升甲醇稀释之后,于室温下搅拌该混合物过夜,添加4.0克蚁酸,使该混合物用酚酞显示呈中性,使之冷却至0℃并加以过滤。用250毫升2份甲醇洗涤滤饼。于70℃下真空干燥后,获得133.1克的浅黄产物,内含98.9%的化学式(2)的化合物及0.7%的化学式(3)的化合物。
B.应用实施例
a)浸染法
在一种着色设备中,于室温及液比1∶20下,用一种其内含极细分散型的0.1重量%的化学式(1)、(2)及(3)光学增白剂的混合物(其比例示于表1)并含分散剂脂肪醇聚乙二醇醚1克/升的水浴,处理一种聚酯编织物(涤纶类型540)。于30分钟的时间内将其温度从室温升至110℃,于此温度下再保持30分钟,随后于15分钟的时间内将其冷却至40℃。然后,在流水下冲洗该纺织材料30秒时间,并在70℃下加以干燥。
如此处理后的聚酯编织物,用Ganz方法测定(见表1),呈现白度高并带中性浅蓝色泽。
b)浸轧热固化染色方法
采用浸轧-堆放复苏法,用一种水溶液其内含1.2克/升%由化学式(1)、(2)及(3)光学增白剂(比例列于表1)的分散型混合物并含1克/升的磺化二羧酸烷基酯的碱金属盐,在室温下对一种聚酯编织物(涤纶类型540)进行处理。其浸轧效应(pinch-off effect)为65%。随后,在70℃下干燥该编织物样品30分钟,接着在180℃下热固化30秒时间。
如此处理后的聚酯编织物按Ganz方法测定(见表1)呈现白度高,带有中性浅蓝色泽。
表1
实施例 | 化合物(1)% | 化合物(2)% | 化合物(3)% | 白度方法a) | 白度方法b) |
4 | 63.75 | 34.75 | 1.5 | 211 | 216 |
5 | 63.0 | 34.5 | 2.5 | 211 | 215 |
6 | 62.5 | 34.0 | 3.5 | 210 | 216 |
7 | 58.75 | 37.75 | 1.5 | 208 | 216 |
8 | 39.25 | 59.5 | 1.25 | 206 | 210 |
9 | 29.5 | 69.5 | 1.0 | 204 | 210 |
10 | 20.0 | 79.0 | 1.0 | 207 | 210 |
Claims (9)
2.按照权利要求1的混合物,包括50-70重量%的化学式(1)化合物、30-50%的化学式(2)化合物及0.5-5%的化学式(3)化合物。
3.按照权利要求1或2的混合物,包括55-70重量%的化学式(1)的化合物、30-45%%的化学式(2)的化合物及0.5-3%的化学式(3)的化合物。
4.按照权利要求1-3的混合物,包括58-62重量%的化学式(1)的化合物,38-42%%的化学式(2)的化合物及0.5-3%的化学式(3)的化合物。
5.一种制备按照权利要求1定义的萤光增白剂的混合物的方法,它包括使对苯二亚甲基醛与4-二烷基膦酰甲基苄腈进行缩合,然后使所得中间产物4-氰基-4’-甲酰基二苯乙烯与2-或3-二烷基膦酰甲基苄腈进一步进行缩合。
6.一种用于增白合成纤维的组合物,它含水、按照权利要求1-4的萤光增白剂的混合物及任选的助剂。
7.按照权利要求6的增白剂组合物,包含水、及在每种情况下均按配方重量计的3-25重量%,优选5-15重量%的上述定义的荧光增白剂混合物以及0-60%的,优选5-50重量%的助剂。
8.权利要求1-4任一项用于增白合成纤维的混合物的应用。
9.权利要求8的用于增白聚酯纤维的混合物的应用。
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