AEO3季铵化衍生物的制备

本文讨论了由ＡＥＯ３催化胺化制得的叔胺同氯甲烷和氯化苄之间的季铵化反应并制得了由ＡＥＯ３衍生的三种季铵盐。     

脂肪醇醚的催化胺化及其季铵化衍生物的制备

描述了用带气相循环的１０Ｌ反应系统进行醇醚（ＡＥＯ３）的催化胺制备醚叔胺的工艺以及醇醚叔胺的氯甲烷季铵化反应,制得两种醇醚叔胺及其季铵化衍生物,其中双烷基醚胺含量〉７０％,单烷基醚含量〉６５％,两种季铵盐活化物浓度为４０％,未反应胺〈１．３％。     

二硬脂酰二甲基氯化铵(DSDMAC)作织物柔软剂

在阳离子表面活性剂中，脂肪胺和季胺盐型阳离子应用越来越广泛，其中用量最大的是织物柔软剂。织物柔软剂的品种很多，但在美国和西欧大量销售的还是DSDMAC。它是二硬脂酰一甲基叔胺不用氯甲烷改用硫酸二甲酯季胺化的产物，在衣服洗涤后的漂     

叔胺及季铵盐的合成和应用

1 前言胺类萃取剂的研究和应用始于本世纪四十年代末期,较磷系萃取剂出现得较晚,但其发展迅速,现已广泛应用于化学工业和湿法治金工业。胺类萃取剂包括伯胺、仲胺、叔胺和季铵盐,其中伯胺、仲胺应用很少,应用较多的是叔胺和季铵盐,其分子结构示意如下:     

乙氧基化三酯基季铵盐的性能研究

考察了不同平均EO数的乙氧基化二酯基季铵盐的柔软性、再润湿性、去污力和对织物白度的影响等性能,并分别与单、双、三和混合酯基季铵盐进行了对比。结果表明,3EQDMS-6EO是一种性能良好的新型柔软剂,其柔软性与MEQDMS相近,再润湿性优于MEQDMS、EQDMS和2EQDMS,多次处理后对织物白度影响不大,具有酯基季铵盐所不具备的去污力。     

乙氧基化三酯基季铵盐的合成与性能

以硬脂酸和三乙醇胺为原料合成硬脂酸三乙醇胺三酯,对该酯先进行乙氧基化改性,再进行季铵化反应得到了不同平均EO数的乙氧基化三酯基季铵盐——乙氧基化三硬脂酸乙酯基甲基硫酸甲酯铵(3EQDMS-nEO)。采用IR和1HNMR对产物结构进行了表征。考察了不同平均EO数的乙氧基化三酯基季铵盐的柔软性、再润湿性、去污力和对织物白度的影响等性能,并与硬脂酸乙酯基羟乙基甲基硫酸甲酯铵(EQDMS)进行了对比。结果表明,3EQDMS-6EO是一种性能良好的新型柔软剂,其柔软性与EQDMS相近,再润湿性优于EQDMS,多次处理后对织物白度影响不大,具有EQDMS所不具备的去污力。     

合成双棉籽油基二甲基氯化铵新工艺的研究

双脂肪烷基季铵盐类产品是一种性能优良的织物柔软剂。在烷基链中引入不饱和键,经处理后织物的亲水性得到提高。以棉籽油基伯胺为原料合成了棉籽油基仲胺,再将棉籽油基仲胺季铵化,合成了双棉籽油基二甲基氯化铵。经放大实验,产品具有优良的柔软性,且具有更好的织物润湿性和生物降解性。     

单,双和三长链烷基叔胺及其季铵盐制备技术新进展

综述了单、双和三长链烷基叔胺及季铵盐的合成技术新进展。从传统的脂肪酸法，脂肪醇经氯代烷胺化法以及近年来国内外开发的新路线。重点介绍了脂肪醇常压一步法制叔胺的新方法，也涉及到脂肪肪酸甲酯、醇醚与原料催化胺化制叔胺的最新进展和各种路线的比较。     

双酯柔软剂2,3-二(硬脂酰氧基)-丙基三甲基胺季铵盐的合成

合成了一种织物柔软剂2,3-二(硬脂酰氧基)-丙基三甲基胺季铵盐,通过正交实验研究了反应温度、反应物的摩尔比等因素对酯胺化反应的影响。从而确定了酯胺化反应的最优反应条件:n(硬脂酸)/n(3-二甲胺基-1,2-丙二醇)=1.8,190℃反应8 h。在最优条件下,制得的酯胺的酸价为0.75 mg KOH/g。用红外光谱和核磁共振氢谱对酯胺的结构进行了表征。最后,与硫酸二甲酯进行季铵化反应,得到了目标产物。     

研发动态

甲基二乙氧基硅烷季铵盐惠州工学院的彭忠利等人以3-氯丙基甲基二乙氧基硅烷和叔胺为原料,合成了甲基二乙氧基硅烷季铵盐;考察了溶剂、反应时间等对甲基二乙氧基硅烷季铵盐的影响。较佳的反应条件是:在N2氛围中,以乙醇为溶剂回流反应40h。产品色泽较好,季铵盐质量分数达80%以上     

几种常用织物柔顺剂的性能研究

通过研究6种柔顺剂原料对织物的白度、柔软性能、表面抗静电性能及再润湿性能的影响,得出氨基硅油乳液、酰胺季铵盐与咪唑啉季铵盐对方巾白度影响较大;双烷基二甲基季铵盐柔软效果最好,聚醚硅油柔软效果最差;季铵盐类柔顺剂抗静电效果优于硅油类柔顺剂;酯基季铵盐与双烷基二甲基季铵盐的再润湿性能较差。     

含酯基Gemini季铵盐柔软剂的合成工艺研究

以2-二甲氨基乙醇、硬脂酸为原料,合成了二甲基硬脂酸乙酯基叔胺,再与由十八烷基二甲基叔胺(DMA18)和环氧氯丙烷(ECH)为原料合成的中间体氯化铵反应,合成了一种含酯基的Gemini季铵盐柔软剂。通过单因素实验和正交实验考察了反应的影响因素。确定二甲基硬脂酸乙酯基叔胺的优化工艺条件为:n(2-二甲氨基乙醇)∶n(硬脂酸)=1.15∶1,反应温度100～110℃,m(甲苯)∶m(2-二甲氨基乙醇)=1.3∶1,反应时间7h,w(次磷酸)=1.0%,收率达96.6%以上;中间体氯化铵的优化工艺条件为:n(ECH)∶n(DMA18)=0.95:1,w(异丙醇)=50%,反应温度40～50℃,反应时间60min,收率达90.9%以上;含酯基Gemini季铵盐柔软剂的优化工艺条件为:n(中间体氯化铵)∶n(二甲基硬脂酸乙酯基叔胺)=1∶1.1;反应温度100℃;反应时间10h,收率达95.3%以上。该合成工艺已在河南省道纯化工技术有限公司成功进行了500L中试。     

双季铵盐杀菌剂的合成

以十二胺、甲酸和甲醛为原料制备出中间体长链叔胺，又以长链叔胺和1，3-二溴丙烷合成出双季铵盐杀菌剂，研究了长链叔胺和双季铵盐的合成工艺条件，应用红外光谱对其结构进行表征，双季铵盐收率可达85．4％。     

Studies in the development of antibacterial surfactants. I. institutional use of antibacterial fabric softeners

Summary It has been determined that the incorporation of a highly active antibacterial agent, phenylmercuric propionate, into an aqueous solution of a fabric softener of the quaternary ammonium type results in a most effective antibacterial laundry rinse additive. The presence of the quaternary ammonium compound appears to enhance the antibacterial activity of the mercurial. When applied at a level of 63 parts of available mercurial to one million parts of fabric, the treated cloth is rendered bacteriostatic to several strains ofS. aureus and to ammonia-producing organisms of theProteus group, also mildewstatic toChaetomium globosum. The formulated antibacterial softener as well as the treated linens appear to be entirely safe to humans. In longer-term application tests in a hospital laundry the total bacterial load carried by the soiled treated linens is practically zero. There is no excessive build-up of antibacterial agent on fabric upon repeated applications, and it is readily washed out of the fabric by conventional laundering.     

Alkyldimethylamine oxides as synergistic fabric softeners

The interaction of solid alkyldimethylamine oxide and ditallowdimethylammonium chloride (DTMAC) and ditallow dimethylammonium sulfate (DTMAS) quats in representative types of fabric softener systems was studied with particular focus on synergistic behavior. Softening, whiteness retention, wetting, static build-up and detersiveness were evaluated for laundry rinses, laundry detergents and dryer sheets. In laundry rinses, blends of amine oxide and DTMAC proved to be synergistic for improving the wetting of cotton towels. Although no synergism was observed in laundry detergents, formulations containing amine oxide gave better detersiveness than systems with DTMAC without the splotching associated with the quaternary salt. In dryer sheets, it was discovered that blends of amine oxide and DTMAS gave synergistic softening of cotton towels and were unexpectedly effective in preventing static charge build-up on polyester fabric.     

Cationic surfactants in laundry detergents and laundry aftertreatment aids

Cationic surfactants have a positively charged nitrogen atom and at least one hydrophobic, long-chain substituent in the molecule. Because of their fabric-softening and antistatic properties, they are used as active materials in fabric-softening agents. Suitable cationic surfactants are mostly quaternary ammonium salts, and to a lesser extent, imidazolinium salts with two long hydrophobic alkyl chains. Alkylated, partly ethoxylated polyamines, amine amides, ester amines and di-quaternary compounds also have recently been used or proposed. Fabric softeners generally are aqueous dispersions of distearyl dimethyl ammonium chloride or tallow alkylated imidazolinium derivatives in concentrations of 1–9%. Concentrated fabric softeners have recently been pushed into the market as double, triple or 10-fold concentrates. Fabric softeners used in the forms of acrosol sprays, pads or sheets, are not used in the washing machine but can be used in the laundry dryer. The combination of laundry detergent and fabric softener is a single product is impaired by anionic surfactants normally contained in laundry detergents because they react with the cationics to form neural salts. With the so-called soft detergents, one attempts to circumvent these difficulties by means of special formulations, e.g., with nonionics or by using definite physical-chemical mechanisms. They represent a compromise with regard to detergency performance and softening effect.     

Microscopy Study of Distribution of Laundry Fabric Softener on Cotton Fabric

Distribution of fabric softeners on cotton terry cloth was studied using scanning electron microscopy and energy dispersive X-ray analysis. The unsaturated groups in the quaternary fabric softeners were tagged with osmium tetroxide to provide contrast in the microscopy. Longitudinal specimens showed the fabric softeners distributed over the cotton fiber surfaces with more in the crenulation of the fiber. Cross sectional specimens revealed that the fabric softener was distributed throughout the cotton fibers with higher concentrations of fabric softener observed in the lumen and crenulation than in the secondary wall and non-crenulated fiber surface. This distribution of fabric softener is consistent with deposition on both external fiber surfaces and internal fibril surfaces. The deposition and final surface coverage is strongly dependent on the pH value of the washing medium. Repeated treatment cycles with fabric softener using a higher pH washing media resulted in higher concentrations of fabric softener on and within the cotton fibers. Neutral or lower pH washing media resulted in a somewhat constant concentration of fabric softener on and with cotton fibers with increased number of treatment cycles. Differences in perception of softness of the treated fabrics are not explained by differences in distribution of the fabric softener; it appear that there is an optimum amount of softener to achieve the desired sensory response and that further deposition build-up does not increase perception of softness.

酯基有机硅季铵盐柔软整理剂的合成与表征

以硬脂酸和N-甲基二乙醇胺(MDEA)为原料进行酯化反应得到中间体硬脂酸甲基二乙醇胺酯,再与γ-氯丙基甲基二甲氧基硅烷季铵化反应制备二烷基酯基甲基二甲氧基硅烷季铵盐。通过单因素和正交实验,考察了反应温度、反应时间、反应物摩尔比及催化剂用量等对酯化反应的影响。酯化反应优化工艺条件:反应温度为180℃,反应时间为8 h,反应物摩尔比n(硬脂酸)∶n(MDEA)=1.6∶1.0,次磷酸催化剂质量分数为0.9%,转化率达98%;二甲基亚砜作为季铵化反应的溶剂。通过溴酚蓝显色反应以及红外光谱、1HNMR、ESI-MS分析中间体和产物的结构。测定了目标产物在298 K下的表面活性以及柔软性能,临界胶束质量浓度CMC为0.197 g/L,γCMC为24.25 mN/m,柔软性能优于同类市售产品。     

季铵化改性氨基硅油的应用研究

本文采用环氧丙基十二烷基二甲基氯化铵对氨基硅油进行季铵化改性,合成了一种新型季铵化改性氨基硅油柔软剂。对氨基硅油及其改性产物进行乳化,可得到性能稳定的柔软剂乳液。将所得乳液在纯棉平纹织物和涤纶织物上进行了柔软整理。测试结果表明:该新型季铵化改性氨基硅油柔软剂可使织物的柔软性、抗黄变性和亲水性显著提高。在应用于涤纶织物时,可以获得良好的抗静电效果。