新型双季铵盐二氯化N,N-双(十二烷基二甲基)-3-氮杂-1,5-戊二胺杀菌剂的合成

新型杀菌剂双季铵盐以其杀菌效果好、毒性低、水溶性好等特点在工业中具有广泛应用前景。本文以十二胺、甲酸和甲醛为原料制备出中间体十二烷基二甲基叔胺,以二乙醇胺、氯化亚砜为原料合成连接基团分子2,2-二氯二乙胺,将合成的二种中间体进行加成反应得到二氯化N,N-双(十二烷基二甲基)-3-氮杂-1,5-戊二胺——一种新型双季铵盐。实验考察了十二烷基二甲基叔胺、2,2-二氯二乙胺以及双季铵盐的合成工艺条件,以单因素法考察了反应时间、反应温度及醇胺/氯化剂配比对合成产物的影响,筛选了较适宜的工艺条件。结果表明:在十二烷基二甲基叔胺的合成中,较适宜的总反应时间为12h左右;在2,2-二氯二乙胺的合成中,较适宜的n(二乙醇胺)∶n(氯化亚砜)为1∶2.5,反应时间为2h;在双季铵盐的合成中,较适宜的反应温度为80℃,反应时间为4h,在此工艺条件下,双季铵盐的收率可达81.2%。     

双季铵的合成及其反应动力学研究

长链烷基叔胺和1，2-二溴乙烷以1：1和2：1摩尔比反应，得到单季铵盐和双季铵盐。比较了不同链长、极性和非极性容剂及反应温度对反应速率的影响，经动力学推导和计算，求得反应速率常数k，，初步推断了反应级数。对化合物进行了元素分析、IR、CMR、DTA、TLC等分析和测试。     

含咪唑啉环不对称双季铵盐的合成及其缓蚀性能

以长链烷基叔胺、长链烷基叔胺盐酸盐、环氧氯丙烷为原料合成了N-(3-氯-2-羟丙基)-N,N-二甲基长链烷基季铵盐,利用其与长链烷基咪唑啉季铵化合成了含咪唑啉环的不对称双季铵盐。通过FTIR,1HNMR验证了中间体和目标产物结构,考察了其合成工艺。合成含咪唑啉环不对称双季铵盐的最佳反应条件为:n[N-(3-氯-2-羟丙基)-N,N-二甲基长链烷基季铵盐]∶n(长链烷基咪唑啉)=1∶1.1,反应溶剂采用异丙醇,反应温度80℃。用失重法测定了25℃时含咪唑啉环不对称双季铵盐在1.0mol/L盐酸溶液中的缓蚀性能,结果表明,仅添加50mg/L,对Q235钢缓蚀率达98.89%。     

一锅煮法合成联结基团含羟基的季铵盐Geminie表面活性剂

以长链烷基叔胺、环氧氯丙烷、浓盐酸一锅煮的方法合成了联结基团含羟基的季铵盐Gemini表面活性剂。较佳合成条件为：反应物最佳配比为n（叔胺）：n（浓盐酸）：n（环氧氯丙烷）=2．2：1．1：1．0，反应时先加长链叔胺和盐酸，使之充分反应后再加环氧氯丙烷，在乙醇中回流条件下反应16h，收率达93．5％。     

双季铵盐杀菌剂的合成及其杀菌性能研究

利用自制的双卤代醚与长链叔胺,合成了双季铵盐杀菌剂,并对其结构进行了红外表征,评价了其杀菌效果,并与12 2 7进行了杀菌性能的对比。实验结果表明:双季铵盐对SRB具有良好的杀菌性能,而且杀菌能力也明显优于12 2 7,在菌量较高的情况下(1.5×10 8个·mL-1)杀菌浓度仅为5 0mg·L-1,就能10 0 %杀死SRB ,是一种很有应用前景的新型杀菌剂。     

新型阳离子表面活性剂γ—双季铵盐的合成（II）

本文以不同碳链的脂肪伯胺、丙烯腈和氯甲烷为原料合成新型阳离子表面活性剂－γ－双季铵盐系列产品，该以季铵盐广泛应用于沥青乳化、矿石浮选、织物整理等领域。     

含酯基不对称双季铵盐表面活性剂的合成

以长链烷基叔胺、盐酸、环氧氯丙烷为原料,合成了N (3 氯 2 羟丙基) N,N 二甲基长链烷基氯化铵,研究了其合成工艺,优化反应条件为:n(长链烷基叔胺)∶n(盐酸)∶n(环氧氯丙烷)=1∶1∶1 1,反应温度为40℃,体系pH=6～7。以月桂酸及2 二甲氨基乙醇为原料,酯化得到二甲基月桂酸乙基叔胺(Ⅲ),利用其与N (3 氯 2 羟丙基) N,N 二甲基长链烷基氯化铵季铵化得到含酯基不对称双季铵盐阳离子表面活性剂〔长链烷基分别为(Ⅰ)C12H25和(Ⅱ)C14H29〕。经测定,产物的临界胶束浓度CMC分别为6 61×10-3、8 31×10-3mol·L-1,γCMC分别为37 6、39 2mN·m-1,证明所合成的含酯基不对称双季铵盐阳离子表面活性剂具有较高的表面活性。     

季铵盐型双子表面活性剂的合成和性能

以烷基二甲基叔胺R(CH32N(R为C12H25、C14H29和C16H33)、盐酸、环氧氯丙烷为原料合成了系列季铵盐型双子表面活性剂GnCl2(n=12,14,16),样品经核磁共振及元素分析证实其结构.研究了其水溶液的表面活性、泡沫性能和杀菌性能.结果表明,所合成的双子阳离子表面活性剂具有较高的表面活性,烷基链越长,临界胶束浓度越小;不同链长的GnCl2体系中,G12Cl2溶液的起泡和稳泡效能最高,起泡和稳泡效率最低;通过纸片扩散法测定其杀菌性能表明,双季铵盐型表面活性剂具有优良的杀菌能力.     

新型双季铵盐杀菌剂的合成及其杀菌性能研究

以乙二胺、甲酸、甲醇和氯乙酸乙酯为原料,合成了双季铵盐杀菌剂,以绿藻为模型,探讨了双季铵盐的浓度和投加时间对其杀菌性能的影响。结果表明,当双季铵盐的浓度为0.3 g/mL时,杀菌效果较好,3 d可实现79.25%的杀菌率,且投加时间越长,灭菌效果越显著。     

新型阳离子表面活性剂γ-双季铵盐的合成(Ⅱ)

本文以不同碳链的脂肪伯胺、丙烯腈和氯甲烷为原料合成新型阳离子表面活性剂——γ-双季铵盐系列产品,该双季铵盐广泛应用于沥青乳化、矿石浮选、织物整理等领域.     

新型两性Gemini表面活性剂的合成及工艺条件优化

利用两步法合成了双季铵盐一羧甲基钠盐新型两性Gemini表面活性剂,表征了结构,探讨了表面活性,优化了合成工艺条件。研究结果表明：合成产物结构与设计目标相符,表面活性优于双季铵盐阳离子Gemini表面活性剂及传统两性表面活性剂;两步最佳合成条件分别为：n叔胺：n盐酸盐：“环氧氯丙烷为2．2：1．1：1．0,反应时间16h,溶剂采用正丙醇;n双季铵盐：n氯乙酸为1．0：1．5,反应温度50℃,反应时间3．5h,NaOH浓度为20％,产物收率96．8％。     

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。     

双季铵盐类化合物的研究现状及合成进展

双季铵盐类化合物是一类具有较强杀菌活性的杀菌剂,属于Gemini表面活性剂中的一种.目前国内外对双季铵盐类化合物的结构、性质及合成已经取得很大的进展.本文简略介绍了此类化合物的结构和杀菌性能,详细阐述了其目前的研究状况和合成方法.     

The effect of different ammonium structure of quaternary ammonium resin on the electrochemical properties

The quaternary ammonium resin is synthesized by the ring-opening reaction of an epoxy resin with a tertiary amine in the presence of a proton donor in the solution. This kind of resin can be dispersed in the water phase to form a conductible milky dispersion. In this study, different kinds of tertiary amines including the full-alkyl group and the ester group-containing or urethane group containing tertiary amine are reacted with DGEBA-type epoxy resin to synthesize the quaternary ammonium resins. The resin characteristics and the electrochemical properties of its emulsion are investigated. In addition, properties of the emulsion prepared from tertiary amine salt resin are also measured for comparison. It is found that if the substituted groups of the ammonium structure of the quaternary ammonium resin are all alkyl groups, rupture voltage of the emulsion is very low. But when one of the substituted group contains an ester group or an urethane group, rupture voltage increases remarkably and the resin can be used for electrodeposition. Meanwhile, the electrodeposition theory of quaternary ammonium resin and its thermal cross-linking reaction and the electrochemical properties of coemulsion prepared by mixing the quaternary ammonium resin and the tertiary amine salt resin are also discussed. © 1993 John Wiley & Sons, Inc.     

一种有机硫杀菌剂的合成及性能评价

以对二氯苄、十二烷基二甲基叔胺、硫氰酸钠为原料,在100℃时恒温反应4 h,制备了一种含硫杀菌灭藻剂TBDA,对其杀菌性能及灭藻性能进行评价。结果表明,对于油田回注水系统,当TBDA的投加量为50mg/L时,对TGB、SRB的杀菌率达100%;对于工业循环冷却水系统,当TBDA的投加量为100 mg/L时,灭藻率为99.99%。TBDA的杀菌及灭藻效果明显优于1227及双季铵盐等常规杀菌剂。     

Use of cationic starch derivatives for the removal of anionic dyes from textile effluents

Six types of cationic starch derivatives were prepared. These types were (1) cationic starch derivatives containing primary, secondary, and tertiary amino groups and quaternary ammonium salt and (2) etherified and grafted cationic starch derivatives. These cationic starch derivatives were treated with three types of dyes, an acid dye, a hydrolyzed reactive dye, and a direct dye. Different factors affecting the dye sorption value (mmol/100 g of sample) were been studied. These factors were the pH of the medium, treatment time, amine type, amine content, dye type and molecular size, and the distance between the amine groups. The dye sorption value and the sorption efficiency percentage were determined. The dye sorption value increased with increasing amine content to a maximum value and then decreased. This phenomenon occurred with all of the amine types. The maximum dye sorption values on with the acid dye depended on the amine type. These values were 73.8 (at an amine content of 155), 90 (at an amine content of 150), 84.9 (at an amine content of 133), and 72.5 (at an amine content of 75) for primary, secondary, and tertiary amines and the quaternary ammonium salt, respectively. The sorption efficiency percentage at these maximum values were 47.6, 60, 63.8, and 96.3%, respectively. The maximum sorption values were acid dye > hydrolyzed reactive dye > direct dye. The dye sorption value and the sorption efficiency percentage of the etherified cationic starch derivatives had higher values than that of the grafted cationic starch derivatives. The prepared cationic starch derivatives that had amine contents of 155, 150, 133, and 75 m atom/100 g of sample for primary, secondary, and tertiary amines and the quaternary ammonium salt, respectively, had the best ability to adsorb anionic dyes. © 2004 Wiley Periodicals, Inc. J Appl Polym Sci 93: 227–234, 2004     

双季铵盐杀菌剂的杀菌试验研究

为解决循环冷却水的微生物问题,克服目前较多使用的一些杀菌剂的若干不足之处。本文在多种杀菌剂研究的基础上,进行了双季铵盐杀菌剂静态实验研究。发现双季铵盐具有高效低毒、作用时效长的特点,是一种优良的杀菌剂。     

有机硅季铵盐单组分环氧树脂胶的制备

研究了利用有机硅季铵盐在热分解时释放叔胺作为环氧树脂固化剂，释放多官能活性有机硅作为交联剂，从而达到潜固化和改性环氧树脂的目的。     

The electrodeposition properties of coemulsion-contained quaternary ammonium/tertiary amine salt epoxy–amine adducts and the composition analysis of its electrodeposited film

Two-component electrodepositable coemulsion-contained quaternary ammonium resin Q , as a pigment grinding vehicle, and DGEBA–N-methylethanolamine (MEA) tertiary amine salt resin T , as the principal resin, were obtained and then deposited to form a resinous film on the cathode during electrodeposition. The resin composition of this deposited film was determined by the quantitative analysis of FTIR and it was found different from the resin composition of the original coemulsion. The electrodeposition behaviors of the coemulsion were deeply affected by the quaternary ammonium resin. In addition, the electrodeposition properties of emulsions dispersed by quaternary ammonium resin and tertiary amine salt resin were also studied for comparison. © 1994 John Wiley & Sons, Inc.     

新型双季铵盐杀菌剂的合成及杀菌性能研究

季铵盐类杀菌剂是目前最常用的杀菌剂之一,常用于工业循环冷却水及油田水处理。以十二烷基二甲基叔胺、1,3-二氯丙烷为原料,合成了一种新型双季铵盐杀菌剂TA-08,并探讨了其杀菌性能。结果表明,在投加浓度为50mg/L时,TA-08的杀菌率达99.99%,明显优于1227及异噻唑啉酮等常规杀菌剂。