两步法合成双氰胺工艺

采用两步法由氰氨化钙合成双氰胺,通过正交试验,考察了水解温度、聚合温度、聚合时间对产品收率的影响,确定了最佳的工艺条件:水解温度42℃、聚合温度70℃、聚合时问150 min,此条件下,双氰胺收率可达85.73％。     

Zinc Coated Steel/Epoxy Adhesive Systems: Investigation of the Interfacial Zone by FTIR Spectroscopy

The present study takes advantage of the ability of Fourier Transform Infrared Spectroscopy (FTIR) for the analysis of ultrathin organic films on metals. FTIR in the reflection mode (IRRAS) is used in order to study the interaction of ultrathin films of dicyandiamide (hardener of most one-pack epoxy resins) with various substrates, model ones such as gold or zinc and industrial ones such as steel and zinc-coated steels.

Pure zinc surfaces and, to a lesser extent, zinc-coated steels are shown to react with dicyandiamide after heating at 180°C, as evidenced by the frequency shift of the absorption band (at about 2200 cm^-1) characteristic for nitrile groups. As real systems consist of thick layers of a fully formulated adhesive cured onto a metallic substrate, the direct investigation of such a buried interphase is no longer possible by FTIR and by most of the known spectroscopies. Some mechanically tested specimens are then analysed, after failure, by FTIR microspectrometry. The spectra obtained, corresponding to the fracture initiation zone which is about 100 μm in diameter, advocate for the presence of an ultrathin layer of modified polymer still covering the substrate.     

利用腈纶废丝合成絮凝剂PAN—DCD

本文以腈纶废丝为原料与双氰双胺在碱性溶液中反应，成功地制得含有多种活性基因的聚合物ＰＡＮ－ＤＣＤ，并用于染料废水脱色及炼油厂废水除油，除酚的处理研究，与常规使用的几种絮凝剂进行处理结果对照，实验结果表明：该产品单独使用处理效果明显优于其他絮凝剂，与聚铝复合使用处理效果更为理想。     

The synergistic effect of dicyandiamide and resorcinol in the curing of epoxy resins

The synergistic effect of dicyandiamide (Dicy) and phenolic substances was studied, with resorcinol as a model compound. It was found that when Dicy and resorcinol are used jointly, the curing temperature of epoxy resin can be significantly lowered. FTIR and DSC data were used to illustrate the mechanism of the synergism. The addition of the phenolic hydroxyl group to epoxide was facilitated by Dicy, which favors the formation of phenoxy anions. The reaction of Dicy with epoxide was facilitated by resorcinol, which can exert “electrophilic assistance” for the addition of the amino group to epoxide. The presence of resorcinol also favors the addition of the hydroxyl group to the cyano group. The thermal and mechanical properties of the epoxy resins cured with Dicy/resorcinol or Dicy/phloroglucinol were studied. © 2003 Wiley Periodicals, Inc. J Appl Polym Sci 89: 1869–1874, 2003     

2—氨基—4—甲氧基—6—甲基均三嗪的合成

着重介绍了2-氨基-4-甲氧基-6-甲基均三嗪的合成方法。     

双氰胺/环氧粉末涂料的研究

以E-12环氧树脂为基础树脂、双氰胺(Dicy)为固化剂、2-甲基咪唑(2-MI)为促进剂,并配以其他助剂,经熔融共混制备出双氰胺/环氧粉末涂料。考察双氰胺、2-甲基咪唑用量对固化反应、涂膜附着力及耐冲击性的影响,并确定了两者的较佳用量。利用非等温差示扫描量热法研究了环氧/双氰胺/2-甲基咪唑体系的固化反应,并通过动力学分析得出了理论固化温度等固化动力学参数。在此基础上,根据实验得到了较好的固化时间和固化温度。另外,根据Kissinger和Crane方程拟合了固化反应动力学方程。结果表明,涂膜附着力及耐冲击性随着双氰胺及2-甲基咪唑用量增加先提高后减小。双氰胺、2-甲基咪唑用量分别为环氧树脂用量的4.00%、0.40%时,体系固化温度较低,130.00°C下固化30 min所得涂膜综合性能最好。     

温度和组成对苄基二甲胺/双氰胺/环氧树脂体系固化反应历程的影响

本文用红外光谱法研究了温度和组成对苄基二甲胺催化双氰胺固化环氧树脂体系的固化反应历程的影响.结果表明在100℃和170℃均不利于醚化竞争反应,体系中环氧树脂和叔胺量越少,越不利于醚化反应.在100℃环氧基只与伯氨基进行加成反应.但在140℃或170℃,除了环氧基与氨基的加成反应外,还包括氰基与体系中羟基和环氧基反应形成亚氨醚键,然后经重排反应得到含有酰胺键的化合物.     

间甲苯胺改性双氰胺固化环氧树脂的DSC研究

采用化学改性合成的间甲苯胺改性双氰胺衍生物作为环氧树脂潜伏性固化剂，通过差示扫描量热法（DSC）研究了间甲苯胺改性双氰胺／环氧树脂E-44体系的固化反应。结果表明，间甲苯胺改性双氰胺与双氰胺相比，具有较高的固化反应活性，显著降低了固化反应的温度，而且间甲苯胺改性双氰胺／环氧树脂E-44体系也具有较好的贮存稳定性。同时间甲苯胺改性双氰胺／E-44环氧树脂体系的动力学研究也表明该固化体系的活化能明显降低，固化反应活性与未改性前相比，有很大程度的提高。     

双模板分子印迹聚合物在奶粉检验中的应用研究

采用本体聚合法制备三聚氰胺(MEL)与双氰胺(DCD)双模板分子印迹聚合物(MEL/DCD-MIPs),将其作为固相萃取介质,实现了奶粉中MEL与DCD富集与纯化,建立了奶粉中两种物质同时检测的方法。通过热力学、选择性和动态结合试验表明,与单模板分子印迹聚合物相比,双模板分子印迹聚合物由于双模板-功能单体分子间的多位点协同作用而有更好的印迹效应,对MEL和DCD结合能力高于结构类似物三聚氰酸(CYA)。固相萃取试验显示,MEL/DCD-MIPs可以从市售奶粉中选择性地分离、富集MEL与DCD,对MEL与DCD的加样回收率分别为93.1%~100.1%和75.7%~82.5%,RSD均小于5.2%。所制得的MEL/DCD-MIPs可应用于奶粉等食品中氰胺类物质的检测。     

对双胍基苯甲酸盐酸盐的合成

实验以对氨基苯甲酸、双氰胺为原料,在盐酸存在下,经对氨基苯甲酸直接与双氰胺反应,一步合成对双胍基苯甲酸盐酸盐。较佳反应条件为:n(盐酸):n(对氨基苯甲酸)=1.0:1,反应温度80℃,反应时间6.0h,收率约86%,双胍基苯甲酸盐酸盐质量分数大于97%。