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《化工进展》2016,(Z2)
目前有关荧烷染料中间体的合成方法国内少有报道。2-羟基-4-(N-乙基-N-异丁基)氨基-2’-羧基二苯酮是一种重要的荧烷类压热敏染料中间体,本文以N-乙基-N-异丁基间氨基苯酚为原料与邻苯二甲酸酐在氮气保护下反应合成,并在反应后使用NaOH溶液分解副产物,以提高产物纯度,通过HPCE测定产物纯度达到96.36%(面积归一法)。使用TLC对反应进程进行监测,并通过UV对TLC检测结果进行确认,详细讨论了物料比、温度和时间等条件对反应的影响,并得出二苯酮合成反应中N-乙基-N-异丁基间氨基苯酚与邻苯二甲酸酐摩尔比为1∶1.5,温度为110℃,时间为15h时反应效果最佳。副产物若丹明染料分解反应中NaOH溶液浓度为33.3%,N-乙基-N-异丁基间氨基苯酚与NaOH的质量比为1∶7.5,温度为90℃,时间为9h时反应效果最佳。最后通过IR和UV对目标产物结构进行确认。 相似文献
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N-甲基-N-(4'-氨基苄基)-4-甲苯磺酰胺的合成包括三步反应,首先由对甲苯磺酰氯与甲胺反应得到N-甲基-4-甲基苯磺酰胺,再与对硝基苄基溴反应引入苄基,然后在铁催化剂存在下用水合肼将硝基还原,得到N-甲基-N-(4'-氨基苄基)-4-甲苯磺酰胺;该工艺重现性好,三废少,三步反应总收率81%.得到的N-甲基-N-(4'-氨基苄基)-4-甲苯磺酰胺与溴胺酸反应即得C.I.酸性蓝264,该染料染色时对染浴的pH不敏感、竭染率高、水洗牢度好. 相似文献
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以全氟丁基磺酰氟与N,N’-二甲基-1,3-丙二胺为原料制备得到全氟丁基磺酰胺,然后分别与己基磺酰氯和辛基磺酰氯反应得到带烷基支链的全氟丁基磺酰胺,最后将两中间产物与过氧化氢氧化得N’-3-(二甲基)-丙基-(N-全氟丁基磺酰基-N-烷基磺酰基)-亚胺氧化物。通过MS和1H NMR等方法对产物进行了表征,表面张力等性能测试表明,产物具有较好的表面活性,可以作为全氟辛基磺酰胺类表面活性剂的替代品。 相似文献
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报道了9-[(4氟-)-3羟-基甲基丁基]鸟嘌呤(FHBG,Ⅱ)的改进合成方法,对起始原料喷昔洛韦(Ⅲ)的氨基和一个羟基用4-甲氧基氯化三苯甲烷保护,对另一个羟基磺酯化,得到N2-(p-甲氧基苯酰基二苯基甲基)-9-[(4甲-苯磺酰)-3-p-甲氧基苯酰基二苯基-甲氧基甲基丁基]鸟嘌呤(Ⅴ),收率为70.5%;再用四丁基氟化铵(TBAF)对化合物Ⅴ亲核取代4-甲苯磺酰基团,水解脱去保护基,即得FHBG。产品经1HNMR、IR、MS表征,并用HPLC分析了Ⅴ和Ⅱ,保留时间分别为5.89 m in和4.41 m in,积分计算质量分数分别为w(Ⅴ)=99.5%和w(Ⅱ)=99.3%。 相似文献
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用DTA和XRD方法研究了K_2O-Al_2O_3-WO_3三元系中Al_2(WO_4)_3-K_2O和Al_2(WO_4)_3-K_2WO_4截面相平衡关系。在Al_2(WO_4)_3-K_2O赝二元系中由包晶反应形成三个化合物:2Al_2(WO_4)_3·K_2O_4、Al_2(WO_4)_3·K_2O和Al_2(WO_4)_8·3K_2O。其包晶反应温度分别为937±3℃、786±3℃和902±3℃。在Al_2(WO_4)_3-K_2WO_4截面中,33.3mol%K_2WO_4和50mol%K_2WO_4组份其主要成份分别为2Al_2(WO_4)_3K_2O和Al_2(WO_4)_3K_2O。 相似文献
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Photoluminescence properties of Eu-doped WO3-Eu2(WO4)3 composites and single-phase Eu2(WO4)3 powders
《Ceramics International》2022,48(2):1560-1566
The development of highly stable and efficient oxide-based red phosphors is urgently required for next-generation lighting devices. Herein, we report the micro/crystal structures and luminescent properties of single-phase Eu2(WO4)3 and Eu3+-doped WO3-Eu2(WO4)3 composite phosphors prepared by a one-step conventional solid-state reaction method in air atmosphere. As increasing Eu contents in the mixtures of WO3 and Eu2O3, the intensities of the X-ray diffraction peaks of Eu2(WO4)3 increased while that of WO3 decreased. The photoluminescence intensity of the synthesized phosphors increased with increase in the Eu content when calcined at 900 °C, while it degraded at a higher temperature. Red-emitting single-phase Eu2(WO4)3 powders were successfully obtained when the WO3 and Eu2O3 powders were calcined in the ratio of 3:1. The intensity of the red emission spectra of the Eu2(WO4)3 phosphor was higher than those of the 6, 12, and 24 at.% Eu-added WO3 composites at excitation wavelengths of 394 and 465 nm. On the other hand, the intensity of emission from the single-phase phosphor was lower than that of the Eu-doped WO3-Eu2(WO4)3 composites under excitation of UV light at 254 nm. Thus, we propose two prospective phosphors for application as red phosphors at various wavelengths. 相似文献
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Yong K. Kim A. William Frazier Cheryl L. Griffin 《Nutrient Cycling in Agroecosystems》1989,20(2):115-121
Solubility data were obtained in the system CO(NH2)2-NH4NO3-H3PO4-H2O at 0° and 15°C. The results show that high-analysis solution fertilizers can be produced from standard urea-ammonium nitrate (UAN) and phosphoric acid materials. These acidic solution fertilizers contain up to 35% total plant nutrient (TPN = N + P2O5 + K2O), with N:P2O5 ratios varying from 20:1 to 1.5:1. Potential liquid products having fertilizer grades of 23-12-0, 26-9-0, 28-6-0, and 31-3-0 are feasible. 相似文献
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4-Hydroxy-2-trans-nonenal, the most abundant and toxic unsaturated aldehyde generated during membrane lipid peroxidation, was synthesized starting
from fumaraldehyde dimethyl acetal. In the first step of the synthesis, the fumaraldehyde dimethyl acetal was partially hydrolyzed
using amberlyst catalyst to obtain the monoacetal. The 4-hydroxy-2-trans-nonenal was synthesized by the Grignard reaction of the fumaraldehyde monoacetal with 1-bromopentane. 4-Hydroxy-2-trans-nonenal, obtained as its dimethylacetal, was oxidized to its corresponding 4-keto derivative using pyridinium chlorochromate
buffered with sodium acetate as the oxidizing agent. 4-(3H) 4-Hydroxy-2-trans-nonenal was obtained in one step by the sodium borotriteride reduction of the 4-keto derivative. 相似文献
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Raman spectra of (NH4)4H2(SeO4)3 protonic conductor were studied at room temperature using a 1064 nm - excited Fourier transform (FT) - Raman spectroscopy. A tentative assignment of the external and internal vibrations is proposed. 相似文献
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