合成硝基麝香溶液结晶分离研究

为了开发低共熔组成酮麝香、二甲苯麝香混合物溶液结晶新过程,计算得到酮麝香、二甲苯麝香、溶剂三元相图。在此基础上研究了麝香混合物溶液结晶分离方法,提出了轮流加入乙腈和庚烷从低共熔组成麝香混合物中,分级冷却结晶分离得到2种产品的过程。由三元相图得到理论产量并进行试验验证,结果表明加入乙腈一级结晶可得到纯度为97.5%的二甲苯麝香,加入庚烷二级结晶后酮麝香的纯度为98.1%。     

气相色谱串联质谱法测定儿童护肤用品中10种合成麝香

建立了采用气相色谱串联三重四级杆质谱(GC-MS/MS)同时测定护肤品中10种人工合成麝香的分析方法。其中包括萨利麝香(ADBI)、粉檀麝香(AHMI)、佳乐麝香(HHCB)、特拉斯麝香(ATII)、吐纳麝香(AHTN)、二甲苯麝香(MX)、伞花麝香(MM)、葵子麝香(MA)、西藏麝香(MT)、酮麝香(MK)。样品用乙酸乙酯进行超声萃取,DB-WAXetr(30 m×0.250 mm×0.25μm)毛细管色谱柱分离,对碎片离子进行选择性扫描,以离子丰度比定性,外标法定量。实验数据显示:10种人工合成麝香在1～25 ug/L范围内线性关系良好,相关系数均大于0.996,当加标水平在0.25～1.25 mg/kg时,回收率为89.2%～96.1%,相对标准偏差(RSD,n=6)为3.4%～5.6%,方法的最低检出限(S/N=3)为0.4 mg/L～0.6 ug/L,满足检测要求。     

气相色谱-质谱法检测日用香精中3种禁用麝香物质

建立了一种同时检测日用香精中葵子麝香、伞花麝香和西藏麝香等3种禁用麝香类物质的气相色谱-质谱(GCMS)方法,采用外标法结合离子(SIM)扫描对3种物质进行了定性定量分析。结果表明:该方法在质量浓度0.001到0.500 mg/mL范围内的响应线性关系良好,相关系数均大于0.9980;检出限为0.005μg/mL(S/N≥3)。在100μg/mL和200μg/ml加标浓度下,三种麝香的回收率在80%至120%之间,精密度10%,重复性较好。该方法满足分析检测要求,可用于日用香精中葵子麝香、伞花麝香和西藏麝香的定性定量分析。同时将此方法应用到不同薄荷香精样品中3种禁用麝香类物质的检测,未检测到目标化合物。     

粉檀麝香的合成研究

用均匀设计对粉檀麝香中间体 1,1,2 ,3,3,5 -六甲基茚满 (HMI)合成实验条件进行优化 ,使HMI的收率提高 7% ,达到了 5 7%。进而对HMI用乙酰氯进行酰化合成出合格的粉檀麝香产品 ,其总收率可达 48.1%     

气相色谱-质谱联用法测定驱蚊产品中6种合成麝香

[目的]建立气相色谱-质谱联用法分离测定驱蚊产品中萨利麝香、葵子麝香、酮麝香、佳乐麝香、吐纳麝香、二甲苯麝香6种合成麝香定性定量的分析方法。[方法]采用TG-1MS,30 m×0.25 mm×0.25μm毛细柱和质谱(EI离子源)检测器,同时测定试样中6种合成麝香的含量。[结果] 6种合成麝香(萨利麝香、葵子麝香、酮麝香、佳乐麝香、吐纳麝香、二甲苯麝香)在1.0～100 mg/L质量浓度范围内线性关系良好,线性相关系数R为0.9927～0.9987;方法检出限(3S/N)为0.015～0.052 mg/L;定量限(10S/N)为0.049～0.173 mg/L;相对标准偏差(RSD)为0.6%～1.9%;平均回收率为81.3%～107.2%。[结论]该方法操作简便,分离效果好,精密度与准确度高,可同时快速测定驱蚊产品中6种合成麝香的含量。     

麝香保心丸治疗冠心病心绞痛的临床观察

目的 是应用麝香保心丸治疗冠心病心绞痛无明显不良反应.方法 选择用口服消心痛不能耐受的20例服用麝香保心丸为治疗组,20例用消心痛作为对照组进行观察.结果 麝香保心丸治疗组心绞痛症状疗效总有效率为85%.心电图疗效总有效率为60%;对照组心绞痛症状疗效总有效率为55%,心电图疗效总有效率为45%;两组有显著差异性,但治疗组无明显不良反应.     

佳乐麝香的合成及其应用

概述了佳乐麝香的理化性质和香气特征,对佳乐麝香的合成工艺进行了综述,并介绍了佳乐麝香的应用.     

酮麝香与二甲苯麝香体系相平衡研究

为了判断酮麝香、二甲苯麝香固相存在状态,改进Lennard-Jonnes位能函数后得到了适用于极性和非极性分子的位能函数式,计算得到酮麝香、二甲苯麝香体系相互作用能量参数λ,结合NRTL方程计算确认酮麝香、二甲苯麝香为简单低共熔体系,采用差分扫描量热热分析法进行了实验验证。     

日用化学品用合成麝香

简要介绍了合成麝香的分类及其代表物质,综述了目前合成麝香的毒性研究成果,比较了我国和欧盟对于合成麝香在化妆品中添加量的法规限定,阐述了日化产品中合成麝香的主要前处理和仪器检测方法,并对未来合成麝香的研究进行了展望。     

麝香类香料的合成研究进展

结合当前法规现状综述了天然麝香主要香气成分的研究进展以及麝香类香料的合成方法和几种合成麝香的研究现状,重点介绍了以手性香茅醛为原料合成左旋麝香酮的各种路线,以及第四代麝香中应用较为广泛的几个脂环麝香的制备工艺,并提出了自己的观点。最后对合成麝香的发展前景进行了展望。     

酮麝香，二甲苯麝香溶液结晶研究

1 INTRODUCTION Musk ketone and musk xylene are important syn- thetic nitro-musks. They are high boiling substances and subject to decomposition under the condition of heat and light. When they are melted, the liquid mix- ture is very sticky, which lead to high resistance to heat and mass transfer and difficulty in solidification. As a result, it is reasonable to employ solution crys- tallization to separate and purify musk mixture. As the basis of solution crystallization, the solubility …     

杂多酸固相催化合成麝香DDHI的研究

以杂多酸为催化剂 ,2 ,6 二异丙基酚 (DIPP)与异戊二烯 (IP)经环烷基化反应合成麝香DDHI。研究了催化剂种类和用量、原料配比、反应温度及时间对反应结果的影响。反应最佳条件为∶催化剂为磷钨酸固载于活性炭上 ,n(DIPP)∶n(IP) =2 .0 ,m(C1)∶m(IP) =0 .8～ 0 .9,反应温度 36℃～ 4 2℃ ,滴加时间 2h ,保温时间 1h ,产品收率 83.7%。     

麝香T生产工艺的改进

对麝香T的主要生产过程－聚合、解聚、精馏、脱色、过滤的改进进行了论述，提出了比较理想的操作条件和操作过程。新工艺粗品的收率由70％－75％提高到90％－92％，纯度由90％－92％提高到95％以上，外观亦有很大改善，而且聚合、解聚由30h缩短为23－34h，精馏缩短1／3，同时大大降低了生产成本。     

西藏麝香合成新工艺

以催化重整C9芳烃分离装置分离出均三甲苯、偏三甲苯后的副产品重组分溶剂(169～178℃馏分)—混合C9芳烃为原料,其中含连三甲苯40%～50%,以三氯化铝为催化剂与异丁烯进行烷基化反应,合成出5 叔丁基 1,2,3 三甲基苯中间体,经蒸馏后,用混酸进行硝化反应得到西藏麝香。本方法不但具有工艺路线简单,生产成本低的特点,同时也解决了富集连三甲苯的利用问题。     

Background,importance and production volumes

The importance of the fatty acid industry today is reflected by the estimated 1978 production in the U.S. of 956 M lbs., exclusive of tall oil fatty acids. The 1978 U.S. production of various fatty acids as reported monthly and annually by the FAPC of SDA, is broken down into 9 saturated categories, and 5 unsaturated categories, as follows: (1) stearic and 127.2 M lbs. (13.3%); (2) hydrogenated animal and vegetable acids (2a) 97.3 M lbs. (10.2%), (2b) 158 M lbs. (16.5%), (2c) 32 M lbs. (3.4%); (3) high palmitic, 14.6 M lbs. (1.5%); (4) hydrogenated fish, 6.5 M lbs. (0.7%); (5) lauric acid types, 88.8 M lbs. (9.3%); (6) fractionated fatty acids, (6a) C₁₀ or lower, 18.5 M lbs. (1.9%), (6b) C₁₂ and C₁₄ 55% 17 M lbs. (1.9%); (7) oleic acid, 158.3 M lbs. (16.6%); (8) animal fatty acids other than oleic, 156.3 M lbs. (16.3%); (9) vegetable or marine fatty acids, 0.1 M lbs. (less than 1%); (10) unsaturated fatty acids, 57 M lbs. (6.0%); (11) unsaturated fatty acids I.V. over 130, 24.2 M lbs (2.5%). Reported 1977 fatty acid derivative production from fatty acids (not fats and oils) is 1,980 M lbs. The average price of fatty acids has increased from 23￠/lb.. to 60￠/lb. within the last 5 years.     

制浆煤粉燃烧固硫添加剂的复配研究

对新汶原煤进行了TG—FTIR分析 ,确定了主固硫剂 ,进行了助剂对固硫率的影响研究。助剂M1、M2和M3分别提高固硫率 2 6 1 3 %、1 8 5 0 %和 1 3 5 0 % ,三者复配后的固硫率达到 5 8 7%。分析煤粉燃尽后的渣相及对固硫添加剂固硫机理的初探表明 ,助剂M1、M2能促进固硫反应的进行 ,并提高了渣的灰熔点 ,助剂M3对SO2 向SO3的转化起重要的催化作用     

头孢曲松母液中回收2-巯基苯并噻唑新工艺

研究从头孢曲松生产母液中回收2 巯基苯并噻唑(以下简称M),提出了蒸发结晶 加碱联合处理回收M的新工艺。采用失重法首次研究了M在不同溶剂体系中的溶解度,采用HPLC法测定母液蒸发浓缩结晶和加碱处理回收得到的M的质量分数。结果表明,M在丙酮中溶解度为15 g(常温),在乙醇中溶解度为2.5 g(常温),水的存在会使M在溶媒中的溶解度大幅降低,1.3 g［m(乙醇)∶m(水)=0.4∶0.6,75 ℃］;母液蒸发浓缩至85%时,M的收率可达98.6%,蒸发结晶和加碱处理回收得到的M的质量分数分别为98.2%和98.7%。该工艺不需要大量水的加入,降低了溶剂回收系统的能耗,酸碱用量少,无二次污染,不堵塞管道,已成功用于工业化生产。     

Inhibition of Propylene Oxidation to Acrylic Acid by Amorphous Overlayers on MoV(Nb)TeO Based M2 Catalysts

One of the most effective catalysts for the selective oxidation of propane to acrylic acid (AA) and ammoxidation to acrylonitrile (AN) is the MoV(Nb,Ta)(Te,Sb)O system, comprised of two phases, with M1 the major catalyst and M2 the co-catalyst in symbiosis with M1, converting intermediately formed propylene to the respective desired end products. An improvement in either phase should enhance the overall desired yields of a combined M1/M2 conglomerate. The current study concentrates on the M2 phase (variously substituted and/or doped) where depending on composition and preparation technique crystalline materials or crystalline materials with amorphous overlayers are obtained. Crystalline M2 catalysts without amorphous overlayers are vastly superior to those encumbered with overlayers. In a comparative study the former give a maximum AN yield of ~45% in propylene ammoxidation, the latter ~24%. In the selective oxidation of propylene to acrylic acid, the difference in performance between the two types of catalysts becomes enormous: The crystalline M2 catalyst gives a maximum AA yield of ~34% while the Te–molybdate overlayered M2 a meager ~3%. Doping of crystalline M2 phase with P significantly enhances AA yields over the base and should be seriously considered in future attempts to improve M1/M2 propane/propylene catalyst systems.     

Changes in Chemical Signature and Host Specificity from Larval Retrieval to Full Social Integration in the Myrmecophilous Butterfly Maculinea rebeli

The ant social parasite, Maculinea rebeli shows high levels of host specificity at a regional scale. While 68-88% of caterpillars in the field are adopted by nonhost Myrmica ants, 95-100% of the butterflies emerge from the natural host M. schencki the following year. While retrieval of preadoption caterpillars is specific to the genus Myrmica, it does not explain differential survival with different Myrmica species. We present survival data with host and nonhost Myrmica species suggesting that, with nonhosts (M. sabuleti and M. rubra), survival depends on the physiological state of the colony. We also compared the similarities of the epicuticular surface hydrocarbon signatures of caterpillars that were reared by host and nonhost Myrmica for 3 weeks with those from tending workers. Counterintuitively, the hydrocarbons of postadoption caterpillars were more similar (78%, 73%) to the ant colony profiles of the nonhost species than were caterpillars reared in colonies of M. schencki (42% similarity). However, caterpillars from M. schencki nests that were then isolated for 4 additional days showed unchanged chemical profiles, whereas the similarities of those from nonhost colonies fell to 52 and 56%, respectively. Six compounds, presumably newly synthesized, were detected on the isolated caterpillars that could not have been acquired from M. sabuleti and M. rubra (nor occurred on preadoption caterpillars), five of which were found on the natural host M. schencki. These new compounds may relate to the high rank the caterpillars attain within the hierarchy of M. schencki societies. The same compounds would identify the caterpillars as intruders in non-schencki colonies, where their synthesis appeared to be largely suppressed. The ability to synthesize or suppress additional compounds once adopted explains the pattern of mortalities found among fully integrated caterpillars in Myrmica colonies of different species and physiological states.     

Effect of Medium on Transients and on Observed Quantum Yields in Photoreduction of Benzophenone by 2-Propanol

The quantum yield for photoreduction of 0.1 M benzophenone by 2-propanol, at 313 mμ, light intensity 1 × 10¹⁶ quanta/sec cm² is ?1.16. The quantum yield increases on dilution with benzene to 1.70 at 3.13 M 2-propanol. A Stern-Volmer plot of data below 3 M 2-propanol leads to an extrapolated limiting quantum yield of ?1.9. The quantum yield in 2-propanol decreases with extent of conversion from 1.1 at 17% to 0.74 at 37% photoreduction. Quantum yields for photoreduction of 0.1 M benzophenone by 1 M 2-propanol and by 1 M benzhydrol in benzene remain constant with conversion. A light absorbing transient builds up strongly and progressively during photoreduction in 2-propanol, and to a much lesser extent in 1 M 2-propanol and 1 M benzhydrol in benzene. Photoreduction in 1 M 2-propanol in t-butyl alcohol appears to behave like that in 2-propanol; 1 M 2-propanol in acetonitrile shows behavior intermediate between that in alcoholic and in hydrocarbon solutions. Efficiency of quenching by naphthalene in alcoholic and in hydrocarbon media indicates that k_r is about twice as great in the hydrocarbon as in the alcohol solvents. The effect of the hydrocarbon in diminishing build up of the light absorbing intermediate, which may mask and possibly quench, is largely responsible for the increase in quantum yield on dilution with hydrocarbon.