绝缘材料, 2010, 43(5): 57-60. doi: 10.3969/j.issn.1009-9239.2010.05.015
TGDDM/3,3'-二氨基-4,4'-二羟基联苯固化反应动力学研究
徐永芬 单脂肪酸甘油酯中单软脂酸甘油酯、单硬脂酸甘油酯、单油酸甘油酯和单亚油酸甘油酯4种单甘酯的测定方法.以葵花籽油为原料,通过脂肪酶催化甘油解反应制备单甘酯.样品用正己烷/异丙醇(体积比7∶3)溶解,采用超临界CO2-甲醇/乙腈(体积比1∶1)梯度洗脱,经ACQUITY UPC2BEH 2-EP(100 mmx2.1 mm,1.7 μm)色谱柱分离,通过质谱检测器在正离子电喷雾模式下对目标化合物进行分析,外标法定量.结果表明,4种单甘酯化合物在线性范围内线性关系良好,线性相关系数(R2)均大于0.9983;目标物的检出限(S/N≥3)为0.036 ～0.093 mg/L;3个加标水平下的回收率在88.50％ ～ 110.00％之间,相对标准偏差为1.01％ ～4.04％.本方法具有检出限低、分析速度快、分离效果好、分析成本低等优点,为脂肪酸酯类物质的分离测定提供了新的色谱技术平台.","authors":[{"authorName":"林春花","id":"05b63541-4622-4053-8da7-7413f8cfea58","originalAuthorName":"林春花"},{"authorName":"芮培欣","id":"7669fd24-ae85-4e78-90f9-f92b38583815","originalAuthorName":"芮培欣"},{"authorName":"雷志伟","id":"b8726cea-38b5-460b-b966-816d78140ee4","originalAuthorName":"雷志伟"},{"authorName":"严楠","id":"de3b5b9e-33a4-40db-80b9-2be8b8578634","originalAuthorName":"严楠"},{"authorName":"许招会","id":"3bbd1ef3-403e-41f9-b6b5-913b7829ee2a","originalAuthorName":"许招会"},{"authorName":"廖维林","id":"a471450e-0c56-4eb6-941e-aad5b9fc5427","originalAuthorName":"廖维林"}],"doi":"10.11944/j.issn.1000-0518.2016.02.150188","fpage":"238","id":"309def33-940e-41a8-8f09-9220b2ab5c87","issue":"2","journal":{"abbrevTitle":"YYHX","coverImgSrc":"journal/img/cover/YYHX.jpg","id":"73","issnPpub":"1000-0518","publisherId":"YYHX","title":"应用化学"},"keywords":[{"id":"bd5cff5e-3fd9-4d40-b807-285910a4e3bd","keyword":"超高效合相色谱-质谱法","originalKeyword":"超高效合相色谱-质谱法"},{"id":"d6268fb7-876d-465c-9840-123858560c52","keyword":"单脂肪酸甘油酯","originalKeyword":"单脂肪酸甘油酯"},{"id":"a825889d-3973-4c17-a387-a6a510647170","keyword":"甘油解","originalKeyword":"甘油解"},{"id":"3a5ffcc5-6da0-48a2-b720-9dfcbd2d2519","keyword":"葵花籽油","originalKeyword":"葵花籽油"}],"language":"zh","publisherId":"yyhx201602016","title":"超高效合相色谱-质谱法快速分离测定4种单脂肪酸甘油酯","volume":"33","year":"2016"},{"abstractinfo":"","authors":[{"authorName":"邢艳","id":"0c41a712-e907-4541-b6b2-b4488208d267","originalAuthorName":"邢艳"},{"authorName":"褚莹","id":"bba47cc2-7e74-4625-aaf3-d0f934d4fa09","originalAuthorName":"褚莹"},{"authorName":"吴子生","id":"9676cd86-714f-421b-9d2a-8c04f0b7d993","originalAuthorName":"吴子生"},{"authorName":"曹淑桂","id":"59364ac9-8b59-4c0b-9918-8b4397a411af","originalAuthorName":"曹淑桂"}],"doi":"10.3969/j.issn.1000-0518.2000.02.021","fpage":"189","id":"012473a0-6f30-4caa-a7d2-85d3049524d8","issue":"2","journal":{"abbrevTitle":"YYHX","coverImgSrc":"journal/img/cover/YYHX.jpg","id":"73","issnPpub":"1000-0518","publisherId":"YYHX","title":"应用化学"},"keywords":[{"id":"4467394c-112a-4d75-bc84-5a7a19ee45ab","keyword":"反向胶束","originalKeyword":"反向胶束"},{"id":"cfa53096-0053-4f99-b031-03ee9c80ab07","keyword":"甘油解反应","originalKeyword":"甘油解反应"},{"id":"307076be-903e-4b34-bbef-bafaec86cdfa","keyword":"单脂肪酸甘油酯","originalKeyword":"单脂肪酸甘油酯"}],"language":"zh","publisherId":"yyhx200002021","title":"反向胶束中脂肪酶催化猪油的甘油解反应","volume":"17","year":"2000"},{"abstractinfo":"以自制二聚甘油和油酸为原料进行酯化反应合成聚甘油不饱和脂肪酸多酯,再与乙酸酐反应得到乙酰聚甘油不饱和脂肪酸多酯.采用单因素试验研究反应温度、反应时间、聚甘油与油酸摩尔比、催化剂用量对酯化率的影响,确定最优合成工艺条件为反应温度215℃、反应时间3h、油酸与聚甘油摩尔比4∶1、催化剂用量1.5％,该条件下酯化率为87.7％.采用红外光谱、热重分析、凝胶渗透色谱对产物进行了表征.热重分析表明当温度达到500℃时,残留质量为0.21％;凝胶渗透色谱分析结果表明,(-M)n为2354,(-M)w为3050,Mz为6549,相对分子质量分布指数为1.2957;拉伸强度为(22.69±3.10)MPa,断裂伸长率为(65.21±5.25)％.","authors":[{"authorName":"胡云","id":"41871232-e6c2-4c73-95a0-a9bd2b5f4e65","originalAuthorName":"胡云"},{"authorName":"冯国东","id":"f9b23aaf-add7-41d4-89d9-588975a515e2","originalAuthorName":"冯国东"},{"authorName":"许彬","id":"09b07c8d-8555-4a2f-b267-bfa5d6088b13","originalAuthorName":"许彬"},{"authorName":"刘朋","id":"bf133cff-1b13-4601-b11c-a30f3acdbe0d","originalAuthorName":"刘朋"},{"authorName":"周永红","id":"84e2ecc8-63e1-434a-89fc-81cdf8d62b57","originalAuthorName":"周永红"}],"doi":"","fpage":"31","id":"63bf0a0a-5297-4d63-bfca-0b0194d196eb","issue":"4","journal":{"abbrevTitle":"GFZCLKXYGC","coverImgSrc":"journal/img/cover/GFZCLKXYGC.jpg","id":"31","issnPpub":"1000-7555","publisherId":"GFZCLKXYGC","title":"高分子材料科学与工程"},"keywords":[{"id":"56ed8582-7561-4c13-9406-d8816ba568c6","keyword":"增塑剂","originalKeyword":"增塑剂"},{"id":"72dac0c1-c09e-4319-87d7-550d1dedea46","keyword":"酯化","originalKeyword":"酯化"},{"id":"524064c7-6bf7-4928-9d37-03085df65be7","keyword":"不饱和脂肪酸","originalKeyword":"不饱和脂肪酸"},{"id":"b13628ca-00cf-485b-8737-8e58af250863","keyword":"聚甘油","originalKeyword":"聚甘油"}],"language":"zh","publisherId":"gfzclkxygc201504007","title":"增塑剂乙酰聚合甘油不饱和脂肪酸多酯的合成及应用","volume":"31","year":"2015"},{"abstractinfo":"建立了一种采用高效液相色谱法(HPLC)分析猪油甘油三酯中的脂肪酸组成及其位置分布的方法.利用sn-1,3位专一性脂肪酶对甘油三酯sn-1,3位上的脂肪酸进行水解,形成sn-2位甘油单酯和游离脂肪酸;之后,通过甘油三酯中脂肪酸总含量和sn-1,3位上脂肪酸含量之间的差值计算出sn-2位上的脂肪酸含量.利用2-溴苯乙酮仅同游离脂肪酸作用的特点,将脂肪酸酯化为苯乙酰甲酯,然后进行HPLC分析.分析所用色谱柱为ZORBAX SB C18柱,以十七酸作为内标,甲醇-乙腈-水为流动相,采用梯度洗脱(梯度洗脱程序为甲醇-乙腈-水由80∶10∶10(体积比,下同)在35 min内线性变化到86∶10∶4,然后在5 min内恢复到起始比例,流动相流速为1 mL/min),通过测定苯乙酰甲酯在254 nm处的吸光度值来测定脂肪酸含量.结果表明,猪油甘油三酯中的脂肪酸主要是棕榈酸和油酸(分别占总量的26.61%和43.18%),其中油酸主要分布于sn-1,3位上,而棕榈酸分布于sn-2位上.这些测定结果与传统气相色谱法的测定结果相吻合.该方法简单可行,省去了传统测定中费时的薄层色谱分离步骤,可成为一种有效的实验室分析方法.","authors":[{"authorName":"赵海珍","id":"2d9d8ce4-9452-4812-b6f0-bbe671f354f0","originalAuthorName":"赵海珍"},{"authorName":"陆兆新","id":"96854ef9-0cc7-4f9e-99c7-1035d0614f0e","originalAuthorName":"陆兆新"},{"authorName":"别小妹","id":"ed463fed-9b17-4fda-879b-9cc468fdac17","originalAuthorName":"别小妹"},{"authorName":"吕凤霞","id":"fca515d7-6343-49f1-9bda-586d6d5a3b2a","originalAuthorName":"吕凤霞"}],"doi":"10.3321/j.issn:1000-8713.2005.02.006","fpage":"142","id":"f70fbdf1-5f11-4f38-9259-d6af95bc76dd","issue":"2","journal":{"abbrevTitle":"SP","coverImgSrc":"journal/img/cover/SP.jpg","id":"58","issnPpub":"1000-8713","publisherId":"SP","title":"色谱 "},"keywords":[{"id":"fd5cfe66-1fef-450e-adae-7f2d90779b04","keyword":"高效液相色谱","originalKeyword":"高效液相色谱"},{"id":"43c8d860-f6ed-4447-9eeb-c97b9a923f05","keyword":"脂肪酸","originalKeyword":"脂肪酸"},{"id":"e8b3b6f3-0e5d-4887-9bf6-abaf33ffb7a5","keyword":"位置分布","originalKeyword":"位置分布"},{"id":"936b7af8-5476-42ac-89df-3559a2a498e3","keyword":"甘油三酯","originalKeyword":"甘油三酯"},{"id":"b245b912-4c92-4165-b042-0f673a474c51","keyword":"脂肪酶","originalKeyword":"脂肪酶"},{"id":"8883ddf7-9537-457f-b7d5-d06636a2ff20","keyword":"猪油","originalKeyword":"猪油"}],"language":"zh","publisherId":"sp200502006","title":"高效液相色谱法测定猪油甘油三酯中的脂肪酸位置分布","volume":"23","year":"2005"},{"abstractinfo":"以α-单硬脂酸甘油酯的水解反应为指示反应,初步研究了琥珀酸二辛酯磺酸钠(AOT)-正庚烷-明胶微乳液凝胶固定化脂肪酶在有机相中的水解催化活性. 结果表明,明胶和AOT含量、R值(水与AOT的摩尔数之比)对酶催化活性均有影响,确定了较佳的凝胶组成:微乳液配比为m(正庚烷)∶ m(缓冲液)∶ m(AOT)=75∶ 9∶ 16,明胶质量分数为17%,R值为72;当酶含量固定,底物浓度大于0.10 mol/L时,脂肪酶可发挥最大催化活性;反应时间超过15 h,水解反应达到平衡.","authors":[{"authorName":"宋少芳","id":"05f6376b-f555-434e-a89c-f12c10232cd3","originalAuthorName":"宋少芳"},{"authorName":"栾玉霞","id":"ec8e2244-46a4-4610-92af-faf6268dddb5","originalAuthorName":"栾玉霞"},{"authorName":"路福绥","id":"dc657931-0f00-4968-a826-4a5976c0bfa5","originalAuthorName":"路福绥"}],"doi":"10.3969/j.issn.1000-0518.2006.02.017","fpage":"188","id":"c66cb57f-a4f8-4bd2-a194-f37eae239b3d","issue":"2","journal":{"abbrevTitle":"YYHX","coverImgSrc":"journal/img/cover/YYHX.jpg","id":"73","issnPpub":"1000-0518","publisherId":"YYHX","title":"应用化学"},"keywords":[{"id":"8490adb2-1848-4491-ba63-9a8291b458e9","keyword":"微乳液凝胶","originalKeyword":"微乳液凝胶"},{"id":"f44ed5ce-354c-4e9e-8a70-53e1bb5e2b0e","keyword":"固定化脂肪酶","originalKeyword":"固定化脂肪酶"},{"id":"08f5ccfd-7cbc-43df-95f2-3464f3ea3356","keyword":"催化活性","originalKeyword":"催化活性"},{"id":"1e53e15e-979a-475e-ac46-05c55097c81c","keyword":"水解反应","originalKeyword":"水解反应"},{"id":"4eaa6ee5-92b2-4408-ad0c-b8765df1e19e","keyword":"α-单硬脂酸甘油酯","originalKeyword":"α-单硬脂酸甘油酯"}],"language":"zh","publisherId":"yyhx200602017","title":"微乳液凝胶固定化脂肪酶催化α-单硬脂酸甘油酯水解反应活性","volume":"23","year":"2006"},{"abstractinfo":"以聚醚210(N-210)、IPDI(异佛尔酮二异氰酸酯)为基本单体,用含有18个碳脂肪侧链的硬脂酸单甘油酯改性,合成了一种以十八碳脂肪链为疏水链段的水性聚氨酯.研究了硬脂酸单甘油酯用量对树脂外观、稳定性、耐水性、表面能的影响,以及硬脂酸单甘油酯的引入对水性聚氨酯热稳定性的影响.结果表明引入脂肪链可以提高水性聚氨酯的表面活性、热稳定性和耐水性.","authors":[{"authorName":"詹媛媛","id":"0fb06ba9-1043-480f-becd-2f50a9ea17b8","originalAuthorName":"詹媛媛"},{"authorName":"张彪","id":"c2a69ac4-1d2d-4798-88cf-e5457f094862","originalAuthorName":"张彪"},{"authorName":"黄毅萍","id":"95ce7a94-3e48-496e-9e03-97371a167e03","originalAuthorName":"黄毅萍"},{"authorName":"许戈文","id":"24c18df7-bc0a-48d5-a1d6-ad713b121e54","originalAuthorName":"许戈文"}],"doi":"10.3969/j.issn.0253-4312.2010.01.017","fpage":"63","id":"f5ebd06b-36d3-4c34-a913-5e7ef2b9b140","issue":"1","journal":{"abbrevTitle":"TLGY","coverImgSrc":"journal/img/cover/TLGY.jpg","id":"61","issnPpub":"0253-4312","publisherId":"TLGY","title":"涂料工业 "},"keywords":[{"id":"ef60847d-c60a-48b7-87df-7a38e9a6e183","keyword":"水性聚氨酯","originalKeyword":"水性聚氨酯"},{"id":"f9171bd4-70c9-427e-8715-0d355d386897","keyword":"硬脂酸单甘油酯","originalKeyword":"硬脂酸单甘油酯"},{"id":"8099da34-b9c6-45c4-8dc3-6889b49d1df7","keyword":"表面活性","originalKeyword":"表面活性"},{"id":"a942cc98-eb55-4225-a9be-1d6b062c32f0","keyword":"耐水性","originalKeyword":"耐水性"},{"id":"f2897bcb-f9d1-4055-afe8-2a73319e2814","keyword":"热稳定性","originalKeyword":"热稳定性"}],"language":"zh","publisherId":"tlgy201001017","title":"硬脂酸单甘油酯改性水性聚氨酯的研究","volume":"40","year":"2010"},{"abstractinfo":"本文简述了脂肪酸酯的历史,提出了将此原料应用于制漆时应采用的方法,分析了这种方法的可行性.例举了用脂肪酸酯制备白色氨基烘漆、蓝色聚氨酯漆及浅灰色自干醇酸磁漆的配方及涂料性能.","authors":[{"authorName":"王其超","id":"13bebd9c-e7d5-4afe-8848-75eace808b03","originalAuthorName":"王其超"},{"authorName":"马喜顺","id":"20f6f19a-69df-4489-8459-680ceaae810c","originalAuthorName":"马喜顺"},{"authorName":"黄新竹","id":"d94dec31-9f42-46e8-9a98-61a8c75c092c","originalAuthorName":"黄新竹"},{"authorName":"陈广明","id":"b4bad55b-8402-44fc-822a-07f4b89d8a7d","originalAuthorName":"陈广明"},{"authorName":"孙胜民","id":"ef108b5e-28d6-414a-b120-8dd26c5989f6","originalAuthorName":"孙胜民"}],"doi":"10.3969/j.issn.0253-4312.2006.01.014","fpage":"48","id":"c169a7ea-ba28-43c6-a1d5-7659ea1f5cdc","issue":"1","journal":{"abbrevTitle":"TLGY","coverImgSrc":"journal/img/cover/TLGY.jpg","id":"61","issnPpub":"0253-4312","publisherId":"TLGY","title":"涂料工业 "},"keywords":[{"id":"0d528d0b-cda8-4df6-82cb-a892642b6456","keyword":"脂肪酸酯","originalKeyword":"脂肪酸酯"},{"id":"bb7848cc-3ef6-4b19-a281-cf0b283d34fa","keyword":"酯交换反应","originalKeyword":"酯交换反应"},{"id":"fe4719fb-9eea-465f-a866-ddb2700e1cc3","keyword":"烘漆","originalKeyword":"烘漆"},{"id":"a0f7cdbe-4db1-4068-9210-87a3f24b95a4","keyword":"自干漆","originalKeyword":"自干漆"}],"language":"zh","publisherId":"tlgy200601014","title":"脂肪酸酯在制漆中的应用","volume":"36","year":"2006"},{"abstractinfo":"以线性低密度聚乙烯为原料,向其中加入单油酸甘油酯,采用共混挤出的方法,吹塑出了厚度约为0.11mm的棚膜,研究了单油酸甘油酯对聚乙烯棚膜性能的影响.结果表明,单油酸甘油酯有较好的防雾效果;随着其添加量的增加,棚膜的水滴接触角减小,水浴法防雾时间增长;但与此同时,单油酸甘油酯的加入降低了棚膜的透光率和力学强度.当单油酸甘油酯的添加量为2％时,棚膜在60℃水浴中的防雾时间达到183 h,而普通聚乙烯棚膜的防雾时间只有5min.","authors":[{"authorName":"韦佳程","id":"fbad3620-81fe-4984-b866-9b320c551e47","originalAuthorName":"韦佳程"},{"authorName":"罗学刚","id":"10c2c022-a7b6-48fe-8e9f-4d608b9a79d1","originalAuthorName":"罗学刚"},{"authorName":"林晓艳","id":"ea87b7a2-5780-4c0f-9c05-20ea3199e89e","originalAuthorName":"林晓艳"},{"authorName":"张红平","id":"26cebf05-69c5-45b3-9205-ea5274220d62","originalAuthorName":"张红平"}],"doi":"","fpage":"71","id":"5124c621-ce00-489d-9264-f1fb6839dcce","issue":"5","journal":{"abbrevTitle":"GFZCLKXYGC","coverImgSrc":"journal/img/cover/GFZCLKXYGC.jpg","id":"31","issnPpub":"1000-7555","publisherId":"GFZCLKXYGC","title":"高分子材料科学与工程"},"keywords":[{"id":"4f7e6fe6-d582-44b9-b5a9-5df9b409a4cd","keyword":"单油酸甘油酯","originalKeyword":"单油酸甘油酯"},{"id":"96f35ee7-26f0-4afb-9051-84efbed6be3b","keyword":"聚乙烯","originalKeyword":"聚乙烯"},{"id":"22779c45-7181-4680-a295-6cf356fed3a4","keyword":"棚膜","originalKeyword":"棚膜"},{"id":"21ba6964-965c-405a-94ee-553cb6682ad8","keyword":"防雾","originalKeyword":"防雾"}],"language":"zh","publisherId":"gfzclkxygc201305018","title":"单油酸甘油酯对聚乙烯棚膜的防雾性影响","volume":"29","year":"2013"},{"abstractinfo":"介绍了异氰脲酸三缩水甘油酯(TGIC)的合成方法、反应原理及用途,并介绍了TGIC的异构体与毒性等.","authors":[{"authorName":"黄俊峰","id":"21c66ff6-dc3b-49cf-b5b6-285c5c82c2f4","originalAuthorName":"黄俊峰"}],"doi":"10.3969/j.issn.0253-4312.2009.07.018","fpage":"68","id":"c87a7695-4723-413c-b063-e7b80c468104","issue":"7","journal":{"abbrevTitle":"TLGY","coverImgSrc":"journal/img/cover/TLGY.jpg","id":"61","issnPpub":"0253-4312","publisherId":"TLGY","title":"涂料工业 "},"keywords":[{"id":"b3f1c3a0-0d47-4f39-b40b-2af8edaab64c","keyword":"异氰脲酸三缩水甘油酯","originalKeyword":"异氰脲酸三缩水甘油酯"},{"id":"acfaedad-6a62-4b3e-8c52-39ec5a702967","keyword":"合成方法","originalKeyword":"合成方法"},{"id":"f59c3c14-9064-41dc-859f-9b940e5be533","keyword":"异构体","originalKeyword":"异构体"},{"id":"7e4c3ec3-132b-477e-a796-44b2ed43e61c","keyword":"粉末涂料","originalKeyword":"粉末涂料"},{"id":"7f4378f3-a928-4bd2-bd05-9428e2061cb2","keyword":"毒性","originalKeyword":"毒性"}],"language":"zh","publisherId":"tlgy200907018","title":"异氰脲酸三缩水甘油酯的合成及应用","volume":"39","year":"2009"},{"abstractinfo":"采用乙酸酐为共反应剂合成了纤维素高级脂肪酸酯.用FT-IR、1H-NMR对合成产物的结构进行了表征.结果表明,在纤维素分子骨架上同时接枝上了高级脂肪酸酯基以及乙酸酯基,产物为纤维素混合酸酯.产物的酯化度值通过1H-NMR确定,酯化度可达到1.66.研究了纤维素与系列高级脂肪酸的酯化反应,结果表明,随着高级脂肪酸中碳原子数目的增加,产物的酯化度逐渐减小,而产物质量有一个先增加-后减小的趋势.","authors":[{"authorName":"宋毅","id":"97a44531-01da-49a8-b1aa-444d915af7d5","originalAuthorName":"宋毅"},{"authorName":"马风国","id":"a89c1ebf-cfd8-46d9-9f4d-0528ef82f169","originalAuthorName":"马风国"},{"authorName":"邵自强","id":"5fbce7fa-ab58-4938-bd12-c2c6bb91493f","originalAuthorName":"邵自强"},{"authorName":"谭惠民","id":"bed904c0-cb83-41ed-9b0e-90ff569207b7","originalAuthorName":"谭惠民"}],"doi":"","fpage":"66","id":"2270c874-7f93-40c3-86ae-ed02b2f19164","issue":"4","journal":{"abbrevTitle":"GFZCLKXYGC","coverImgSrc":"journal/img/cover/GFZCLKXYGC.jpg","id":"31","issnPpub":"1000-7555","publisherId":"GFZCLKXYGC","title":"高分子材料科学与工程"},"keywords":[{"id":"88ee608f-b02d-418d-8718-4af9e465ee52","keyword":"纤维素","originalKeyword":"纤维素"},{"id":"23af30d6-a637-4108-87e1-755e9f6d78fa","keyword":"高级脂肪酸","originalKeyword":"高级脂肪酸"},{"id":"31c8817f-aca7-4946-b63a-b4f03a4cfed8","keyword":"酯化","originalKeyword":"酯化"}],"language":"zh","publisherId":"gfzclkxygc200204016","title":"共反应剂法合成纤维素高级脂肪酸酯","volume":"18","year":"2002"}],"totalpage":2364,"totalrecord":23631}