高效液相色谱法测定低聚果糖

提出用高效液相色谱法（ Ｈ Ｐ Ｌ Ｃ）, Ｂｏｎｄａｐａｋ Ｎ Ｈ２ 柱为分析柱,乙腈—水（３∶１, Ｖ／ Ｖ）为流动相,示差折 光仪为检测器,一次进样能同时测定低聚果糖样品中的果糖、蔗糖、蔗果三糖（ Ｇ Ｆ２ ）、蔗果四糖（ Ｇ Ｆ３ ）、蔗果五糖（ Ｇ Ｆ４ ）、蔗果六糖（ Ｇ Ｆ５ ）等。本法测定了样品“博爱生命素”和“火麻仁内清液”,所得结果良好,变异系数为 ０９ ％ ～１５ ％ ,线性相关系数 ｒ 为 ０９９９０～０９９９９。     

新型钛系催化剂在直接酯化工艺路线中应用探讨

选用特定的含钛化合物作为缩聚催化剂，以ＰＴＡ路线，在２Ｌ小釜规模上进行ＰＥＴ的合成研究，并利用ＤＳＣ、ＴＧＡ、ＧＰＣ等手段对合成的ＰＥＴ进行性能研究．得到催化剂的用量为（０．５～０．７）／万。酯化时间为５０～５５ｍｉｎ，缩果时间为７０－８０ｍｉｎ．聚酯各项指标均在合格范围之内，与Ｓｂ（Ａｃ）３催化体系比较，其用量为锑系的１／３，酯化时间缩短２０～３０ｍｉｎ，缩聚时间缩短２５ｍｉｎ。     

硫化剂TCY在活性氯型聚丙烯酸酯橡胶胶料中的应用研究

研究了国产硫化剂 Ｔ Ｃ Ｙ（１ ,３ ,５三巯基２ ,４ ,６均三嗪） 对国产活性氯型聚丙烯酸酯橡胶（ Ａ Ｃ Ｍ） 硫化胶性能的影响。结果表明,与皂（ 钠皂／ 钾皂）／ 硫黄和３ ＃ 硫化剂（ Ｎ, Ｎ双肉桂叉１ ,６己二胺） 硫化体系相比,硫化剂 Ｔ Ｃ Ｙ 硫化体系硫化的活性氯型 Ａ Ｃ Ｍ 硫化胶压缩永久变形小,物理性能和耐热老化性能良好;在硫化剂 Ｔ Ｃ Ｙ硫化体系中,硫化剂 Ｔ Ｃ Ｙ 的用量为０７５ ～１００ 份较合适,促进剂可采用促进剂 Ｐ Ｚ, Ｚ Ｄ Ｃ 和 Ｂ Ｚ;活性氯型 Ａ Ｃ Ｍ 一段硫化胶的硫化程度高,可不进行二段硫化,若要使硫化胶的压缩永久变形大幅度减小,可进行短时间（６ ｈ） 的高温（１８０ ℃） 二段硫化。     

乙酰乙酸异丙酯的气相色谱分析

以３％ＰＥＧＡ／ｃｈｒｏｍｏｓｏｒｂＧ．ＡＷ－ＤＭＣＳ为固定相，Ｈ２作载气、在１１５℃的柱温下用ＴＣＤ检测器，直接对乙酰乙酸异丙酯及杂质分离含量测定。各组分得到很好的分离。分离度Ｒ〉１。标准偏差０．０７，变异系数为０．０７％。     

烷基多苷稀溶液的泡沫特性研究

本系统地研究了烷基多苷（ＡＰＧ）稀水溶液的泡沫特性，当ＡＰＧ的浓度大于临界胶束浓度时，起泡力与浓度的关系与Ｈ＝０．１１１Ｃ＋５４（ｍｍ）。实验研究发现ＡＰＧ与ＡＥＳ有较好的正协同效应。当０．９５（重量）ＡＥＳ与０．０５ＡＰＧ配伍时，所配制的稀水溶液具有最高的泡沫高度。ＡＰＧ的起泡能力受水溶液中无机盐浓度的影响。在同一浓度下，无机盐对ＡＰＧ起泡能力的影响大小次序为：ＣａＣｌ２〉ＭｇＣｌ２〉ＮａＣｌ     

涕灭威及其代谢物在苹果和土壤中残留量分析

本文概述了涕灭威及其代谢物在苹果和土壤中残留量的分析方法。样品以丙酮提取，过氧乙酸氧化，二氯甲烷萃取，气谱火焰光度检测器（ＧＣ／ＦＰＤ）测定。涕灭威在土壤和苹果中的最低检测浓度分别为０００４、０００４毫克／公斤，空白样品添加０１～２０毫克／公斤，涕灭威及其代谢物的平均回收率和变异系数分别为８４７～１０９７％及１０～７８％。     

α_1-抗胰蛋白酶制剂的制备及其病毒灭活

目的 从Ｃｏｈｎ　ＦⅣ中提纯α１－抗胰蛋白酶（α１－Ａｎｔｉｔｒｙｐｓｉｎ　α１－ＡＴ，制备较高纯度α１－ＡＴ制剂。方法 对Ｃｏｈｎ ＦⅣ抽提液经沉淀、超滤、离子交换及凝胶过滤，提纯 α１－ＡＴ用巴氏法（液态，６０℃，１０ｈ加热）作病毒灭活， 并考察其效果。用免疫单扩散、双向交叉免疫电泳、ＳＤＳ－ＰＡＧＥ及合成基质法检测α１－ＡＴ蛋白及生物活性。用区带 扫描法测定α１－ＡＴ制剂的纯度。结果３批试制的α１－ＡＴ制剂的纯度为９１．３±１．５２％，比活０．４９±０．０８μ／ｍｇ，比活性 比抽提液提高了２７．４倍。巴氏法处理可使ＶＳＶ、Ｓｉｎｄｂｉｓ、Ｐｏｌｉｏ　Ｉ型疫苗病毒分别降低１０．０±０．３，１０．０±０．３１及７．１１ ±０．３ｌｇＴＣＩＤ５０／ｍｌ，但仍能检出Ｐｏｌｉｏ型疫苗病毒。结论 可从 Ｃｏｈｎ ＦⅣ中制得较高纯度的 α１－ＡＴ制剂，巴氏法能对 α１－ＡＴ制剂作有效的病毒灭活处理。     

聚乙二醇-400催化合成橙花醚的研究

研究了利用多种相转移催化剂在不同条件下合成橙花醚。结果表明：采用聚乙二醇 ４００（ＰＥＧ ４００）为催化剂，当β 萘酚：溴乙烷：催化剂＝１：１２：００７（摩尔比）、温度为７６℃、反应７ｈ时，产率可高达９８１％。     

T M E D A/ n - Bu Li 体系丁二烯- 苯乙烯溶液共聚的偶联反应(英文)

研究了 Ｔ Ｍ Ｅ Ｄ Ａ 与 Ｓｎ Ｃｌ４ 用量对丁苯共聚偶联反应的影响。结果表明, 取 Ｔ Ｍ Ｅ Ｄ Ａ／ Ｌｉ 为０ ．１ ,当 Ｓｎ Ｃｌ４／ Ｌｉ 为０ ．１３ 时, Ｈ Ｉ达到最大值１ ．７３ ;当 Ｓｎ Ｃｌ４／ Ｌｉ 为０ ．２５ 时, Ｃ Ｅ 达到最大值６８ ．２５ ％ 。取 Ｓｎ Ｃｌ４／ Ｌｉ 为０ ．１３ ,发现 Ｔ Ｍ Ｅ Ｄ Ａ 加入量对 Ｃ Ｅ 及 Ｈ Ｉ 无明显影响。     

四氯邻苯二甲酸二辛酯的合成

以四氯苯酐和辛醇为原料进行催化酯化反应,产物经固体碱和吸附剂后处理合成了新型阻燃增塑剂四氯邻苯二甲酸二辛酯,四氯苯酐的转化率９９６％,产品的酯含量９９９７％、酸值００１５ｍｇＫＯＨ／ｇ、体积电阻１４６×１０１３Ω·ｃｍ、色泽（铂 钴）１０～２０号。最佳工艺条件是,原料摩尔比为ＴＣＰＡ∶辛醇∶催化剂＝１∶３∶１２４×１０－２,反应温度为２１０±２℃,反应时间为３～３５ｈ。     

复配型受阻酚类抗氧剂对聚甲醛的稳定作用

将受阻酚类抗氧剂Irganox245和Irganox1010进行复配并加入聚甲醛中，通过将物料在设定温度下多次挤出，测定挤出物料的黄色指数、拉伸强度、冲击强度、熔体质量流动速率、热失重率等方法对单剂和复配抗氧剂在聚甲醛中的稳定作用进行了研究。结果表明：将抗氧剂Irganox245和Irganox1010复配后，提高了聚甲醛的分解温度，较好地保持了聚甲醛的各项性能，没有发生劣化现象，作用效果介于两种抗氧剂单独作用效果之间；在聚甲醛的热氧稳定性能方面起到一定的协同作用。     

Study on the High Efficiency Antioxidant of Polyoxymethylene

This article reports on the properties and uses of antioxidant F/B, a type of high efficiency antioxidant for polyoxymethylene (POM), consisting of the hindered phenolic main antioxidant, the secondary thermostabilizer phosphite ester, and lactone compound. Our experimental studies focused on the thermostabilization effect of antioxidant F/B on POM, which was measured by isothermal weight loss analysis at 220°C, isothermal weight loss rate analysis at 222°C, balance torque analysis, nonisothermal gravity analysis (TGA), oxidation induction time (OIT) analysis, and multiple processing and long-term aging analysis as compared to the commonly used antioxidant Irganox245 of POM. The results showed that the thermal stability of POM can be improved remarkably by using antioxidant F/B. The aging mechanism of POM under heat and oxygen was studied by the measurements of polarized light microscopy (PLM), differential scanning calorimetry (DSC), and X-ray photoelectron energy spectrum (XPS), which showed very slight changes of spherulites dimension, crystallinity, and the surface atom concentration after 15 days of aging at 140°C. Furthermore, the small amount of degradation of POM only occurred in the amorphous region of POM. These experiments demonstrated that lower amounts of antioxidant F/B can reach the same level of thermal stabilization of POM as is achieved with higher amounts of Irganox245, and can replace Irganox245 for use in the production of POM, which can further improve the thermal stabilization and reduce the production cost of POM.     

Performance and synergistic effect of phenolic and thio antioxidants in ABS graft copolymers

The synergistic effect of phenolic and thio antioxidants on the stabilization of acrylonitrile-butadiene-styrene (ABS) graft copolymers has been studied. Three commercial antioxidants Irganox245, Irganox1076 and dilauryl thiodipropionate (DLTP) were selected. Formulations based on hindered phenols and secondary antioxidant DLTP were prepared. Stabilization was monitored in terms of changes in the functional groups (oxidation products), tensile properties and yellowness index. Differential scanning calorimetry (DSC) and thermogravimetry (TG) were also used to assess the stability. The results indicated that the combination of Irganox245 and DLTP showed much better stabilization effect than the individual components due to the strong synergistic effect. Only weak synergism could be observed in the formulation that contained Irganox1076 and DLTP. Irganox1076 and Irgnox1076/DLTP exhibited similar behaviors between antioxidants with the highest and lowest efficiencies.     

受阻酚抗氧剂Ky—586的合成及应用

介绍了受阻酚类抗氧剂Ｋｙ－５８６的合成路线及性能特点，了Ｋｙ－５８６、Ｉｒｇａｎｏｘ１０７６、Ｉｒｇａｎｏｘ２４５在通用聚苯乙烯、高冲聚苯乙烯和聚甲醛中的应用。     

Influence of binary combined systems of antioxidants on the stabilization of peroxide‐cured low‐density polyethylene

The secondary antioxidants Irganox 168 and 242 and dilaurylthiodipropionate (didodecyl‐3,3′‐thiodipropionate) (DLTP) were chosen to be combined with the primary phenol antioxidants Irganox 300, 1010, 1035, and 1076, and the effects of the binary combined systems of antioxidants on the peroxide curing reaction and the long‐term stability of crosslinked low‐density polyethylene (XLPE) were studied through isothermal dynamic rheological and mechanical testing. The results show that the primary phenol antioxidants with lower melting points had better resistance to scorching and exhibited good synergistic effects with the secondary antioxidants. Irganox 168 had little resistance to scorching, whereas Irganox DLTP had moderate resistance, and Irganox 242 had the greatest resistance. Irganox 168 and DLTP guaranteed the mechanical properties well, whereas Irganox 242 reduced the tensile strength obviously. Irganox 300 and 1035 combined with secondary antioxidants performed poorly in long‐term thermal aging test, whereas Irganox 1076 in combination with secondary antioxidants displayed a moderate effect of aging resistance, and Irganox 1010 showed the best effect. © 2012 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2012     

新型功能复合型抗氧剂的合成及性能研究

以4-羟基苯乙酰胺和六氯环三磷腈为原料合成六（4-氨基苯氧基)环三膦腈;再通过β（3,5-二叔丁基4羟基苯基）丙酰氯与六（4-氨基苯氧基)环三膦腈的酰胺化缩合反应,最终合成了一种具有膦腈环结构和6个受阻酚单元的新型功能复合型枝化大分子抗氧剂六［β-（3,5-二叔丁基-4-羟基苯基）丙酰胺苯基］环三膦腈（HACP）。通过红外吸收光谱与核磁共振谱图对HACP的结构进行了表征。以HACP或抗氧剂1010为抗氧组分成功制备聚丙烯（PP）树脂共混物,并对共混物进行了热稳定性、耐老化性能的研究。结果表明,热失重过程中PP/HACP的失重5 %时的温度（T5 %）最高,为391.9 ℃(空气气氛)和410.0 ℃(N2气氛);同时,纯PP在老化7 d后失去力学性能,而PP/HACP或PP/抗氧剂1010,即使在老化14 d后依旧保持一定的力学性能,其中PP/HACP的拉伸强度由38.8 MPa下降到34.1 MPa,衰减率为11.6 %;PP/抗氧剂1010则以25.1 %的衰减率由38.7 MPa下降到29.0 MPa。     

胺处理聚甲醛的热稳定化研究

针对聚甲醛由于合成中残留催化剂及不稳定端基导致其热稳定较差的问题，采用胺对聚甲醛进行处理，并考察了胺种类、胺处理工艺及水用量对聚甲醛热稳定性能影响；采用等温热质量损失率、等温热质量损失速率、甲醛释放量分析等方法对三乙醇胺对POM的热稳定作用进行了进一步研究。结果表明：以三乙醇胺为胺处理剂、采用熔融后处理法可有效提高聚甲醛热稳定性能，三乙醇胺最佳用量为0.2％。     

The effect of carbon black on the oxidative induction time of medium-density polyethylene

An extensive series of: (i) oxidative induction time (OIT) measurements derived from differential scanning calorimetry experiments, and (ii) stabilizer analyses by high performance liquid chromatography were conducted on medium-density polyethylene (MDPE) stabilized with various levels of Irganox 1010 (penta-erythrityl-tetrakis-(3,5-di-tert-butyl-4-hydroxyphenyl propionate), Irgafos 168 (tris-(2,4-di-tert-butyl-phenyl)-phosphite), and carbon black (CB). The OIT data were analyzed using a novel interpretation method, which is described and applied. It was found that: (i) addition of CB to base-stabilized MDPE increases stability and reduces OIT variability; (ii) the optimum effective concentrations of Irganox 1010, Irgafos 168 and CB are 1690 ppm, 1580 ppm and 2.5% w/w, respectively; and (iii) interactions between CB and the base co-stabilizers may occur at high loadings of the latter but CB does not affect the extraction of the base co-stabilizers which are extracted with efficiencies of ca. 80% and 100% for Irganox 1010 and Irgafos 168, respectively.     

Evaluation of the oxidative stability of multiextruded polypropylene as assessed by physicomechanical testing and simultaneous differential scanning calorimetry–chemiluminescence

Common physicomechanical tests comprising impact strength, the melt flow index (MFI), and the yellowness index (YI) were used to study the thermooxidative stability of polypropylene (PP) following multipass extrusion. Differential scanning calorimetry (DSC) coupled with chemiluminescence (CL) monitoring was also used to assess the stability. Three PP formulations were studied: (i) PP‐1 containing 0.050% w/w of the phenolic antioxidant Irganox 1010^™, (ii) PP‐2 containing 0.028% w/w Irganox 1010, 0.056% w/w of the phosphite costabilizer Irgafos 168^™ and 0.014% w/w of the lactone processing stabilizer HP 136^™, and (iii) PP‐3 containing 0.050% w/w Irganox 1010 and 0.100% w/w of the phosphite Ultranox 641^™. All formulations contained 0.045% w/w of the hydrotalcite acid scavenger DHT‐4A^™. The results suggest that physicomechanical tests cannot reliably detect the small difference in the stability between PP‐2 and PP‐3 but can detect the larger difference between these and the less stable PP‐1. The oxidative induction time (OIT) determined by CL monitoring (i.e., CL– OIT) is consistent with the OIT determined by DSC but has better reliability. The CL–OIT data suggest that PP‐3 has superior oxidative stability to PP‐2 in the early stages of multipass extrusion. However, PP‐2 exhibits a better resistance to yellowing. A correlation between the CL–OIT data and each of the MFI and YI data was found. © 2000 John Wiley & Sons, Inc. J Appl Polym Sci 79: 733–741, 2001     

The influence of molecular weight on the properties of polyacetal/hydroxyapatite nanocomposites. Part 2. In vitro assessment

A series of polyoxymethylene (POM)/hydroxyapatite (HAp) nanocomposites for long-term bone implants were prepared by melt processing using POM with different molecular weight. Bioactivity was examined by incubating the samples in simulated body fluid. Moreover, in vitro stability, wettability, thermal stability, and formaldehyde release process were investigated. Results of in vitro investigations show that an increase in HAp content in POM nanocomposites facilitates the formation of an apatite layer on the sample surface. There is no significant influence of HAp concentration on the contact angle values as revealed by wettability studies. Thermogravimetric analysis results indicate that with an increase in HAp content the thermal stability of POM matrix decreases significantly depending upon the POM molecular weight. Finally, it was found the amount of formaldehyde leached out of the samples during the incubation period depends on the HAp content: amounts in excess of 3 ppm were emitted for the samples containing only 10% HAp.