三组份酚醛树脂冷压制备离合器摩擦材料

提出采用三组份改性酚醛树脂和混杂纤维冷压工艺制备离合器摩擦材料.三组份酚醛树脂为硼改性腰果壳油液体树脂、三聚氰胺改性酚醛液体树脂和芳烷基改性酚醛固体树脂.混杂纤维由玻璃纤维和复合包芯纱混杂构成.结果表明,采用三组份酚醛树脂和混杂纤维可以制备出摩擦性能良好,350℃不发生热衰退的离合器摩擦材料,且材料具有合适的孔隙率.     

低聚端羟基聚硅氧烷接枝增韧酚醛树脂的制备及性能

由低聚羟基封端聚硅氧烷（HO-PDM）与甲醛和苯酚的接枝反应制备了增韧改性酚醛树脂,用FT-IR对改性酚醛树脂的结构进行表征,用电子万能试验机测试了改性前后酚醛树脂的力学性能,用热重分析仪测试改性酚醛树脂的热稳定性。 测得改性酚醛树脂的断裂伸长率、冲击强度、抗拉强度分别为2.8%、2.875 kJ/m2和23.2 MPa;树脂失重20%的温度为431.28 ℃,峰值温度为441.8 ℃,800 ℃的残重率为51.02%。     

硼改性酚醛树脂的制备及其耐热性能研究

酚醛树脂因其材料成本低、工艺简单、原料易得等优点，在工业上得到了广泛应用。但由于其耐热性不足以及游离酚含量较高等因素，限制了其应用范围。本文利用硼酸对酚醛树脂进行改性，利用红外和质谱对其结构进行表征，改性后酚醛树脂的耐热性能、游离酚等指标得到明显改善。当失重20%时酚醛树脂改性前后耐热性能提高了56℃,可能是由于硼酚醛树脂中含有硼的三维交联网状结构，提高了树脂的交联密度；游离酚含量从改性前的4.12%降低到了2.21%,说明硼元素的引入改变了苯酚的活性，提高了树脂聚合度。     

Co改性高残炭率酚醛树脂的合成研究

以亚氨基二乙酸为螯合剂,采用配位法在热固性酚醛树脂中引入Co离子,通过热失重(TGA)、扫描电子显微镜(SEM)、红外光谱(FT-IR)和X射线光电子能谱(XPS)等表征对Co改性的酚醛树脂进行分析。FT-IR发现Co离子以配位键方式成功地引入到了树脂结构中;XPS发现酚醛树脂中存在配位结构;TGA发现酚醛树脂经过改性后的热稳定性明显提高;SEM发现通过Co改性的方式,树脂在结构中排布更加紧密。Co改性后的酚醛树脂其固含量和残炭率均有明显提高,分别达到87.19%和52.68%。     

四乙基氢氧化铵改性聚偏氟乙烯接枝聚丙烯酸油水分离膜的制备

使用四乙基氢氧化铵(TEAH)液相本体改性聚偏氟乙烯(PVDF), 以过氧化苯甲酰(BPO)为引发剂, 将丙烯酸(AA)接枝到改性PVDF骨架上, 合成了聚偏氟乙烯接枝聚丙烯酸(PVDF-g-PAA)共聚物, 通过浸没沉淀法制备了PVDF-g-PAA亲水性油水分离膜. 通过傅里叶变换红外光谱(FTIR)、 扫描电子显微镜(SEM)和过滤试验分析了膜的结构和分离性能. 研究了不同接枝条件对PVDF-g-PAA膜接枝率的影响. 同时, 通过膜接枝率与膜表面接触角的关系确定最佳接枝条件. 结果表明, TEAH使PVDF脱去HF产生碳碳双键且PAA接枝到改性的PVDF骨架上, 膜内外孔隙分布均匀; PVDF-g-PAA膜的接触角随着接枝率的提高而降低. 接枝单体AA含量为45%, 接枝温度为85 ℃, 接枝4 h制备的PVDF-g-PAA膜的接枝率为20.1%, 孔隙度为65.3%, 平均孔径为78.0 nm, 接触角为57.5°, 且在60 s内接触角降至14.3°; 纯水通量提高到571.33 L/(m²·h), 截留率和水通量恢复率分别达到94.3%和88.7%, 且通量衰减率仅为9.8%. 与纯PVDF膜相比, PVDF-g-PAA膜的分离性能显著提高.     

带环氧基团纳米二氧化硅改性酚醛树脂的合成及热性能

以苯酚、甲醛、带环氧基团纳米二氧化硅(RNS-E)为原料,采用原位聚合法合成了RNS-E改性酚醛树脂.利用红外光谱(FT-IR)对其结构进行了分析,并利用热重分析(TGA)对其热性能进行了研究.结果表明,改性后的酚醛树脂热稳定性得到提高,当RNS-E的加入量为4%时(质量分数),失重10%时的热分解温度(t10%)较酚醛树脂的提高了15℃,1 000℃下残炭率较酚醛树脂提高了7%.     

高亲水性聚四氟乙烯微粉的制备及其性能研究

通过预辐射接枝方法在聚四氟乙烯(PTFE)微粉上成功接枝丙烯酸(AAc)和2-丙烯酰胺-2-甲基丙磺酸(AMPS),制备了高亲水性的PTFE微粉.采用红外光谱(FTIR)、X射线光电子能谱(XPS)和接触角(CA)测试表征了改性PTFE微粉的化学结构和亲水性变化;采用扫描电子显微镜(SEM)观察改性PTFE微粉表面形貌;采用电泳法测试了改性PTFE微粉的zeta电位;通过热重分析(TGA)测试了辐射接枝对PTFE微粉热稳定性的影响.结果表明,改性PTFE微粉亲水性和分散稳定性随着接枝率的增加而增强;在单体浓度为20%,AAc与AMPS之比为2且反应温度为70℃时接枝率达到26.6%,此时改性样品PTFE-g-P(AAc-co-AMPS)在水溶液中的分散稳定性效果较好,并能够长期稳定存在.水接触角由改性前的148.8°下降到改性后的30.2°,对应的zeta电位从-4.3 m V降为-83.4 m V.     

长链双马来酰亚胺改性氰酸酯树脂及其复合材料

制备了长链双马来酰亚胺改性的氰酸酯树脂及其复合材料, 并对其进行了表征. 结果表明, 当长链双马树脂(MTHMI)占改性树脂的质量分数为37.5%时, 改性树脂(MTI/T₃)的5%热失重温度为414℃, 复合材料在室温和200℃时的拉伸强度分别为431.2和331.0 MPa, 弯曲强度分别为631.5和278.4 MPa, 复合材料的X-Y轴热膨胀系数为18.1×10^-6℃^-1, 吸湿率为1.4%. 实验结果表明, 该类树脂与普通双马改性氰酸酯树脂及分别由质量分数为20%和30% MTHMI改性的氰酸酯树脂MTI/T₁和MTI/T₂相比, 具有良好的加工性, 优异的耐热性和力学性能, 较低的吸湿性和热膨胀系数.     

丙烯腈在聚丙烯上接枝共聚

丙烯腈在聚丙烯上非均相接枝共聚，得杨梅形氰基树脂。研究了接枝共聚条件对单体转化率和接枝率的影响。表观聚合速度可表示为，碰撞频率因子和聚合活化能分别是1．36×1011s-1和99．2kJ．mol-1。从光学显微镜观察到改性树脂在水中接枝连束的分布状态。丙烯腈和二乙烯基苯在聚丙烯上接校共聚，再经二甲苯率取，得笼形氰基树脂。二乙烯基苯在单体中的相对含量对树脂的溶胀性能和笼孔尺寸有很大的影响，制取功能材料时应予适当调节。扫描电镜照片展示了笼形树脂的笼腔和网络结构形态。     

纳米二氧化硅改性苯硼酸型酚醛树脂的制备及热性能

以苯酚、甲醛、苯硼酸和含羟基的纳米二氧化硅(RNS-O)制备了酚醛树脂纳米复合材料,利用红外光谱(FT-IR)对复合材料的结构进行了分析;利用扫描电镜(SEM)对RNS-O在树脂中的分布情况进行了研究,并通过热分析(TGA)考察了RNS-O含量对复合材料热性能的影响.结果表明:当RNS-O含量仅为1%时,RNS-O可均匀的分布在树脂中,且纳米复合材料的耐热性最高,T_(d10%)较改性前提高了134℃,800℃的残炭率提高了7%.     

二氧化碳和丙烯直接合成甲基丙烯酸的NiPMo/TiO2催化剂的研究

用溶胶-凝胶法以磷钼酸(MPA)的镍盐溶液水解钛酸四丁酯制备了NiPMo/TiO2催化剂.使用ICP、 XRD、 TG-DTA、 IR、 TPD-MS和微反应技术研究了催化剂的化学组成、热稳定性、化学吸附性质和催化反应性能.杂多钼酸盐与TiO2通过O2-在TiO2表面发生了键合.在623 K下,杂多阴离子仍保持原有的Keggin结构.CO2在Lewis酸位Ni(Ⅱ)和Lewis碱位Ni-O-Mo的桥氧协同作用下生成CO2卧式吸附态Ni(Ⅱ)←O-(CO)←(O--Ni).丙烯有多种吸附态在催化剂上吸附.在563 K、 1 MPa和空速1500 h-1的反应条件下,丙烯的摩尔转化率为3.2%,产物MAA选择性为95%.     

Synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives

Different approaches for the synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives from simple amino acids have been investigated. A library of 33 precursors for the preparation of N-hydroxy pyrazinones was obtained in moderate to good yields.     

Toward new camptothecins. Part 6: Synthesis of crucial ketones and their use in Friedländer reaction

In the context of the preparation of camptothecin and luotonin A analogs, the synthesis of some key keto-precursors and their use in Friedländer condensation are described. This paper also focuses on the stability of these keto intermediates and emphasizes the major differences between indolizinones and pyrroloquinazolinones series. Noteworthy is also the report of some original structures isolated as by-products of some experiments.     

CoFe2O4自形成磁性液体场致结构化对磁化的影响

The Langevin paramagnetic theory can’t describe the relation between magnetization of ferrofluids and applied magnetic field. The structuralization of ferrofluids, which is considered the main influence factor of the magnetization, is regarded. The part of magnetization works is deposited when the structure is forming. This action influences the magnetization of ferrofluids directly or indirectly. On the base of the “compressing” model, the Langevin function that usually describes the magnetization of ferrofluid is modified, and a well-fitted curve is obtained. An equation of the relation between the equivalent volume fraction after being “compressed” and the intensity of magnetic field is discovered, which approximately describes the process of magnetization. The relation between the approximate initial susceptibility and the volume fraction can be obtained from modified formula.     

Highly regioselective Buchwald–Hartwig amination at C-2 of 2,4-dichloropyridine enabling a novel approach to 2,4-bisanilinopyridine (BAPyd) libraries

The highly regioselective Buchwald–Hartwig amination at C-2 of the cheap and readily accessible reagent, 2,4-dichloropyridine with a range of anilines and heterocyclic amines is described. This new methodology is robust and provides a facile access to 4-chloro-N-phenylpyridin-2-amines on 0.25 mol scale. These intermediates undergo a further Buchwald–Hartwig amination at higher temperature to enable rapid exploration of the chemical space at C-4 and to provide a library of 2,4-bisaminopyridines.     

KMnO4-mediated oxidative CN bond cleavage of tertiary amines: Synthesis of amides and sulfonamides

KMnO₄-mediated oxidative CN bond cleavage of tertiary amines producing secondary amine was introduced, which was trapped by electrophiles (acyl chloride and sulfonyl chloride) to form amides and sulfonamides. The reaction could take place at mild condition, tolerating a wide range of function groups and affording products in moderate to excellent yields.     

Chemistry of heterocyclic compounds at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences, over 50 years (Review)

The review contains a concise historical account and information on the most significant researches undertaken by the staff at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences on the Chemistry of Heterocyclic Compounds. Dedicated to Academician of the Russian Academy of Sciences B. A. Trofimov on his 70th jubilee. Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 10, pp. 1443–1502, October, 2008.     

A general and convenient synthesis of 4-(tosylmethyl)semicarbazones and their use in amidoalkylation of hydrogen,heteroatom, and carbon nucleophiles

A general synthesis of previously unknown semicarbazone-based α-amidoalkylating reagents, 4-(tosylmethyl)semicarbazones, has been developed. The synthesis involved three-component condensation of semicarbazones of aliphatic or aromatic aldehydes with the same or other aldehydes and p-toluenesulfinic acid. The scope and limitations of this reaction were investigated. The compounds obtained were demonstrated to be an efficient α-(4-semicarbazono)alkylating agents. They were reacted with H- (sodium borohydride), O- (sodium methylate), S- (sodium phenylthiolate), N- (pyrrolidine, sodium succinimide), P- (trialkyl phosphites), and C-nucleophiles (sodium diethyl malonate) to give the corresponding products of the tosyl group substitution, 4-substituted semicarbazones, including analogues of nitrofurazone. Among the prepared compounds tested in vitro for antibacterial and antifungal activity, three nitrofuryl-containing semicarbazones exhibited high biological activities with minimum inhibitory concentration (MIC) values of 8–32 μg/mL.     

Sulfur-directed metal-free and regiospecific methyl C(sp3)–H imidation of thioanisoles

Regiospecific and direct imidation of the methyl C(sp³)–H bond of thioanisoles is realized under mild and metal-free conditions with N-fluorobis(benzenesulfonyl)imide as an oxidant and nitrogen source. Proposed mechanism suggests that thionium ion intermediates and a Pummerer-type reaction are involved. The imidation has advantages such as high step-economy, excellent functionality tolerance, and regiospecificity, giving structurally diverse imidation products.     

Synthesis of novel chiral bidentate hydroxyalkyl-N-heterocyclic carbene ligands and their application in palladium-catalyzed Mizoroki–Heck couplings and asymmetric addition of diethylzinc to benzaldehyde

A small library of new chiral bidentate hydroxyalkyl-imidazolium salts 1 is conveniently synthesized on multi-gram scale from inexpensive and commercially available chiral pool amino acids. The corresponding carbenes, generated by deprotonation of imidazolium salts 1, in combination with palladium(II) chloride were tested in the Mizoroki–Heck coupling reaction. The most significant results in terms of yields and reactivities were achieved with low catalyst loading. The catalytic activities of these imidazolium salts were also investigated in the asymmetric addition of diethylzinc to benzaldehyde. The use of MgO nanoparticles as an additive in conjunction with these ligands played a crucial role in increasing the efficiency of these reactions.