A novel method for determination of polyester end-groups by NMR spectroscopy

An efficient, convenient and quantitative method for characterising polyester end-groups is described. We have found that trichloroacetyl isocyanate (TAI) reacts rapidly and quantitatively with both carboxyl [C(O)OH] and hydroxyl (OH) chain ends to form derivatives that can be readily determined by ¹H NMR spectroscopy. The TAI capped end-groups give rise to characteristic imidic NH resonances in a normally clear region of the ¹H NMR spectrum [δ∼10-11.5 for C(O)-O-C(O)-NH-C(O)CCl₃ from C(O)OH, δ∼8-9 for O-C(O)-NH-C(O)CCl₃ from OH]. The method has been successfully applied to quantitative determination of the end-groups of a wide variety of oligomeric polyesters. It has also been applied to higher molecular weight polyesters including commercial, bottle grade, poly(ethylene terephthalate) (PET) and PET based copolyesters (e.g. PETG).     

Synthesis and characterisation of N-toluyl methacrylatoethyl carbamates,homopolymers and copolymers with methyl methacrylate

The paper describes the synthesis of N-2/4-toluyl methacrylatoethyl carbamates using 2/4-toluyl isocyanate and 2-hydroxyethyl methacrylate. Homopolymerisation and copolymerisation of these novel monomers with methyl methacrylate was carried out using benzoyl peroxide as an initiator and tetrahydrofuran as solvent. Photopolymerisation of N-4-toluyl methacrylatoethyl carbamate could be carried out without the use of photosensitiser. Structural characterisation of copolymers was done using ¹H-NMR. Thermal stability of copolymers was evaluated in a nitrogen atmosphere by dynamic thermogravimetry.     

国内外异氰酸酯生产状况及展望

介绍近年来国内外主要异氰酸酯生产厂商生产能力的现状及发展前景，并提出了对我国异氰酸酯工业的建议。     

Environmental etch performance, and scratch and mar of automotive clearcoats

Environmental etch damage to automotive coatings, and scratch and mar of these coatings are an important element of customer satisfaction as well as a significant warranty repair consideration for automotive companies. The conditions that result in environmental etch are examined and a laboratory test proposed. Data from this test are compared to automotive hoods exposed in Florida. The performance of various crosslinking chemistries is discussed and the requirements for improved environmental etch are outlined. Scratch and mar performance of these systems is also reviewed. We have found that coatings respond to physical stress by elastic recovery, by plastic flow and by brittle fracture. Classifying types of damage in this way is important for understanding the chemistry needed for improved scratch and mar of coatings.     

封闭型异氰酸酯固化剂的制备及应用

以甲苯二异氰酸酯、三羟甲基丙烷为原料合成预聚物,分别与甲乙酮肟和多种醇醚类混合物进行封端反应,合成溶剂性和水性封闭异氰酸酯固化剂。采用红外光谱和化学滴定等方法对预聚物和固化剂进行表征和分析。合成的固化剂与树脂按比例混合,制备涂膜,并对漆膜的性能作了初步探讨。     

Effects of apitong (Dipterocarpus spp.) extractives on bond strength development and curing rate of adhesives

Emulsion polymer isocyanate ( ), polyvinyl acetate ( ) and resorcinol-formaldehyde ( ) adhesives were used to produce single lap shear specimens using resinous and non-resinous apitong (Dipterocarpus spp.) timbers. Tests showed that joints made with highly resinous apitong were about 40% weaker than similar joints made with non-resinous apitong. The resinous apitong was treated with different solvents to yield five different extractives which were characterized by infra-red analysis. Apitong extractives were then added to and adhesives and joints made with buna (Fagus crenata), a timber known to be low in extractives and easy to bond. Joints prepared using extractive-containing adhesives were generally weaker than those made with the unmodified adhesives. RF adhesives containing extractives cured more slowly than unmodified . It is thought that the acidic nature of the extractives changes the pH of the system sufficiently to affect the curing mechanism     

全水发泡硬质聚氨酯泡沫塑料技术研究进展

对CFC 11发泡替代技术中全水发泡技术路线进行了分析 ,指出水作为发泡剂存在的优点与不足。着重阐述了全水发泡中几种主要因素如水的用量、聚醚多元醇性质和结构以及异氰酸酯指数对泡沫性能的影响 ,并对国外近些年来全水发泡用聚醚多元醇研究现状进行了详细论述     

异氰酸酯增强二氧化硅气凝胶的力学性能

采用有机无机复合的方式,制得异氰酸酯增强的SiO2气凝胶。将硅酸甲酯(TMOS)、甲基三甲氧基硅烷(MTMS)、3-氨丙基三乙氧基硅烷(APTES)配成混合硅源,经水解缩聚后形成凝胶,老化后浸泡在含六亚甲基二异氰酸酯单体(HDI)的乙腈溶液中,最后经CO₂超临界干燥,获得了具有良好机械性能的SiO₂气凝胶。制备过程中引入的MTMS增加了凝胶与有机物间的浸润性,与使用有机物低聚体相比,使用单体可使有机物更易进入凝胶网络,反应更充分,形成纳米尺度更均匀的复合气凝胶。复合后的气凝胶密度为330 mg/cm³、比表面积为446.3 m²/g、热导率为0.068 W•m^-1•K^-1,该气凝胶良好的力学性能(压缩强度为19.96 MPa、压缩模量为82.37 MPa)使气凝胶的机械加工成为可能。     

三(2-羟乙基)异氰尿酸酯的合成研究

研究了用环氧乙烷在常压下合成三(2-羟乙基)异氰尿酸酯的方法。探讨了原料配比、反应温度、溶剂、催化剂等对反应的影响,并对溶剂的回收利用做了研究。讨论了产品的后处理工艺。通过红外光谱和核磁共振谱分析表征了化合物的结构。     

TPU增韧改性POM的研究

利用双螺杆挤出机制备了聚甲醛(POM)/热塑性聚氨酯弹性体(TPU)和POM/TPU/异氰酸酯预聚物(Z)共混物.采用力学性能测试方法、偏光显微镜(PLM)、傅立叶转换红外线光谱 (FTIR)、扫描电子显微镜(SEM)等研究了共混物的力学性能、结晶行为及形态结构.结果表明,不同种类TPU增韧的共混物的缺口冲击强度和断裂伸长率都随TPU含量的增加而增加,TPU(95A)增韧的POM/TPU共混物的刚性较好,TPU(250)增韧的POM/TPU共混物的韧性较好;Z能促进TPU在基体树脂中的均匀分散,增强两相界面的粘结力,并能细化球晶.