上海双龙混合设备制造有限公司总经理 李臣浩——领军“专业品质”扩大“海外市场”

本文介绍了一种苝系颜料的颜料化加工方法,采用干式球磨法,在有助磨剂、分散剂、有机溶剂及固体有机酸存在下球磨5～6小时,球磨结束以后,将球磨料倒入含表面活性剂的酸性的水介质中沸煮1～2小时,经过滤、水洗、干燥得苝系颜料成品.采用本文所说的颜料化加工方法所获得的颜料成品,其色光鲜艳、着色力高,在应用介质中易分散.     

Characterisation of separated melamine—formaldehyde adducts (methylolmelamines) and adduct mixtures by h.p.l.c. and by n.m.r. and u.v. spectroscopy

Most of the individual methylolmelamines that occur in melamine–formaldehyde adduct mixtures have been separated by preparative high-performance liquid chromatography (h.p.l.c.) and recovered in amounts sufficient to allow their characterisation by high-field ¹H- and ¹³C-n.m.r. Particular attention has been paid to the chemical shifts of the aromatic azine carbons of the melamine nuclei. These carbon shifts are shown broadly to be in agreement with some values previously published, but additional assignments have been made. It is shown that a satisfactory quantitative analysis of the methylolmelamines in a melamine–formaldehyde adduct mixture can be carried out either by h.p.l.c. or by ¹³C-n.m.r.     

H.p.l.c. separation and g.c. characterization of polynuclear aromatic fractions of bitumen,heavy oils and their synthetic crude products

Characterization of bitumen, heavy oils, crude oil distillation residues and their processed products involves separation of the mixtures into several compound classes according to their molecular structure. However, these fractions are still very complex and often need further separation in order to get a better insight into their composition as well as the processing reactions involved in their upgrading. In this paper, the polynuclear aromatic fraction is divided into three subfractions by high performance liquid chromatography. Gas chromatography is then used to quantify these fractions and to determine their average molecular weight by a new method derived from simulated distillation. Crude oil distillation residues and their hydrocracked products are used to demonstrate this method.     

Ageing of low-temperature coal-tar pitch. 1. Influence of weather and u.v. light

Outdoor weathering or exposure to u.v. light causes chemical changes on the surface of pitch which can be studied with infrared spectroscopy. Several changes — increase of oxygen content and aromaticity — take place at the same time but at different rates. Carbonyl groups are formed considerably faster than phenols or aromatics. The changing properties are hyperbolic function of time and approach a definite limit.     

E.s.c.a. studies of the nitration and denitration of cellulosic materials

The relative rates of the nitration and denitration of cellulose and cellulose nitrate, respectively (in the form of linters paper), have been monitored in the outermost few tens of Angstroms of the fibres using e.s.c.a. (X-ray photoelectron spectroscopy). Important conclusions are drawn on the equilibrium conditions at the surface and it has been shown that in mixed acid nitrations sulphate esters, (often thought to be a cause of instability in cellulose nitrates), are confined to the outermost few tens of Angstroms of the material. Comparison of the degree of substitution at the surface and that determined for the bulk by Kjeldahl methods provides a new insight into this complex problem.     

Polymerization of Lactams: 57. G.l.c. and n.m.r. analysis of the anionic copolymers of 2-pyrrolidone with 6-caprolactam and 8-octanelactam

The activated anionic copolymerization of 2-pyrrolidone (PD) with 6-caprolactam (CL) or 8-octanelactam (OL) proceeds even above the ceiling temperature for PD homopolymerization. At high temperatures, the copolymerizations are accompanied by the depolymerization of PD sequences, which is more pronounced with the copolymers with CL. The copolymers obtained probably exhibit a constitutional heterogeneity and contain considerable amounts of low-molecular weight fractions. This may be the reason why the content of comonomers in the prepared copolymers determined by g.l.c. did not agree with that found by ¹H n.m.r. or ¹³C n.m.r. spectroscopy. The copolymers with CL had in part a block structure and also an alternating character, depending on temperature and polymerization time, while random copolymers were obtained at high temperatures. The copolymers with OL tended mostly to alternation.     

B.t.蛋白的纯化与鉴定

通过碱溶、碱解的方法溶解B．t．蛋向,采用60％饱和度的硫酸钱粗提,Sephadex G-50层析凝胶分离,加1．5倍的95％乙醇可得晶体沉淀计冻干,所得B．t．蛋白含量为92％,SDS-PAGE电泳图谱显示所纯化的B．t．蛋白分子量为130KD,生物学检测时,幼虫至3铃虫的死亡卒均大于90％,生物活性达18000IU／mg,可T作抗原用。     

A rapid technique for the qualitative analysis of polymers and additives using stop-and-go g.p.c. and i.r.

The use of gel permeation chromatography operated in a stop-and-go mode combined with an infrared spectrometer detector permits rapid qualitative and quantitative analysis of additives in polymers. Additionally, the chemical composition of the polymer and its molecular weight and molecular weight distribution may be determined. The method does not require any preliminary separation steps.     

Proton and carbon n.m.r. spectra of butylated coal

The proton and carbon n.m.r. spectra of butylated Illinois No. 6 coal which has been fractionated by gel-permeation chromatography (GPC) are reported. The chemical shifts and spin-lattice relaxation times of model compounds provide the bases for the assignment of the spectroscopic results. The spectra of the various molecular weight fractions are clearly different. There are significant variations in the degree of aromaticity, the presence of linear alkanes, the ratio of C-butylation to O-butylation, the extent of butylation on aliphatic and aromatic carbon atoms, and the amount of carbonyl and vinyl derivatives. The results suggest that electron transfer, proton abstraction, ether cleavage, and elimination reactions are important under the conditions of the Sternberg process and that both nucleophilic and free-radical substitution reactions occur. The results also strongly suggest that the distribution of functional groups in coal is not uniform.     

Chromatographic and n.m.r. analysis of coal liquefaction products

An efficient Chromatographic separation scheme has been developed to characterize the SYNTHOIL hydrodesulphurization coal liquefaction product. Chromatographic fractions were analysed by nuclear magnetic resonance to determine carbon and hydrogen aromatic/aliphatic distribution ratios of major molecular types. The SYNTHOIL product and its coal-derived asphaltenes were found to contain intermolecularly hydrogen-bonded complexes that may affect the physical properties of the oil.     

Characterization of coal-derived liquids by C n.m.r. and FT-i.r. spectroscopy: Fractions of middle and heavy distillates of SRC-II

Coal-derived products of the SRC-II liquefaction of Powhatan Mine (Pittsburgh Seam) bituminous coal were separated into various fractions either by solvent extraction or by distillation. Subsequently, the middle and heavy distillates were separated by sequential elution solvent chromatography into fractions differing in chemical functionality. These fractions were examined by ¹³C n.m.r. and FT-i.r. spectroscopic techniques. In addition to developing the techniques, the work was undertaken to relate the product composition to the possible reactions occurring during the solvent-induced pyrolytic fragmentation of coal. The bulk of the SRC-II generated middle distillate is composed of two-ring nonpolar aromatic compounds, tetralins, one-ring phenols, indoles, and some alkanes. The heavy distillate contains three-and four-ring systems.