50 Jahre helle Montanwachse - Stand der Montanwachsveredelung nach 50jähriger Entwicklung

Fifty Years of Light Colored Montana Wax - State of Montana Wax Refining since 50 Years of Development Since 50 years, light colored montana waxes are technically prepared by refining of crude montana wax which occurs in certain varieties of lignite. By this process, the dark colored crude montana wax, which is of limited use, is converted into valuable light colored wax products. Since many years of development work, process are now available for montana wax refining that permit the production of wax products which are suitable for every field of application. According to these processes, the crude montana wax having complex composition is depolymerized and bleached. Subsequently, the product can be modified by a variety of chemical transformations. The processes known for the refining of montana wax are reviewed.     

Einfluß der Raffination auf die Zusammensetzung der Säuremontanwachse

Refining Effect on Acid Montana Wax Composition Three acid montana waxes which result from industrial refining process in ZA Kedzierzyn were investigated with respect to their group composition and chemical composition. The subsequent wax types were investigated: 1. wax MR - weakly refined (one step, by HNO₃), 2. wax MR moderately refined (two step, by HNO₃ and Na₂Cr₂O₇), 3. wax R - highly refined (two step, by Na₂Cr₂O₇). These acid waxes were used in Poland as raw materials for production of various semisynthetic montana waxs. The characteristical values of the waxes have been determined. Besides that the examined acid montana waxes were separated by ion exchange methods and adsorption chromatography in free and esterified wax acids, wax alcohols and hydrocarbons. By GC methods the components separated from the substance groups have been qualitatively and quantitively analyzed. The effect of the refining methods on the chemical conversion processes of the waxes is explained.     

Wachse mit hoher Dispergierfähigkeit unter besonderer Berücksichtigung ihrer Eignung für die Herstellung von Kohlepapierfarbmassen

Waxes Having High Dispersibility and Special Consideration of Their Suitability in the Manufacture of Colouring Masses for Carbon Paper Increasing amounts of waxes having fundamentally different chemical composition are being used as dispersion aids. In the manufacture of colouring masses for carbon papers, the materials used as vehicle of the colour and as dispersing agent for carbon black are hydrocarbons, wax acids and their natural esters. Whereas low-priced paraffins are mainly used for cheap carbon papers meant for a single use, carnauba wax is used for better quality carbon papers which can be used several times. The latter wax is especially suited because of its carbon black-dispersing and oil-binding properties. Since crude montana wax does not have these properties to such an extent as the carnauba wax, it was attempted to improve the carbon black-dispersing and oil-binding of montana wax by chemical synthesis. This was achieved by reacting crude montana wax with maleic anhydride and subsequent esterification of the reaction products with glycols. The results were successfully applied to the solution of problems involving dispersion of pigments and plastic additives.     

废塑料热解聚乙烯蜡的羧基化改性和表征

以废弃聚乙烯塑料热解得到的粗蜡为原料,用溶液催化氧化法制备了羧基化改性的氧化聚乙烯蜡,考察了催化剂种类和用量、引发剂用量、反应时间、反应温度对产物酸值的影响。结果表明,在催化剂加入量为1%、引发剂用量为10%、反应时间为8 h、反应温度为90℃的条件下,可制得酸值为16.26 mg KOH/g和16.17 mg KOH/g的氧化蜡。利用红外光谱和热重分析对产品进行表征。     

Bilanz der Schnellpyrolyse des Rohmontanwachses

Rapid Pyrolysis of Raw Montana Wax Raw montana wax from Slovakian Lignite was subjected to rapid pyrolysis at a temperature of 600° and 700° C. The products of pyrolysis were segregated into a solid, a liquid and highly volatile fraction. The products of pyrolysis were determined in each fraction. Both the pyrolysis products as well as the original wax were fractionated by column chromatography. The individual eluates were analyzed by gas chromatography and mass spectrometry.     

Schnellpyrolyse von Rohmontanwachs

Rapid Pyrolysis of Raw Montana Wax Montana wax of different origins has been subjected to rapid pyrolysis in a quartz apparatus according to the method reported by Romová?ek and Kubát, and the products of fragmentation have been identified chromatographically. The thermal splitting was generally carried out at 650° C, however, with the montana wax of Russian origin temperatures between 500° and 900° C were chosen. The individual products were identified and determined quantitatively.     

石蜡改性制备汽车上光用蜡

采用聚乙烯蜡为原料,通过催化氧化反应对石蜡进行改性研制出质量和性能与天然巴西棕榈蜡相似的氧化蜡,用其代替天然巴西棕榈蜡制备乳化型汽车上光蜡。对氧化蜡制备微乳液进行了研究,考察了微乳液的配方组成以及乳化条件对制备氧化蜡微乳液的影响,结果表明蜡样和乳化剂的质量比为1∶0.50,乳化时间为50min,乳化温度为90~95℃,搅拌速度为1200~1500r/min时可制得外观、光泽、成膜性等方面性能优良的汽车上光用蜡。     

Physikalisch-chemische Eigenschaften von Braunkohlenextrakten und abgetrennten Wachs- und Harzstoffen

Physico-chemical Properties of Brown-Coal Extracts and Separated Wax and Resin Substances The component composition and the physico-chemical properties of the raw montane wax Romonta as well as of three samples of the toluene extracts from the mine Turów, obtained at different extraction temperatures, were determined. The wax and resin substances were separated from the raw montane wax Romonta and from the toluene extract of brown-coal from the mine Turów, obtained at 100°C, and then characterized. The rheological properties of the extracts, the separated components and the four selected processing products of the raw montane waxes Romonta (means of hydrophobation Romonta 55, acid wax R, ester wax K-60, partly saponified ester wax REW II) were determined by the rotation viscosity metre Rheotest 2. The viscosity measurements were carried out at higher temperatures than the dropping point of the investigated substance, in case of extracts rich on resin also at lower temperatures. A significant influence of the sort of coal and the extraction temperature on the component composition of the obtained extracts as well as on the properties of the separated wax and resin substances was established. Furthermore a different rheological behaviour of the wax substances and wax containing extracts in comparison to the resin components of brown-coal bitumen was observed. Concerning the extracts of brown-coal from the mine Turów it was found out that the viscosity slowly increases in case of an increase of the resin content up to 50%, but at higher resin content it increases very quickly.     

新型无催化剂石蜡氧化改性研究

分别以硬脂酸和H2O2为引发剂进行了石蜡氧化改性研究,考察了空气流量、氧化引发剂的质量分数、反应温度和反应时间对石蜡氧化过程的影响,以及反应条件对氧化石蜡性质的影响,并确定了最佳的氧化工艺条件:其中氧化温度为145~150℃,氧化时间为6~8 h。并对两种引发剂的反应效果进行了比较,其中硬脂酸效果更佳。结果表明,采用上述两种引发剂,在不添加任何催化剂的前提下,选取适当的反应条件,可以制备出酸值高、颜色浅、气味轻的氧化蜡。制得的氧化石蜡性质与天然蜂蜡相近,而且能替代天然蜂蜡制成稳定的乳化蜡。     

Eigenschaften und Anwendungsmöglichkeiten von Montanharz

Properties and Application Feasibilities of Montan Resin In raw montan wax raffination the process of resin extraction is the first stage. In this process a large amount of montan resin is obtained, which is a waste product without corresponding application possibilities. The common combustion of montan resin with fuel oil is certainly no ideal solution of the problem. Therefore the physical and chemical properties of montan resin were determined and investigations of the use of montan resin in practice were carried out. The softening point, the characteristic values and the IR-spectrum of the obtained montan resin were determined, furthermore elementary analysis and X-ray structural analysis. To obtain from montan resin products with altered properties, the following laboratory experiments were carried out: heating, air blowing, condensation with furfurol, nitration and saponification. The aerial oxidized products showed only a little increased softening point, with furfurol condensed montan resins were deep black coloured and brittle, the nitrogen content of the obtained nitrocompounds was very low. If saponified montan resin is applicated as air entraining agent in air beton positive results were obtained.     

Influence of heating time and oxygen availability on lipid oxidation in meat emulsions

The aim of the present study was to investigate the effect of heating time and oxygen availability on lipid oxidation during chill storage, using different step indicators, in a meat emulsion model. Lipid oxidation was measured by conjugated dienes, hydroperoxides and 2‐thiobarbituric acid reactive substances formation on raw and cooked meat emulsion at 80 °C in different oxygen availability bags, at 0 °C during 35 d. The results obtained showed that heat treatment and oxygen availability affected conjugated dienes, hydroperoxides and 2‐thiobarbituric acid reactive substances formation during chill storage. Besides cooked meat emulsion did not have a similar behaviour to that of raw samples. Thus, is very important to follow primary and secondary products of oxidative deterioration to understand the effect of heat treatment and oxygen availability overall lipid oxidation process in meat emulsion.     

铅笔板乳化蜡的研制

传统铅笔板制造工艺采用烤板法加蜡,利用铅笔板本身的余热,石蜡被熔化并渗入木板中。这种方法虽然简便,但铅笔板中石蜡分布不均,铅笔仍会发生活芯或膨胀变形等问题。采用石蜡、C5石油树脂以及氧化蜡等为原料,制备铅笔板乳化蜡,并对其性能进行了研究。实验确定了铅笔板用乳化蜡微乳液的配方,考察了乳化条件对制备微乳液的影响。研究结果表明:当石蜡、C5石油树脂、氧化蜡的质量比为1∶0.6∶0.4,乳化时间为30min,乳化温度为90～95℃,搅拌速度为1100r/min时可制得性能稳定的铅笔板专用防护蜡乳液。     

Über den Einfluß von Licht auf den oxydativen Verderb von Speiseölen IV: Abhängigkeit der Oxydationsgeschwindigkeit von der Wellenlänge des eingestrahlten Lichts

Influence of Light on Oxidative Deterioration of Edible Oils IV: Dependence of Rate of Oxidation on Wave-Length of Incident Light A distinct decrease in the rate of oxidation with increasing wave-length is observed for soybean, sunflower and peanut oils when these oils are irradiated with various coloured lights having the same quantum-density. While studying the causes of this behaviour, pure absorption curves for the aforesaid oils were determined. Light of short wave was completely absorbed, whereas long-wave light was barely absorbed to any measurable extent. A considerable increase in quantum yield during oxidation occurs with increasing wave-length. Inspite of this, the oxidation of oils is catalysed most strongly by short-wave light, because the influence of pure absorption exceeds the increase in quantum yield. Pure absorption is therefore considered as the decisive factor with regard to the dependence of photooxidation on wave-length. Finally, the rate of oxidation, as determined in darkness, was found to increase with decreasing wave-length of light used for pre-oxidation of the oil.     

Trennung halbsynthetischer Montanwachse in Gruppenkomponenten und physikalischchemische sowie rheologische Eigenschaften der Wachssäure-Glykolester-Systeme

Separation of Semisynthetic Montana Wax into Component Groups and Physico-Chemical as well as Rheological Properties of Wax Acids and Glycol Ester Systems Crude montana wax Romonta, acid wax R, as well as two ester waxes MR-150B and KPS were separated into their component groups. Two methods of separation were employed, namely, chromatography and extraction. Using these methods free wax acids, esters, alcohols and hydrocarbons were separated. Purity of each fraction was determined in the same manner. One part of the separated acids was esterified with ethylene glycol and from the reaction product six wax esters were synthesized. Slip point, penetration and rheological properties of these six wax esters were studied.     

陶瓷制造用乳化蜡的制备研究

以58#号石蜡及其氧化蜡为原料,采用非离子表面活性剂吐温系列和司盘系列作为添加剂,通过全实验筛选出符合陶瓷用乳化蜡制备的乳化条件及各原料用量及配比,在最佳实验条件下制得优于市场同类产品的乳化蜡。考察确定的乳化剂为复合乳化剂Ⅲ,其HLB值为9.50,乳化剂加入量为蜡质量的25%;在最佳工艺条件,乳化温度90℃、乳化时间40min、搅拌速度850r/min的条件下,制备出的陶瓷用乳化蜡,具有稳定性好、可塑性强、流动性适宜、粘度适中、铺膜性好等特点。     

Gas-chromatographische Untersuchung von Naturwachsen

Gas Chromatographic Investigation of Natural Waxes A rapid gas chromatographic method for the identification of natural Waxes is described, according to which the wax acids and the unsaponifiables are investigated after saponification. The methyl esters of the wax acids as well as the acetates and oxidation products from the unsaponifiables showed a characteristic pattern of distribution amongst the individual natural waxes. In the characterization of natural waxes it is desirable to investigate the methyl esters of the wax acids, because after saponification the wax acids are obtained as a more uniform class of substances than the unsaponifiables.     

反应条件对石蜡深度氧化制取二元酸的影响

研究了石蜡液相深度氧化过程中氧吸收量与氧化蜡组成变化的关系。结果说明,深度氧化蜡绝大部分是由多官能团酸组成,其官能团除羧基为主外,次为酯基,其量为羧基的一半,羰基较少,而羟基几无。C_4～C_（10）二元酸在氧化醋酸价为250毫克KOH/克左右时开始有明显的含量,并且随着氧化深度的增加而含量迅速增加。在适宜的催化剂和较好的气液接触情况下,石蜡能否快速定向深度氧化的关键在于恰当的选择温度和氧分压;使整个反应过程中氧化尽可能在化学动力学控制范围内进行,减少扩散因素的影响。试验结果表明,氧化蜡的酯价/酸价比值可作为反映氧扩散速度是否满足氧化动力学速度的需要,也可以估计氧化所能达到的最高酸价。氧化过程中物料收率变化的规律说明,在反应后期氧化蜡收率的显著降低,与此时CO_2和冷凝水相的生成速度迅速增加有关。氧化至酸价400以上后,C_4～C_（10）二元酸的收率最高可达40％（对原料石蜡）。从色谱分析结果得知,在C_4～C_（10）的单体二元酸分布中,一般皆以丁二酸为最多,次为戊二酸,并且C_4～C_5和C_6～C_（10）二元酸的收率相近。     

氧化蜡的制备及其性能研究

以石蜡为主要原料,加入一定量的微晶蜡,采用纯氧气进行催化氧化改性,考察了反应温度、反应时间、氧气流速、催化剂用量、助剂用量等因素对氧化蜡性质的影响。结果表明,氧化蜡的结构中出现羰基官能团;在以质量分数为0.52%的硫酸锰为催化剂,质量分数为12%的硬脂酸为助剂,氧气流速为75~85 mL/min,150℃条件下4 h,可以得到色泽浅、气味轻、酸值为23.44 mg KOH/g,皂化值为49.13 mg KOH/g的优质氧化蜡。     

尿素脱蜡装置改型生产轻液蜡

异丙醇水溶液尿素脱蜡装置设计目的是利用尿素分子在一定条件下能够与正构烷烃发生络合反应的特性，以常二线含蜡油为原料，生产高纯度300#重液蜡和低凝柴油。因市场对200#轻液蜡产品的需求旺盛，某公司准备利用现有生产设备，通过改造原料油组成、改变尿液组成、反应终温等工艺指标，使络合反应时的络合物具有一定的选择性，在保证产品质量和收率的前提下，使尿素脱蜡装置顺利改型生产200#轻液蜡和300#重液蜡。