Fatty acids,fatty alcohols,and wax esters fromLimnanthes douglassi (Meadowfoam) seed oil

Limanathes douglasii seed oil glycerides contain fatty acids which predominantly (97%) have 20 or more carbon atoms. Fatty acids were prepared by saponification; fatty alcohols, by sodium reduction of the glycerides; and liquid wax esters, byp-toluenesulfonic acid-catalyzed reaction of the fatty acids with the fatty alcohols. Solid waxes were prepared by hydrogenation of the glyceride oil and of the wax esters. Chemical and physical constants were determined forLimnanthes douglasii seed oil and its derivatives. The liquid wax esters had properties very similar to those of jojoba (Simmondsia chinensis) seed oil. The solid hydrogenated wax ester was identical in physical appearance and melting point to hydrogenated jojoba seed oil. A laboratory of the Northern Utilization Research and Development Division, Agricultural Research Service, USDA.     

Jojoba oil analysis by high pressure liquid chromatography and gas chromatography/mass spectrometry

Two analytical procedures for determining com-positions of jojoba liquid wax esters are described and compared. One, the more tedious, involves separation of wax ester homologs by high pressure liquid chro-matography followed by determination of the acid and alcohol moieties from each homolog. The second allows rapid determination of wax ester composition by gas Chromatographic separation of hydrogenated jojoba wax esters according to chain length, followed immediately by ancillary mass spectrometric identifi-cation of the acid and alcohol moieties. Double bonds in the alkyl chains in jojoba liquid waxes were almost exclusively (98%) ω-9, when examined by gas chro-matography/mass spectrometry (GC/MS) and ozonolysis/GC/MS. Presented in part at the 2nd International Conference on Jojoba and Its Uses, Ensenada, Mexico, February, 1976.     

Effect of the extraction and bleaching processes on jojoba (Simmondsia chinensis) wax quality

The aim of the work was to evaluate the effect of extraction method and bleaching on the quality of jojoba waxes from Argentina. Jojoba waxes obtained by cold pressing, Golden wax (expeller‐pressed wax) and Lite wax (bleached wax) were analyzed using standard methods adopted as recommended practices by the American Oil Chemists Society. Physical parameters, fatty acid and alcohol compositions were unchanged among waxes. Cold‐pressed wax was noteworthy by its lower peroxide value, higher amounts of tocopherol and total phenol contents. Accordingly, it presented the best oxidative stability. Bleaching caused a strong decrease in both tocopherol and phenol contents; consequently the bleached wax showed poor oxidative stability.     

Extraction of Surface Wax from Whole Grain Sorghum

Sorghum has potential as a domestic source of wax for applications in the food and nonfood industries. The waxes extracted from sorghum have similar physical properties to those of Carnauba wax, a common imported commercial wax. This work focused on the extraction, fractionation, and characterization of waxes from sorghum kernels. Extraction was performed by varying the extraction conditions including temperature and solvents (hexane, ethanol, and methanol). A fractionation technique was developed to separate and quantify waxes from nonwaxes. The fractions were then characterized using a reverse‐phase high‐performance liquid chromatography method developed in our laboratory that utilizes an evaporative light‐scattering detector for quantification. The results showed that the average amount of wax extracted from the surface of intact sorghum kernels was about 0.3 wt% using hexane at temperatures between 25 and 120°C and 1000 psi. The yield of wax via hexane extraction increased with temperature and ranged from about 0.06 to 0.39 wt%. Extraction with alcohols resulted in higher yields of extracts, but after fractionation to remove nonwax components, the yield of waxes was reduced by 31% for ethanol and 47% for methanol compared to hexane.     

Separation and Analysis of Wax from Egyptian Sugar Cane Filter Press Cake

Waxes from filter press cake of the by-product of the Sugar Cane Industry gained from various Egyptian Cane Sugar Factories were studied. A method for continuous extraction of wax filter cake using different solvent i. e. toluene, naphtha, acetone, fractionated gasoline, denatured and refined alcohol was investigated. The speed and ease of extraction using different solvents were compared. By using toluene as solvent the highest percentage of crude wax was obtained from Edfu, which gave 14.55%, while extraction with refined alcohol produced 12.65% crude wax from Qus. Decolorization of crude wax was carried out by sodium hypochlorite, nitric acid, chlorine, sulphur dioxide and acetone. The pure wax was separated from the fatty oil fraction by fractional crystallization from 70° to 0° C. The greater portion of wax can be obtained at 30° C. Hard, brittle wax was obtained between 45° to 20° C. The crude and refined waxes had properties comparable to carnauba wax and other commercial waxes. The Egyptian cane sugar waxes can be utilized in paper, ink, coating, varnishes, pharmaceuticals, cosmetics and fertilizer industries.     

Oil from deep water fish species as a substitute for sperm whale and jojoba oils

The lipid fraction of the deep water fish species orange roughy (Hoplostetbus atlanticus), black oreo (Allocyttus sp.) and small spined oreo (Pseudocyttus maculatus) had wax esters with even carbon numbers over the range C₃₀ to C₄₆ as the major components. The component acids and alcohols of the wax ester fraction were analyzed by gas liquid chromatography and compared with those of jojoba and sperm whale oils. Orange roughy oil was refined and deodorized and its chemical, physical and mechanical properties were determined. Hydrogenation of orange roughy oil produced a range of white crystalline waxes with melting points between 34 and 66 C. The characteristics of these waxes were very similar to those of hydrogenated jojoba oil and spermaceti. Lubricant tests performed on sulfurized orange roughy oil indicated it is comparable to sulfurized jojoba and sperm whale oils as an extreme-pressure additive in lubricants. The results show a sound technical basis on which to consider an industry based on orange roughy oil and the oreo oils as replacements for sperm whale oil and as substitutes for jojoba oil. Applications for the oil could be in the cosmetic and high-grade lubricant fields, the waxes in the polish, textile, cosmetic and pharmaceutical industries and the sulfurized derivative of orange roughy oil in the lubricant industry.     

Co-crystals of Beeswax and Various Vegetable Waxes with Sterols Studied by X-ray Diffraction and Differential Scanning Calorimetry

In this study, mixtures of purified wax and sterols were melted and subsequently cooled. Using X-ray diffraction of the mixed, solid phase, it was shown that for up to 30–40 wt% sterols no measurable re-crystallisation of sterols occurred, i.e. the sterols became dissolved at a molecular level. Probably a form of amorphous co-crystals of sterols and wax is formed if the molecular ratio does not exceed 1:1. Differential scanning calorimetry (DSC) suggests that a minor amount of pure sterols could already be present at lower sterol levels. This may be because of the higher temperature at which the microstructure is probed when using DSC—melting of the wax might lead to crystallisation of the sterols. For application in foods, the structure as probed by X-rays at ambient temperatures is more relevant. When sunflower wax and rice bran wax are used, prevention of sterol crystallisation is even more pronounced, probably because the melting temperatures of these waxes are closer to the melting temperature of sterol crystals. Replacing the beeswax with a saturated fat (heRP70), sunflower oil, or jojoba wax (a liquid wax) substantially increases the amount of crystalline sterols. The difference between the various waxes and fats was qualitatively the same for X-ray diffraction and DSC. Stanols can be incorporated in the same manner and up to similar concentrations. Another insoluble nutritional compound, ursolic acid, has a greater tendency to crystallise in wax. This is probably because the melting temperature of ursolic acid is much higher than that of wax.     

A Simplified Method for Fractionation and Analysis of Waxes and Oils from Sorghum (Sorghum bicolor (L.) Moench) Bran

In the United States, sorghum is primarily used for animal feed and ethanol production but has potential to provide value-added coproducts including waxes and oil. The surface of sorghum contains 0.1–0.4% wax; however, wax extraction from whole kernels before fermentation may not be economical. An alternative method for this extraction could be facilitated through decortication, abrasion of the surface to remove bran. Decortication increases the starch content of decorticated sorghum, potentially improving ethanol yields, while concentrating wax and oil to the bran. Typically, oil (triacylglycerols) and waxes are extracted from bran in one extraction and waxes are precipitated from oil using cold temperatures then filtration. This research compared traditional fractionation (simulated with a two-step, single-temperature extraction) to a two-step, dual-temperature extraction, whereby oil is first extracted at room temperature and then waxes at elevated temperature. Extractions were performed using an accelerated solvent extractor with hexane or ethanol as solvents. Ethanol extraction showed greater yields (~15% w/w) compared to those of hexane (~11% w/w) because polar materials were extracted. Using hexane, the two-step, dual-temperature fractionation separated waxes from oils via the temperature of extraction solvent with similar purity to the traditional method that fractionated via cold precipitation and filtration. For ethanol, the traditional single-step method fractionated with higher wax purity but lower oil purity compared to the two-step, dual-temperature fractionation.     

Wachssynthese mittels der Guerbet-Reaktion

Synthesis of Waxes by Guerbet Reaction Branched chain waxes possess better liquifying properties and superior solubility in organic solvents than straight chain waxes. Branched chain waxes having both of the above properties were therefore synthesized by a new principle, namely the Guerbet reaction. Guerbet alcohols, based on technical octadecyl alcohol were esterified with various mono- and dicarboxylic acids. Strongly branched and relatively low melting waxes were thus obtained which, inspite of their greater solubility in organic solvents, exhibit insignificant liquifying effect in wax pastes. As against these, when the Guerbet alcohols from stearyl alcohol are oxidized, branched chain wax alcohols are obtained which in native as well as saponified state show liquifying action on wax pastes. The Guerbet reaction is explained taking the example of a mixture of two primary alcohols.     

Separation of some paraffin wax grades using solvent extraction technique

Solvent extraction technique has been used to separate paraffin wax grades; with different characteristics; from El-Ameria light, middle and heavy slack waxes. The wax deoiling has been done by solvent extraction at different extraction temperatures and different solvent feed ratios (S/F by weight). The extraction solvents used are furfural, N-methyl-2-pyrrolidone (NMP) and N, N, dimethylacetamide (DMA). The wax products are evaluated according to TAPPI-ASTM equation and petroleum wax specifications. The data revealed that DMA and NMP are suitable extracting solvents for isolating of semi- and scale-refined grades of paraffin waxes from light and middle slack waxes. But furfural solvent can separate only semi-microcrystalline waxes from heavy slack wax.     

Holdup and extraction characteristics of jojoba meal

Holdup and drainage characteristics have been determined for three jojoba meals of different nature and size distribution, using hexane and isopropanol as solvents. Density and viscosity properties of the oil-solvent solutions have been measured. The experimental information should be of value in the design of solvent extraction equipment for jojoba nuts.     

Solubility of 1-monostearin in various solvents

Summary The practical limits of the solubility of pure monostearin in various solvents at different temperatures has been determined for isopropyl alcohol, ethanol, acetone, methanol, and commercial hexane. The synthetic method was employed, in which the temperature of known quantities of solvent and solute was decreased until crystallization of the solute began. This temperature, corrected for supercooling and heat loss to the surrounding bath, was taken as the equilibrium temperature between the known weight of solute and the known weight of solvent. The solubility-temperature data of monostearin in each of the various solvents are presented both graphically and in tabular form. A comparison of the solubility of monostearin in the various solvents at comparative temperatures indicates that its solubility is greatest in isopropyl alcohol and decreases in the order ethanol, acetone, methanol, and hexane. Presented at the 45th annual meeting of the American Oil Chemists' Society, San Antonio, Tex., April 12–14, 1954. One of the laboratories of the Southern Utilization Research Branch, Agricultural Research Service, U. S. Department of Agriculture.     

Adsorptive removal of aflatoxins

Physical removal of aflatoxins from cottonseed by solvent extraction with ethanol or isopropyl alcohol is technically feasible. These solvents used in the removal process are recycled to extraction systems after regeneration by distillation. However, distillation is costly due to high latent heat of the solvents. Adsorption techniques have been explored as a method to remove aflatoxins from these solvents. Enzyme-linked immunosorbent assays method and a high-performance liquid chromatography method with fluorescence detector were used to determine the toxins in the feed and eluates from the adsorption columns. Experimental data indicate that montmorillonite is highly effective for adsorptive aflatoxin removal. Adsorption data with neutral alumina and silica are also presented. Ethanol and ethanol-based miscellas, obtained from alcoholic cottonseed extractions were spiked with aflatoxins for this investigation. Presented in part at the 1991 AOCS Annual Meeting, Chicago, Illinois.     

Sunflower-Oil Wax Reduction by Seed Solvent Washing

Wax distribution in sunflower seeds was determined by capillary-gas chromatography, as well as both the wax composition in sunflower oils obtained from washed seeds and the wax composition in the solvent extracts. The dehulling efficiency was evaluated by using a laboratory centrifugal process. The washing effect on hull morphology and on wax distribution was observed by scanning-electron microscopy. Washing preferentially removed the crystallized fraction, hexane being the most effective solvent. Short contact times (20 s) at 25–40 °C were sufficient to extract the insoluble waxes by hexane washing. The extracted material consisted of C40–C54 waxes with higher percentages of extracted C44, C46 and C48. These are superficially in the hull of sunflower seed presenting a non-uniform distribution as observed by microscopy. Solvent washing with pre-heating of the seeds caused a decrease in sample moisture content, which reduced dehulling ability. Ethanol-washed seeds were the easiest to dehull, but higher production of fines was also observed. Solvent washing improves both the dehulling-seed ability increment and the recovery of sunflower waxes as a by-product for commercial use.     

Investigation of parameters affecting atmospheric extraction yields and extract qualities of two Turkish lignites

Four sets of extractions of two Turkish lignites have been performed at atmospheric pressure in Soxhlet-type extractors varying the time of extraction, particle size of the lignite, its moisture, and the solvent. Extractions performed in small-size Soxhlet extractors (capacity 90 g coal) with benzene as the solvent have shown that for the Mengen lignite the most appropriate size range is 20–60 Tyler mesh and the moisture content leading to highest yield is 10–12 per cent. For the Elbistan lignite the corresponding values are 10–60 Tyler mesh and 20 per cent moisture. Extractions carried out with benzene in a larger-size Soxhlet apparatus (capacity 1–1.5 kg coal) have shown that Mengen lignite should be extracted for 30 hours and Elbistan lignite for 24 hours for exhaustion. Most of the extractable material can be obtained in the first five hours in the case of Elbistan lignite and in the first 10 hours in the case of Mengen lignite; the difference is attributed to different porosities.Extractions carried out using various solvents in larger-size Soxhlet extractors under the most appropriate conditions as determined from the first three sets of experiments have indicated that Mengen lignite may be a promising raw material for industrial-scale montan wax production. Yields varying between 10 and 14 per cent on dry basis have been obtained from Mengen lignite with benzene—ethanol, benzene—methanol and tetrahydrofuran as solvents. Elbistan lignite gives a maximum yield of 3.5 per cent with tetrahydrofuran. Solvents characterized by a high substitution ability yield more extract. Montan waxes obtained from Mengen and Elbistan lignites are found to be richer in free acids and esters compared with commercially available ones. Infrared spectra results indicate the raw wax to be predominantly aliphatic. The melting points of the waxes obtained with various solvents are generally found to increase as the asphaltic matter content increases and resinous matter content decreases.     

Solvent hydrogenation of cottonseed oil

Refined and bleached cottonseed oil was dissolved in a solvent (hexane, isopropyl alcohol, or di-isopropyl ether) and was then hydrogenated in a dead-end hydrogenator. Hydrogenation runs were conducted at temperatures from 115 to 145°C., at hydrogen partial pressures from 44 to 74 p.s.i.a., with catalyst concentrations varying from 0.05 to 0.40% nickel, and at high rates of agitation to climinate mass-transfer resistances. A series of hydrogenation runs was also made in which no solvent was used. The rates of hydrogenation for the various series of runs were in the same order of magnitude but decreased in the following order: nonsolvent, hexane, isopropyl alcohol, and di-isopropyl other runs. Selectivity and isomerization were low in all cases and essentially identical for solvent and nonsolvent runs. The rate of hydrogenation increased in all cases with higher catalyst concentrations. For the isopropanol runs, the reaction rate was maximum as a function of temperature at about 135°C. In the case of the other solvents, the rate of hydrogenation increased with increased temperature in the range from 115 to 145°C., but the rate increases of the solvent runs were less than those of the nonsolvent runs.     

Chemical Quality Evaluation of Damaged Jojoba Seeds (Simmondsia chinensis)

The objective of the research was to characterize the quality of damaged and undamaged jojoba seeds. The study was performed on jojoba seeds grown in La Rioja, Argentina. Proximal composition, fatty acid composition, acid value, peroxide value, conjugated dienes and trienes and protein electrophoresis profiles were determined in undamaged (JS) and damaged jojoba seeds (DJS). The fat content (wax) was lower in DJS (39.11%) than in JS (50.82%). The values of acid, peroxide, conjugated dienes and trienes were higher in DJS than in JS. No difference in fatty acid composition was observed between DJS and JS. The protein content was not significantly different between JS and DJS. However, DJS had lower soluble protein values. In the electrophoresis profiles, the band located at 50 kDa disappeared in DJS and the intensity of the band located at 25 kDa decreased. The deterioration process in jojoba kernels significantly affects the chemical quality of their proteins and waxes.     

环境友好型脱漆剂的制备

以苯甲醇(BA)、二丙二醇丁醚(DPNB)和二甲基亚砜(DMSO)等为主溶剂制备环境友好型脱漆剂,采用单因素试验法研究了有机溶剂、促进剂、缓蚀剂以及封闭剂等助剂对脱漆效率的影响。试验结果表明:以BA、DPNB和DMSO为主溶剂,异丙醇(IPA)为助溶剂,表面活性剂AR-10和十二烷基苯磺酸钠(LAS)复配,复配有机酸为促进剂,微晶蜡为封闭剂,氨基磺酸与有机羧酸醇铵盐类缓蚀剂复配。当复合主溶剂的用量范围为60%～70%,m(DMSO)∶m(DPNB)=8∶6,m(AR-10)∶m(LAS)=1∶0.8,复配用量为2.5%～3%,异丙醇用量为5%～l0%,复配有机酸用量为7.5%～10%,微晶蜡用量为2.5%～3%时,脱漆效率最高。其组成均为低挥发性的物质,符合绿色化学"高效、洁净、经济、环保"的要求。     

The removal of pesticide residues from wool wax by solvent extraction

A range of suitable solvents for the removal of dieldrin and diazinon residues from wool wax by solvent-solvent extraction was evaluated. Extraction of a 10% solution of wool wax in hexane with N,N-dimethylformamide was shown to be the most effective. These solvents were then used to meanure the partition coefficients of 36 organochlorine, organophosphorus, and pyrethroid pesticides that have the potential to be found in wool wax. Repeated batchwise extraction of a raw wool wax, which had been spiked to produce typical pesticide residue levels, yielded a high-quality wax in which all pesticide residues had been reduced to below detectable levels. The treated wool wax was lighter in color with a lower acid number and a lower free alcohol content and had excellent water absorption characteristics. All detergents associated with the recovery of wool wax from an aqueous scour were also removed.     

异丙醇尿素脱蜡工艺改进

异丙醇尿素水溶液脱蜡过程中得到的脱蜡液和蜡液溶含有异丙醇、水和少量尿素,采用闪蒸方法分出水和部分异丙醇。在压力60.80 kPa、闪蒸温度90~95℃或以上时,脱蜡液和蜡液中的水全部分出,部分异丙醇也被分出,在脱蜡液和蜡液中的尿素全部结晶析出。过滤分出尿素后,脱蜡液和蜡液可直接蒸馏。