Methanol impurities

Ah H was measured in ethanol and corrected for the heat of solution. The value given is for a liquid —> liquid reaction. Hydrogen uptake was slightly under theoretical indicating the possibility of 2-4% methanol impurity. 

It is most important that the feed does not contain even a small impurity that harms the phase separation. A small amount of methanol in n-butanol feed for instance will build up at the head of the column because both exits from the plant are for less volatile materials. The methanol impurity eventually stops the n-BuOH separating from the water. 

As well as Methanol Impure methanol Error at supplier Exothermic reaction, explosion... 

An internal standard of 1-butanol is used to determine the concentrations of one or more of the following impurities commonly found in whiskey acetaldehyde, methanol, ethyl acetate, 1-propanol, 2-methyl-1-propanol, acetic acid, 2-methyl-1-butanol and 3-methyl-1-butanol. A packed column using 5% Garbowax 20m on 80/120 Garbopak B and an EID detector were used. 

Another example is the purification of a P-lactam antibiotic, where process-scale reversed-phase separations began to be used around 1983 when suitable, high pressure process-scale equipment became available. A reversed-phase microparticulate (55—105 p.m particle size) C g siUca column, with a mobile phase of aqueous methanol having 0.1 Af ammonium phosphate at pH 5.3, was able to fractionate out impurities not readily removed by hquid—hquid extraction (37). Optimization of the separation resulted in recovery of product at 93% purity and 95% yield. This type of separation differs markedly from protein purification in feed concentration ( i 50 200 g/L for cefonicid vs 1 to 10 g/L for protein), molecular weight of impurities (<5000 compared to 10,000—100,000 for proteins), and throughputs ( i l-2 mg/(g stationary phasemin) compared to 0.01—0.1 mg/(gmin) for proteins). 

The alcoholysis reaction may be carried out either batchwise or continuously by treating the triglyceride with an excess of methanol for 30—60 min in a well-agitated reactor. The reactants are then allowed to settle and the glycerol [56-81-5] is recovered in methanol solution in the lower layer. The sodium methoxide and excess methanol are removed from the methyl ester, which then maybe fed directiy to the hydrogenolysis process. Alternatively, the ester may be distilled to remove unreacted material and other impurities, or fractionated into different cuts. Practionation of either the methyl ester or of the product following hydrogenolysis provides alcohols that have narrow carbon-chain distributions. 

Anhydrous, monomeric formaldehyde is not available commercially. The pure, dry gas is relatively stable at 80—100°C but slowly polymerizes at lower temperatures. Traces of polar impurities such as acids, alkahes, and water greatly accelerate the polymerization. When Hquid formaldehyde is warmed to room temperature in a sealed ampul, it polymerizes rapidly with evolution of heat (63 kj /mol or 15.05 kcal/mol). Uncatalyzed decomposition is very slow below 300°C extrapolation of kinetic data (32) to 400°C indicates that the rate of decomposition is ca 0.44%/min at 101 kPa (1 atm). The main products ate CO and H2. Metals such as platinum (33), copper (34), and chromia and alumina (35) also catalyze the formation of methanol, methyl formate, formic acid, carbon dioxide, and methane. Trace levels of formaldehyde found in urban atmospheres are readily photo-oxidized to carbon dioxide the half-life ranges from 35—50 minutes (36). 

The quahty of formamide suppHed by BASE is certified as having a minimum assay of 99.5%. The principal impurities in the material are ammonium formate, methanol, water, and traces of iron. The quaUty of formamide supphed by BASE is certified to meet the specifications given in Table 3. 

Methanol can be converted to a dye after oxidation to formaldehyde and subsequent reaction with chromatropic acid [148-25-4]. The dye formed can be deterruined photometrically. However, gc methods are more convenient. Ammonium formate [540-69-2] is converted thermally to formic acid and ammonia. The latter is trapped by formaldehyde, which makes it possible to titrate the residual acid by conventional methods. The water content can be determined by standard Kad Eischer titration. In order to determine iron, it has to be reduced to the iron(II) form and converted to its bipyridyl complex. This compound is red and can be determined photometrically. Contamination with iron and impurities with polymeric hydrocyanic acid are mainly responsible for the color number of the merchandized formamide (<20 APHA). Hydrocyanic acid is detected by converting it to a blue dye that is analyzed and deterruined photometrically. 

Although there are no new methane VPO competitive processes, current technology may be usehil for the production of impure methanol in remote areas for use as a hydrate inhibitor in natural gas pipelines (119,120). 

Fumaric acid is sold as resia-grade and food-grade. The general sales specification under which resia-grade fumaric acid is sold ia the United States specifies white, crystalline granules with a minimum assay of 99.6% and maximum ash content of 0.05%. The moisture specification is 0.3% maximum with < 10 ppm heavy metals. The color of a 5% solution ia methanol is to be less than 10 APHA. Food-grade fumaric acid calls for somewhat lower impurity levels. Particle size and particle size distribution are important ia many appHcations. 

Hydrolysis of Dimethyl Terephthalate. Hoechst Celanese and Eormosa Chemical Eibers Corp. produce a polymer-grade terephthahc acid by hydrolysis of high purity dimethyl terephthalate. Hbls-Troisdorf AG hcenses a process with this step (70). Hydrolysis occurs at 260—280°C and 4500—5500 kPa (45—55 atm) in a hydrolysis reactor without catalysis. The overhead methanol and water vapor is separated and the methanol is returned to the dimethyl terephthalate section for reuse. The reactor hquid is crystallized, cycloned, washed, and further cooled. Einahy, the slurry is centrifuged and dried. The product has less than 25 ppm of 4-formylbenzoic acid and very low levels of other impurities. There may be several hundred parts per million of monomethyl terephthalate, which is incompletely hydrolyzed dimethyl terephthalate. 

Fiaal purification of propylene oxide is accompHshed by a series of conventional and extractive distillations. Impurities ia the cmde product iaclude water, methyl formate, acetone, methanol, formaldehyde, acetaldehyde, propionaldehyde, and some heavier hydrocarbons. Conventional distillation ia one or two columns separates some of the lower boiling components overhead, while taking some of the higher boilers out the bottom of the column. The reduced level of impurities are then extractively distilled ia one or more columns to provide a purified propylene oxide product. The solvent used for extractive distillation is distilled ia a conventional column to remove the impurities and then recycled (155,156). A variety of extractive solvents have been demonstrated to be effective ia purifyiag propylene oxide, as shown ia Table 4. 

The impure product is dissolved in methanol. Subsequent reaction with ammonium fluoride forms ammonium hexafluorotitanate. This soHd, obtained in high purity, reacts with water vapor in a stream of air at 250°C to give anatase. 

Pure (9-terphenyl can be obtained by fractional distillation. To obtain high purity m- or -terphenyl, the appropriate distillation fraction has to be further purified by recrysta11i2ing, 2one refining, or other refining techniques. Currently, litde demand exists for pure isomers, and only a mixture is routinely produced. Small amounts of acetone, ethanol, or methanol are used to promote dehydrocondensation, and as a result, minor amounts of methyl- or methylene-substituted polyphenyls accompany the biphenyl and terphenyls produced. For most purposes, the level of such products (<1%) is so small that their presence can be ignored. For appHcations requiring removal of these alkyl-polyphenyl impurities, an efficient process for their oxidative destmction has been described (38). 

Improvements to the methanol reductant processes may be found in the patent Hterature. These include methods of operation to reduce acidity in the crystallisation 2one of the generator to promote crystallisation of sodium sulfate and to reduce sulfuric acid consumption (48). Other improvements sought are the elimination of formic acid and chlorine impurities from the chlorine dioxide, as weU as methods of recovering acid and sodium hydroxide, or acid and neutral sodium sulfate from the soHd sodium sesquisulfate salt waste stream (48—52). 

A representative technical grade of methyl chloride contains not more than the following indicated quantities in ppm of impurities water, 100 acid, such as HCl, 10 methyl ether, 20 methanol, 50 acetone, 50 residue, 100. No free chlorine should be detectable. Traces of higher chlorides are generally present in methyl chloride produced by chlorination of methane. The boiling point should be between —24 and —23° C, and 5—95% should distill within a range of about 0.2°C. It should be clear, colorless, and free from visible impurities. 

Hydrogen Liquefaction. Hydrogen can be produced from caustic—chlorine electrolytic cells, by decomposition of ammonia or methanol, or by steam—methane reforming. Hydrogen recovered by these methods must be further purified prior to Hquefaction. This is generally achieved by utilizing pressure swing adsorption methods whereby impurities are adsorbed on a soHd adsorbent. 

Specifications. Eor fuel-grade MTBE, the typical specification of merchant product is 95 wt % minimum purity ia the United States and 98% minimum ia Europe. The maximums for impurities are usually 0.5 wt % for methanol, and 0.15 wt % for water. To maintain quaUty, fuel-grade MTBE is normally stored ia fixed-roof tanks, to keep rain water out, with internal floaters, to minimise vapor losses. 

Formaldehyde is a gas with a boiling point of -21 °C. It is usually supplied as a stabilised aqueous solution ( 40% formaldehyde) known as formalin. When formalin is used as the source of the aldehyde, impurities present generally include water, methanol, formic acid, methylal, methyl formate and carbon dioxide. The first three of these impurities interfere with polymerisation reactions and need to be removed as much as possible. In commercial polymerisation the low polymers trioxane and paraformaldehyde are convenient sources of formaldehyde since they can be obtained in a greater state of purity. 

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