Methyl alcohol reactors

Manufacture is either by reaction of molten sodium with methyl alcohol or by the reaction of methyl alcohol with sodium amalgam obtained from the electrolysis of brine in a Castner mercury cell (78). Both these methods produce a solution of sodium methylate in methanol and the product is offered in two forms a 30% solution in methanol, and a soHd, which is a dry, free-flowing white powder obtained by evaporating the methanol. The direct production of dry sodium methylate has been carried out by the introduction of methanol vapors to molten sodium in a heavy duty agitating reactor. The sohd is supphed in polyethylene bags contained in airtight dmms filled in a nitrogen atmosphere. 

Methylene dichloride and chloroform may be produced by modified methods using a mixture of chlorine, methane, and methyl chloride as feed. Chlorination is run at 350-400°C reactor temperature at slightly above atmospheric pressure. A 2.6 1 chlorine methane ratio results in an optimal yield of chloroform. Alternatively, excess methane is reacted with chlorine at 485-510°C to produce methylene dichloride as the main product.181 The predominant method, however, still is the chlorination of methyl chloride manufactured by the reaction of methyl alcohol and hydrogen chloride.181... 

The bottom layer, the methanol solution of muriatic carbamide, is poured off. The top layer, the toluene solution of methylphenyldimethox-ysilane, is left in the reactor, backflow cooler 5 is switched in the direct operation mode and the reactor jacket is filled with vapour. The contents of the apparatus are heated and at the tank temperature below 150 °C the mixture of methyl alcohol and toluene is distilled into receptacle 6 until the distillation stops (the distillation speed is regulated by sending vapour into the reactor jacket 7). The toluene methanol mixture (97% of toluene and 3% of methyl alcohol) is sent from receptacle 6 into batch box 3, from where it enters reactor 7. After the toluene methanol mixture is distilled completely, the contents of reactor 7 are cooled with water sent into the jacket down to 30 °C and sent by nitrogen flow into receptacle 7. 

Because pH of the medium is so essential for the alcoholysis of triace-toxyphenylsilane, at this stage the acidity of the reactive mixture is monitored. pH should be about 1+2. If pH >2, reactor 5 is filled with an additional quantity of phenyltrichlorosilane from batch box 2, reducing the temperature to 30-40 °C prior to that. After phenyltrichlorosilane has been added, the mixture in the apparatus is held at 45-55 °C at least for 1 more hour and then checked for acidity and appearance. If the analysis is positive (pH 1+2), the mixture is sampled and sent to the laboratory, where tri-acetoxyphenylsilane is subjected to alcoholysis with methyl alcohol to determine the onset temperature for the distillation of methylacetate (58-68 °C in the reactive mixture). If at this temperature methylacetate does not distil, reactor 5 is filled from batch box 2 with an additional amount of phenyltrichlorosilane. The sample is chosen in such a way that the solid and liquid phases are approximately 1 1. 

Methyl dichloride is obtained by the interaction of phosphorus thiotri-chloride with methyl alcohol. The process is carried out in an excess of alcohol (2 moles of CH3OH per 1 mole of PSCI3), which serves to absorb released hydrogen chloride. Phosphorus thiotrichloride from batch box 2 and methyl alcohol from batch box 3 are pumped with batching pumps through siphons into reactor 1. The synthesis occurs when the components are fed simultaneously at 0-5 °C. To withdraw the heat and maintain the temperature in reactor 1, the coil and jacket of the reactor are filled with -15 °C salt solution. The products of the reaction, which include dichloride, unreacted... 

Preparation of methyl monochloride. Methyl monochloride is synthesised in reactor 10 (see Fig. 110), which is made of stainless steel and has a propeller agitator, a jacket and a coil. Methyl dichloride is sent from batch box 9 by compressed nitrogen into reactor 10 and is cooled there to 0 °C by sending -15 °C salt solution into the coil and the jacket of the apparatus. Then, reactor 10 is filled at agitation with a necessary amount of methyl alcohol from batch box 11. After mixing dichloride and methyl alcohol, the temperature in reactor 10 is brought to 0 °C at this temperature and agitation the apparatus receives metered amounts of 40-42% solution of sodium hydroxide from batch box 12. 

Alcoholysis of l-chloro-2,4-dinitrobenzene to 2,4-dinitroanisole. To 800 kg of methyl alcohol in the reactor 196 kg of sodium hydroxide and 600 kg of chloro-dinitrobenzene are added in 10 equal portions. The reagents are added alternately. During this operation, which requires 7 hr, a temperature at 40-45°C is maintained. Then the temperature is raised to 50°C by heating the reactor jacket and kept there for 30 min, before cooling the whole mixture to 35°C (which takes 3 hr). The crystals of the product together with the mother liquor are then transferred to a vacuum filter for separation. The product obtained is washed four times with water, centrifuged and finally transferred to the nitration plant. 

A C4 fraction and methyl alcohol (molar ratio methyl alcohol i-C4 = 1 1) is preheated to about 70°C before being sent to the reactor containing a fixed bed of sulphonated polystyrene resin. The reaction is exothermic (AH298=-37.7 kj/mol) and the heat produced is removed by means of cooling jackets so as to keep the temperature below 120°C. The reaction mixture from the top of the reactor is distilled and any unreacted butene is collected overhead with the azeotropic amount of methyl alcohol. The bottom contains pure MTBE. The distillate, together with additional methyl alcohol, is passed to a second reactor. The products from the second stage are extracted with water to remove residual methyl alcohol. The water-methyl alcohol solution is distilled to recover methyl alcohol, which is recycled. 

A reactor was charged with 10 ml liquid ammonia at —78°C to which was added lithium (4 eq) and the product from Step 1 (53 mg) in 4 ml THF. The mixture was stirred and a blue color appeared an additional amount of lithium was added to maintain the color of the mixture. The mixture was stirred 1 hour at —78°C, several drops of methyl alcohol added until the blue color disappears, and the mixture warmed to ambient temperature and concentrated. The residue was treated with 6 ml water and 10 ml diethyl ether, cooled to 0°C, then treated with iodine (3.00 mmol) dissolved in 15 ml 20% aqueous KL The... 

Methyl bromide (5.1 kg) was piped into the product from Step 3 at 20 °C and the mixture stirred for 3 days at 30°C. Thereafter, 70L DMF was distilled off in vacuo at 50°, the solution transferred to a smaller reactor, and then rinsed with 10 L DMF. An additional lOOL DMF was distilled off and the remainding solution stirred 2 hours at 15°C. The product was isolated by filtration in 88% yield, mp = 200-230 °C. The yield increased to 96% yield after recrystallizing 10.3 kg crude material in 66 L methyl alcohol, mp = 228 °C. 

A reactor was charged with 3,4-dioximino-2-oxotetrahydrofuran (9.4 g) suspended in 50 ml methyl alcohol, isopropylamine (4.2 g) added, and the mixture stirred 3 hours. The mixture was cooled in an ice bath and 8.5 g product isolated by filtration, mp = 133-134°C. 

A reactor was charged with N,N-dimethylformamide dimethyl acetal (700 mmol) and pyruvaldehyde dimethyl acetal (700 mmol), heated to 110°C 4 hours, cooled to 85 °C, and thiourea (636.4 mmol) and sodium methoxide (700 mmol) dissolved in 160 ml methyl alcohol added. Thereafter, the mixture stirred 4 hours. The mixture was cooled to 65 °C and 1-bromopropane (700mmol) added over 15 minutes. After 1 hour, 100ml EtOAc was added and the mixture heated to 95 °C. The solvents were distilled off, 120 ml water added, the mixture stirred 10 minutes at 50°C, cooled, concentrated, and the product isolated as a yellow oil. NMR data supplied. 

To 1-aminocyclohexane-l-carboxylic acid (350 mmol) dissolved in 1.25 L of methyl alcohol in a glass reactor was added 51 ml thionyl chloride in portions at —5°C. The mixture was stirred 5 hours then stood overnight. Thereafter, the mixture was concentrated, the residue mixed with water, the solution pH adjusted to 9 using Na2C03, and extracted twice with CH2CI2. The organic phase was dried, re-concentrated, and the product isolated in 66% yield. 

A reactor was charged with paraformaldehyde (30.5 g), N-methyl-N -nitroguanidine (20 g), triethylamine (17 g) and 100 ml apiece toluene and dioxane, and the mixture refluxed 16 hours. Thereafter, the solvent was evaporated, the residue purified by column chromatography on silica using CH2Cl2/methyl alcohol, 95 5, and the product isolated, mp= 137-139 °C. 

The esterification reaction of jasmonic acid with methyl alcohol was carried out in a high-pressure reactor to reduce epimerization. It was known that the cis-form of methyl jasmonate easily epimerized to the trans-form of methyl jasmonate under acid, base and high temperature conditions. The resulting methyl jasmonate mixture was recovered and purified by solvent extraction followed by fractional distillation. To improve the methyl epijasmonate concentration, additional steps of fractionation, such as the use of silica gel, were applied. 

The reaction was carried out in a fixed-bed quartz reactor at 90-400 C The reaction products were analyzed by a GLC technique. Carbon dioxide and formaldehyde were found to be the only products of methanol oxidation in no case the formation of CO was detected. In parallel to oxidation, the dehydration of methyl alcohol also occurs, dimethyl ether (DME) being a product. 

An explosion within the vapour space of a reactor resulted when methyl alcohol vapour reacted with incoming halogen. The explosion ruptured a 51 mm graphite rupture disc on the reactor. The alcohol vapour resulted from a slurry, which was usually washed three times to remove the excess alcohol prior to transfer to the reactor. 

Markets and Miscellaneous Information Methanol is methyl alcohol and at the present 99% of the production of methanol in the world is produced either from natural gas or gases out of oil. The reformed gas is compressed and passed to a methanol reactor. Carbon monoxide and carbon dioxide react with hydrogen over a catalyst to produce methanol. Also it is possible to produce methanol and ammonia... 

Esterifica.tlon. The process flow sheet (Fig. 4) outlines the process and equipment of the esterification step in the manufacture of the lower acryflc esters (methyl, ethyl, or butyl). For typical art, see References 69—74. The part of the flow sheet containing the dotted lines is appropriate only for butyl acrylate, since the lower alcohols, methanol and ethanol, are removed in the wash column. Since the butanol is not removed by a water or dilute caustic wash, it is removed in the a2eotrope column as the butyl acrylate a2eotrope this material is recycled to the reactor. 

Patty esters (wax esters), formed by ester interchange of the product alcohol and the starting material in the hydrogenolysis reactors, are later separated from the product by distillation. Unreacted methyl esters are also converted to fatty esters in the distillation step... 

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. 

Liquid mixtures of methanol and hydrochloric acid slowly yield methyl chloride even at 0°C (20,21), The typical process is carried out by contacting the alcohol with hydrochloric acid at 70 to 160°C and 0.1—1 MPa (15—150 psig) in the presence of a catalyst such as zinc chloride, quaternary amines (18,19,22), or with no catalyst at aH (23,24). TypicaHy 0.5 to 3% of the methanol is converted to dimethyl ether. Product methyl chloride is taken out of the reactor as a vapor and is cooled to condense as much of the water vapor and HCl as possible. Dimethyl ether and the residual water is then removed and the finished methyl chloride is condensed. 

In the manufacture of methyl ethyl ketone (MEK) from 2-butanol, the reactor products are precooled and then partially condensed in a shell and tube exchanger. A typical analysis of the stream entering the condenser is, mol fractions MEK 0.47, unreacted alcohol 0.06, hydrogen 0.47. Only 85 per cent of the MEK and alcohol are condensed. The hydrogen is non-condensable. 

The butyl alcohol is pumped from storage to a steam-heated preheater and then to a vaporiser heated by the reaction products. The vapour leaving the vaporiser is heated to its reaction temperature by flue gases which have previously been used as reactor heating medium. The superheated butyl alcohol is fed to the reaction system at 400°C to 500°C where 90 per cent is converted on a zinc oxide-brass catalyst to methyl ethyl ketone, hydrogen and other reaction products. The reaction products may be treated in one of the following ways ... 

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