Acetic anhydride reactor

Acetic acidMBK/water extraction, 468 Acetic acid purificatibn, 547 Acetic anhydride reactor, 573 Acetone/methanol equilibria, 416 Acetone/water equilibria, 423 Acetonitrile... 

Production of ketene and acetic anhydride reactor and internals up to 850 °C oxidation/carburization... 

G. Production of acetic anhydride and acetic acid. In the final step of the process, purified carbon monoxide from the gas separation plant is reacted with methyl acetate to form acetic anhydride by using a proprietary catalyst system and process developed by Eastman (U.S. Patent 4,374,070). Part of the acetic anhydride is reacted with methanol to coproduce acetic acid. The methyl acetate resulting from this reaction is recarbonylated in the acetic anhydride reactor system. The acetic acid and acetic anhydride are refined in the distillation section of this plant. A reactor liquid purge stream removes high molecular weight by-products, and a catalyst recycle process recovers and regenerates the catalyst from the purge stream (U.S. Patent 4,388,217). 

Figure 14.8a shows a simplified flowsheet for the manufacture of acetic anhydride as presented by Jeffries. Acetone feed is cracked in a furnace to ketene and the byproduct methane. The methane is used as furnace fuel. A second reactor forms acetic anhydride by the reaction between ketene from the first reaction and acetic acid. 

Polymer is separated from the polymerisation slurry and slurried with acetic anhydride and sodium acetate catalyst. Acetylation of polymer end groups is carried out in a series of stirred tank reactors at temperatures up to 140°C. End-capped polymer is separated by filtration and washed at least twice, once with acetone and then with water. Polymer is made ready for extmsion compounding and other finishing steps by drying in a steam-tube drier. 

Under sufficient pressure to permit a Hquid phase at 55—56°C, the acetaldehyde monoperoxyacetate decomposes nearly quantitatively into anhydride and water in the presence of copper. Anhydride hydrolysis is unavoidable, however, because of the presence of water. When the product is removed as a vapor, an equiUbrium concentration of anhydride higher than that of acetic acid remains in the reactor. Water is normally quite low. Air entrains the acetic anhydride and water as soon as they form. 

Reaction in a Centrifugal Pump In the reaction between acetic acid and gaseous ketene to make acetic anhydride, the pressure must be kept low (0.2 atm) to prevent polymerization of ketene. A packed tower with low pressure drop could be used but the required volume is very large because of the low pressure. Spes (Chem. Ing. Tech., 38, 963-966 [1966]) selected a centrifugal pump reactor where... 

Eastman Chemical Company has operated a coal-to-methanol plant in Kingsport, Tennessee, since 1983. Two Texaco gasifiers (one is a backup) process 34 Mg/h (37 US ton/h) of coal to synthesis gas. The synthesis gas is converted to methanol by use of ICl methanol technology. Methanol is an intermediate for producing methyl acetate and acetic acid. The plant produces about 225 Gg/a (250,000 US ton/a) of acetic anhydride. As part of the DOE Clean Coal Technology Program, Air Products and Cnemicals, Inc., and Eastman Chemic Company are constructing a 9.8-Mg/h (260-US ton/d) slurry-phase reactor for the conversion of synthesis gas to methanol and dimethyl... 

Acetic anhydride is hydrolyzed at 40°C in a CFSTR. The reactor is initially charged with 0.57 m of an aqueous solution containing 0.487 kmol/m of anhydride. The reactor is heated quickly to 350 K, and at tliat time, a feed solution containing 0.985 kmoFm of anhydride is run into the reactor at the rate of 9.55 x 10 m /sec. At the instant the feed stream is introduced, the product pump is started and the product is withdrawn at 9.55 x 10 m /sec. The reaction is first order... 

A solution containing 0.25 kmol/m of acetic anhydride is to be hydrolyzed in a single CFSTR to give an effluent containing an anhydride concentration of 0.05 kmol/m. The volumetric flowrate is 0.05 m /min and the working volume of the reactor is 0.75 m. ... 

The one-pot MCR of methylene active nitriles 47 has been used in the synthesis of both pyrano- and pyrido[2,3-d]pyrimidine-2,4-diones in a single-mode microwave reactor [90]. Microwave irradiation of either barbituric acids 61 or 6-amino- or 6-(hydroxyamino)uracils 62 with triethyl-orthoformate and nitriles 47 (Z = CN, C02Et) with acetic anhydride at 75 °C for 2-8 min gave pyrano- and pyrido[2,3-d]pyrimidines in excellent yield and also provided a direct route to pyrido[2,3-d]pyrimidine N-oxides (Scheme 27). 

The process begins with a gasification process that converts coal into carbon monoxide and hydrogen. Part of this gas is sent to a water-gas shift reactor to increase its hydrogen content. The purified syngas is then cryogenically separated into a carbon monoxide feed for the acetic anhydride plant and a hydrogen-rich stream for the synthesis of methanol. 

Eastman uses acetic anhydride primarily for esterification of cellulose, producing acetic acid as a byproduct. This acetic acid is used to convert the methanol into methyl acetate in a reactor-distillation column in which acetic acid and methanol flow countercurrently. 

Acylations of Amines Investigated in Micro Reactors Organic synthesis 8 [OS 8] Acetic anhydride acylation of diverse amines... 

Acetic acid and 10, 15, or 20% acetyl chloride were fed as a mixture into a modified falling film micro reactor (also termed micro capillary reactor in [57]) at a massflow rate of 45 g min and a temperature of 180 or 190 °C [57]. Chlorine gas was fed at 5 or 6 bar in co-flow mode so that a residual content of only 0.1% resulted after reaction. The liquid product was separated from gaseous contents in a settler and collected. By exposure to water, acetyl chloride and acetic anhydride were converted to the acid. The hydrogen chloride released was removed. 

HYDROL - Batch Reactor Hydrolysis of Acetic Anhydride... 

The liquid phase hydrolysis reaction of acetic anhydride to form acetic acid is carried out in a constant volume, adiabatic batch reactor. The reaction is exothermic with the following stoichiometry... 

Bromohydroxybiphenyl was O-acetylated with excess acetic anhydride in pyridine. The excess anhydride was to be hydrolysed by addition of water, but this was done without proper control using a hosepipe. The hydrolysis reaction ran away, causing boiling and evaporation of the reactor contents. 

The hydrolysis of acetic anhydride is being studied in a laboratory-scale continuously stirred tank reactor (CSTR). In this reaction acetic anhydride [(CH3C0)20] reacts with water to produce acetic acid (CH3COOH). 

The initial experimental design is shown in Figure 10-14. Water and acetic anhydride are gravity-fed from reservoirs and through a set of rotameters. The water is mixed with the acetic anhydride just before it enters the reactor. Water is also circulated by a centrifugal pump from the temperature bath through coils in the reactor vessel. This maintains the reactor temperature at a fixed value. A temperature controller in the water bath maintains the temperature to within 1°F of the desired temperature. 

Consider the hydrolysis of acetic anhydride carried out in dilute aqueous solution in a batch reactor ... 

P4.07.09. ACETIC ANHYDRIDE HYDROLYSIS. ADIABATIC AND COOLED REACTORS. 

A batch reactor has a 500 lb charge of a solution of acetic anhydride at a concentration of 0.0135 lbmol/cuft. The solution density is 65.5 lb/cuft and its specific heat is 0.9 Btu/(lb)(). The heat of reaction is -90,000 Btu/lbmol and the specific rate is... 

Transient Holdup Profiles in an Agitated Extractor 459 Homogeneous Free-Radical Polymerisation 310 Batch Reactor Hydrolysis of Acetic Anhydride 247 Continuous Bioreactor with Inhibitory Substrate 543 Dynamic Oxygen Electrode 462... 

Other companies (e.g. Hoechst, now Celanese) have developed a slightly different process in which the water content is low in order to save CO feedstock [1], In the absence of water it turned out that the catalyst precipitates. Also, the regeneration of ihodium(III) is much slower. The formation of the trivalent rhodium species is also slower because the HI content is much lower when the water concentration is low. The water content is kept low by adding part of the methanol in the form of methyl acetate. Indeed, the shift reaction is now suppressed. Stabilisation of the rhodium species and lowering of the HI content can be achieved by the addition of iodide salts (Li, ammonium, phosphonium, etc). Later, we will see that this is also important in the acetic anhydride process. High reaction rates and low catalyst usage can be achieved at low reactor water concentration by the introduction of tertiary phosphine oxide additives [1]. 

The acetylation over protonic zeolites of aromatic substrates with acetic anhydride was widely investigated. Essentially HFAU, HBEA, and HMFI were used as catalysts, most of the reactions being carried out in batch reactors, often in the presence of solvent. Owing to the deactivation effect of the acetyl group, acetylation is limited to monoacetylated products. As could be expected in electrophilic substitution, the reactivity of the aromatic substrates is strongly influenced by the substituents, for example, anisole > m-xylene > toluene > fluorobenzene. Moreover, with the poorly activated substrates (m-xylene, toluene, and fluoroben-zene) there is a quasi-immediate inhibition of the reaction. It is not the case with activated substrates such as anisole and more generally aromatic ethers. It is why we have chosen the acetylation of anisole and 2-methoxynaphtalene as an example. 

The above observations allow the selective formation of RDX, HMX or the two linear nitramines (247) and (248) by choosing the right reaction conditions. For the synthesis of the linear nitramine (247), with its three amino nitrogens, we would need high reaction acidity, but in the absence of ammonium nitrate. These conditions are achieved by adding a solution of hexamine in acetic acid to a solution of nitric acid in acetic anhydride and this leads to the isolation of (247) in 51 % yield. Bachmann and co-workers also noted that (247) was formed if the hexamine nitrolysis reaction was conducted at 0 °C even in the presence of ammonium nitrate. This result is because ammonium nitrate is essentially insoluble in the nitrolysis mixture at this temperature and, hence, the reaction is essentially between the hexamine and nitric acid-acetic anhydride. If we desire to form linear nitramine (248) the absence of ammonium nitrate should be coupled with low acidity. These conditions are satisfied by the simultaneous addition of a solution of hexamine in acetic acid and a solution of nitric acid in acetic anhydride, into a reactor vessel containing acetic acid. 

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