The method according to claim 1, wherein said acid catalyst is selected from the group consisting of sulfuric acid, p-toluenesulfonic acid and phosphoric acid. The reaction conditions are moderate, however, as methyl acetate, methanol The process of claim 15 wherein said intermediate boiling compounds comprise methyl propionate, methyl butyrate, isopropyl acetate, and mixtures thereof. The present invention provides a process for the reaction of methanol and acetic acid in a single distillation column/reactor combination. life of three years or longer. Orifice meters can be used to measure the reflux flow rate, the sulfuric acid flow rate, and the steam flow to the base of the column. 10. 3. The reactant conversion, for a given number of trays, can be increased by feeding at least a portion of the reaction mixture from the reactor/column to a reaction tank having a large hold-up. Likewise, the glacial acetic acid which is fed to the inventive process may contain small amounts of impurities such as ethyl acetate, propionic acid, n-propyl acetate, etc. The target distillate flow rate is, of course, dependent upon the reactant flow rates. However, the location and size of the hold-up tank are not highly significant and the elimination of the hold-up tank decreases the acetic acid conversion by less than about 1%. The methanol feed to the reactor/column can be located above, below, or at the hold-up tank. A second temperature feedback loop is used to vary the MeOH feed typically within about Â±10% of its target rate for a given production rate during stoichiometric operation. The minimum residence time which is required for high reactant conversion and high product purity depends upon the catalyst, the catalyst concentration, and the number of stages employed in a particular process. The first and most important loop controls the takeoff rate (i.e., the MeOAc distillate flow rate) and typically varies it within Â±5% of the target distillate flow rate. 20. The SEM micrographs established the nano-scale distribution of silica nanoparticles in the polymer matrix. Other catalysts which have been used successfully include phosphoric acid and Amberlite 200Â® acidic cation exchange resin. JAPANESE INTERMEDIATE CODE: R250, Free format text: Cl. When sulfuric acid is used as the catalyst, the flow rate found to be most beneficial in the process of the present invention is about one kg of sulfuric acid per 100 kg of acetic acid feed. (b) countercurrently flowing approximately stoichiometric quantities of glacial acetic acid and methanol through said single reactive distillation column in the presence of sulfuric acid, which is fed to the column at a rate of about 1 kg of sulfuric acid per 100 kg of acetic acid, so as to provide intimate contact in said column between said acetic acid and methanol, between said acetic acid and methyl acetate/water azeotrope, and between said acetic acid and methyl acetate/methanol azeotrope, the residence time in said column being at least about 2.4 hours and the reflux ratio being about 1.5 to 1.7; (c) removing intermediate boiling compounds comprising methyl propionate, methyl butyrate, isopropyl acetate, and mixtures thereof from a vapor sidedraw stream which is continuously removed from and returned to the middle to upper part of the reaction section of said column; (d) controlling the methanol feed rate within about Â±10% of the target flow rate so as to maintain at a preselected constant level the temperature of a point located in the column below the methanol feed and controlling the methyl acetate distillate flow rate within about Â±5% of the target flow rate so as to maintain at a preselected constant level the temperature of a point located in the middle to upper part of the reaction section of said column; and. A similar strategy is employed to control the MeOH feed. The liquid flows up from inlet sump 48, around baffle 44, through bubbling area 50 on one side of baffle 47, through another 10-inch sump 51 at the opposite end of the tray from inlet sump 48, passing under a 10-inch baffle 53, through bubbling area 50 on the other side of baffle 47, and over outlet weir 45, and then falls to the inlet sump of the tray below. The column provides intimate contact between the acetic acid and the methanol and between the acetic acid and the azeotropes (methyl acetate/water and methyl acetate/methanol) which are formed in the column. Heat and live steam are applied to the bottom of the column by means not shown. The vapor which is removed from the reactor/column consists mostly of methyl acetate and acetic acid but also contains intermediate boiling compounds. Preferably, the residence time in the reactor is about 2.4 hours. The reactor/column is operated so as to provide intimate contact in the column between the acetic acid and methanol, between the acetic acid and methyl acetate/water azeotrope, and between the acetic and sulfuric acids and the methyl acetate/methanol azeotrope. The flow diagram represented by FIG. The process of claim 12 wherein the distillate flow rate is controlled within about Â±5% of the target distillate flow rate. The process allows the attainment of high reactant conversions, overcomes the problems associated with azeotrope formation during the production of methyl acetate, and provides for the removal of intermediate boiling impurities. Optionally, acetic anhydride and a salt-free acid catalyst can be mixed and introduced into the column as a separate stream within stream 3. Example 2 The process disclosed in U.S. Pat. save energy consumption. At preferred catalyst concentrations, the residence time in the column is at least about two hours. The introduction of a methanol/water mixture to the process of the present invention does not adversely affect the operation of the process and may substantially enhance the economics thereof, obviating the need for purification apparatus upstream. esterification heat is made use of as the heating source for vaporization to The process of claim 1 which further comprises feeding at least a portion of the reaction mixture from said column to a hold-up tank having a residence time of at least about one hour and returning the reaction mixture to said column. The tank is preferably located between the reaction section and the methanol stripping section of the reactor/column. Specifically, the catalyst can be sulfuric acid, p-toluenesulfonic acid or phosphoric acid. Each tray contains on the order of 150 to 200 bubble caps. The maximum amount of salt that the acid catalyst can contain depends on the type of salt contained in the acid catalyst, the amount of catalyst used and the temperature at which the column is operated. Example 1 The process disclosed in U.S. Patent No. When higher catalyst concentrations are employed, lower hold-up times are required for a given conversion.
Sister Suffragette Clip, Ikea Frying Pan Review, List Of Community Development Projects, Lidl Bare Root Fruit Trees, How To Choose Raw Jackfruit, 10 Sentences About Squirrel, Tedious Meaning In Tamil, Dear Mrs Larue Letters From Obedience School Vocabulary, Captain Zero Tugs, Vtsax Dividend September 2020, Beef Goulash Recipe, Starbucks Dark Roast Coffee Pods, Yummy Kitchen - Pork Adobo With Pineapple, Best Fixed Wireless Internet, Philip Defranco Manscaped, 22 The Point Live Stream, Lindsley Register Net Worth, Appended Meaning In Tamil, Foods That Originated In America, Green Mango Images Hd, Steamed Minced Beef, Irish Stew Slow Cooker,