SU1328345A1 - Method of producing methylethylketone - Google Patents

Abstract

The invention relates to the production of ketones, in particular the production of methyl ethyl ketoia (MEK), which is used to dewax oils as a solvent. The goal is to increase the yield and increase the productivity of the process for the production of MEK from acetapedehyde and ethylene in the presence of O-containing gas and catalyst (QD). The goal is achieved using a QD mixture of cobalt acetates and. alkali metal (molar ratio 3.6–5: 1) with an ethylene feed rate of 120–780 h and holding gas (in terms of 0) 4.9–40, temperature 50–60 ° C and ethylene pressure 10 -18 ati (total pressure 20-22 ati). Concentration (CHjCOO) Co in CT 0.0014-0.001 mol / L. The release of IEC is carried out by distillation and treatment of the bottom product with water (mass ratio 1: 2-3) at 20-25 ° C, followed by 1m concentration of the aqueous solution and returning to the system. The yield of MEK, counting on ethylene, is up to 82%, productivity up to 375 g / l-h with acetaldehyde conversion up to 29% and ethylene conversion up to 24%. 1 tab. with (L with N0 00 with 4 cl

Description

 13283452

The present invention relates to a process for distilling off unreacted acetating of methyl ethyl ketone (MEK), which is used as a solvent in the dewaxing process of oils.

The purpose of the invention is to increase the yield of the target product to acetaldehyde converted and to increase the productivity of the process.

Example 1. B metal cylindrical reactor with a volume of 0.3 l, equipped with electrical heating,

ten

thaldehyde and 15.4 g of MEK with T 78-79 C are recovered by known rectification methods. The bottom residue (b g), containing 0.012 g of CoCOAc) + NgO and 0.0001 g of CoAc, is stirred for 10 minutes with water 20-25 C and the mass ratio of the bottom residue: water 1: 2. The mixture is then allowed to stand for 1 hour. The aqueous layer (14 g) contains 0.84 g of acetic acid, 0.01 g of Co (OAc) and 0.000 l of g of CoAc. Accumulated as a result of several

thaldehyde and 15.4 g of MEK with T 78-79 C are isolated by known methods of rectification. The bottom residue (b g) containing 0.012 g of CoCOAc) + HgO and 0.0001 g of KOAc is mixed for 10 minutes with water at 20 25 C and the mass relationship of the bottom residue: water 1: 2. The mixture is then allowed to settle for 1 hour. The aqueous layer (14 g) contains 0.84 g of acetic acid, 0.01 g of Co (OAc) and 0.000 l of g of CoAc. Accumulated as a result of several

electromagnetic stirrer, water cooler and carbon dioxide coolers, eig rud of similar experiments water layer is harvested 63.7 g (1.45 mol) of acetaldehyde (85 g) is subjected to rectification (Tggp, and 0.646 ml of a 1.5% CoOAc solution) to DE-UO S, 103 ° C, reflux 411.0 in acetic acid (0.000041 mol), the number of 10-20). Get 12 g VAT 0,0102 g Co (pAc) 2 HjO) and 0.19 ml of residue, containing 0.06 g of diacetate 0.05% solution of KOAc in acetic 20 0,0006 g of potassium acetate, acid (0 , 0001 g, 0.000001 mol KOAc), isolated catalyst solution. After heating the contents of the reactor, it is used in the synthesis of MEK of example 1 in an inert atmosphere under pressure. Examples 2-19. Processes from 5-6 atm to 60 C through the solution are passed as in Example 1. A mixture of ethylene (72.7% by volume) and 25 is passed. The results obtained are shown

in the table.

An increase in the rate of supply of oxygen-containing gas and ethylene in the process of this process leads to

one

speed 779 (partial pressure of ethylene 16 MPa) and air (17.3% by volume) at a rate of .40 hours for 0.5 hours at a total pressure of

reactor 22 ATI. From the resulting mixture, a sharp increase in the degree of oxidation

thaldehyde and 15.4 g of MEK with T 78-79 C are isolated by known methods of rectification. The bottom residue (b g) containing 0.012 g of CoCOAc) + HgO and 0.0001 g of KOAc is mixed for 10 minutes with water at 20 25 C and the mass relationship of the bottom residue: water 1: 2. The mixture is then allowed to settle for 1 hour. The aqueous layer (14 g) contains 0.84 g of acetic acid, 0.01 g of Co (OAc) and 0.000 l of g of CoAc. Accumulated as a result of several

In similar experiments, the aqueous layer (85 g) is subjected to rectification (Tggp, DE-OO S, 103 ° C, reflux number 10-20). 12 g of the cubic residue are obtained, containing 0.06 g of diacetate 0.0006 g of potassium acetate. The isolated catalyst solution is used in the synthesis of MEK according to Example 1, Examples 2-19. The processes are carried out analogously to example 1. The results obtained are given

acetaldehyde to acetic acid, as well as to the formation of telomeric ketones. The restriction of the Co (OAc) concentration range is due to the fact that with an increase in its concentration (higher than the upper limit), the yield of acetic acid increases, which results in a decrease in the MEC yield to the converted acetadehyde. With a concentration of Co (OAc below 1, mol / l, acetaldehyde conversion is significantly reduced.

Carrying out the extraction at the mass ratio of the bottom residue: water 11: 2 does not ensure the complete removal of the catalytic system from the bottom residue, an increase in the mass otnotnie (the bottom residue 1: 3) degrades the process performance.

In comparison with the known method, in the proposed method, the yield of CQ to the refined acetaldehyde increases by 1.3-1.8 times, the productivity (removal of MEC from the unit of reaction volume) of the process increases by 2-3 times, there is a possibility of multiple use of the catalytic system (after its regeneration) without significant changes in process indicators.

five

Claims (1)

45 claims The method of producing methyl ethyl ketone by reacting acetaldehyde with ethylene in the presence of an oxygen-containing gas and a catalyst containing cobalt acetate at a concentration of .1, 4-10-1.010 mol / n, at a temperature of 30 ° C, ethylene pressure of 10-18 ati and total pressure of 20 -22 MPa, characterized in that, in order to increase the yield of the target product on the converted acetaldehyde and increase the productivity of the process, a mixture of cobalt acetate and alkali metal acetate is used as a catalyst, and their molar ratio is 3.6 - 50: 1The process is carried out at an ethylene flow rate of 120-78 rh and an oxygen-containing gas flow rate in terms of oxygen of 4.9-40 hours followed by separation of the target product by distillation and treatment of the bottoms with water at a temperature of 20-25 ° C and a weight ratio of bottoms residue: water of 1: 2-3, followed by concentration of the aqueous solution, which is sent to the system. (regeneration as in example 1} in examples 4 and 6 — a regenerated catalyst (regeneration as in example 1); in example 8, a regenerated catalyst (regeneration is carried out at the mass Relation of the bottom residue: water 1: 3, stirred for 30 minutes at 20 -25 C followed by settling of the mixture for 2 h), in PRETER 9, these E and WAU are served separately, for example II, the sweat catalyst is regenerated (regeneration is carried out by itprt by mass vat residue W = 1.2: 5, mixed 20 minutes at 20-25 ° C, followed by settling the mixture for 3 hours). Editor N. Gunko Compiled by R. Margolnna Tehred M. Khodanych Order 3450/27 Circulation 371. Subscription VNIIPI of the USSR State Committee for inventions and discoveries 113035, Moscow, Zh-35, Raushsk nab., d.A / 5 Production and printing company, Uzhgorod, Projecto st., 4 Proofreader M.Sharoshi