CS201299B1 - Method of regenerating oetone and dl-methylformamide and apparatus for carrying it out - Google Patents

Abstract

The invention provides a method for the regeneration of acetone and dimethylformamide from dimethylformamide used in the production of gases from high-temperature pyrolysis of gasoline, commonly referred to as the HTP process, and also a device for its implementation. The regeneration takes place in such a way that the lower-value substances enriched in dimethylformamide are first separated by continuous rectification at a vapor temperature before condensation in the range of 100 to 135 °C, and from the condensate thus obtained, a acetone fraction with a maximum water content of 2 wt. and residual dimethylformamide with a maximum water content of 1 wt. are returned* to the continuous rectification, dimethylformamide from the continuous rectification, containing caustic components, and next to it back to the absorption-desorption circuit, with 15 to 40 $ wt. of it will be subjected to continuous before being introduced into this circuit! to the distillate.

Description

1 au

Vynlloau is produced by the separation of olefins and palotylfumane used in the separation of gases of the oxotepolar pyrroleine, either as an HTP prooaa. In the production of aootyll and otylan with a high temperature pyrolyte, the alumina and aylalcohol and the high biodiesel blend have a propellant of pyrolysis gas with water, such as aythic and Ihkin banalaon. The main aloikaui of the pyrolyzed gas of this type and the usual oethylin, otylin, kyallBnlk uhllBlack, kyallBnlkHalk, Betl and Hydrogen · Potterifiers, mainly oatylin and ethylin, aa alacava in alollton abaorpBno-desorpBnon ayatlnaa alakotepel koudanalol and rectlcliol as aelective abeorpBhl Blnldll pouilvajd oetlna dluhetyllormtald · In aet & ne and firstly abeorbujd oetylln a kyelBnlkhlllk, Yellow, aaoddolla from ootat aloorpoil in a pyrolytic gas ·

Okran aeetylian and kyallBnlka uhliBltiho proohldaajú to tav · dlaotylf oraanldovihopraala also SalBlo substances such aootln, water Anaa uhPovodlkov poured anaiatvl kyollBnlkovduolka and olónyoh aldBonla, Unoh and týohto lltok AA pyrolýaaon gas aaohldaajd lfeavo veltal nalýoh anoiotvloh ala inappropriately aplaofea repanorloie dlaotylforuauldu aaakuuulujd in pouiíváaou dinotylfomnaldo, and after Laton relatively short Bsa AI, aajdnepriaaaivý effect aa prleboh dlaotylf omnuldovlho praala · VB effect aallho oboahu apo-aouutýeh lltok in dluatylfomaulda aa ahoriuja dBlaaostf abaorpola, aparatdra rýohlo coronal recentrifuged and engaged akunulovaal aloBky alúBealn Olry pradatavujd Vlin aebaqpeBeaetvb havárieprevddafcy v ddoledka of the production of the fire-proofing agent · From the following sources 1 and dBu dolahuu-press autlndlaej production efficiency is ddleiiti to proceed so that and to avoid the accusation-oll nailaddoioh lltok, ala prl aajni consumption of absorptionBialdlel and energy ·

Doteraa pouilvaný apdaob reeenerdole rektlflklolou Basta dlnetylfomaaldu by continuous on odoberanlho and abaorpBnlho circuit neeplna laid poiladavky and naprlefc pouiitlu vyao-koúBlunej rektiflkaBnej Kölln · Distillate odohádaajdol head and knees endowed rektiflkaBnej-oestrus okran beaoenaej water and veltal oooný aootln and dlaetylfomauold, Bia oa eltaShe avylu- They need nonqr to do this, but also in Bletenl, the defect of vanadium anobllucyl.

Shortcomings dotorajiloho opBoobu rogonerdolo aoetluu and dluotylforaauldu pouiitlhopri vyplaranl gases and vyaokotepelnej pyrolýay bonalau in aboorpBnou-daoorpBnou circuit jdooho hire a content aooiln, Science, as well salile naiiototy removes spBaob rogonoriolopodl'a this vyndloau, PRL by OA nliMlevrúoo substances obohateai dlmotylfomaaldoa, oddePujd firstly with a continuous steam at a temperature pair prior to the condonalol at 100 ° C and 135 ° C, preferably at 104 and 116 ° 0, after the water and at a temperature of about 8% by weight, preferably at 1% by weight of water. the abundance of the residual glycolphthalate of water and the volume of water 1 ton of aralaric acid into a contiguous rectifluoride. %, and preferably 20 to 30% by weight, and then, prior to introduction into the circuit, performs a cont flax &

The spdaob regenerate, the acetone and the dimethylformamide of dimethylformamide dimethylformamide and convert to the rectifying and deacidifying apparatus and auxiliary tuning, where the output of the dimethylformamide from the absorption-desorption circuit is connected to a continuous rectification column which is coupled to the diaphragm rectifier. The reaction medium consisting of the rectification column and the cooker, which is connected by a pipeline and a coating of dimethylformamide, in which case the continuous rectification column is both a pipeline directly and a technological branch formed by a pipeline, a continuous deactivating apparatus comprising a single-stage distillation apparatus, a pipe and a condenser coupled to absorption-deactivation circuit ·

Surprisingly, the effect of aa reached the rectal with the alkali at the indicated vapor temperatures before condensation, whereby the lower components degrade completely quantitatively, e.g., to reduce the acetone in dimethylformamide to a value of less than 0.05% by weight. A further surprising effect and has reached the equilibrium of traffic. They behave and these ayatems are not ambiguous, because the properties of the multi-constituent compound in the range of the small-scale extremities are neither theoretical nor empirical.

Surprisingly, the high purity of the dimethylformamide in the absorption-deactivation circuit is achieved and shown in the figure.

The dimethylformamide destined for regeneration is fed from the absorption-desorption circuit 17a via line J through a continuous rectification column 2a and next to the continuous recycle together with dimethylformamide, generally supplied continuously from the cooking column 2 via line 15 via a continuous rectification column. 2, usually by pipe 1. The condensate is removed from the continuous rectification column 2 and the conduit 2, and the condensate is discharged as a poor flow through the conduit and the conduit 6, and the condensate is discharged and converted into a continuous rectification tunnel. comprising a brewing unit 2 of a rectification column 8, a duct for a phase memory 6, a condenser 10 of a conduit 11, and a conduit 12, 13, 14 for individual distilled components or deatillation sections. The number of pipes aa determines the advantage of separating the acetone, the intermediate and the water according to the technological intent. Thus, and obtains a low content of water and dimethylformamide.

The continuous rectification column 2 is connected via line 16 and to the absorption-deactivation circuit 17. The dimethylformamide is completely dispensed with the line 16a and returned to the absorption-desorption circuit 17. Thus, the removal of the hardening agent results in a portion of the dimethylformamide removed from the continuous rectification column 2 via a pipe 18 " connected to the pipe 16 and a single-stage distillation apparatus 19, whereby the de-vaporized solids are discharged via line 23 to the liquid and the dimethylformamide vapors are continuously discharged via line 20 to condenser 21a and the condensed pure dimethylformamide is returned via line 22 either directly or through line 16 to the absorption-desorption circuit 17.

The technological scheme in the figure includes commonly used apparatuses such as cartridges, copperisers, meraoie and indicating devices, as well as fittings such as valves.

The proposed process and apparatus, by a simple, simple solution, allows the recovery of contaminated selective solvents of the desired high degree of purity, while at the same time reducing the risk of an accident caused by corrosion and by increasing the concentration of substances that may be pyrophoric. At the same time, the proposed procedure is economically unpretentious and energy demands are not high.

The following examples illustrate, but do not limit, the mode of use. Example 1

Dimethylformamide withdrawn from dimethylformamide washing, containing 0.9% by weight of aetone, 0.2% by weight. water, dissolved ethylene and other substances are continuously rectified at a vapor temperature before condensing 114 ° C at normal pressure. In this way, a distillate containing 80 mol% is obtained. dimethylformamide, 5 mol%; water and 15 # mol. By discontinuous rectification in the temperature range of 55 to 157 ° C, an aethone of 0.9 wt. % water and dimethylformamide containing 1 wt. water. The efficiency of removal of undesirable substances in the acetone and dimethylformamide circuit is high, so that even in long-term operation, the required maximum water content in dimethylformamide and acetone are not exceeded. The content of pyrophoric substances is not increased, or completely negligible, if about 15% of dimethylformamide is made from continuous rectification in a single-stage continuous distillation. Example 2

Dimethylformamide from dimethylformamide washing initially had 0.9% w / w acetone and 0.15% w / w. water, dissolved ethylene, and other substances are first continuously rectified at a vapor temperature of 90 ° C at normal pressure prior to condensation. Rectification is irregular, the amount of water and aetone in the circuit gradually rises to an inadmissible value. In this way, the initial parameters are achieved by discontinuous rectification of the entire amount of dimethylformamide at a particular level.

Claims (2)

OBJECT OF THE INVENTION 1. A process for the recovery of azetone and dimethylformamide by rectifying the dimethylformamide used in scrubbing gases from high-temperature pyrolysis gasoline in the absorption-deaorption circuit containing at least acetone, water and, more importantly, it is difficult to separate the materials by making the amides more difficult. and at first a continuous rectification at a temperature in front of the condenser in the range of 100-135 ° C, preferably 104-116 ° C, after the condensed condensate and discontinuous rectification of the fraction of acetone and a maximum water content of 2% by weight, preferably $ 1 and residual dimethylformamide having a maximum water content of $ 1 wt. In addition to the continuous rectification, dimethylformamide from the continuous rectification comprises the fining components in addition to the epoxy-desorption circuit, with an addition of 15 to 40% by weight. therefrom, and preferably 20 to 30% by weight ·, and prior to introduction into this circuit subjected to continuous de-cold diethyl · 2. Apparatus according to claim 1 operating from rectified and de-ethylene apparatuses and auxiliary apparatus, and facilitating the output of the dimethylformamide (1) from the absorption-desorption circuit (17) as a spray to the continuous rhombus (1). 2), its upper data being connected via a duct (6) to a continuous rectification device, starting from a rectification column (8) and a boil (7), the bottom of which is connected via a duct (15) and sprayed with dimethylformamide (1); the rectification of each column (2) is on the one hand a pipe (10), and on the other hand a thyologologic branch consisting of a pipe (18,22), a continuous distillation apparatus consisting of a one-stage distillation apparatus (19), a pipe (20) and a condenser (21). connected to absorption-de-absorption circuit (17) ·