CS255372B1 - The method of detoxifying waste water after arylation by diazonium salts - Google Patents

The method of detoxifying waste water after arylation by diazonium salts Download PDF

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CS255372B1
CS255372B1 CS855394A CS539485A CS255372B1 CS 255372 B1 CS255372 B1 CS 255372B1 CS 855394 A CS855394 A CS 855394A CS 539485 A CS539485 A CS 539485A CS 255372 B1 CS255372 B1 CS 255372B1
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Czechoslovakia
Prior art keywords
arylation
waste water
rectification
solvent
diazonium salts
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CS855394A
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Czech (cs)
Slovak (sk)
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CS539485A1 (en
Inventor
Ladislav Szoecs
Marian Zajac
Mikulas Buday
Pavol Dano
Jan Uhlar
Eva Kohutova
Walter Waradzin
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Ladislav Szoecs
Marian Zajac
Mikulas Buday
Pavol Dano
Jan Uhlar
Eva Kohutova
Walter Waradzin
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Application filed by Ladislav Szoecs, Marian Zajac, Mikulas Buday, Pavol Dano, Jan Uhlar, Eva Kohutova, Walter Waradzin filed Critical Ladislav Szoecs
Priority to CS855394A priority Critical patent/CS255372B1/en
Publication of CS539485A1 publication Critical patent/CS539485A1/en
Publication of CS255372B1 publication Critical patent/CS255372B1/en

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  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

Riešenie sa zaoberá detoxikáciou odpadových vůd po arylácii diazoinovými solami. Po rozdělení reakčnej zmesi sedimentáciou, vodná vrstva obsahujúca menšie množstvá rozpúšťadla a východzej suroviny, sa podrobí defirenciálnej rektifikácii s premenlivým refluxným pomerom. Získaný destilát pozostáva z rozpúšťadla a východzej arylovej látky a za malého množstva vody. Zvyšok po rektifikácii neobsahuje toxické látky v koncentráciach závadných pri biologickom čistění odpadových vod aktivovaným kalom.The solution deals with the detoxification of wastewater after arylation with diazoin salts. After separation of the reaction mixture by sedimentation, the aqueous layer containing smaller amounts of solvent and starting material is subjected to differential rectification with a variable reflux ratio. The obtained distillate consists of solvent and starting aryl substance and a small amount of water. The residue after rectification does not contain toxic substances in concentrations harmful to biological wastewater treatment with activated sludge.

Description

(54) Sposob detoxikácie odpadových vQd po arylácii diazoniovýmí solami(54) Method of detoxifying wastewater after arylation with diazonium salts

Riešenie sa zaoberá detoxikáciou odpadových vůd po arylácii diazoinovými solami. Po rozdělení reakčnej zmesi sedimentáciou, vodná vrstva obsahujúca menšie množstvá rozpúšťadla a východzej suroviny, sa podrobí defirenciálnej rektifikácii s premenlivým refluxným pomerom. Získaný destilát pozostáva z rozpúšťadla a východzej arylovej látky a za malého množstva vody. Zvyšok po rektifikácii neobsahuje toxické látky v koncentráciach závadných pri biologickom čistění odpadových vod aktivovaným kalom.The solution deals with the detoxification of waste leads after arylation with diazoin salts. After partitioning of the reaction mixture by sedimentation, the aqueous layer containing minor amounts of solvent and feedstock is subjected to a liquid rectification with varying reflux ratio. The distillate obtained consists of a solvent and a starting aryl material and a small amount of water. The residue after rectification does not contain toxic substances in concentrations that are harmful in biological treatment of waste water by activated sludge.

Vynález sa zaoberá detoxikáciou odpadových vod po arylácii diazoniovými sol'ami.The invention is concerned with the detoxification of waste water after arylation with diazonium salts.

Po arylácii diazoniovými solami vzniknutá reakčná zmes sa rozdělí na vodnú a organická vrstvu. V závislosti od koncentrácie zložiek a hodnot rozdělovačích koeficientov vo vodnej vrstvě sa nachádza zmes rozpúšťadla a nezreagovaných zbytkov vstupnej suroviny. S ciel'om spatného získavania rozpúšťadla tento vodný roztok sa v ďalšom spracováva v dvoch stupňoch. V prvom vodná vrstva po arylácii sa podrobí diferenciálnej destilácii. Z destilátu diferenciálnou rektilikáciou sa oddělí zmes rozpúšfadla a východzej suroviny od vody. Zvyšok po destilácii a rektifikácii je voda znečistěná organickými látkami, takže je potřebné jej čistenie. Tento sposob detoxikácie má niekolko nevýhod. Viacnásobným tepelným namáháním dochádza k reakciám vedúcim k tvorbě biologicky pomaly rozložitelných toxických látok. Nedostatečné vydestilovanie zložiek pri diferenciálnej destilácii a diskontinuálnej rektifikácii s konštantným refluxným pomerom vedie k dalším stratám suroviny a znečisteniu odpadových vod.After arylation with diazonium salts, the resulting reaction mixture was separated into an aqueous and an organic layer. Depending on the concentration of the components and the partition coefficient values in the aqueous layer, there is a mixture of solvent and unreacted feedstock residues. In order to recover the solvent poorly, this aqueous solution is further processed in two stages. In the first aqueous layer after the arylation, it is subjected to differential distillation. The mixture of solvent and starting material is separated from water from the distillate by differential rectification. The residue after distillation and rectification is water contaminated with organic substances, so it is necessary to purify it. This method of detoxification has several drawbacks. Multiple thermal stresses lead to reactions leading to the formation of biodegradable toxic substances. Insufficient distillation of the components by differential distillation and discontinuous rectification with a constant reflux ratio leads to further raw material losses and waste water pollution.

Uvedené nedostatky odstraňuje námi předložený vynález. Sposob detoxikácie odpadových vod po arylácii diazonovými sofami podlá uvedeného vynálezu je založený na principe diferenciálnej rektifikácie vodnej fázy s premenlivým refluxným pomerom v rozmedzí 0,5 do 10.These disadvantages are overcome by the present invention. The method for detoxifying waste water after arylation with diazone salts according to the present invention is based on the principle of differential rectification of the aqueous phase with a variable reflux ratio in the range of 0.5 to 10.

Odpadová voda po diferenciálnej rektifikácii vykazuje nízké znečistenie a nevyskytuji! sa problémy pri jej biologlckom čistění. Neobsahuje toxicky ťažko rozložitelné látky. Výhodami sposobu podfa předloženého vynálezu sú zmenšenie strát suroviny a rozpúšťadla, zmenšenie energetickej náročnosti procesu a zmenšenie ekologickej závadnosti produkované] odpadovej vody.Waste water after differential rectification shows low contamination and does not occur! problems with its biological purification. It does not contain toxic substances that are difficult to decompose. Advantages of the process of the present invention are the reduction of raw material and solvent losses, the reduction of the energy consumption of the process, and the reduction of the environmental harmfulness of the waste water produced.

Příklad 1Example 1

Aryláciou akrylonitrilu s 4-chlórfenyldiazoniumchloridom za katalýzy chloridom meďnatým a acetónom vzniká 3-(4-chlórfenyl)-2-chlórpropionitril. Reakčná zmes sa dělí na vodnú a organická vrstvu. Voda obsahovala aceton a akrylonitril v množstve 15 %. Aceton a akrylonitril od vody sa oddělí v dvoch etapách. Najprv diferenciálnou destiláciou sa získala zmes s obsahom vody 38 %, pričom destilačný zvyšok ako odpadová voda, aceton a akrylonitril v množstve 2 % hmotnostných. Destilát bol podrobený diferenciálnej rektifikácii s konštantným refluxným pomerom R = 4. Vzniknutá odpadová voda obsahovala 0,9 % acetonu a akrylonitrilu.Arylation of acrylonitrile with 4-chlorophenyldiazonium chloride under catalysis with cuprous chloride and acetone affords 3- (4-chlorophenyl) -2-chloropropionitrile. The reaction mixture is separated into aqueous and organic layers. The water contained acetone and acrylonitrile in an amount of 15%. Acetone and acrylonitrile are separated from the water in two stages. First, by differential distillation, a mixture with a water content of 38% was obtained, with a distillation residue such as waste water, acetone and acrylonitrile in an amount of 2% by weight. The distillate was subjected to differential rectification with a constant reflux ratio R = 4. The resulting waste water contained 0.9% acetone and acrylonitrile.

Delením zmesi podfa předmětného vynálezu s refluxným pomerom 0,5 až 10 sa získal destilát o zložení 20 % akrylonitrilu a 80 % acetonu. Vodu obsahovala v stopových množstvách. Přítomnost acetonu a akrylonitrilu vo zvyšku nebola dokázaná běžnými analytickými postupmi.Separation of the mixture of the present invention with a reflux ratio of 0.5 to 10 gave a distillate of 20% acrylonitrile and 80% acetone. The water contained in trace amounts. The presence of acetone and acrylonitrile in the residue was not detected by conventional analytical procedures.

Příklad 2Example 2

Arylácia ako v příklade 1. Obsah acetonu a akrylonitrilu bol 13,5 %. Destilát diferenciálnou destiláciou obsahoval aceton a akrylonitril v množstve 32,1 % a destilačný zvyšok 2,2 %. Po diferenciálnej rektifikácii s refluxným pomerom 4 v odpadovej vodě bol dokázaný aceton a akrylonitril v množstve 0,8 %. Podfa předmětného vynálezu destilát obsahoval vodu v množstve 0,3 %. V odpadovej vodě aceton a akrylonitril nebol dokázaný běžnými analytickými postupmi.Arylation as in Example 1. The acetone and acrylonitrile content was 13.5%. The distillate by differential distillation contained acetone and acrylonitrile in an amount of 32.1% and a distillation residue of 2.2%. After differential rectification with a reflux ratio of 4 in the waste water, acetone and acrylonitrile were detected in an amount of 0.8%. According to the present invention, the distillate contained 0.3% water. In wastewater, acetone and acrylonitrile were not detected by conventional analytical procedures.

Claims (1)

PREDMETSUBJECT Sposob detoxikácie odpadových vod po arylácii diazoniovými solami vyznačujúci sa tým, že rozpúšťadlo a nezreagovaná zlúčenina sa oddělí diferenciálnou rektifikáciou s premenlivým refluxným pomerom v rozmedzí 0,5 do 10.A process for detoxifying waste water after arylation with diazonium salts, characterized in that the solvent and the unreacted compound are separated by differential rectification with a variable reflux ratio in the range of 0.5 to 10.
CS855394A 1985-07-22 1985-07-22 The method of detoxifying waste water after arylation by diazonium salts CS255372B1 (en)

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CS255372B1 true CS255372B1 (en) 1988-03-15

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