CS209588B1 - The process for obtaining phenylhydrazide hydrochloride from the waste solution after filtration of the phenylhydrazine hydrochloride suspension - Google Patents

The process for obtaining phenylhydrazide hydrochloride from the waste solution after filtration of the phenylhydrazine hydrochloride suspension Download PDF

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CS209588B1
CS209588B1 CS323780A CS323780A CS209588B1 CS 209588 B1 CS209588 B1 CS 209588B1 CS 323780 A CS323780 A CS 323780A CS 323780 A CS323780 A CS 323780A CS 209588 B1 CS209588 B1 CS 209588B1
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phenylhydrazine
hydrochloride
filtration
phenylhydrazine hydrochloride
suspension
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CS323780A
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Czech (cs)
Slovak (sk)
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Robert Poor
Vojtech Holka
Imrich Svitek
Vladimir Kopinic
Stefan Leska
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Robert Poor
Vojtech Holka
Imrich Svitek
Vladimir Kopinic
Stefan Leska
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Priority to CS323780A priority Critical patent/CS209588B1/en
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Abstract

Sposob získania fenylhydrazín hydrochloridu z odpadného roztoku po filtrácii suspenzie fenylhydrazín hydrochloridu vyznačujdci sa tým, že sa do odpadného roztoku získaného po filtrácii suspenzie fenylhydrazín hydrochloridu, nasýteného anorganickými soíami a rozpuštěným fenylhydrazín hydrochloridom, přidá pri teplote 5 až 40 °C za miešania alkalický hydroxid, alebo jeco vodný roztok, pričom sa neutralizuje rozpuštěný fenylhydrazín hydrochlorid až po dosiahnutie pH 6,5 až 7,5 a reakciou vznikajúci fenylhydrazín sa po ochladení na teplotu +5 až +20 °C izoluje z odpadného roztoku filtráciou s výhodou, i premývaním vodou a. áalej sa odyselí kyselinou chlorovodíkovou.A method of obtaining phenylhydrazine hydrochloride from a waste solution after filtration of a suspension of phenylhydrazine hydrochloride, characterized in that an alkali hydroxide or an aqueous solution is added to the waste solution obtained after filtration of a suspension of phenylhydrazine hydrochloride, saturated with inorganic salts and dissolved phenylhydrazine hydrochloride, at a temperature of 5 to 40 °C with stirring, while neutralizing the dissolved phenylhydrazine hydrochloride until a pH of 6.5 to 7.5 is reached, and the phenylhydrazine formed by the reaction is isolated from the waste solution by filtration, preferably also by washing with water, and is further extracted with hydrochloric acid.

Description

(54)(54)

Sposob získania fenylhydrazím hdrochloridu z odpadného roztoku po filtrácii suspenze fenylhydrazín hydrochloriduMethod for obtaining phenylhydrazine hydrochloride from waste solution after filtration of the phenylhydrazine hydrochloride suspension

Sposob získania fenylhydrazín hydrochloridu z odpadného roztoku po filtrácii suspenzie fenylhydrazín hydrochloridu vyznačujdci sa tým, že sa do odpadného roztoku získaného po filtrácii suspenzie fenylhydrazín hydrochloridu, nasýteného anorganickými soíami a rozpuštěným fenylhydrazín hydrochloridom, přidá pri teplote 5 až 40 °C za miešania alkalický hydroxid, alebo jeco vodný roztok, pričom sa neutralizuje rozpuštěný fenylhydrazín hydrochlorid až po dosiahnutie pH 6,5 až 7,5 a reakciou vznikajúci fenylhydrazín sa po ochladení na teplotu +5 až +20 °C izoluje z odpadného roztoku filtráciou s výhodou, i premývaním vodou a. áalej sa odyselí kyselinou chlorovodíkovou.A process for recovering phenylhydrazine hydrochloride from a waste solution after filtration of a phenylhydrazine hydrochloride suspension, characterized in that an alkali hydroxide is added to the waste solution obtained after filtration of the suspension of phenylhydrazine hydrochloride saturated with inorganic salts and dissolved phenylhydrazine hydrochloride at 5 to 40 ° C, or is an aqueous solution, wherein the dissolved phenylhydrazine hydrochloride is neutralized to a pH of 6.5 to 7.5 and the phenylhydrazine formed by reaction is, after cooling to +5 to +20 ° C, isolated from the waste solution by filtration, preferably by washing with water and. It is then de-acidified with hydrochloric acid.

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Vynález sa týká spfisobu získania fenylhydrazín hydrochloridu z odpadného roztoku po filtrécii suspenzie fenylhydrazín hydrochloridu, pričom sa do odpadného roztoku přidá alkalický hydroxid a vykrystalizuje fenylhydrazín, ktorý sa izoluje filtráciou a okyselením kyselinou chlorovodíkovou a prevedie na fenylhydrazín hydrochlorid.The invention relates to a process for obtaining phenylhydrazine hydrochloride from a waste solution after filtration of a suspension of phenylhydrazine hydrochloride, adding alkali hydroxide to the waste solution and crystallizing phenylhydrazine, which is isolated by filtration and acidification with hydrochloric acid and converted to phenylhydrazine hydrochloride.

Fenylhydrazín hydrochlorid sa vyrába hydrolýzou fenylhydrazíndisulfonétu sodného mineiálnou kyselinou. V áalšom technologiekom stupni so po ochladení a nasýtení roztoku z reakčnej zmesi vykrystalizuje fenylhydrazín hydrochlorid, ktorý sa izoluje filtráciou . reakčnej zmesi. Odfiltrovaný krystalický fenylhydrazín sa áalej spracúva na přípravu roznych zlúčenín.Phenylhydrazine hydrochloride is produced by hydrolyzing sodium phenylhydrazine disulfonate with a mineial acid. In a further technology, phenylhydrazine hydrochloride crystallizes from the reaction mixture after cooling and saturating the solution, which is isolated by filtration. of the reaction mixture. The filtered crystalline phenylhydrazine is further processed to prepare various compounds.

Filtrát získaný po izolácii fenylhydrazín hydrochloridu sa podía potřeby riedi vodou a bez dalšej možnosti zúžitkovania odtéká vo formě odpadných vod.The filtrate obtained after isolation of the phenylhydrazine hydrochloride is diluted with water if necessary and, without further utilization, flows as waste water.

Po filtrácii kryátalickej suspenzie fenyhlydrazín hydrochloridu odtéká odpadný filtrát s priemerným obsahom 0,03 až 12 g/1 fenylhydrazín hydrochloridu v závislosti ód sposobu vedenia technologie výroby fenylhydrazín hydrochloridu i v závislosti .od stupňa nasýtenia roztoku suspenzie fenylhydrazín hydrochloridu před jej'filtruciou soíami NaCl, NaHSO^ Na množstvo rozpuštěného fenylhydrazín hydrochloridu vplývai teplota a pH roztoku.After filtration of the crystalline phenyhlydrazine hydrochloride suspension, the waste filtrate with an average content of 0.03 to 12 g / l of phenylhydrazine hydrochloride flows off depending on the method of conducting the phenylhydrazine hydrochloride production process and depending on the degree of saturation of the phenylhydrazine hydrochloride solution before filtration with NaCl. The amount of dissolved phenylhydrazine hydrochloride is affected by the temperature and pH of the solution.

Uvedené nevýhody odstraňuje spSsob získania fenylhydrazín hydrochloridu z odpadného roztoku po filtrácii jeho suspenzie podía vynálezu, ktorého podstatou je, že sa do odptdného roztoku, získaného po filtrécii suspenzie fenylhydrazín hydrochloridu nasýteného anorganickými soíami a fenylhydrazín hydrochloridom přidá za mieaania alkalický hydroxid, alebo jeho vodný roztok, pričom sa neutralizuje rozpuštěný fenylhydrazín hydrochlorid až po dosiahnutie pH 6,5 až 7,5»These disadvantages are overcome by the method of recovering phenylhydrazine hydrochloride from the waste solution after filtration of the suspension thereof according to the invention, which comprises adding alkaline hydroxide or an aqueous solution thereof to the waste solution obtained after filtration of the suspension of phenylhydrazine hydrochloride saturated with inorganic salts and phenylhydrazine hydrochloride. neutralizing dissolved phenylhydrazine hydrochloride to pH 6.5 to 7.5 »

Pridévanie alkalického hydroxidu sa uskutočňuje při teplete +5 až +40 °C za miešania.The addition of the alkali hydroxide is carried out at a temperature of +5 to +40 ° C with stirring.

Z alkalických hydroxidov sa dá použit hydroxid sodný, draselný, ale i hydroxid amonný.. S výhodou ea použije hydroxid sodný vo formě vodného roztoku.Of the alkali hydroxides, sodium, potassium, but also ammonium hydroxide can be used. Preferably ea is used in the form of an aqueous solution.

Rozpuštěný fenylhydrazín hydrochlorid sa alkalickým hydroxidem neutralizuje a prechádza na fenylhydrazín, ktorý je vo vodnom roztoku nerozpustný a kryštalizuje.The dissolved phenylhydrazine hydrochloride is neutralized with alkaline hydroxide and converted to phenylhydrazine, which is insoluble in aqueous solution and crystallizes.

Vy.kryštalizovaný fenylhydrazín sa odliltrujé, pričom sa získá fenylhydrazín a odpadný filtrát. Pretože pri filtrácii fenylhydrazín hydrochloridu sa získává filtrát obsahujúci okrem rozpuštěného fenyhlyďřazínu i anorganické soli, ako napr. Naď, NBgHSO^, NagSO-j, NaHSOp připadne i voínú HC1, je výhodné po neutralizécii rozpuštěného fenylhydrazín hydrochloridu alkalickým hydroxidom vzniknutý a odfiltrovaný fenylhydrazín v kryštalickej formě premývat vodou s cieíom odstránií uvedené soli z fenylhydrazínu. Uvedeným postupom sa získá fenylhydrazín, zbavený od anorganických solí, ktorý sa v áalšom stupni rozpúšta v kyselině chlorovodíkovéj za vzniku roztoku fenylhydrazín hydrochloridu. Filtrát získaný po filtrovaní fenylhydrazínu sa áalej nespracúva.The crystallized phenylhydrazine is filtered off to give phenylhydrazine and waste filtrate. Because filtration of phenylhydrazine hydrochloride yields a filtrate containing in addition to the dissolved phenylacrylate also inorganic salts such as e.g. For example, NBlHSO4, NagSO4, NaHSO3, optionally free HCl, it is preferable to wash and filter the phenylhydrazine in crystalline form after neutralization of the dissolved phenylhydrazine hydrochloride with an alkaline hydroxide to remove said salt from the phenylhydrazine. This procedure gives phenylhydrazine, free from inorganic salts, which is dissolved in hydrochloric acid in the next step to form a solution of phenylhydrazine hydrochloride. The filtrate obtained after filtering the phenylhydrazine is not further processed.

Příklad 1Example 1

V 2-litrovej kádinke sa 1000 ml matečného roztoku.po filtrácii suspenzie fenylhydrazín hydrochloridu pomaly za miešania neutralizuje 43 % hmot roztokom NaOH tak, aby teplota reakčnej zmesi nepřekročila 30 °C. Celkove sa přidá 150 aš 160 ml 43 % hmit. NaOH, kým sa nedošiahne pH 7,5· Po dosiahnutí neutrálnej reakcie sa z reakčnej zmesi vylučujú kryštálky fenylhydrazínu, pričom-sa. nápadné změní zafarbenie roztoku /narůžovělé farba prechádza v hnědozelené sfarbenie/. Po cca 10 minutách kryštalizácie kryštály fenylhydrazínu rýqhle sedimentu jú. Získaný podiel kryátalickej suspenzie sa odfiltruje cez odsévtečku, premyje 100 ml destilovanej vody a získaný koláč fenylhydrazínu saprevedie na vodný roztok fenylhydrazín hydroehlqridu tak, že do 500 ml kádinky sá předloží 190 ml vody a 10 ml 32 % HC1. Předloha sa predohreje na 40 °C a potom sa za miešania rozpustí fehylhycirazín na vodný roztok fepylhydrazín hydrochloridu.In a 2 L beaker, 1000 mL of the mother liquor was slowly neutralized with 43% w / w NaOH solution with stirring until the temperature of the reaction mixture did not exceed 30 ° C after filtration of the phenylhydrazine hydrochloride suspension. A total of 150 to 160 ml of 43% hmit is added. NaOH until pH 7.5 is reached. After neutral reaction, phenylhydrazine crystals are precipitated from the reaction mixture while being stirred. it noticeably changes the color of the solution (pinkish color becomes brownish green). After about 10 minutes of crystallization, the phenylhydrazine crystals of the reddish sediment are yellow. The obtained crystalline suspension is filtered through a sieve, washed with 100 ml of distilled water and the obtained phenylhydrazine cake is transferred to an aqueous phenylhydrazine hydrochloride solution by adding 190 ml of water and 10 ml of 32% HCl to a 500 ml beaker. The flask was preheated to 40 ° C and then the phthylhycirazine was dissolved with stirring to an aqueous solution of fepylhydrazine hydrochloride.

200 ml yodný roztoko hustotě 1,020 kg/nP mé obsah 0,035 % hmot. fenylhydrazín hydrochloridu, čo zodpovedá koncentrácii 7 g/1.200 ml of an iodine solution having a density of 1.020 kg / nP and a content of 0.035% by weight. phenylhydrazine hydrochloride, corresponding to a concentration of 7 g / l.

Claims (1)

PREDMET VYNÁLEZUOBJECT OF THE INVENTION Spósob získania fenylhydrazín hydrochloridu z odpadného roztoku po filtrácii sespenzie henylhydrazín hydrochloridu vyznačujúci sa tým, že sa do odpadného roztoku získaného po filtrácii suspenzie fenylhydrazín hydrochloridu., nasýteného anorganickými sóíami a rozpuštěným fenylhydrazín hydrochlori dom, přidá pri teplote 5 až 40 °G za' miešania alkalický hydroxid, ale-o jeho .vodný roztok, pričom sa neutralizuje rozpuštěný fenylhydrazín hydrochlořid až po dosiahnutie pH 6,5 až 7,5 a reakciou vznikajúci fenylhydrazín sa po ochladení na teplotu +5 až +20 °C'izoluje z odpadného roztoku filtréciou s výhodou, i premývaním vodou a áalej sa okyselí kyselinou chlorovodíkovou.A process for recovering phenylhydrazine hydrochloride from a waste solution after filtration of a henylhydrazine hydrochloride suspension by adding to the waste solution obtained after filtration of a suspension of phenylhydrazine hydrochloride saturated with inorganic salts and dissolved phenylhydrazine hydrochloride at 5 to 40 ° C with stirring. hydroxide, or an aqueous solution thereof, neutralizing the dissolved phenylhydrazine hydrochloride until a pH of 6.5 to 7.5 is achieved and, after cooling to +5 to +20 ° C, the phenylhydrazine formed is isolated from the waste solution by filtration with preferably by washing with water and further acidifying with hydrochloric acid.
CS323780A 1980-05-08 1980-05-08 The process for obtaining phenylhydrazide hydrochloride from the waste solution after filtration of the phenylhydrazine hydrochloride suspension CS209588B1 (en)

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