CS209588B1 - Method of gaining the hydrochloride phenylhydrazine from the refuse solution after filtration of the hydrochloride phenylhydrazine suspension - Google Patents
Method of gaining the hydrochloride phenylhydrazine from the refuse solution after filtration of the hydrochloride phenylhydrazine suspension Download PDFInfo
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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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- Czechoslovakia
- Prior art keywords
- phenylhydrazine
- hydrochloride
- filtration
- suspension
- phenylhydrazine hydrochloride
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- JOVOSQBPPZZESK-UHFFFAOYSA-N phenylhydrazine hydrochloride Chemical compound Cl.NNC1=CC=CC=C1 JOVOSQBPPZZESK-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 238000001914 filtration Methods 0.000 title claims abstract description 21
- 239000000725 suspension Substances 0.000 title claims abstract description 14
- 238000000034 method Methods 0.000 title claims abstract description 9
- 229940038531 phenylhydrazine hydrochloride Drugs 0.000 claims abstract description 37
- 239000000243 solution Substances 0.000 claims abstract description 22
- 239000002699 waste material Substances 0.000 claims abstract description 16
- HKOOXMFOFWEVGF-UHFFFAOYSA-N phenylhydrazine Chemical compound NNC1=CC=CC=C1 HKOOXMFOFWEVGF-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229940067157 phenylhydrazine Drugs 0.000 claims abstract description 15
- 239000007864 aqueous solution Substances 0.000 claims abstract description 7
- 150000003839 salts Chemical class 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 5
- 238000001816 cooling Methods 0.000 claims abstract description 4
- 229920006395 saturated elastomer Polymers 0.000 claims abstract description 4
- 238000005406 washing Methods 0.000 claims abstract description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims description 4
- 230000003472 neutralizing effect Effects 0.000 claims description 2
- 229910001854 alkali hydroxide Inorganic materials 0.000 abstract description 5
- 150000008044 alkali metal hydroxides Chemical class 0.000 abstract description 5
- 239000002253 acid Substances 0.000 abstract description 3
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 239000000706 filtrate Substances 0.000 description 5
- 239000011541 reaction mixture Substances 0.000 description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 102100030624 Proton myo-inositol cotransporter Human genes 0.000 description 1
- 101710095091 Proton myo-inositol cotransporter Proteins 0.000 description 1
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 description 1
- 239000000908 ammonium hydroxide Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- ZJSZOKWFNBLCFL-UHFFFAOYSA-L disodium;n-phenyl-n-(sulfonatoamino)sulfamate Chemical compound [Na+].[Na+].[O-]S(=O)(=O)NN(S([O-])(=O)=O)C1=CC=CC=C1 ZJSZOKWFNBLCFL-UHFFFAOYSA-L 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- -1 e.g. For example Chemical class 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 230000020477 pH reduction Effects 0.000 description 1
- WRAQQYDMVSCOTE-UHFFFAOYSA-N phenyl prop-2-enoate Chemical compound C=CC(=O)OC1=CC=CC=C1 WRAQQYDMVSCOTE-UHFFFAOYSA-N 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 238000009738 saturating Methods 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
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.Process for obtaining phenylhydrazine hydrochloride from the waste solution after filtration a suspension of phenylhydrazine hydrochloride characterized by being in a waste solution obtained by filtration of the suspension with phenylhydrazine hydrochloride saturated with inorganic with salts and dissolved phenylhydrazine hydrochloride is added at 5 to 40 ° C with stirring alkali hydroxide, or The aqueous solution is neutralized dissolved phenylhydrazine hydrochloride to to a pH of 6.5 to 7.5 and by reaction the resulting phenylhydrazine is upon cooling to a temperature of +5 to +20 ° C isolates from the waste solution by filtration, preferably washing water and. with acid 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.
209 588209 588
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.
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Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS323780A CS209588B1 (en) | 1980-05-08 | 1980-05-08 | Method of gaining the hydrochloride phenylhydrazine from the refuse solution after filtration of the hydrochloride phenylhydrazine suspension |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS323780A CS209588B1 (en) | 1980-05-08 | 1980-05-08 | Method of gaining the hydrochloride phenylhydrazine from the refuse solution after filtration of the hydrochloride phenylhydrazine suspension |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CS209588B1 true CS209588B1 (en) | 1981-12-31 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CS323780A CS209588B1 (en) | 1980-05-08 | 1980-05-08 | Method of gaining the hydrochloride phenylhydrazine from the refuse solution after filtration of the hydrochloride phenylhydrazine suspension |
Country Status (1)
| Country | Link |
|---|---|
| CS (1) | CS209588B1 (en) |
-
1980
- 1980-05-08 CS CS323780A patent/CS209588B1/en unknown
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