CS249484B1 - A method for obtaining 3-methyl-4-nitrophenol sodium from the waste solution - Google Patents
A method for obtaining 3-methyl-4-nitrophenol sodium from the waste solution Download PDFInfo
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- CS249484B1 CS249484B1 CS620185A CS620185A CS249484B1 CS 249484 B1 CS249484 B1 CS 249484B1 CS 620185 A CS620185 A CS 620185A CS 620185 A CS620185 A CS 620185A CS 249484 B1 CS249484 B1 CS 249484B1
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Abstract
Spósob ziskavania 3-metyl-4-nitrofenolátu sodného z odpadného roztoku po filtrá- cii jeho suspenzie, pri ktorom sa filtrát přečerpává cez hydrocyklon pri teplote 25°C a pH 6,5 až 8, v ktotom sa odlučujú jemné čiastočky 3-metyi-4-nitrofenolátu sodného a ktoré vo formě zahuštěného roztoku sa vracajú spať do procesu kryštalizácie.A method of obtaining sodium 3-methyl-4-nitrophenolate from a waste solution after filtration of its suspension, in which the filtrate is pumped through a hydrocyclone at a temperature of 25°C and pH 6.5 to 8, in which fine particles of sodium 3-methyl-4-nitrophenolate are separated and which, in the form of a concentrated solution, are returned to the crystallization process.
Description
Vynález sa týká spósobu získavania 3-metyl-4-nitrofenolátu sodného z odpadného filtrátu po izolácii suspenzie 3-mety1-4-nitrofenolátu sodného. Odpadný filtrát získaný po izolácii suspenzie 3-metyl-4-nitrofenolátu sodného sa přečerpává cez hydrocyklon, kde sa odlučovacou schopnosfou zachytává 3-metyl-4-nitrofenolát sodný.The present invention relates to a process for recovering sodium 3-methyl-4-nitrophenolate from a waste filtrate after isolation of a sodium 3-methyl-4-nitrophenolate suspension. The waste filtrate obtained after isolation of the sodium 3-methyl-4-nitrophenolate suspension is pumped through the hydrocyclone, where sodium 3-methyl-4-nitrophenolate is collected by separating capability.
3-mety1-4-nitrofenolát sodný je významným medziproduktom pri róznych organických syntézách napr. pri výrobě insekticídneho přípravku 0,0-dimetyl-0-3-metyi-4-nítro-fenyl-tiofosfát.Sodium 3-methyl-4-nitrophenolate is an important intermediate in various organic syntheses, e.g. in the preparation of the insecticidal preparation O, O-dimethyl-0-3-methyl-4-nitro-phenyl-thiophosphate.
3-metyl-4-nitrofenolát sodný sa móže vyrábať například nitrozáciou m-krezolu dusitanom sodným v prostředí kyseliny sírovej pri znížených teplotách, přitom sa získá 3-metylnítrozofenol, ktorý sa v ďalšom technologickom stupni oxiduje kyselinou dusičnou pri teplotách 40 až 45 °C.Sodium 3-methyl-4-nitrophenolate can be produced, for example, by nitrosation of m-cresol with sodium nitrite in sulfuric acid at reduced temperatures, thereby obtaining 3-methylnitrosophenol which is oxidized in a further process with nitric acid at temperatures of 40-45 ° C.
3-metyl~4-nitrofenol sa získá izoláciou z reakčnej zmesi. Dalej sa 3-metyl-4-nitrofenol neutralizuje roztokom hydroxidu sodného pri teplotách 60 až 90 °c, krystalizuje ochladením a vytěsňuje z roztoku chloridom sodným alebo uhličitanom sodným. Ďalej sa 3-mety1-4-nitrofenolát sodný izoluje z vodnej suspenzie.3-Methyl-4-nitrophenol is obtained by isolation from the reaction mixture. Next, the 3-methyl-4-nitrophenol is neutralized with sodium hydroxide solution at temperatures of 60-90 ° C, crystallized by cooling and displaced from the solution by sodium chloride or sodium carbonate. Furthermore, sodium 3-methyl-4-nitrophenolate is isolated from the aqueous suspension.
Takto získaný 3-metyl-4-nitrofenolát sodný sa upotrebuje v ďalších technologických stupňoch. Filtrát sa zhromažďuje v sedimentačnom zásobníku a po vysedimentovaní sa spodná vrstva odpúšta do chemickej kanalizácie, čo je nevýhodou, pretože obsahuje 0,5 až 15 g/1 jemne rozptýleného tuhého i z Časti rozpustného 3-metyl-4-nitrofenolu v odpadnom filtráte, ktorý sa získá spósobom popísaným v predchádzajúcej časti.The sodium 3-methyl-4-nitrophenolate thus obtained is used in further technological steps. The filtrate is collected in a sedimentation tank and after sedimentation, the bottom layer is drained into a chemical sewer, which is a disadvantage since it contains 0.5 to 15 g / l of finely dispersed solids as well as partially soluble 3-methyl-4-nitrophenol in the waste filtrate. obtained as described above.
Po filtrácii kryštaiickej suspenzie 3-metyl-4-nitrofenolátu sodného odtéká odpadný filtrát s priemerným obsahom 0,5 až 15 g/1 3-metyl-4-nitrofenoiátu sodného v závislosti od spósobu vedenia technologie výroby 3-mety1-4-nitrofenolu i v závislosti od stupňa nasýtenia roztoku hydroxidom sodným alebo uhličitanom sodným. Na množstvo rozpuštěného 3-metyl-3-nitrofenolu vplýva i teplota a pH roztoku.After filtration of the crystalline suspension of sodium 3-methyl-4-nitrophenolate, the waste filtrate with an average content of 0.5 to 15 g / l of sodium 3-methyl-4-nitrophenoate flows out depending on the method of production technology of 3-methyl-4-nitrophenol and from the degree of saturation of the solution with sodium hydroxide or sodium carbonate. The temperature and pH of the solution also influence the amount of dissolved 3-methyl-3-nitrophenol.
Uvedené nevýhody odstraňuje sposob ziskania 3-metyl-4-nitrofenolu sodného z odpadného roztoku po filtrácii suspenzie podlá vynálezu, ktorého podstatou je to, že sa filtrát získaný po izolácii 3-metyl-4-nitrofenolátu sodného přečerpává cez hydrocyklon pomocou přídavného čerpadla za konštantnej prietokovej rýchlosti, kde sa odlučovacou schopnostou cyklonu zachytává rozptýlená sodná sol 3-metyl-4-nitrofenolátu. ktorá sa vracia v zahustenej formě do procesu kryštalizácie 3-metyl-4-nitrofenolátu sodného.These disadvantages are eliminated by the method of recovering sodium 3-methyl-4-nitrophenol from the waste solution after filtration of the suspension according to the invention, which is based on the fact that the filtrate obtained after isolation of sodium 3-methyl-4-nitrophenolate is pumped through hydrocyclone using an additional pump at constant flow. at which the suspended sodium salt of 3-methyl-4-nitrophenolate is trapped by the cyclone separation capability. which is returned in a concentrated form to the crystallization process of sodium 3-methyl-4-nitrophenolate.
Matečné luhy z hydrocyklonu zbavené sodnej soli 3-metyl-4-nitrofenolátu sodného odchádzajú do chemickej kanalizácie a ďalej na chemické a biologická čistiareň. Je výhodné, ak teplota vstupujúceho filtrátu do cyklona obsahujúca jemne rozptýlený 3-metyl-4-nitrofenolát sodný nepresiahla 35 °C a pH prostredia bolo v oblasti 6,5 až tí, výhodné 7,5. Ďalej sa zahuštěný 3-metyi-4-nitrofenolát sodný recirkuluje /vracia/ spát do procesu kryštalizácie 3-metyl-4-nitrofenoiátu sodného.The mother liquors from the hydrocyclone free of sodium 3-methyl-4-nitrophenolate are discharged to the chemical sewerage and further to the chemical and biological treatment plant. It is preferred that the temperature of the inlet filtrate to the cyclone containing finely divided sodium 3-methyl-4-nitrophenolate does not exceed 35 ° C and the pH of the environment is in the range of 6.5 to 3, preferably 7.5. Further, the concentrated sodium 3-methyl-4-nitrophenolate is recirculated (returned) to the crystallization process of sodium 3-methyl-4-nitrophenolate.
P r í k 1 n dExample 1 d
Pri výrobě 3-mety1-4-nitrofenólátu sodného sa po izolácii 3-metyl-4-nitrofenolátu sodného odstreďovaním získalo 6 200 1 filtrátu, ktorý sa zhromažďdoval v 16 m sedimentačněj nádobě. Filtrát z 3 nádob sa spojil a po vysedimentovaní sa horná vrstva v množstve 15 tis. 1, obsahujúce 8 g/1 , -dnej soli 3-mety1-4-nitrofenolátu sodného pri teplote 25 °C a pH 7,8, dávkovala přídavným čerpadlom za konštantnej prietokovej rýchlosti do hydrocyklona, ktorý bol umiestnený nad kryštalizačným kotlom.' Silné zahuštěný roztok 3-metyl-4-nitrofenolátu sodného sa priamo dostane do kryštalizačného kotlá, pričom po stanovení sušiny - obsahu účinnej látky 3-metylfenolátu sodnéno a jeho čistoty sa získalo 120 kg 3-metylfenolátu sodného. Matečný roztok z hydrocyklonu sa ďalej nespracovával.In the preparation of sodium 3-methyl-4-nitrophenollate, after isolation of sodium 3-methyl-4-nitrophenolate by centrifugation, 6,200 L of filtrate was collected, which was collected in a 16 m sedimentation vessel. The filtrate from 3 vessels was combined and after sedimentation, the upper layer was 15,000. 1, containing 8 g / l of sodium 3-methyl-4-nitrophenolate at 25 ° C and pH 7.8, was metered into the hydrocyclone, which was placed above the crystallization boiler, at a constant flow rate by an additional pump. A strong concentrated sodium 3-methyl-4-nitrophenolate solution is directly transferred to the crystallization cauldron, yielding 120 kg of sodium 3-methylphenolate after determining the dry substance content of the sodium 3-methylphenolate and its purity. The hydrocyclone mother liquor was not further processed.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS620185A CS249484B1 (en) | 1985-08-30 | 1985-08-30 | A method for obtaining 3-methyl-4-nitrophenol sodium from the waste solution |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS620185A CS249484B1 (en) | 1985-08-30 | 1985-08-30 | A method for obtaining 3-methyl-4-nitrophenol sodium from the waste solution |
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| Publication Number | Publication Date |
|---|---|
| CS249484B1 true CS249484B1 (en) | 1987-03-12 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CS620185A CS249484B1 (en) | 1985-08-30 | 1985-08-30 | A method for obtaining 3-methyl-4-nitrophenol sodium from the waste solution |
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| CS (1) | CS249484B1 (en) |
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1985
- 1985-08-30 CS CS620185A patent/CS249484B1/en unknown
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