CS228402B1 - Method of sulphuric acid purification - Google Patents

Method of sulphuric acid purification Download PDF

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CS228402B1
CS228402B1 CS241382A CS241382A CS228402B1 CS 228402 B1 CS228402 B1 CS 228402B1 CS 241382 A CS241382 A CS 241382A CS 241382 A CS241382 A CS 241382A CS 228402 B1 CS228402 B1 CS 228402B1
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sulfuric acid
nitro
weight
solution
purification
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CS241382A
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Czech (cs)
Slovak (sk)
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Robert Ing Csc Poor
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Poor Robert
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Description

Vynález sa týká čistenia kyseliny sírovejj vznikajúcej pri nitračných, oxidačných a sulfonačných procesoch.The invention relates to the purification of sulfuric acid resulting from nitration, oxidation and sulfonation processes.

Kyselina sírová, ktorá odpadá po nitračných, oxidačných, sulfonačných procesoch, má koncentráciu 20 až 80 % hmotnosti. Obsahuje organické látky, kyselinu dusičná, oxidy dusíka, anorganická kyslé sírany a pod. Takáto kyselina sírová sa používá napr. pri výrobě superfosfátu. Sá známe postupy k odstraňovaniu nečistfit z použitej kyseliny sírovej, například ak obsahuje kysličníky dusíka, tieto sa z nej odstraňujá denitréciou.Sulfuric acid, which falls off after nitration, oxidation, sulfonation processes, has a concentration of 20 to 80% by weight. It contains organic substances, nitric acid, nitrogen oxides, inorganic acid sulphates and the like. Such sulfuric acid is used e.g. in the production of superphosphate. Known processes for removing impurities from the sulfuric acid used, for example if it contains nitrogen oxides, are removed from the sulfuric acid by denitration.

PodTa patentu DD 120 184 sa odstraňujá kysličníky dusíka z kyseliny sírovej močovinou, alebo karbamidami. Kyselina sirové o koncentráoii 70 % hmotnosti, získané z nitrozačných procesov, sa koncentruje v Paulingovom přístroji, pričom dochádza k oxidácii organických nečistot kyselinou sírovou alebo dusičnou.According to the patent DD 120 184, nitrogen oxides are removed from the sulfuric acid by urea or carbamides. Sulfuric acid, with a concentration of 70% by weight, obtained from nitrosation processes, is concentrated in a Pauling apparatus, oxidising organic impurities with sulfuric or nitric acid.

PodTa patentu SU 316 648 sa čistenie použitej kyseliny sírovej uskutočňuje extrakciou fenolmi. Extrakciou organických nečistot s mastnými alkoholmi z kyseliny sírovej udává patent SU 416 3Í2. SpOsob čistenia upotrebenej kyseliny sírovej po nitrozácii aromatických zlúčenín, obsahujúcich fluór, popisuje čsl. AO 167 207.According to patent SU 316 648 the purification of the sulfuric acid used is carried out by extraction with phenols. The extraction of organic impurities with fatty alcohols from sulfuric acid is disclosed in SU 416 3112. The method of purification of spent sulfuric acid after nitrosation of fluorine-containing aromatic compounds is described in U.S. Pat. AO 167 207

Alkalická sírany a sírany těžkých kovov sa oddeTujá zo zriedenej kyseliny sírovej koncentrováním kyseliny sírovej na 96 až 98 % hmotnosti a potom sa izolujú napr. filtráciou.The alkaline and heavy metal sulfates are separated from the dilute sulfuric acid by concentrating the sulfuric acid to 96-98% by weight and then recovering e.g. filtration.

Organická látky sa odstraňujá z kyseliny sírovej extrakciou organickými rozpáčtadlami. Pri extrakci! sa čésť rozpáčťadla rozpustí v kyselině sírovej.The organic material is removed from the sulfuric acid by extraction with organic solvents. When extracting! the solvent of the solvent is dissolved in sulfuric acid.

Kyselina sírová použitá vo vyššie uvedených procesoch sa používá na výrobu síranu vápenatého, bárnatáho alebo zinočnatého, alebo pri výrobě superfosfátu.The sulfuric acid used in the above processes is used for the production of calcium, barium or zinc sulfate, or for the production of superphosphate.

čistěním kyseliny sírovej o koncentrácii 20 až 40 % hmotnosti obsahujúcej kyslý síran sodný, kyselinu dusičná, 3-metylfenol a jeho nitro-, dinitro-, nitrozo- i sulfoderiváty popisuje čsl. AO 209 967 a AO 208 337, priSom podstatou čistenia je, že sa organické nečistoty adsorbujá kremičitanmi, aktívnym uhlím, aktívnym bentomitom alebo použitím niekol’ko stupňovej adsorbcie za využitia uvedených adsorbčných činidiel.Purification of 20 to 40% by weight sulfuric acid containing sodium sulphate, nitric acid, 3-methylphenol and its nitro-, dinitro-, nitroso- and sulfoderivatives is described in U.S. Pat. AO 209 967 and AO 208 337, the essence of the purification is that the organic impurities are adsorbed by silicates, activated carbon, active bentomite or by the use of several step adsorption using said adsorbent agents.

Nevýhodou postupu je, že sa používá 2-stupňová adsorbcia, pričom je nutné v následnosti zahušťovaníe kyseliny sírovej a po zahušťovaní sa oddělí síran od kyseliny sírovej.A disadvantage of the process is that 2-stage adsorption is used, whereby it is necessary to concentrate the sulfuric acid and, after concentration, the sulfate is separated from the sulfuric acid.

Vyššie uvedené nedostatky sú odstránené spOsobom čistenia kyseliny sírovej podl’a vynálezu. Kyselina sírová koncentrácie 18 až 40 % hmotnostných, obsahujúca hydrogensírany alkalického kovu, kyselinu dusičnú, 3-metyl-4-nitrofenol, 3-metylfenol a jeho nitro-, nitrozo-, dinitro-, sulfoderiváty a oxidy dusíka, sa čistí podlá vynálezu tak, že sa neutralizuje amoniakom, alebo vodným roztokom amoniaku, pričom sa před, behom alebo po neutralizácii uvedle do styku s aktívnym uhlím, čistěním roztoku aktívnym uhlím a po izolácii použitého aktívneho uhlia sa získá roztok síranu amonného, obsahujúci i dusičnan amdnny a malé množstvo síranu sodného.The above drawbacks are overcome by the method of purification of the sulfuric acid of the invention. Sulfuric acid at a concentration of 18 to 40% by weight, containing alkali metal hydrogen sulphates, nitric acid, 3-methyl-4-nitrophenol, 3-methylphenol and its nitro-, nitroso-, dinitro-, sulfoderivatives and nitrogen oxides, is purified according to the invention by: by neutralizing with ammonia or aqueous ammonia, contacting with activated carbon before, during or after neutralization, purifying the solution with activated carbon, and isolating the spent activated carbon to give an ammonium sulfate solution containing also ammonium nitrate and a small amount of sodium sulfate .

Výhodou spdsobu podlá vynálezu je, že sa uskutočňuje 1 stupňová adsorbcia spojená s neutralizácloujbez zahusťovania sa získává výsledný produkt.An advantage of the process according to the invention is that a 1-step adsorption coupled with neutralization is carried out without concentration, the resulting product is obtained.

PřikladlEXAMPLE

200 ml použitej kyseliny sírovej, obsahujúcej 32 % hmotnosti H^SO^, 1,4 % hmotnosti kyseliny dusičnej, 0,1 % hmotnosti oxidov dusíka, 0,19 % hmotnosti 3-metyl-4-nitrofenolu a 0,10 % hmotnosti 3-metylfenolu a jeho nitro-, nitrozo-, dinitro- a sulfoderivátov sa neutralizovala za použitia 39 % roztoku NH^, pričom na neutralizáciu do neutrálneho pH sa spotřebovalo 86 ml tohto roztoku. Teplota pozvolné vystúpila na 60 až 70 °C, za miešania sa přidalo 10 g aktívneho uhlia a po 1/2 hodině miešania sa roztok přefiltroval, pričom sa oddělilo aktivně uhlle a získal sa roztok, obsahujúci 108 g síranu amonného; obsah 3-metyl-4-nitrofenolu poklesol na hodnotu 0,038 % a stopové množstvá 3-metylnitrofenolu a jeho derivétov.200 ml of sulfuric acid used containing 32% by weight of H 2 SO 4, 1,4% by weight of nitric acid, 0,1% by weight of nitrogen oxides, 0,19% by weight of 3-methyl-4-nitrophenol and 0,10% by weight of 3 methylphenol and its nitro-, nitroso-, dinitro- and sulfoderivatives were neutralized using a 39% NH 4 solution, 86 ml of this solution being consumed to neutralize to neutral pH. The temperature gradually rose to 60-70 ° C, 10 g of charcoal were added with stirring, and after stirring for 1/2 hour the solution was filtered while separating actively charcoal to give a solution containing 108 g of ammonium sulfate; the 3-methyl-4-nitrophenol content decreased to 0.038% and the trace amounts of 3-methylnitrophenol and its derivatives.

Příklad 2Example 2

Postup i východiskové látky sú rovnaké ako v příklade 1, rozdiel bol len v tom, že aktivně uhlie sa přidalo priamo do kyseliny sírovej, v ňalšóm sa uskutočnila neutralizácia a po neutralisácii sa aktivně uhlie oddělilo filtráciou. Získaný roztok síranu amonného obsahoval po Izolácii aktívneho hhlia 0,03 % p-nitro-m-krezolátu a stopové množstvá 3-metylnitrofenólu a jeho derivétov.The procedure and the starting materials are the same as in Example 1, the only difference being that the activated carbon was added directly to the sulfuric acid, the neutralization was carried out and after neutralization the activated carbon was removed by filtration. The ammonium sulfate solution obtained after isolation of active carbon contained 0.03% p-nitro-m-cresolate and trace amounts of 3-methylnitrophenol and its derivatives.

Vynález možno použiť pri čistění kyseliny sírovej, vznikájúcej pri výrobě 3-metyl-4-nitřof enolu.The invention can be used in the purification of sulfuric acid resulting from the production of 3-methyl-4-nitrophenol.

Claims (1)

3 PREDMET VYNÁLEZU 228402 Spdsob čistenia kyseliny sírovej, obsahujúcej ako nečistoty 3-metyl-4-nitrofenol, 3--metylfenol a jeho nitro-, nitrozp-, dinitro- a sulfoderivéty, kyselinu dusičná, oxidy dusí-ka a hydrogensírany alkalického kovu, je význačný tým, že kyselina sírová sa neutralizuje amo-niakom alebo roztokom amoniaku,přičom sa před, počas, alebo po neutralizácii přidá ku kyse-lina sírovej alebo připadne ku zneutralizovanému roztoku kyseliny sirovej aktivně uhlie,ktoré sa potom oddělí od roztoku síranu amonného. 9BACKGROUND OF THE INVENTION 228402 A method of purifying sulfuric acid containing 3-methyl-4-nitrophenol, 3-methylphenol and its nitro, nitro-, dinitro- and sulfoderivatives, nitric acid, nitrogen oxides and alkali metal hydrogen sulphates as impurities is characterized in that sulfuric acid is neutralized with ammonia or ammonia solution, and charcoal is added to sulfuric acid or to a neutralized sulfuric acid solution before, during or after neutralization, which is then separated from the ammonium sulfate solution. 9
CS241382A 1982-04-05 1982-04-05 Method of sulphuric acid purification CS228402B1 (en)

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