CS228402B1 - Method of sulphuric acid purification - Google Patents
Method of sulphuric acid purification Download PDFInfo
- Publication number
- 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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- CS
- Czechoslovakia
- Prior art keywords
- sulfuric acid
- nitro
- weight
- solution
- purification
- Prior art date
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- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 title claims description 56
- 238000000034 method Methods 0.000 title claims description 12
- 238000000746 purification Methods 0.000 title description 8
- 235000011149 sulphuric acid Nutrition 0.000 title 1
- 239000001117 sulphuric acid Substances 0.000 title 1
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 claims description 18
- -1 nitro- Chemical class 0.000 claims description 9
- RLSSMJSEOOYNOY-UHFFFAOYSA-N m-cresol Chemical compound CC1=CC=CC(O)=C1 RLSSMJSEOOYNOY-UHFFFAOYSA-N 0.000 claims description 8
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 6
- 229910017604 nitric acid Inorganic materials 0.000 claims description 6
- PIIZYNQECPTVEO-UHFFFAOYSA-N 4-nitro-m-cresol Chemical compound CC1=CC(O)=CC=C1[N+]([O-])=O PIIZYNQECPTVEO-UHFFFAOYSA-N 0.000 claims description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 5
- 239000012535 impurity Substances 0.000 claims description 5
- 238000006386 neutralization reaction Methods 0.000 claims description 5
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 4
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 4
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 4
- 239000003610 charcoal Substances 0.000 claims description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 2
- 229910052783 alkali metal Inorganic materials 0.000 claims description 2
- 229910021529 ammonia Inorganic materials 0.000 claims description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims 1
- 235000011114 ammonium hydroxide Nutrition 0.000 claims 1
- 125000000449 nitro group Chemical group [O-][N+](*)=O 0.000 claims 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 13
- 238000004519 manufacturing process Methods 0.000 description 4
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 3
- 238000000605 extraction Methods 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- QIORDSKCCHRSSD-UHFFFAOYSA-N 3-methyl-2-nitrophenol Chemical compound CC1=CC=CC(O)=C1[N+]([O-])=O QIORDSKCCHRSSD-UHFFFAOYSA-N 0.000 description 2
- YYRMJZQKEFZXMX-UHFFFAOYSA-N calcium;phosphoric acid Chemical compound [Ca+2].OP(O)(O)=O.OP(O)(O)=O YYRMJZQKEFZXMX-UHFFFAOYSA-N 0.000 description 2
- 235000013877 carbamide Nutrition 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 238000006396 nitration reaction Methods 0.000 description 2
- 230000009935 nitrosation Effects 0.000 description 2
- 238000007034 nitrosation reaction Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 description 2
- 235000011152 sodium sulphate Nutrition 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000006277 sulfonation reaction Methods 0.000 description 2
- 239000002426 superphosphate Substances 0.000 description 2
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 description 1
- LWKMVGXFANTKBP-UHFFFAOYSA-N 6-hydroxy-2-methyl-3-nitrobenzoic acid Chemical compound CC1=C(C(O)=O)C(O)=CC=C1[N+]([O-])=O LWKMVGXFANTKBP-UHFFFAOYSA-N 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 150000001491 aromatic compounds Chemical class 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Inorganic materials [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Inorganic materials [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 150000002191 fatty alcohols Chemical class 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 150000003672 ureas Chemical class 0.000 description 1
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 1
- 229960001763 zinc sulfate Drugs 0.000 description 1
- 229910000368 zinc sulfate Inorganic materials 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
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)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS241382A CS228402B1 (en) | 1982-04-05 | 1982-04-05 | Method of sulphuric acid purification |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS241382A CS228402B1 (en) | 1982-04-05 | 1982-04-05 | Method of sulphuric acid purification |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CS228402B1 true CS228402B1 (en) | 1984-05-14 |
Family
ID=5361211
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CS241382A CS228402B1 (en) | 1982-04-05 | 1982-04-05 | Method of sulphuric acid purification |
Country Status (1)
| Country | Link |
|---|---|
| CS (1) | CS228402B1 (en) |
-
1982
- 1982-04-05 CS CS241382A patent/CS228402B1/en unknown
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