PL417B1 - A method of purifying acetic acid containing mercury. - Google Patents
A method of purifying acetic acid containing mercury. Download PDFInfo
- Publication number
- PL417B1 PL417B1 PL417A PL41720A PL417B1 PL 417 B1 PL417 B1 PL 417B1 PL 417 A PL417 A PL 417A PL 41720 A PL41720 A PL 41720A PL 417 B1 PL417 B1 PL 417B1
- Authority
- PL
- Poland
- Prior art keywords
- acetic acid
- mercury
- acid
- acid containing
- containing mercury
- Prior art date
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- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 title claims description 57
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 title claims description 20
- 229910052753 mercury Inorganic materials 0.000 title claims description 19
- 238000000034 method Methods 0.000 title claims description 12
- 239000002253 acid Substances 0.000 claims description 11
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 claims description 2
- 239000003054 catalyst Substances 0.000 claims description 2
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 claims description 2
- 150000007513 acids Chemical class 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 claims 1
- 230000001590 oxidative effect Effects 0.000 claims 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 3
- BDAGIHXWWSANSR-UHFFFAOYSA-M Formate Chemical compound [O-]C=O BDAGIHXWWSANSR-UHFFFAOYSA-M 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 229940117975 chromium trioxide Drugs 0.000 description 2
- WGLPBDUCMAPZCE-UHFFFAOYSA-N chromium trioxide Inorganic materials O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 description 2
- GAMDZJFZMJECOS-UHFFFAOYSA-N chromium(6+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Cr+6] GAMDZJFZMJECOS-UHFFFAOYSA-N 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 238000010992 reflux Methods 0.000 description 2
- VZSRBBMJRBPUNF-UHFFFAOYSA-N 2-(2,3-dihydro-1H-inden-2-ylamino)-N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]pyrimidine-5-carboxamide Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C(=O)NCCC(N1CC2=C(CC1)NN=N2)=O VZSRBBMJRBPUNF-UHFFFAOYSA-N 0.000 description 1
- IKHGUXGNUITLKF-XPULMUKRSA-N acetaldehyde Chemical compound [14CH]([14CH3])=O IKHGUXGNUITLKF-XPULMUKRSA-N 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- ZCDOYSPFYFSLEW-UHFFFAOYSA-N chromate(2-) Chemical class [O-][Cr]([O-])(=O)=O ZCDOYSPFYFSLEW-UHFFFAOYSA-N 0.000 description 1
- KRVSOGSZCMJSLX-UHFFFAOYSA-L chromic acid Substances O[Cr](O)(=O)=O KRVSOGSZCMJSLX-UHFFFAOYSA-L 0.000 description 1
- BUACSMWVFUNQET-UHFFFAOYSA-H dialuminum;trisulfate;hydrate Chemical compound O.[Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O BUACSMWVFUNQET-UHFFFAOYSA-H 0.000 description 1
- SOCTUWSJJQCPFX-UHFFFAOYSA-N dichromate(2-) Chemical compound [O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O SOCTUWSJJQCPFX-UHFFFAOYSA-N 0.000 description 1
- -1 for example Substances 0.000 description 1
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 description 1
- AWJWCTOOIBYHON-UHFFFAOYSA-N furo[3,4-b]pyrazine-5,7-dione Chemical compound C1=CN=C2C(=O)OC(=O)C2=N1 AWJWCTOOIBYHON-UHFFFAOYSA-N 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 150000002730 mercury Chemical class 0.000 description 1
- 229940008718 metallic mercury Drugs 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 239000012286 potassium permanganate Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000001577 simple distillation Methods 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 238000005292 vacuum distillation Methods 0.000 description 1
Description
. Wynalazek dotyczy sposobu oczy¬ szczania kwasu octowego, zawierajacego rtec a otrzymywanego, np. przy bezpo¬ srednim wyrobie z acetylenu w obecnosci katalizatorów rteciowych, który to wy¬ nalazek daje moznosc otrzymania kwasu zupelnie wolnego od rteci. Sposób*polega na tern, ze kwas octowy zawierajacy rtec podgrzewa sie czas dluzszy az do wrzenia. Przytem rtec wydziela sie.Jezeli poprzestac na tej metodzie, otrzymuje sie rtec w postaci metaliczne¬ go osadu, a po oddzieleniu, zupelnie wol¬ ny od rteci kwas octowy, który nastep¬ nie oczyszcza sie zwyklem destylowa¬ niem.Sposób przyspiesza sie przez zasto¬ sowanie pewnych dodatków. Jako takie okazaly sie stosownemi: stezony kwas siarczany, kwas fosforowy, siarczany me¬ tali alkalicznych, metali ciezkich, glinu it. d., nastepnie sole kwasu nadmanganowego, kwasu chromowego i kwasu nadsiarcza- nowego. Temi srodkami osiaga sie po¬ wazne skrócenie czasu podgrzewania.Wyniki powyzsze osiaga sie takze, gdy podgrzewac do wrzenia kwas octowy, zawierajacy rtec, przez krótki X)kres cza¬ su, z cialami odtleiiiajacemi, np. kwa¬ sem mrówczanym. Przy zastosowaniu niektórych dodatków, np. • mieszanin dwuchromianów lub chromianów lub nad¬ manganianów i t. d. z kwasem siarcza- nym, przechodzi rtec czesciowo lub cal¬ kowicie w odpowiednia sól rteciowa, od której oddziela sie kwas octowy, np. przez destylowanie w prózni. Przy od¬ dzialywaniu na kwas octowy, zawieraja¬ cy rtec, silnych srodków utleniajacych, jak trójtlenek chromu, nadmanganiani kwas siarczany, dwuchromian i kwas siarczany i t. d., otrzymuje sie jeszcze te korzysc, ze kwas octowy uwalnia sie równoczesnie od pewnych domieszek zanieczyszczajacych,np. od aldehydu octo¬ wego.Ponizej podano kilka przykladów wy¬ konania niniejszego sposobu.Przyklad 1. 1 kg kwasu octowego, zawierajacego rtec, podgrzewa sie do wrzenia okolo 20 godzin pod chlodnica zwrotna, odle¬ wa od wydzielonej metalicznej rteci i de¬ styluje przy zwyklem cisnieniu. Otrzy¬ many jako destylat kwas octowy jest zupelnie wolny od rteci.Przyklad 2. 1 kg kwasu octowego, jak w przy¬ kladzie 1, podgrzewa sie wraz z 40 g siarczanu glinowego w ciagu 8 godzin, az do wrzenia. Dalszy przebieg jak w przykladzie 1.Przyklad 3. 1 kg kwasu octowego z zawartoscia rteci podgrzewa sie wraz z 10 g kwasu mrówczanego w ciagu i—2 godzin do wrze¬ nia. Dalszy przebieg jak w przykladzie 1.Przyklad 4. 1 kg kwasu octowego, zawierajacego rtec i okolo 1% aldehydu octowego, miesza sie z 25 g nadmanganianu po¬ tasu i 20 g stezonego kwasu siarcza- nego i podgrzewa w ciagu 1 godziny pod chlodnica zwrotna. Nastepnie kwas pod¬ daje sie przedestylowaniu, bez uprzed¬ niego oddzielania od utworzonego osadu, w prózni przy temperaturze 60 — 70°.Destylat jest zupelnie wolny od rtecj i aldehydu.Przyklad 5. 1 kg kwasu octowego, jak w przykla¬ dzie 4 miesza sie »z 30 g sproszkowa¬ nego trójtlenku chromu i podgrzewa w ciagu 1 godziny do wrzenia, poczem postepuje sie jak w przykladzie 4.Wedlug wynalazku, kwas octowy, do¬ wolnego pochodzenia, z zawartoscia rte¬ ci, mozna przerobic na chemicznie czysty kwas octowy. PL. The invention relates to a process for the purification of acetic acid containing mercury obtained, for example, by making a direct product from acetylene in the presence of mercury catalysts, which invention makes it possible to obtain an acid that is completely mercury free. The method * is based on the fact that the mercury-containing acetic acid is heated for a longer time until it boils. The mercury is then released. If one persists in this method, the result is mercury in the form of a metallic precipitate, and after separation, completely mercury-free acetic acid, which is then purified by simple distillation. The method is accelerated by the stagnation. ¬ the use of certain additives. As such, the following have proved to be suitable: concentrated sulfate acid, phosphoric acid, sulfates of alkali metals, heavy metals, aluminum, etc. d., then salts of permanganic acid, chromic acid and persulfic acid. By these means the heating time is considerably shortened. The above results are also obtained when the mercury-containing acetic acid is boiled for a short time period with de-oxygenating bodies such as formate acid. With the use of certain additives, for example, mixtures of dichromates or chromates or permanganates, etc. with sulfuric acid, the mercury is converted partially or completely into the corresponding mercury salt, from which the acetic acid is separated, for example by vacuum distillation. By treating acetic acid, which contains mercury, with strong oxidizing agents, such as chromium trioxide, permanganate sulfate acid, dichromate and sulfate acid, etc. . Some examples of the present process are given below. EXAMPLE 1 1 kg of acetic acid, containing mercury, is boiled for about 20 hours under reflux, casts from the separated metallic mercury, and distorts at I used to pressure. The acetic acid obtained as the distillate is completely mercury free. Example 2.1 kg of acetic acid, as in Example 1, is heated with 40 g of aluminum sulphate in 8 hours until boiling. Further procedure as in Example 1. Example 3. 1 kg of acetic acid with mercury content is heated with 10 g of formate acid for 1-2 hours until September. The procedure is as in example 1. Example 4.1 kg of acetic acid, containing mercury and about 1% of acetaldehyde, is mixed with 25 g of potassium permanganate and 20 g of concentrated sulfuric acid and heated for 1 hour under reflux. . The acid is then distilled, without separating from the precipitate formed, under a vacuum at a temperature of 60-70 °. The distillate is completely free of mercury and aldehyde. Example 5.1 kg of acetic acid, as in Example 4 is mixed with 30 g of powdered chromium trioxide and boiled for 1 hour, then proceed as in Example 4 According to the invention, acetic acid of any origin, containing mercury, can be converted into chemically pure acid acetic. PL
Claims (4)
Publications (1)
| Publication Number | Publication Date |
|---|---|
| PL417B1 true PL417B1 (en) | 1924-08-30 |
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