METHOD AND DEVICE FOR PROCESSING WASTE SULPHURIC ACIDS FROM NITRATION PROCESSES
Processing waste acid obtained from nitroaromatics production, preferably dinitrotoluene- or trinitrotoluene production, comprises: adding a pre-heated waste acid comprising sulfuric acid, water, nitric acid, nitrosylsulfuric acid and nitro-organics, into a stripping column in a counter-flow to the...
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| description | Processing waste acid obtained from nitroaromatics production, preferably dinitrotoluene- or trinitrotoluene production, comprises: adding a pre-heated waste acid comprising sulfuric acid, water, nitric acid, nitrosylsulfuric acid and nitro-organics, into a stripping column in a counter-flow to the steam obtained from the bottom of the stripping column by heating a pre-concentrated sulfuric acid; separating nitric acid, optionally nitro-organics and the pre-concentrated sulfuric acid into at least one vapor phase; and processing the obtained nitric acid and the nitro-organics. Processing waste acid obtained from nitroaromatics production, preferably dinitrotoluene- or trinitrotoluene production, under recovery of concentrated and purified sulfuric acid and nitric acid, comprises: (i) adding a pre-heated waste acid comprising sulfuric acid and water (up to 80 wt.%), nitric acid, nitrosylsulfuric acid and nitro-organics, preferably dinitrotoluene and mononitrotoluene, into a stripping column in a counter-flow to the steam, which is obtained from the bottom of the stripping column by heating a pre-concentrated sulfuric acid in a first phase; (ii) separating nitric acid, optionally nitro-organics and the pre-concentrated sulfuric acid into at least one vapor phase; and (iii) supplying the obtained pre-concentrated sulfuric acid from the bottom of the stripping column for further purification to separate the highly concentrated nitro-organics in a first downstream stage, and processing nitric acid obtained from the nitric acid vapor phase, and the nitro-organics including the nitro-organics obtained during the further purification and concentration of the pre-concentrated sulfuric acid, and returning back to the nitration process in a second downstream stage. The step (i) comprises: adding the pre-heated waste acid into the stripping column for stripping in the counter-flow to the steam obtained from the pre-concentrated sulfuric acid in concentrating the stripping steam containing nitric acid in the counter-flow to the purified and optionally fresh concentrated sulfuric acid (75-97 wt.%, preferably 80-96 wt.%); and condensing the nitric acid vapors obtained from the top of the column of the first stage, and thus directly obtaining a highly concentrated form of nitric acid for returning back to the nitration process. An independent claim is also included for a device for performing the above method comprising: a first stripping column (K1) with a feeding line f |
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| fullrecord | <record><control><sourceid>epo_EVB</sourceid><recordid>TN_cdi_epo_espacenet_EP2295375A1</recordid><sourceformat>XML</sourceformat><sourcesystem>PC</sourcesystem><sourcerecordid>EP2295375A1</sourcerecordid><originalsourceid>FETCH-epo_espacenet_EP2295375A13</originalsourceid><addsrcrecordid>eNqNyrEKwjAQANAsDqL-w_2AQ1uKOIbkYg5sLuTSOpYicSpaqP-Pi-5Ob3lbxR1mzxZ0sGBxIIPgOEFMbFCEwgVuWjKC9Nfo-0QGtCEr4BJ3ECgnnYnD76Ps1eYxzWs5fN0pcJiNP5blNZZ1me7lWd4jxro-t82p1VXzR_kA8cEukg</addsrcrecordid><sourcetype>Open Access Repository</sourcetype><iscdi>true</iscdi><recordtype>patent</recordtype></control><display><type>patent</type><title>METHOD AND DEVICE FOR PROCESSING WASTE SULPHURIC ACIDS FROM NITRATION PROCESSES</title><source>esp@cenet</source><creator>DICHTL, GOTTFRIED ; STEEG, HARALD</creator><creatorcontrib>DICHTL, GOTTFRIED ; STEEG, HARALD</creatorcontrib><description>Processing waste acid obtained from nitroaromatics production, preferably dinitrotoluene- or trinitrotoluene production, comprises: adding a pre-heated waste acid comprising sulfuric acid, water, nitric acid, nitrosylsulfuric acid and nitro-organics, into a stripping column in a counter-flow to the steam obtained from the bottom of the stripping column by heating a pre-concentrated sulfuric acid; separating nitric acid, optionally nitro-organics and the pre-concentrated sulfuric acid into at least one vapor phase; and processing the obtained nitric acid and the nitro-organics. Processing waste acid obtained from nitroaromatics production, preferably dinitrotoluene- or trinitrotoluene production, under recovery of concentrated and purified sulfuric acid and nitric acid, comprises: (i) adding a pre-heated waste acid comprising sulfuric acid and water (up to 80 wt.%), nitric acid, nitrosylsulfuric acid and nitro-organics, preferably dinitrotoluene and mononitrotoluene, into a stripping column in a counter-flow to the steam, which is obtained from the bottom of the stripping column by heating a pre-concentrated sulfuric acid in a first phase; (ii) separating nitric acid, optionally nitro-organics and the pre-concentrated sulfuric acid into at least one vapor phase; and (iii) supplying the obtained pre-concentrated sulfuric acid from the bottom of the stripping column for further purification to separate the highly concentrated nitro-organics in a first downstream stage, and processing nitric acid obtained from the nitric acid vapor phase, and the nitro-organics including the nitro-organics obtained during the further purification and concentration of the pre-concentrated sulfuric acid, and returning back to the nitration process in a second downstream stage. The step (i) comprises: adding the pre-heated waste acid into the stripping column for stripping in the counter-flow to the steam obtained from the pre-concentrated sulfuric acid in concentrating the stripping steam containing nitric acid in the counter-flow to the purified and optionally fresh concentrated sulfuric acid (75-97 wt.%, preferably 80-96 wt.%); and condensing the nitric acid vapors obtained from the top of the column of the first stage, and thus directly obtaining a highly concentrated form of nitric acid for returning back to the nitration process. An independent claim is also included for a device for performing the above method comprising: a first stripping column (K1) with a feeding line for the processed waste acid, an associated evaporator for obtaining the pre-concentrated sulfuric acid and a discharging for the nitric acid containing vapor phase; an additional stripping column (K2) with an associated evaporator for producing a purified sulfuric acid and at least one additional evaporator for highly concentrating the purified sulfuric acid; heat exchanger condensers for vapor phases, which are obtained as top products from the stripping columns and the evaporators; optionally a washing column for washing of nitrogen-containing gases; required piping for feeding the starting materials, transporting, distributing and discharging vapor phase, liquid phase, processing products and waste gases obtained as processing streams; and required heating-, cooling- and pressure control equipments. The first stripping column is provided with a feeding line for a highly concentrated purified sulfuric acid, which is produced during the processing of the waste acid.
Verfahren zur Aufarbeitung von Abfallsäure aus Verfahren der Herstellung von Nitroaromaten, insbesondere der Herstellung von Dinitrotoluol (DNT) oder auch Trinitrotouol (TNT), unter Rückgewinnung von aufkonzentrierter und aufgereinigter Schwefelsäure und Salpetersäure, bei dem man in einer ersten Stufe die Abfallsäure in einer Strippkolonne im Gegenstrom zu Wasserdampf aus dem Sumpf der Strippkolonne in mindestens eine dampfförmige Phase, die Salpetersäure sowie gegebenenfalls Nitroorganika enthält, sowie eine vorkonzentrierte Schwefelsäure auftrennt, und man die dampfförmige Phase und die vorkonzentrierte Schwefelsäure in nachgeschalteten Verfahrensstufen kondensiert und/oder aufarbeitet, wobei man in der ersten Stufe des Verfahrens erfindungsgemäß zusätzlich zum Strippen eine Aufkonzentrierung der im Strippdampf enthaltenen Salpetersäure in Gegenwart zusätzlicher konzentrierter Schwefelsäure durchführt, so dass man direkt in der ersten Stufe Salpetersäure in einer für eine Rückführung in das Nitrierverfahren geeigneten hochkonzentrierten Form gewinnt.</description><language>eng ; fre ; ger</language><subject>CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOIDCHEMISTRY ; CHEMISTRY ; COMPOUNDS THEREOF ; INORGANIC CHEMISTRY ; METALLURGY ; NON-METALLIC ELEMENTS ; PERFORMING OPERATIONS ; PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL ; SEPARATION ; THEIR RELEVANT APPARATUS ; TRANSPORTING</subject><creationdate>2011</creationdate><oa>free_for_read</oa><woscitedreferencessubscribed>false</woscitedreferencessubscribed></display><links><openurl>$$Topenurl_article</openurl><openurlfulltext>$$Topenurlfull_article</openurlfulltext><thumbnail>$$Tsyndetics_thumb_exl</thumbnail><linktohtml>$$Uhttps://worldwide.espacenet.com/publicationDetails/biblio?FT=D&date=20110316&DB=EPODOC&CC=EP&NR=2295375A1$$EHTML$$P50$$Gepo$$Hfree_for_read</linktohtml><link.rule.ids>230,308,776,881,25542,76290</link.rule.ids><linktorsrc>$$Uhttps://worldwide.espacenet.com/publicationDetails/biblio?FT=D&date=20110316&DB=EPODOC&CC=EP&NR=2295375A1$$EView_record_in_European_Patent_Office$$FView_record_in_$$GEuropean_Patent_Office$$Hfree_for_read</linktorsrc></links><search><creatorcontrib>DICHTL, GOTTFRIED</creatorcontrib><creatorcontrib>STEEG, HARALD</creatorcontrib><title>METHOD AND DEVICE FOR PROCESSING WASTE SULPHURIC ACIDS FROM NITRATION PROCESSES</title><description>Processing waste acid obtained from nitroaromatics production, preferably dinitrotoluene- or trinitrotoluene production, comprises: adding a pre-heated waste acid comprising sulfuric acid, water, nitric acid, nitrosylsulfuric acid and nitro-organics, into a stripping column in a counter-flow to the steam obtained from the bottom of the stripping column by heating a pre-concentrated sulfuric acid; separating nitric acid, optionally nitro-organics and the pre-concentrated sulfuric acid into at least one vapor phase; and processing the obtained nitric acid and the nitro-organics. Processing waste acid obtained from nitroaromatics production, preferably dinitrotoluene- or trinitrotoluene production, under recovery of concentrated and purified sulfuric acid and nitric acid, comprises: (i) adding a pre-heated waste acid comprising sulfuric acid and water (up to 80 wt.%), nitric acid, nitrosylsulfuric acid and nitro-organics, preferably dinitrotoluene and mononitrotoluene, into a stripping column in a counter-flow to the steam, which is obtained from the bottom of the stripping column by heating a pre-concentrated sulfuric acid in a first phase; (ii) separating nitric acid, optionally nitro-organics and the pre-concentrated sulfuric acid into at least one vapor phase; and (iii) supplying the obtained pre-concentrated sulfuric acid from the bottom of the stripping column for further purification to separate the highly concentrated nitro-organics in a first downstream stage, and processing nitric acid obtained from the nitric acid vapor phase, and the nitro-organics including the nitro-organics obtained during the further purification and concentration of the pre-concentrated sulfuric acid, and returning back to the nitration process in a second downstream stage. The step (i) comprises: adding the pre-heated waste acid into the stripping column for stripping in the counter-flow to the steam obtained from the pre-concentrated sulfuric acid in concentrating the stripping steam containing nitric acid in the counter-flow to the purified and optionally fresh concentrated sulfuric acid (75-97 wt.%, preferably 80-96 wt.%); and condensing the nitric acid vapors obtained from the top of the column of the first stage, and thus directly obtaining a highly concentrated form of nitric acid for returning back to the nitration process. An independent claim is also included for a device for performing the above method comprising: a first stripping column (K1) with a feeding line for the processed waste acid, an associated evaporator for obtaining the pre-concentrated sulfuric acid and a discharging for the nitric acid containing vapor phase; an additional stripping column (K2) with an associated evaporator for producing a purified sulfuric acid and at least one additional evaporator for highly concentrating the purified sulfuric acid; heat exchanger condensers for vapor phases, which are obtained as top products from the stripping columns and the evaporators; optionally a washing column for washing of nitrogen-containing gases; required piping for feeding the starting materials, transporting, distributing and discharging vapor phase, liquid phase, processing products and waste gases obtained as processing streams; and required heating-, cooling- and pressure control equipments. The first stripping column is provided with a feeding line for a highly concentrated purified sulfuric acid, which is produced during the processing of the waste acid.
Verfahren zur Aufarbeitung von Abfallsäure aus Verfahren der Herstellung von Nitroaromaten, insbesondere der Herstellung von Dinitrotoluol (DNT) oder auch Trinitrotouol (TNT), unter Rückgewinnung von aufkonzentrierter und aufgereinigter Schwefelsäure und Salpetersäure, bei dem man in einer ersten Stufe die Abfallsäure in einer Strippkolonne im Gegenstrom zu Wasserdampf aus dem Sumpf der Strippkolonne in mindestens eine dampfförmige Phase, die Salpetersäure sowie gegebenenfalls Nitroorganika enthält, sowie eine vorkonzentrierte Schwefelsäure auftrennt, und man die dampfförmige Phase und die vorkonzentrierte Schwefelsäure in nachgeschalteten Verfahrensstufen kondensiert und/oder aufarbeitet, wobei man in der ersten Stufe des Verfahrens erfindungsgemäß zusätzlich zum Strippen eine Aufkonzentrierung der im Strippdampf enthaltenen Salpetersäure in Gegenwart zusätzlicher konzentrierter Schwefelsäure durchführt, so dass man direkt in der ersten Stufe Salpetersäure in einer für eine Rückführung in das Nitrierverfahren geeigneten hochkonzentrierten Form gewinnt.</description><subject>CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOIDCHEMISTRY</subject><subject>CHEMISTRY</subject><subject>COMPOUNDS THEREOF</subject><subject>INORGANIC CHEMISTRY</subject><subject>METALLURGY</subject><subject>NON-METALLIC ELEMENTS</subject><subject>PERFORMING OPERATIONS</subject><subject>PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL</subject><subject>SEPARATION</subject><subject>THEIR RELEVANT APPARATUS</subject><subject>TRANSPORTING</subject><fulltext>true</fulltext><rsrctype>patent</rsrctype><creationdate>2011</creationdate><recordtype>patent</recordtype><sourceid>EVB</sourceid><recordid>eNqNyrEKwjAQANAsDqL-w_2AQ1uKOIbkYg5sLuTSOpYicSpaqP-Pi-5Ob3lbxR1mzxZ0sGBxIIPgOEFMbFCEwgVuWjKC9Nfo-0QGtCEr4BJ3ECgnnYnD76Ps1eYxzWs5fN0pcJiNP5blNZZ1me7lWd4jxro-t82p1VXzR_kA8cEukg</recordid><startdate>20110316</startdate><enddate>20110316</enddate><creator>DICHTL, GOTTFRIED</creator><creator>STEEG, HARALD</creator><scope>EVB</scope></search><sort><creationdate>20110316</creationdate><title>METHOD AND DEVICE FOR PROCESSING WASTE SULPHURIC ACIDS FROM NITRATION PROCESSES</title><author>DICHTL, GOTTFRIED ; STEEG, HARALD</author></sort><facets><frbrtype>5</frbrtype><frbrgroupid>cdi_FETCH-epo_espacenet_EP2295375A13</frbrgroupid><rsrctype>patents</rsrctype><prefilter>patents</prefilter><language>eng ; fre ; ger</language><creationdate>2011</creationdate><topic>CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOIDCHEMISTRY</topic><topic>CHEMISTRY</topic><topic>COMPOUNDS THEREOF</topic><topic>INORGANIC CHEMISTRY</topic><topic>METALLURGY</topic><topic>NON-METALLIC ELEMENTS</topic><topic>PERFORMING OPERATIONS</topic><topic>PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL</topic><topic>SEPARATION</topic><topic>THEIR RELEVANT APPARATUS</topic><topic>TRANSPORTING</topic><toplevel>online_resources</toplevel><creatorcontrib>DICHTL, GOTTFRIED</creatorcontrib><creatorcontrib>STEEG, HARALD</creatorcontrib><collection>esp@cenet</collection></facets><delivery><delcategory>Remote Search Resource</delcategory><fulltext>fulltext_linktorsrc</fulltext></delivery><addata><au>DICHTL, GOTTFRIED</au><au>STEEG, HARALD</au><format>patent</format><genre>patent</genre><ristype>GEN</ristype><title>METHOD AND DEVICE FOR PROCESSING WASTE SULPHURIC ACIDS FROM NITRATION PROCESSES</title><date>2011-03-16</date><risdate>2011</risdate><abstract>Processing waste acid obtained from nitroaromatics production, preferably dinitrotoluene- or trinitrotoluene production, comprises: adding a pre-heated waste acid comprising sulfuric acid, water, nitric acid, nitrosylsulfuric acid and nitro-organics, into a stripping column in a counter-flow to the steam obtained from the bottom of the stripping column by heating a pre-concentrated sulfuric acid; separating nitric acid, optionally nitro-organics and the pre-concentrated sulfuric acid into at least one vapor phase; and processing the obtained nitric acid and the nitro-organics. Processing waste acid obtained from nitroaromatics production, preferably dinitrotoluene- or trinitrotoluene production, under recovery of concentrated and purified sulfuric acid and nitric acid, comprises: (i) adding a pre-heated waste acid comprising sulfuric acid and water (up to 80 wt.%), nitric acid, nitrosylsulfuric acid and nitro-organics, preferably dinitrotoluene and mononitrotoluene, into a stripping column in a counter-flow to the steam, which is obtained from the bottom of the stripping column by heating a pre-concentrated sulfuric acid in a first phase; (ii) separating nitric acid, optionally nitro-organics and the pre-concentrated sulfuric acid into at least one vapor phase; and (iii) supplying the obtained pre-concentrated sulfuric acid from the bottom of the stripping column for further purification to separate the highly concentrated nitro-organics in a first downstream stage, and processing nitric acid obtained from the nitric acid vapor phase, and the nitro-organics including the nitro-organics obtained during the further purification and concentration of the pre-concentrated sulfuric acid, and returning back to the nitration process in a second downstream stage. The step (i) comprises: adding the pre-heated waste acid into the stripping column for stripping in the counter-flow to the steam obtained from the pre-concentrated sulfuric acid in concentrating the stripping steam containing nitric acid in the counter-flow to the purified and optionally fresh concentrated sulfuric acid (75-97 wt.%, preferably 80-96 wt.%); and condensing the nitric acid vapors obtained from the top of the column of the first stage, and thus directly obtaining a highly concentrated form of nitric acid for returning back to the nitration process. An independent claim is also included for a device for performing the above method comprising: a first stripping column (K1) with a feeding line for the processed waste acid, an associated evaporator for obtaining the pre-concentrated sulfuric acid and a discharging for the nitric acid containing vapor phase; an additional stripping column (K2) with an associated evaporator for producing a purified sulfuric acid and at least one additional evaporator for highly concentrating the purified sulfuric acid; heat exchanger condensers for vapor phases, which are obtained as top products from the stripping columns and the evaporators; optionally a washing column for washing of nitrogen-containing gases; required piping for feeding the starting materials, transporting, distributing and discharging vapor phase, liquid phase, processing products and waste gases obtained as processing streams; and required heating-, cooling- and pressure control equipments. The first stripping column is provided with a feeding line for a highly concentrated purified sulfuric acid, which is produced during the processing of the waste acid.
Verfahren zur Aufarbeitung von Abfallsäure aus Verfahren der Herstellung von Nitroaromaten, insbesondere der Herstellung von Dinitrotoluol (DNT) oder auch Trinitrotouol (TNT), unter Rückgewinnung von aufkonzentrierter und aufgereinigter Schwefelsäure und Salpetersäure, bei dem man in einer ersten Stufe die Abfallsäure in einer Strippkolonne im Gegenstrom zu Wasserdampf aus dem Sumpf der Strippkolonne in mindestens eine dampfförmige Phase, die Salpetersäure sowie gegebenenfalls Nitroorganika enthält, sowie eine vorkonzentrierte Schwefelsäure auftrennt, und man die dampfförmige Phase und die vorkonzentrierte Schwefelsäure in nachgeschalteten Verfahrensstufen kondensiert und/oder aufarbeitet, wobei man in der ersten Stufe des Verfahrens erfindungsgemäß zusätzlich zum Strippen eine Aufkonzentrierung der im Strippdampf enthaltenen Salpetersäure in Gegenwart zusätzlicher konzentrierter Schwefelsäure durchführt, so dass man direkt in der ersten Stufe Salpetersäure in einer für eine Rückführung in das Nitrierverfahren geeigneten hochkonzentrierten Form gewinnt.</abstract><oa>free_for_read</oa></addata></record> |
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| subjects | CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOIDCHEMISTRY CHEMISTRY COMPOUNDS THEREOF INORGANIC CHEMISTRY METALLURGY NON-METALLIC ELEMENTS PERFORMING OPERATIONS PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL SEPARATION THEIR RELEVANT APPARATUS TRANSPORTING |
| title | METHOD AND DEVICE FOR PROCESSING WASTE SULPHURIC ACIDS FROM NITRATION PROCESSES |
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