CS196649B1 - Indication electrode for the potenciometric tracking of the course of the nitrosibstances reduction - Google Patents
Indication electrode for the potenciometric tracking of the course of the nitrosibstances reduction Download PDFInfo
- Publication number
- CS196649B1 CS196649B1 CS750676A CS750676A CS196649B1 CS 196649 B1 CS196649 B1 CS 196649B1 CS 750676 A CS750676 A CS 750676A CS 750676 A CS750676 A CS 750676A CS 196649 B1 CS196649 B1 CS 196649B1
- Authority
- CS
- Czechoslovakia
- Prior art keywords
- electrode
- reduction
- potential
- reaction
- nitro compound
- Prior art date
Links
- 239000003054 catalyst Substances 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 8
- LQNUZADURLCDLV-UHFFFAOYSA-N nitrobenzene Chemical compound [O-][N+](=O)C1=CC=CC=C1 LQNUZADURLCDLV-UHFFFAOYSA-N 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 229910052739 hydrogen Inorganic materials 0.000 claims description 4
- 239000001257 hydrogen Substances 0.000 claims description 4
- 238000012544 monitoring process Methods 0.000 claims description 4
- 150000002828 nitro derivatives Chemical class 0.000 claims description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 3
- 239000007868 Raney catalyst Substances 0.000 claims description 3
- 229910000564 Raney nickel Inorganic materials 0.000 claims description 3
- 239000004020 conductor Substances 0.000 claims description 3
- 239000011521 glass Substances 0.000 claims description 3
- 229910052697 platinum Inorganic materials 0.000 claims description 3
- 238000011946 reduction process Methods 0.000 claims description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 2
- 239000003245 coal Substances 0.000 claims description 2
- 229910052737 gold Inorganic materials 0.000 claims description 2
- 229910002804 graphite Inorganic materials 0.000 claims description 2
- 239000010439 graphite Substances 0.000 claims description 2
- 238000005984 hydrogenation reaction Methods 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 claims description 2
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims 2
- NPXOKRUENSOPAO-UHFFFAOYSA-N Raney nickel Chemical compound [Al].[Ni] NPXOKRUENSOPAO-UHFFFAOYSA-N 0.000 claims 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims 1
- 229910052593 corundum Inorganic materials 0.000 claims 1
- 238000000034 method Methods 0.000 claims 1
- 230000003647 oxidation Effects 0.000 claims 1
- 238000007254 oxidation reaction Methods 0.000 claims 1
- 229910001845 yogo sapphire Inorganic materials 0.000 claims 1
- 239000011541 reaction mixture Substances 0.000 description 6
- 238000006722 reduction reaction Methods 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 150000004982 aromatic amines Chemical class 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000009903 catalytic hydrogenation reaction Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Catalysts (AREA)
Description
Vynález se týká řešení indikační elektrody pro potenciometrická měření, zvláště pro sledování průběhu redukce nitrolátek, k jejichž vedení se používá látek suspendovaných v reakčni směsi.BACKGROUND OF THE INVENTION The present invention relates to a solution for indicating electrodes for potentiometric measurements, in particular for monitoring the progress of the reduction of nitro compounds, for which substances suspended in the reaction mixture are used.
Pro potenciometrická měření se obvykle používají indikační elektrody, jejichž vlastní aktivní , část tvoří jednolitý, popřípadě pórovitý celek o konstantním povrchu, prostorově přesně lokalizovaný.Indication electrodes are usually used for potentiometric measurements, the active part of which consists of a monolithic or porous unit with a constant surface, spatially accurately localized.
V některých případech lze však výhodněji použít pro sledování průběhu chemických redukčních reakcí elektrody podle tohoto vynálezu. Je tomu například v přípa* dech, kdy chemická reakce, jejíž průběh je třeba sledovat, se provádí pomocí suspendovaných částic v reakčni směsi, které vlastní reakci katalýzu jí nebo se jí samy chemicky zúčastňují.However, in some cases, the electrodes of the present invention may be more advantageously used to monitor the progress of chemical reduction reactions. This is the case, for example, where the chemical reaction to be monitored is carried out by means of suspended particles in the reaction mixture which are involved in the catalysis reaction or which are themselves chemically involved.
Indikační elektroda pro potenciometrické sledování průběhu redukce nitrolátek spočívá podle vynálezu v tom, že její aktivní část je tvořena suspendovanými částicemi v měřené kapalině a neaktivní část je tvořena elektrickým vodičem z indiferentního materiálu, například z Pt, Au, skelného grafitu apod.The indicator electrode for the potentiometric monitoring of the nitro-substance reduction process consists in that the active part consists of suspended particles in the measured liquid and the inactive part consists of an electrical conductor of indifferent material, for example Pt, Au, glass graphite and the like.
Na přiloženém výkresu je znázorněno provedení indikační elektrody podle vynálezu. Indikační elektroda 2, 3 obsahuje aktiv2 ní plochu 2, tvořenou přímo suspendovanými částicemi Fe, například katalyzátory Pt čerň, Pt na nosiči, například AI2O3 Pd na nosiči, například uhlí, Raney nikl apod. v reakční nádobě 1, a neaktivní část 3, kterou tvoří přívodní vodič, spojený s potenciometrem 5, se kterým je rovněž spojena srovnávací elektroda 4.The accompanying drawing shows an embodiment of the indicating electrode according to the invention. The indicator electrode 2, 3 comprises an active surface 2 formed by directly suspended Fe particles, for example supported Pt catalysts, supported Pt catalysts, for example Al 2 O 3 Pd supported catalysts, for example coal, Raney nickel and the like in reaction vessel 1, and it forms a lead-in conductor connected to the potentiometer 5, to which the reference electrode 4 is also connected.
Níže uvedené příklady ilustrují provedení redukce za použití elektrody podle vynálezu.The examples below illustrate a reduction using an electrode according to the invention.
Přikladl.He did.
Katalytická hydrogenace nitrobenzenu se provede v uzavřené skleněné reakčni baňce o obsahu 250 ml při laboratorní teplotě a normálním tlaku. Do baňky se napustí 100 ml reakčni směsi, jejíž složení je:The catalytic hydrogenation of nitrobenzene is carried out in a sealed 250 ml glass reaction flask at room temperature and normal pressure. Add 100 ml of the reaction mixture, the composition of which is:
% etylalkoholu,% ethyl alcohol,
0,1 mol/1 KOH, g pasty Raney-nlklu (katalyzátor), a intenzívně se promíchává. Pod hladinu reakční směsi se zavádí vodík rychlostí 20 ml za min. Potenciál indikační suspenzní elektrody (Raney-nikl) je indikován pomocnou Au elektrodou ponořenou do reakčni směsi spolu s referentní elektrodou argentchloridovou. Rozdíl potenciálu obou elektrod je měřen milivoltmetrem. Po nasycení katalyzátoru vodíkem se potenciál suspenzní elektrody ustaví na hodnotě — 1000 ml (proti0.1 mol / l KOH, g of Raney-paste (catalyst), and vigorously stirred. Hydrogen was introduced below the reaction mixture at a rate of 20 ml / min. The potential of the slurry indicating electrode (Raney-nickel) is indicated by an auxiliary Au electrode immersed in the reaction mixture together with a reference chloride electrode. The potential difference between the two electrodes is measured by a millivoltmeter. After saturation of the catalyst with hydrogen, the potential of the suspension electrode is set at -1000 ml (vs
1966 49 ······ 3 argentchloridové elektrodě). Po nadávkování 0,204 g nitrobenzenu v 1 ml etanolu dojde k vzrůstu potenciálu suspenzní elektrody a ustaví se na cca 530 mV. Asi 20 minut před ukončením redukce začíná potenciál klesat a po jejím skončení se ustaví opět na původní hodnotě — 1000 mV. Dosažení této hodnoty indikuje tedy konec redukčního pochodu.1966 49 ······ 3 argent chloride electrode). After dosing 0.204 g of nitrobenzene in 1 ml of ethanol, the potential of the suspension electrode increases and is set to about 530 mV. About 20 minutes before the end of the reduction, the potential begins to decrease and after its completion it returns to its original value - 1000 mV. Reaching this value thus indicates the end of the reduction process.
Přík1 ad 2Example 2
Sledování katalytické tlakové hydrogenace při výrobě aromatických aminůMonitoring of catalytic pressure hydrogenation in production of aromatic amines
Redukce příslušné nitrolátky se provádí v tlakové reakční nádobě 1 vodíkem pomocí niklového katalyzátoru, suspendovaného v reakční směsi. Do této směsi zasahuje indikační elektroda 2, 3 podle vynálezu, přičemž její aktivní část 2 je v tomto případě tvořena přímo . suspendovanými částicemi niklu, který je katalyzátorem použitým pro vlastní vedení redukce. Na jednotlivých čás-The reduction of the respective nitro compound is carried out in the pressure reaction vessel 1 with hydrogen by means of a nickel catalyst suspended in the reaction mixture. The indicator electrode 2, 3 according to the invention intervenes in this mixture, the active part 2 of which is formed directly in this case. suspended nickel particles, which is the catalyst used to conduct the reduction itself. On each part-
Claims (1)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS750676A CS196649B1 (en) | 1976-11-22 | 1976-11-22 | Indication electrode for the potenciometric tracking of the course of the nitrosibstances reduction |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS750676A CS196649B1 (en) | 1976-11-22 | 1976-11-22 | Indication electrode for the potenciometric tracking of the course of the nitrosibstances reduction |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CS196649B1 true CS196649B1 (en) | 1980-03-31 |
Family
ID=5424321
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CS750676A CS196649B1 (en) | 1976-11-22 | 1976-11-22 | Indication electrode for the potenciometric tracking of the course of the nitrosibstances reduction |
Country Status (1)
| Country | Link |
|---|---|
| CS (1) | CS196649B1 (en) |
-
1976
- 1976-11-22 CS CS750676A patent/CS196649B1/en unknown
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