US2199942A - Process for producing nitrogen trichloride - Google Patents

Process for producing nitrogen trichloride Download PDF

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Publication number
US2199942A
US2199942A US149787A US14978737A US2199942A US 2199942 A US2199942 A US 2199942A US 149787 A US149787 A US 149787A US 14978737 A US14978737 A US 14978737A US 2199942 A US2199942 A US 2199942A
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United States
Prior art keywords
electrolyte
nitrogen trichloride
acid
solution
electrolysis
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Expired - Lifetime
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US149787A
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English (en)
Inventor
Staudt Erich
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Ind Mij Nv Deventer
NAAMLOOZE VENNOOTSCHAP INDUSTRIEELE VOORHEEN NOURY and VAN DER LANDE Mij
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Ind Mij Nv Deventer
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C65/00—Compounds having carboxyl groups bound to carbon atoms of six—membered aromatic rings and containing any of the groups OH, O—metal, —CHO, keto, ether, groups, groups, or groups
    • C07C65/01—Compounds having carboxyl groups bound to carbon atoms of six—membered aromatic rings and containing any of the groups OH, O—metal, —CHO, keto, ether, groups, groups, or groups containing hydroxy or O-metal groups
    • C07C65/03—Compounds having carboxyl groups bound to carbon atoms of six—membered aromatic rings and containing any of the groups OH, O—metal, —CHO, keto, ether, groups, groups, or groups containing hydroxy or O-metal groups monocyclic and having all hydroxy or O-metal groups bound to the ring
    • C07C65/05—Compounds having carboxyl groups bound to carbon atoms of six—membered aromatic rings and containing any of the groups OH, O—metal, —CHO, keto, ether, groups, groups, or groups containing hydroxy or O-metal groups monocyclic and having all hydroxy or O-metal groups bound to the ring o-Hydroxy carboxylic acids
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
    • C07F1/00—Compounds containing elements of Groups 1 or 11 of the Periodic Table
    • C07F1/005—Compounds containing elements of Groups 1 or 11 of the Periodic Table without C-Metal linkages
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B1/00—Electrolytic production of inorganic compounds or non-metals
    • C25B1/01—Products
    • C25B1/24—Halogens or compounds thereof
    • C25B1/26—Chlorine; Compounds thereof

Definitions

  • hydrochloric acid as well ⁇ as other acids, may be added to the ammonium chloride solution, or other solution containing ammonium and chloride ions, to impart to the said solutions an acid, reaction, and that the quantity ⁇ of hydrochloric acid or other acid that is used per gram-molecule of ammonium chloride may fluctuate between broad limits, e. g., both with one-tenth and 2 gram-equivalents of acid per gram-molecule of ammonium chloride, good results have been obtained.
  • nitrogen trichloride is removed from the electrolyte by passing or blowing air or other gas through the electrolyte in the cell during electrolysis, or suction or vacuum is applied to the cell to produce a low or n decreased pressure of gas over the electrolyte whereby, in the latter instance also, the nitrogen trichloride is caused to escape from the electrolyte and enters the gases which are sucked or aspirated from the cell-by the suction apparatus or other apparatus 'producing the vacuum or partial vacuum.
  • the nitrogen trichloride pre- 40 pared in this way can be used with advantage for improving the color and the baking quality of our, as well as for maturing our.
  • the devices and apparatuses for the preparation of nitrogen trichloride in the electrolytic way described must accordingly be mounted in our mills when the nitrogen trichloride is usedfor the treatment of flour. Since the production of flour is, as a rule,
  • the electrochemical preparation of' nitrogen trichloride for the treatment of flour should preferably take place in such a way that it can be continued for a long period of time without interruption and without supervision and attendance being necessary.
  • the concentration of the ammonium ions is of importance and this concentration must be as high as possible in order to iet the reaction take place to the right.
  • a concentrated ammonium chloride solution for example, a water solution of ammonium chloride containing grams of ammonium chloride per litre, but the upper limit of the concentration is fixed by the' solubility of ammonium chloride under the circumstances prevailing in the electrolyte.
  • the ammonium chloride in the electrolyte may be wholly or'partly substituted by another ammonium salt, provided that a suiciently high chloride ion concentration is. provided in some other way.
  • a further measure that may be taken in order to attain the object contemplated by the present invention is the provision of a large volume of electrolyte.
  • the best measure for the volume of electrolyte is the volume of electrolyte per square centimeter of active electrode surface. Dependent on the material that is used for the electrodesY this volume may lie at various values.
  • the degree of acidity of h By active surface of electrodes is meant the total surface of both positiva and negative electrodes that-is taking part in the charging and discharging of ions during electrolysis. ⁇ y
  • Another manner of 4influencing theV degree of electrolyte consists in the appropriate choice oi the quantity of air or of the other gas that is blown through the electrolyte during the elecdecomposition of the nitrogen trichloride accordj lng to the present invention, and accordingly for increasing the amount of available acid in the' trolysis according to my above mentioned application in order to eliminate the nitrogen trichloride. formed.
  • the iniiuence of the quantity of air is such that in case of a too small supply of air, the degree o f acidity of the electrolyte will rise because the period'of contact of the nitrogen trichloride with the electrolyte is too long in this case. If, on the contrary, the quantity of air is too large the time of contact ofthe nitrogen trichloride with the' electrolyte will be too small and the degree of acidity of the electrolyte will fall. .It was found that per 100 litres of electrolyte a current of 30-300 litres of air or other gas (measured at 15 C. and 760 mm. pressure) per minute gives the best results. It is, however, necessary to determine by some preliminary tests what quantity of air or other gas must be used inea certain case.-
  • the direction of movement of the air or gas in" the electrolyte is of importance.
  • the air may be given such a movement through the electrolyzing cell or electrolyte that the nitrogen trichloride formed remains in contact with the electrolyte for the required time prior to escaping. By this contact the above mentioned reaction of decomposition may take'place to the desired ex-r tent.
  • the air or other gas used ac- 'cording to the present invention serves also as a means for eliminating the nitrogen trichloride formed from the electrolyte and as a stirring agent for keeping the composition of the ,electrolyte unifor-m. ⁇
  • the stirring movement of theair or other gas may be made such by an appropriate choice of the method of introduction. that the nitrogen trichloride formed at the electrodes, prior to leaving the liquid,'is ⁇ carried away by the current of air and is further brought into contact with the electrolyte.
  • Figures 1, 2 and 4 respectively represent vertical cross sections of three different electrolyzing cells yand Figure 3 represents a top plan view of another electrolyzing cell.
  • the air or gas may be blown into thel electrolytic'cell container I at the bottom, inthe neighborhood of the sidewalls, through perforated pipes 2 and 3,
  • the numeral II indicates the container of the electrolytic cell.
  • Theair is blown into the cell at the bottom, near or at the middle, through a perforated pipe I2, and two sets of electrodes Il and I5 may be employed, one set being positioned near one side of the electrolytic cell and the other set being positioned near the opposite side of the electrolytic cell.
  • 'I'he air orgas introduced causes the contents oi' the cell to be circulated as indicated, by the broken lines I6 and arrow heads I1.
  • the nitrogen trichloride formed at the electrodes is brought into contact with the electrolyte by the air or other gas.
  • Figure 3 illustrates another manner of carryingout the process according to which the electrolyte is'given a' horizontalv rotating movement in a cell container 2
  • 'I'he electrodes in Figure 3 are designated by the numerals 24 and 25, and the move-- ment of the liquid contents of the cell isindicated by broken line 26 and arrow heads 21.
  • the movement of air in the liquid may be caused to ⁇ take place in the desired manner, and theshape of the electrolyzing cell may be chosen to contribute to obtaining the desired movement oi' air or electrolyte.
  • This manner of practicing the ini vention is illustrated in Figure 4.
  • is divided into two compartments of substantially equal volume by means of the partition 38, below which is positioned the perforated pipe 32 from which air is discharged along each side of the partition.
  • Two sets o f electrodes 34 and 35 are provided, one set being placed near one side of the cell container and the other set being placed near the opposite side oi the cell container, there being one set of electrodes, as shown in the drawing, in each compartment of the cell.
  • the air introduced from pipe 32 causes the contents of each compartment of the cell to be circulated as indicated by the broken lines 36 and arrow heads 31.
  • a combination of the various' methods for moving the liquid in the electrolytic cell with one or more of the other measures described above may be used, if only care is taken that the nitrogen trichloride formed is brought into contact with the electrolyte in such a way that a degree of decomposition takes place at which the degree of acidity oi the electrolyte remains constant ,or nearly constant. It is also to be understood that two or more orall of the above described measures for promoting the decomposition of nitrogen trichloride may be used at the same time in connection with the same electrolytic cell for compensating for losses of acid during the production o1 nitrogen trichloride as ⁇ described in my above mentioned application for patent.
  • the loss or consumption of acid produced by the electrolytic action may be compensated or equalled, or even exceeded, according to the amount of nitrogen trichloride that is allowed to be decomposed by the electrolyte with the formation of acid.
  • the initial acid condition of the electrolyte or solution electrolyzed may be produced by the addition of acid. to the electrolyte', it is to be understood that this initial condition may be brought about in any other suitable way, for
  • the initial acid condition may be pro; quizzed by allowing nitrogen trichloride to react withl an electrolyte containing ammonium chloride or ammonium and chloride ions.
  • Process for producing nitrogen trichloride which comprises electrolyzingan aqueous solution containing ammonium and chloride ions in the presence of free acid which imparts to the solution an acidity greater than the acidity of solutions consisting of ammonium chloride dissolved in water, and conducting a gas through the solution during the electrolysis thereof to remove nitrogen trichloride, said gas being oi such a through vthe solution nature that in its passage through the solution nitrogen trichloride is carried out o!

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
US149787A 1936-06-30 1937-06-22 Process for producing nitrogen trichloride Expired - Lifetime US2199942A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
NL494188X 1936-06-30

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US2199942A true US2199942A (en) 1940-05-07

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US (1) US2199942A (pl)
GB (1) GB494188A (pl)
NL (1) NL75730C (pl)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4098668A (en) * 1974-08-21 1978-07-04 Continental Copper & Steel Industries, Inc. Electrolyte metal extraction

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4098668A (en) * 1974-08-21 1978-07-04 Continental Copper & Steel Industries, Inc. Electrolyte metal extraction

Also Published As

Publication number Publication date
GB494188A (en) 1938-10-21
NL75730C (pl)

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