US3028316A - Process for working up of dilute aqueous hydrazine solutions - Google Patents

Process for working up of dilute aqueous hydrazine solutions Download PDF

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Publication number
US3028316A
US3028316A US751543A US75154358A US3028316A US 3028316 A US3028316 A US 3028316A US 751543 A US751543 A US 751543A US 75154358 A US75154358 A US 75154358A US 3028316 A US3028316 A US 3028316A
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United States
Prior art keywords
acetone
hydrazine
solution
distilling
distillation
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Expired - Lifetime
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US751543A
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English (en)
Inventor
Rahlfs Erich
Thraum Werner
Henrich Gunter
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Bayer AG
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Bayer AG
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Publication of US3028316A publication Critical patent/US3028316A/en
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C251/00—Compounds containing nitrogen atoms doubly-bound to a carbon skeleton
    • C07C251/72—Hydrazones
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/02—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in boilers or stills
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B21/00—Nitrogen; Compounds thereof
    • C01B21/082—Compounds containing nitrogen and non-metals and optionally metals
    • C01B21/16—Hydrazine; Salts thereof

Definitions

  • hydrazine hydrate from dilute aqueous solutions such as are obtained for example by Raschig synthesis is very complicated and, in addition, involves considerable expense. In order to reduce the cost, it would be possible to make use of the fact that, by distilling aqueous hydrazine solutions in the presence of suitable quantities of acetone, it is possible to obtain distillate fractions the hydrazine content of which is greater than that of the undistilled solution.
  • the present invention is concerned with a process for the preparation of hydrazine hydrate from dilute aqueous solution by distillation with acetone, which process consists in that the components, ie the aqueous hydrazine solution and the acetone, are held for a finite time (approximately minutes) in homogeneous solution in the liquid state prior to distillation, and the addition of acetone and the holding step are repeated in stages during the process as the acetone content of the solution becomes too greatly reduced.
  • the process can be carried out substantially as follows using an apparatus as shown in the accompanying drawing.
  • the charging vessel 1 contains 2% hydrazine hydrate solution containing 50 g./l. of acetone, this solution being held in the vessel in a homogeneous condition for at least 10 minutes before commencing operations.
  • the solution is supplied continuously at a rate of 34 litres per hour to the upper fractionating column 2.
  • the holding vessels 3a and 3b which are provided so that the solution may remain therein for a period of time, are constantly charged with acetone from the storage vessels 7a and 7b provided for this purpose, the vessel 3a being charged at the rate of 20 g. per hour and the vessel 3b at the rate of 7 g. per hour of acetone.
  • Such an amount of heat is supplied to the sump flask 6 by gas flame heating that about 500-600 cc. of distillate per hour-cooled in cooling device 4-are received in the distillate receiver 5.
  • gas flame heating that about 500-600 cc. of distillate per hour-cooled in cooling device 4-are received in the distillate receiver 5.
  • liquid is constantly ice withdrawn from the sump flask 6 at such a rate that the flask is always half full.
  • the sump discharge is practically free from hydrazine and acetone, while these components are found in correspondingly concentrated form in the distillate.
  • Process for working up dilute aqueous hydrazine solutions by distillation with acetone which comprises the steps of maintaining the aqueous hydrazine solution and the acetone in homogeneous solution in the liquid state until a substantial amount of a hydrazine-acetone compound is formed, thereafter in a vertical distilling zone distilling off the said hydrazine-acetone compound, adding acetone to the undistilled liquid during the distilling at a point along the zone, and repeating the steps of maintaining the aqueous hydrazine solution and the acetone in homogeneous solution in the liquid state until a substantial amount of a hydrazine-acetone compound is formed, distilling ott' the said hydrazine-acetone compound and adding acetone to the undistilled liquid at least one more time at a second point along the zone.
  • Process for working up dilute aqueous hydrazine solutions by distillation with acetone which comprises the steps of maintaining the aqueous hydrazine solution and the acetone in homogeneous solution in the liquid state for about 10 minutes until a substantial amount of a hydrazine-acetone compound is formed, thereafter in a vertical distilling zone distilling off the said hydrazineacetone compound, adding acetone to the undistilled liquid during the distilling at a point along the zone, and repeating the steps of maintaining the aqueous hydrazine solution and the acetone in homogeneous solution in the liquid state until a substantial amount of a hydrazineacetone compound is formed, distilling off the said hydrazine-acetone compound and adding acetone to the undistilled liquid at least one more time at a second point along the zone.
  • the improvement which comprises holding a mixture of aqueous hydrazine solution and acetone for a predetermined period of time in homogeneous solution in the liquid state prior to distillation thereof, passing said mixture of aqueous hydrazine solution and acetone into the upper end portion of a distillation zone, distilling off hydrazine and acetone, adding acetone to the distillation zone at a multiple number of points spaced vertically along said zone to thereby form a series of liquid pockets at said points, holding the aqueous hydrazine solution and the acetone in homogeneous solution in the liquid state at each of said points, distilling off acetone and hydrazine following said holding, and collecting a hydrazine enriched distillate and a hydrazine poor fraction from the sump for said distillation zone and maintaining the volume in said sump substantially constant throughout said distillation.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
US751543A 1957-07-31 1958-07-28 Process for working up of dilute aqueous hydrazine solutions Expired - Lifetime US3028316A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DEF23648A DE1048884B (de) 1957-07-31 1957-07-31 Verfahren zur Aufbereitung von verduennten waessrigen Hydrazinloesungen

Publications (1)

Publication Number Publication Date
US3028316A true US3028316A (en) 1962-04-03

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US751543A Expired - Lifetime US3028316A (en) 1957-07-31 1958-07-28 Process for working up of dilute aqueous hydrazine solutions

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US (1) US3028316A (US07922777-20110412-C00004.png)
BE (1) BE569859A (US07922777-20110412-C00004.png)
CH (1) CH373360A (US07922777-20110412-C00004.png)
DE (1) DE1048884B (US07922777-20110412-C00004.png)
FR (1) FR1201027A (US07922777-20110412-C00004.png)
GB (1) GB839414A (US07922777-20110412-C00004.png)
NL (2) NL105668C (US07922777-20110412-C00004.png)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3485582A (en) * 1966-12-17 1969-12-23 Bayer Ag Process for the preparation of hydrazine from methylethyl- or diethylketazine
US3493469A (en) * 1966-03-12 1970-02-03 Fisons Ind Chem Ltd Distillation and decanting system for separating components
US3494737A (en) * 1966-12-17 1970-02-10 Bayer Ag Process for the preparation of hydrazine by tray column fractionation
US3520367A (en) * 1968-10-28 1970-07-14 Phillips Petroleum Co Method of producing oil using steam condensate trapped in storage zone

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
NL1007442C2 (nl) * 1997-11-04 1998-12-07 Josephus Johannes Petrus Maria Batch-Continue tegenstroomapparatuur met superieure performance.

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2537791A (en) * 1946-08-17 1951-01-09 Edwal Lab Inc Method for production of hydrazine and/or hydrazine hydrate
US2698286A (en) * 1949-05-31 1954-12-28 Battelle Development Corp Dehydration of hydrazine solutions
US2733195A (en) * 1954-09-01 1956-01-31 Process for concentrating aqueous

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2537791A (en) * 1946-08-17 1951-01-09 Edwal Lab Inc Method for production of hydrazine and/or hydrazine hydrate
US2698286A (en) * 1949-05-31 1954-12-28 Battelle Development Corp Dehydration of hydrazine solutions
US2733195A (en) * 1954-09-01 1956-01-31 Process for concentrating aqueous

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3493469A (en) * 1966-03-12 1970-02-03 Fisons Ind Chem Ltd Distillation and decanting system for separating components
US3485582A (en) * 1966-12-17 1969-12-23 Bayer Ag Process for the preparation of hydrazine from methylethyl- or diethylketazine
US3494737A (en) * 1966-12-17 1970-02-10 Bayer Ag Process for the preparation of hydrazine by tray column fractionation
US3520367A (en) * 1968-10-28 1970-07-14 Phillips Petroleum Co Method of producing oil using steam condensate trapped in storage zone

Also Published As

Publication number Publication date
FR1201027A (fr) 1959-12-28
DE1048884B (de) 1959-01-22
GB839414A (en) 1960-06-29
CH373360A (de) 1963-11-30
NL105668C (US07922777-20110412-C00004.png)
BE569859A (US07922777-20110412-C00004.png)
NL229958A (US07922777-20110412-C00004.png)

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