Classifications

• • 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
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B04—CENTRIFUGAL APPARATUS OR MACHINES FOR CARRYING-OUT PHYSICAL OR CHEMICAL PROCESSES
  • B04C—APPARATUS USING FREE VORTEX FLOW, e.g. CYCLONES
  • B04C5/00—Apparatus in which the axial direction of the vortex is reversed
  • B04C5/20—Apparatus in which the axial direction of the vortex is reversed with heating or cooling, e.g. quenching, means

Definitions

• This invention relates to a method of producing hydrazine hydrate, and more specifically is concerned with a method of preparing hydrazine hydrate from ketazines and hydrazones, particularly from dimethyl lietazine and acetone hydrazone.
• This hydrazine salt can, moreover, be worked up by various methods to hydrazine hydrate. Processes are also known, the object of which is to obviate this tedious and costly roundabout method by way of the salts and which permit the hydrate to be produced directly from ketazine solutions. However, all these proposals have basic defects which have prevented them from being carried out industrially.
• the method of the present invention comprises efiecting a decomposition of the dimethyl ketazine and the acetone hydrazone into acetone and hydraz ne by fractionating distillation at excess pressure and at a sump-temperature range between 100 to 250 C., said excess pressure being of about 1 to about 50 atmospheres.
• the decomposition of the ketazine and the hydrazone is effected in an aqueous medium containing about 19 to 25 percent of acetone and about 9 to 12 percent of hydrazine hydrate. Still more particularly the temperature range is between 130 to 210 C. and the excess pressure is from about to 15 atmospheres.
• ketazines and hydrazones are dimethyl ketazine and acetone hydrazone, represented by the following formulae:
• the present invention provides a new and improved method of producing hydrazine hydrate in an economic manner, said method has the advantage of simplicity and avoids the necessity for using complicated apparatus techniques.
• Example 1 An aqueous solution of dimethyl-ketazine containing 9% hydrazine hydrate and 21.9% acetone is fractionated continuously in a column provided with filler bodies at a pressure of 4 atm. The run-in amounts to litres per hour. From the top of the column there have been withdrawn 18 litres per hour of a solution containing 91% acetone and 2.3% of hydrazine hydrate. The sumptemperature amounts to 145 C. The analytical result of the sump-running off shows 10.8% of hydrazine hydrate and 0.8% of acetone.
• Example 3 An aqueous solution of dimethyl-ketazine containing 24.5% of acetone and 10.5% of hydrazine hydrate is fractionated continuously in a column having filler bodies at a pressure of 20 atm. and at a sump-temperature of 216 C. The run-in amounts to 125 litres per hour. At the top of the column there are withdrawn 30 litres per hour of a solution containing 96% of acetone and 1.5% of hydrazine hydrate. The composition of the sumprunning 011 is 0.1% of acetone and 12% of hydrazine hydrate.
• Example 4 An aqueous solution of acetone hydrazone containing 10.4% of acetone and 11.1% of hydrazine hydrate is fractionated in a column with filler bodies at a pressure of 4 atm. and at a sump-temperature of 146 C.
• the run-in amounts to 100 litres per hour and the run oli to 10.8 litres per hour, containing 93.0% of acetone and 1.8% of hydrazine hydrate.
• the sump-running oft contains 0.3% of acetone and 12.1% of hydrazine hydrate.
• Example 5 shows the following compounds: 0.1% of acetone and 14.3 of hydrazine hydrate.
• A'process for the production of hydrazine hydrate which comprises decomposing a hydrazine compound selected from the group consisting "of dimethyl ketazine and acetone hydrazine in the form of an aqueous solution ":7 thereof by fractionally distilling such'a solution under a pressure of between 2 atmospheres and 50. atmospheres and at a sump temperature ranging between 120. and.
• a process .forthe'production of hydrazine hydrate which comprises decomposing acetone hydrazoue in the 5.
• a process for the'productio'n of hydrazine hydrate I Q which comprisesdecomposing dimethylketazine in the form ofan aqueous solution thereofwhich solution addi ltionally contains 24.5% of acetone and 10.5% ofhydrazine hydrate by fractionally distilling such solution under a pressure of 9 atmospheres and at a sump tem-' perature of about 178 C..
• a process for the'production of hydrazine hydrate which comprises decomposingacetone hydrazone in the 'form of an aqueous solution thereof which solution additionally contains 10.4% of acetone and 11.1% ofhyform of an aqueous solution lthereof which solutionu additionally contains 21.0% of acetone and 12.3% Of.' hydrazine hydrate by fractionally distilling such a solution at apressure of 20 atmospheres, and at a sump tem peratureof216 C. e r

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• Chemical & Material Sciences (AREA)
• Organic Chemistry (AREA)
• Inorganic Chemistry (AREA)
• Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

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Citations (1)

• 0
  • NL NL274425D patent/NL274425A/xx unknown
  • NL NL136390D patent/NL136390B/xx unknown
• 1961
  • 1961-02-08 DE DEF33165A patent/DE1130797B/de active Pending
• 1962
  • 1962-01-15 CH CH42962A patent/CH420082A/de unknown
  • 1962-01-23 US US168235A patent/US3189411A/en not_active Expired - Lifetime
  • 1962-02-06 GB GB4541/62A patent/GB952282A/en not_active Expired
  • 1962-02-07 BE BE613588A patent/BE613588A/fr unknown

Patent Citations (1)

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