CA2239253A1 - Preparation of aqueous solutions of free hydroxylamine - Google Patents

Preparation of aqueous solutions of free hydroxylamine

Info

Publication number
CA2239253A1
CA2239253A1 CA002239253A CA2239253A CA2239253A1 CA 2239253 A1 CA2239253 A1 CA 2239253A1 CA 002239253 A CA002239253 A CA 002239253A CA 2239253 A CA2239253 A CA 2239253A CA 2239253 A1 CA2239253 A1 CA 2239253A1
Authority
CA
Canada
Prior art keywords
hydroxylamine
preparation
aqueous solutions
free hydroxylamine
solution
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CA002239253A
Other languages
French (fr)
Other versions
CA2239253C (en
Inventor
Otto Watzenberger
Hans-Michael Schneider
Bernd Leutner
Albrecht Wilhelm Friederang
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
BASF SE
BASF Corp
Original Assignee
Individual
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority claimed from US08/688,281 external-priority patent/US5837107A/en
Application filed by Individual filed Critical Individual
Publication of CA2239253A1 publication Critical patent/CA2239253A1/en
Application granted granted Critical
Publication of CA2239253C publication Critical patent/CA2239253C/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

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
    • C01B21/14—Hydroxylamine; Salts thereof
    • C01B21/1409—Preparation
    • C01B21/1445—Preparation of hydoxylamine from its salts
    • 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
    • B01D3/14—Fractional distillation or use of a fractionation or rectification column
    • B01D3/143—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step
    • B01D3/146—Multiple effect distillation
    • 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
    • B01D3/34—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping with one or more auxiliary substances
    • B01D3/38—Steam distillation
    • 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
    • C01B21/14—Hydroxylamine; Salts thereof
    • C01B21/1463—Concentration
    • 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
    • C01B21/14—Hydroxylamine; Salts thereof
    • C01B21/1472—Separation

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
  • Compounds Of Unknown Constitution (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
  • Extraction Or Liquid Replacement (AREA)
  • Gas Separation By Absorption (AREA)
  • Seasonings (AREA)
  • Disintegrating Or Milling (AREA)

Abstract

A process is disclosed for producing an aqueous solution of free hydroxylamine. A solution obtained by treating an hydroxylammonium salt with a base is treated with water or water vapour at a temperature ? 80 C, so as to separate the solution into an aqueous hydroxylamine fraction and a salt fraction. This process is soft and easy to implement on a Large scale. The risk of decomposition is minimised because of the low thermal stresses, the low hydroxylamine concentration and the short dwelling time during implementation of the process.
CA002239253A 1995-12-20 1996-12-20 Preparation of aqueous solutions of free hydroxylamine Expired - Lifetime CA2239253C (en)

Applications Claiming Priority (5)

Application Number Priority Date Filing Date Title
DE19547758.8 1995-12-20
DE19547758 1995-12-20
US08/688,281 US5837107A (en) 1995-12-20 1996-07-29 Process for production of aqueous solutions of free hydroxylamine
US08/688,281 1996-07-29
PCT/EP1996/005773 WO1997022551A1 (en) 1995-12-20 1996-12-20 Process for producing aqueous solutions of free hydroxylamine

Publications (2)

Publication Number Publication Date
CA2239253A1 true CA2239253A1 (en) 1997-06-26
CA2239253C CA2239253C (en) 2006-01-31

Family

ID=26021480

Family Applications (2)

Application Number Title Priority Date Filing Date
CA002239791A Expired - Lifetime CA2239791C (en) 1995-12-20 1996-12-20 Separation of middle boilers from a mixture of low, middle and high boilers
CA002239253A Expired - Lifetime CA2239253C (en) 1995-12-20 1996-12-20 Preparation of aqueous solutions of free hydroxylamine

Family Applications Before (1)

Application Number Title Priority Date Filing Date
CA002239791A Expired - Lifetime CA2239791C (en) 1995-12-20 1996-12-20 Separation of middle boilers from a mixture of low, middle and high boilers

Country Status (16)

Country Link
EP (2) EP0868399B1 (en)
JP (2) JP2000505033A (en)
CN (2) CN1104376C (en)
AT (1) ATE222565T1 (en)
AU (2) AU704998B2 (en)
BR (2) BR9612053A (en)
CA (2) CA2239791C (en)
DE (2) DE59609580D1 (en)
DK (1) DK0868399T3 (en)
ES (2) ES2177828T3 (en)
HR (1) HRP960601B1 (en)
IL (2) IL124737A (en)
NO (2) NO319309B1 (en)
PT (1) PT868399E (en)
TR (2) TR199801154T2 (en)
WO (2) WO1997022550A1 (en)

Families Citing this family (29)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE19725851A1 (en) * 1997-06-18 1998-12-24 Basf Ag Process for the preparation of high-purity, aqueous hydroxylamine solutions
US5788946A (en) * 1997-07-16 1998-08-04 Ashland Inc. Purification of hydroxylamine
DE19733681A1 (en) 1997-08-04 1999-02-11 Basf Ag Process for the preparation of an aqueous solution of free hydroxylamine
DE19806578A1 (en) * 1998-02-17 1999-08-19 Basf Ag Production of aqueous hydroxylamine solution containing essentially no metal ions, used in electronics industry
US6235162B1 (en) 1998-05-28 2001-05-22 Sachem, Inc. Ultrapure hydroxylamine compound solutions and process of making same
DE19936594A1 (en) 1999-08-04 2001-02-08 Basf Ag Process for the preparation of high-purity stabilized hydroxylamine solutions
DE10004818A1 (en) * 2000-02-04 2001-08-09 Basf Ag Process for recycling stripper solutions containing hydroxylamine
JP3503115B2 (en) * 2000-06-27 2004-03-02 東レ・ファインケミカル株式会社 Method for producing free hydroxylamine aqueous solution
DE10037774A1 (en) * 2000-08-03 2002-02-14 Bayer Ag Method and device for obtaining organic substances from a gas mixture containing these substances
DE10134389A1 (en) * 2001-07-04 2003-01-16 Basf Ag Process for the preparation of a salt-free, aqueous hydroxylamine solution
DE10131787A1 (en) 2001-07-04 2003-01-16 Basf Ag Process for the preparation of a salt-free, aqueous hydroxylamine solution
DE10131788A1 (en) 2001-07-04 2003-01-16 Basf Ag Process for the preparation of a salt-free, aqueous hydroxylamine solution
DE10314492B4 (en) * 2003-03-27 2008-10-16 Domo Caproleuna Gmbh Process for the preparation of an aqueous solution of hydroxylamine
JP4578885B2 (en) * 2003-08-13 2010-11-10 昭和電工株式会社 Method for producing hydroxylamine
EP1663862A2 (en) 2003-08-13 2006-06-07 Showa Denko K.K. Process for producing hydroxylamine
TW200508176A (en) * 2003-08-13 2005-03-01 Showa Denko Kk Process for producing hydroxylamine
FR2860223B1 (en) * 2003-09-26 2005-12-16 Jean Pierre Schirmann PROCESS FOR PRODUCING AQUEOUS HYDROXYLAMINE BASE SOLUTIONS
US7396519B2 (en) 2004-01-26 2008-07-08 San Fu Chemical Company, Ltd. Preparation of a high purity and high concentration hydroxylamine free base
JP2005239702A (en) * 2004-01-28 2005-09-08 Showa Denko Kk Method for producing hydroxylamine
JP2006056742A (en) * 2004-08-19 2006-03-02 Hosoya Fireworks Co Ltd Method for producing aqueous solution of hydroxylamine nitrate
JP4578988B2 (en) * 2005-01-21 2010-11-10 昭和電工株式会社 Method for producing hydroxylamine
JP4578999B2 (en) * 2005-02-10 2010-11-10 昭和電工株式会社 Method for producing hydroxylamine
JP2006219343A (en) * 2005-02-10 2006-08-24 Showa Denko Kk Method for producing hydroxylamine
JP4578998B2 (en) * 2005-02-10 2010-11-10 昭和電工株式会社 Method for producing hydroxylamine
DE102005032430A1 (en) * 2005-07-12 2007-01-25 Bayer Materialscience Ag Process for the preparation of toluenediamine
WO2017204935A1 (en) 2016-05-26 2017-11-30 Exxonmobil Chemical Patents Inc. Production of cyclic imides suitable for oxidation catalysis
WO2017204936A1 (en) 2016-05-26 2017-11-30 Exxonmobil Chemical Patents Inc. Production of cyclic imides suitable for oxidation catalysis
US10584096B2 (en) 2016-10-18 2020-03-10 Exxonmobil Chemical Patents Inc. Cyclic imide slurry compositions
CN108946741B (en) * 2017-05-17 2020-05-12 新特能源股份有限公司 Process method for recovering silicon-containing high-boiling-point substance in polycrystalline silicon cold hydrogenation process and cold hydrogenation process

Family Cites Families (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4111759A (en) * 1976-07-08 1978-09-05 United States Steel Corporation Process for separating ammonia and acid gases from waste waters containing fixed ammonia salts
JPS597313B2 (en) * 1980-02-08 1984-02-17 チツソエンジニアリング株式会社 Alcohol distillation equipment
DE3302525A1 (en) * 1983-01-26 1984-07-26 Basf Ag, 6700 Ludwigshafen DISTILLATION COLUMN FOR THE DISTILLATIVE DISASSEMBLY OF AN INLET PRODUCT MULTIPLE FRACTIONS
DE3528463A1 (en) * 1985-08-08 1987-02-19 Basf Ag Process for the preparation of aqueous solutions of free hydroxylamine
DE3814255A1 (en) * 1988-04-27 1989-11-09 Metallgesellschaft Ag DEVICE FOR DESODORING ORGANIC LIQUIDS
US5266290A (en) * 1992-07-10 1993-11-30 Thiokol Corporation Process for making high purity hydroxylammonium nitrate
DE4324410C1 (en) * 1993-07-21 1994-08-04 Enviro Consult Ingenieurgesell Removing ammonium from process water in effluent water treatment units
US5385646A (en) * 1993-09-03 1995-01-31 Farmland Industries, Inc. Method of treating chemical process effluent

Also Published As

Publication number Publication date
IL124737A (en) 2001-06-14
DE59609580D1 (en) 2002-09-26
CN1104376C (en) 2003-04-02
BR9612053A (en) 1999-02-23
TR199801163T2 (en) 1998-09-21
WO1997022550A1 (en) 1997-06-26
CA2239253C (en) 2006-01-31
IL124737A0 (en) 1999-01-26
HRP960601A2 (en) 1998-04-30
NO319309B1 (en) 2005-07-11
WO1997022551A1 (en) 1997-06-26
NO982849L (en) 1998-08-19
AU1304097A (en) 1997-07-14
ES2181933T3 (en) 2003-03-01
NO982847D0 (en) 1998-06-19
NO322631B1 (en) 2006-11-06
JP4376969B2 (en) 2009-12-02
AU707648B2 (en) 1999-07-15
AU704998B2 (en) 1999-05-13
CA2239791C (en) 2006-01-31
CA2239791A1 (en) 1997-06-26
MX9804788A (en) 1998-10-31
TR199801154T2 (en) 1998-12-21
IL124739A0 (en) 1999-01-26
ES2177828T3 (en) 2002-12-16
NO982847L (en) 1998-08-17
BR9612073A (en) 1999-02-17
NO982849D0 (en) 1998-06-19
EP0868398A1 (en) 1998-10-07
DK0868399T3 (en) 2002-10-07
JP2000505033A (en) 2000-04-25
IL124739A (en) 2001-06-14
CN1209108A (en) 1999-02-24
EP0868398B1 (en) 2002-05-22
DE59609239D1 (en) 2002-06-27
HRP960601B1 (en) 2001-12-31
EP0868399B1 (en) 2002-08-21
JP2000510385A (en) 2000-08-15
CN1102531C (en) 2003-03-05
PT868399E (en) 2003-01-31
AU1303997A (en) 1997-07-14
ATE222565T1 (en) 2002-09-15
CN1205677A (en) 1999-01-20
EP0868399A1 (en) 1998-10-07

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Effective date: 20161220