FR2651776B1 - PROCESS FOR THE SYNTHESIS OF MONOMETHYLHYDRAZINE IN AQUEOUS SOLUTION. - Google Patents
PROCESS FOR THE SYNTHESIS OF MONOMETHYLHYDRAZINE IN AQUEOUS SOLUTION.Info
- Publication number
- FR2651776B1 FR2651776B1 FR8911960A FR8911960A FR2651776B1 FR 2651776 B1 FR2651776 B1 FR 2651776B1 FR 8911960 A FR8911960 A FR 8911960A FR 8911960 A FR8911960 A FR 8911960A FR 2651776 B1 FR2651776 B1 FR 2651776B1
- Authority
- FR
- France
- Prior art keywords
- reactor
- pref
- mixt
- medium
- reaction
- 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.)
- Expired - Lifetime
Links
- 238000000034 method Methods 0.000 title abstract 2
- HDZGCSFEDULWCS-UHFFFAOYSA-N monomethylhydrazine Chemical compound CNN HDZGCSFEDULWCS-UHFFFAOYSA-N 0.000 title abstract 2
- 239000007864 aqueous solution Substances 0.000 title 1
- 230000015572 biosynthetic process Effects 0.000 title 1
- 238000003786 synthesis reaction Methods 0.000 title 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 abstract 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 abstract 3
- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 abstract 2
- 239000002585 base Substances 0.000 abstract 2
- WQYVRQLZKVEZGA-UHFFFAOYSA-N hypochlorite Chemical compound Cl[O-] WQYVRQLZKVEZGA-UHFFFAOYSA-N 0.000 abstract 2
- MXDRPNGTQDRKQM-UHFFFAOYSA-N 3-methylpyridazine Chemical compound CC1=CC=CN=N1 MXDRPNGTQDRKQM-UHFFFAOYSA-N 0.000 abstract 1
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 abstract 1
- QDHHCQZDFGDHMP-UHFFFAOYSA-N Chloramine Chemical compound ClN QDHHCQZDFGDHMP-UHFFFAOYSA-N 0.000 abstract 1
- 229910019093 NaOCl Inorganic materials 0.000 abstract 1
- 239000003513 alkali Substances 0.000 abstract 1
- 229910021529 ammonia Inorganic materials 0.000 abstract 1
- 235000019270 ammonium chloride Nutrition 0.000 abstract 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract 1
- 239000012530 fluid Substances 0.000 abstract 1
- 229910000069 nitrogen hydride Inorganic materials 0.000 abstract 1
- 229910052760 oxygen Inorganic materials 0.000 abstract 1
- 239000001301 oxygen Substances 0.000 abstract 1
- 239000000376 reactant Substances 0.000 abstract 1
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 abstract 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C241/00—Preparation of compounds containing chains of nitrogen atoms singly-bound to each other, e.g. hydrazines, triazanes
- C07C241/02—Preparation of hydrazines
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
Prodn. of monomethylhydrazine (I) in aq. soln. comprises reaction of chloramine (II) with a 1 mol excess of MeNH2 (III) for a time D1 in aq. medium and oxygen-free atmos., in the presence of a strong base, pref. NaOH, and working up the mixt. of (I) and volatile by-prods. obtd., pref. by stripping followed by distn., to give a conc. aq. soln. of (I). The novelty is that, before the reaction mixt. is worked up, it is then heated to 30-100 (pref. 70-100) deg.C for a time D2 such that D2/D1 is greater than 10 (pref. 50-100), in the absence of oxygen and keeping the pH above 13.5, so that the above by-prods. (esp. methyldiazine) are partly or completely removed. - Process is operated continuously; (II) is produced in aq. basic medium with pH 10-14 (pref. in a NH3/NH4Cl buffer) under oxygen-free atmos., by reaction of ammonia with alkali hypochlorite (pref. NaOCl) at -10 to +10 deg.C. (II) is produced in a first reactor with an inlet for the aq. medium and the reactants and an outlet through which the reaction mixt. is transferred by suitable devices to a sec. reactor, from there to a third reactor in which the extra prodn. stage is carried out, and then to the purificn./concn. stage. The third reactor is a tube reactor fitted with a double mantle which enables circulation of a fluid. On leaving the first reactor, the medium contg. (II) is passed to a mixer which is also charged with (III), and the mixt. thus obtd. is transferred to the sec. reactor which is charged with strong base.
Priority Applications (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| FR8911960A FR2651776B1 (en) | 1989-09-13 | 1989-09-13 | PROCESS FOR THE SYNTHESIS OF MONOMETHYLHYDRAZINE IN AQUEOUS SOLUTION. |
| DE19904029119 DE4029119B4 (en) | 1989-09-13 | 1990-09-13 | Process for the preparation of monomethylhydrazine in aqueous solution |
| JP24366790A JP2958351B2 (en) | 1989-09-13 | 1990-09-13 | Method for synthesizing aqueous solution of monomethylhydrazine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| FR8911960A FR2651776B1 (en) | 1989-09-13 | 1989-09-13 | PROCESS FOR THE SYNTHESIS OF MONOMETHYLHYDRAZINE IN AQUEOUS SOLUTION. |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| FR2651776A1 FR2651776A1 (en) | 1991-03-15 |
| FR2651776B1 true FR2651776B1 (en) | 1991-10-25 |
Family
ID=9385408
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| FR8911960A Expired - Lifetime FR2651776B1 (en) | 1989-09-13 | 1989-09-13 | PROCESS FOR THE SYNTHESIS OF MONOMETHYLHYDRAZINE IN AQUEOUS SOLUTION. |
Country Status (3)
| Country | Link |
|---|---|
| JP (1) | JP2958351B2 (en) |
| DE (1) | DE4029119B4 (en) |
| FR (1) | FR2651776B1 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2864078B1 (en) * | 2003-12-17 | 2006-02-10 | Isochem Sa | PROCESS FOR THE CONTINUOUS SYNTHESIS OF MONOALKYL HYDRAZINES WITH FUNCTIONALIZED ALKYL GROUP |
| FR2864081B1 (en) | 2003-12-17 | 2006-04-28 | Isochem Sa | PROCESS FOR THE SYNTHESIS OF EXOCYCLIC CYCLOALKYL HYDRAZINE DERIVATIVES AND EXOCYCLIC HETEROCYCLOALKYL HYDRAZINE DERIVATIVES |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3394184A (en) * | 1964-06-25 | 1968-07-23 | Olin Mathieson | Manufacture of monomethylhydrazine |
| US3423464A (en) * | 1966-08-25 | 1969-01-21 | Olin Mathieson | Process for the manufacture of monomethylhydrazine |
-
1989
- 1989-09-13 FR FR8911960A patent/FR2651776B1/en not_active Expired - Lifetime
-
1990
- 1990-09-13 DE DE19904029119 patent/DE4029119B4/en not_active Expired - Lifetime
- 1990-09-13 JP JP24366790A patent/JP2958351B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| DE4029119A1 (en) | 1991-04-18 |
| JP2958351B2 (en) | 1999-10-06 |
| JPH03109367A (en) | 1991-05-09 |
| FR2651776A1 (en) | 1991-03-15 |
| DE4029119B4 (en) | 2006-10-26 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| CD | Change of name or company name | ||
| TP | Transmission of property |