NO130218B - - Google Patents
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- Publication number
- NO130218B NO130218B NO30373A NO30373A NO130218B NO 130218 B NO130218 B NO 130218B NO 30373 A NO30373 A NO 30373A NO 30373 A NO30373 A NO 30373A NO 130218 B NO130218 B NO 130218B
- Authority
- NO
- Norway
- Prior art keywords
- hydrazine
- solution
- ammonia
- carbonyl compound
- reaction
- Prior art date
Links
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 claims description 28
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 21
- 150000001728 carbonyl compounds Chemical class 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 8
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- 239000005708 Sodium hypochlorite Substances 0.000 claims description 4
- 125000000217 alkyl group Chemical group 0.000 claims description 4
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 claims description 4
- 125000004432 carbon atom Chemical group C* 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- 239000001257 hydrogen Substances 0.000 claims description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims description 2
- 239000000243 solution Substances 0.000 description 14
- 229910021529 ammonia Inorganic materials 0.000 description 9
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 7
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 description 7
- QDHHCQZDFGDHMP-UHFFFAOYSA-N Chloramine Chemical compound ClN QDHHCQZDFGDHMP-UHFFFAOYSA-N 0.000 description 5
- 235000011114 ammonium hydroxide Nutrition 0.000 description 5
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 4
- 239000003292 glue Substances 0.000 description 4
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 3
- 239000000460 chlorine Substances 0.000 description 3
- 229910052801 chlorine Inorganic materials 0.000 description 3
- NBBJYMSMWIIQGU-UHFFFAOYSA-N Propionic aldehyde Chemical compound CCC=O NBBJYMSMWIIQGU-UHFFFAOYSA-N 0.000 description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- PFLUPZGCTVGDLV-UHFFFAOYSA-N acetone azine Chemical compound CC(C)=NN=C(C)C PFLUPZGCTVGDLV-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000004061 bleaching Methods 0.000 description 2
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 description 2
- 150000007857 hydrazones Chemical class 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 108010010803 Gelatin Proteins 0.000 description 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- IKHGUXGNUITLKF-XPULMUKRSA-N acetaldehyde Chemical compound [14CH]([14CH3])=O IKHGUXGNUITLKF-XPULMUKRSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000001299 aldehydes Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000007844 bleaching agent Substances 0.000 description 1
- ZTQSAGDEMFDKMZ-UHFFFAOYSA-N butyric aldehyde Natural products CCCC=O ZTQSAGDEMFDKMZ-UHFFFAOYSA-N 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 229920000159 gelatin Polymers 0.000 description 1
- 239000008273 gelatin Substances 0.000 description 1
- 235000019322 gelatine Nutrition 0.000 description 1
- 235000011852 gelatine desserts Nutrition 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000002429 hydrazines Chemical class 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- FDPIMTJIUBPUKL-UHFFFAOYSA-N pentan-3-one Chemical compound CCC(=O)CC FDPIMTJIUBPUKL-UHFFFAOYSA-N 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000010517 secondary reaction Methods 0.000 description 1
- 235000002639 sodium chloride Nutrition 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
- B01D46/24—Particle separators, e.g. dust precipitators, using rigid hollow filter bodies
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D39/00—Filtering material for liquid or gaseous fluids
- B01D39/14—Other self-supporting filtering material ; Other filtering material
- B01D39/16—Other self-supporting filtering material ; Other filtering material of organic material, e.g. synthetic fibres
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D39/00—Filtering material for liquid or gaseous fluids
- B01D39/14—Other self-supporting filtering material ; Other filtering material
- B01D39/20—Other self-supporting filtering material ; Other filtering material of inorganic material, e.g. asbestos paper, metallic filtering material of non-woven wires
- B01D39/2003—Glass or glassy material
- B01D39/2017—Glass or glassy material the material being filamentary or fibrous
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Filtering Materials (AREA)
- Filtering Of Dispersed Particles In Gases (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Description
Fremgangsmåte til fremstilling av hydrazinhydrat. Process for the production of hydrazine hydrate.
Som kjent lar hydrazin resp. hydrazinhydrat seg fremstille ved oppvarmning av natriumhypoklorittoppløsning med vandig ammoniakkoppløsning, idet ammoni-akken må anvendes i overskudd. Omsetningen forløper på den måten at det først danner seg kloramin av natriumhypoklo-ritt og ammoniakk ifølge ligning (1). As is known, hydrazine resp. hydrazine hydrate is produced by heating sodium hypochlorite solution with aqueous ammonia solution, the ammonia must be used in excess. The reaction proceeds in such a way that chloramine is first formed from sodium hypochlorite and ammonia according to equation (1).
Dette kloramin reagerer videre med overskytende ammoniakk til hydrazin ifølge ligning (2). This chloramine reacts further with excess ammonia to form hydrazine according to equation (2).
Herved følger reaksjonen (1) øyeblik-kelig, uavhengig av temperaturen og am-moniakkoverskuddet, mens reaksjon (2) er en tidsreaksjon og først avslutter med tilsrekkelig hastighet ved forhøyet temperatur og høyere ammoniakkoverskudd. Parallelt til (2) forløper en bireaksjon (3), som ødelegger ennu tilstedeværende kloramin og allerede dannet hydrazin, og dermed nedsetter utbyttet sterkt. Hereby, reaction (1) follows immediately, regardless of the temperature and the ammonia excess, while reaction (2) is a time reaction and only ends with sufficient speed at an elevated temperature and higher ammonia excess. Parallel to (2), a secondary reaction (3) takes place, which destroys the chloramine still present and the hydrazine already formed, and thus greatly reduces the yield.
Det er mulig å trenge reaksjonen (3) tilbake ved tilsetning av lim, gelatin og lig-nende stoffer og dermed fremme reaksjonen (2). It is possible to force reaction (3) back by adding glue, gelatin and similar substances and thus promote reaction (2).
Denne syntese som er funnet av Rasc-hig er med hensyn til sin lønnsomhet inn-skrenket derved at man for å oppnå et til-fredsstillende hydrazinutbytte, må bruke et meget stort overskudd av ammoniakk-oppløsning. Hydrazinet fremkommer da i en meget fortynnet vandig oppløsning, hvorfra det deretter igjen må fjernes med betraktelig energiomkostning. This synthesis, which was found by Rasc-hig, is limited in terms of its profitability by the fact that in order to achieve a satisfactory yield of hydrazine, a very large excess of ammonia solution must be used. The hydrazine then appears in a very dilute aqueous solution, from which it must then be removed again at considerable energy cost.
Av denne grunn er det i løpet av tiden foretatt forskjellige anstrengelser for å øke hydrazinutbyttet resp. å komme ved samme utbyttet til høyere hydrazinkon-sentrasjoner. For eksempel har man straks etter komponentenes blanding oppvarmet synteseoppløsningen meget hurtig under høyt trykk til temperaturer på 150—180° C. Etter andre fremgangsmåter arbeides i to trinn, idet man først fremstiller klor-aminoppløsningen etter (1) under avkjø-ling og tilsetning av et lite ammoniakk-overskudd og deretter omsettes kloramin-oppløsningen etter (2) ved tilsetning av et større overskudd av ammoniakk. For this reason, various efforts have been made over time to increase the hydrazine yield or to arrive at the same yield at higher hydrazine concentrations. For example, immediately after mixing the components, the synthesis solution is heated very quickly under high pressure to temperatures of 150-180° C. According to other methods, work is carried out in two stages, first preparing the chloramine solution according to (1) while cooling and adding a small excess of ammonia and then the chloramine solution is reacted according to (2) by adding a larger excess of ammonia.
Oppfinnelsens gjenstand er en fremgangsmåte til fremstilling av hydrazin av The object of the invention is a method for producing hydrazine from
natriumhypoklorittoppløsning og vandig ammoniakk, karakterisert ved at man sodium hypochlorite solution and aqueous ammonia, characterized in that one
gjennomfører omsetningen i nærvær av en karbonylforbindelse, adskiller det dannede carries out the reaction in the presence of a carbonyl compound, separates the formed
hydrazon eller azin fra koksalt ved destil-lering og opparbeider det derved fremkom-mende vandige destillat på hydrazin, ek-sempelvis ved spaltning av hydrazonet eller azinet med syre til hydrazinsalt og fri karbonylforbindelse. hydrazone or azine from common salt by distillation and thereby processes the resulting aqueous distillate into hydrazine, for example by splitting the hydrazone or azine with acid to hydrazine salt and free carbonyl compound.
Som karbonylforbindelser er ketoner og aldehyder med den generelle formel As carbonyl compounds, ketones and aldehydes have the general formula
egnet, idet R, betyr en alkylgruppe eller vannstoff, R2 betyr en alkylgruppe og R, og R2 tilsammen foreligger ikke mere enn 5 kullstoff atomer, f. eks. acetaldehyd, aceton, propionaldehyd, metyletylketon, di-etylketon og cykloheksanon. suitable, in that R means an alkyl group or hydrogen, R 2 means an alkyl group and R and R 2 together do not contain more than 5 carbon atoms, e.g. acetaldehyde, acetone, propionaldehyde, methyl ethyl ketone, di-ethyl ketone and cyclohexanone.
Karbonylforbindelsens mengde utmå-les fordelaktig slik at på en mol av det ventede hydrazin faller minst 2 mol av karbonylforbindelsen. The amount of the carbonyl compound is advantageously measured so that at least 2 moles of the carbonyl compound fall on one mole of the expected hydrazine.
Ifølge oppfinnelsen kommer man ved den nevnte fremgangsmåten med vesent-lig mindre ammoniakk-overskudd til de samme hydrazinutbytter resp. med det samme ammoniakkoverskudd til høyere hydrazinutbytter. According to the invention, the aforementioned method achieves the same hydrazine yields or with the same ammonia excess to higher hydrazine yields.
Eksempel 1. Example 1.
500 ml blekelut, som inneholder 76 g aktivt klor fortynnes med 500 ml vann, blandes ved værelsestemperatur med 1.500 ml 25 pst.-ig ammoniakk og 10 ml 0,1 pst.-ig limoppløsning og henstår flere minutter ved 50° C. Man får en oppløsning av 1,03 pst. hydrazinhydrat, tilsvarende et utbytte på 43 pst. 500 ml of bleaching liquor, which contains 76 g of active chlorine, is diluted with 500 ml of water, mixed at room temperature with 1,500 ml of 25% ammonia and 10 ml of 0.1% glue solution and allowed to stand for several minutes at 50°C. a solution of 1.03 per cent hydrazine hydrate, corresponding to a yield of 43 per cent.
Eksempel 7: 500 ml av blekeluten som inneholder 76 g aktivt klor blandes ved værelsestemperatur med 500 ml ammoniakkoppløsning (25 pst.-ig) og 10 ml limoppløsning (0,1 pst.-ig) i nærvær av 100 ml aceton. Etter noen minutters reaksjonstid ved 50° C får man en oppløsning av 61,5 g dimetylketazin tilsvarende 27,5 g hydrazinhydrat. Oppløsningen har, beregnet på hydrazinhydrat, en konsentrasjon på 2,6 pst; utbyttet utgjør 52 pst. Example 7: 500 ml of the bleach solution containing 76 g of active chlorine is mixed at room temperature with 500 ml of ammonia solution (25 per cent) and 10 ml of glue solution (0.1 per cent) in the presence of 100 ml of acetone. After a reaction time of a few minutes at 50° C, a solution of 61.5 g of dimethylketazine corresponding to 27.5 g of hydrazine hydrate is obtained. The solution has, calculated on hydrazine hydrate, a concentration of 2.6 percent; the dividend amounts to 52 per cent.
Eksempel 3: 500 ml blekelut som inneholder 76 g aktivt klor fortynnes med 500 ml vann og blandes sammen ved værelsestemperatur med 1.500 ml 25 pst.-ig ammoniakkopp-løsning, så vel som 10 ml 0,1 pst.-ig lim-oppløsning i nærvær av 100 ml aceton og blandingen holdes noen minutter på en temperatur av 50° C. Man får en oppløs-ning av 91,2 g dimetylketazin, tilsvarende 40,7 g hydrazinhydrat. Oppløsningen har beregnet på hydrazinhydrat en konsentrasjon på 1,5 pst.; utbyttet utgjør 77 pst. Example 3: 500 ml of bleaching liquor containing 76 g of active chlorine is diluted with 500 ml of water and mixed together at room temperature with 1,500 ml of a 25% ammonia solution, as well as 10 ml of a 0.1% glue solution in presence of 100 ml of acetone and the mixture is kept for a few minutes at a temperature of 50° C. A solution of 91.2 g of dimethylketazine is obtained, corresponding to 40.7 g of hydrazine hydrate. The solution has a calculated hydrazine hydrate concentration of 1.5 per cent; the dividend amounts to 77 per cent.
Claims (2)
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
SE88672A SE359749B (en) | 1972-01-26 | 1972-01-26 |
Publications (1)
Publication Number | Publication Date |
---|---|
NO130218B true NO130218B (en) | 1974-07-29 |
Family
ID=20257252
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
NO30373A NO130218B (en) | 1972-01-26 | 1973-01-25 |
Country Status (5)
Country | Link |
---|---|
AT (1) | AT349749B (en) |
CH (1) | CH566855A5 (en) |
DE (1) | DE2303460C2 (en) |
NO (1) | NO130218B (en) |
SE (1) | SE359749B (en) |
Families Citing this family (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0068662B1 (en) * | 1981-06-23 | 1987-01-07 | Nippondenso Co., Ltd. | Filter means |
AU540096B2 (en) * | 1982-08-04 | 1984-11-01 | Nippondenso Co. Ltd. | Filter device and manufacturing method |
US4976910A (en) * | 1987-11-30 | 1990-12-11 | Richard Gatley | Method of making a cooling device |
DE10360230A1 (en) * | 2003-12-20 | 2005-07-21 | Mann + Hummel Gmbh | Manufacturing method for filter housing |
EP1657042B1 (en) * | 2004-11-15 | 2014-06-25 | Ip Ag | Centrifugal casting for edge encapsulation and mould therefore |
-
1972
- 1972-01-26 SE SE88672A patent/SE359749B/xx unknown
-
1973
- 1973-01-24 CH CH101573A patent/CH566855A5/xx not_active IP Right Cessation
- 1973-01-25 DE DE19732303460 patent/DE2303460C2/en not_active Expired
- 1973-01-25 AT AT62073A patent/AT349749B/en not_active IP Right Cessation
- 1973-01-25 NO NO30373A patent/NO130218B/no unknown
Also Published As
Publication number | Publication date |
---|---|
AT349749B (en) | 1979-04-25 |
DE2303460C2 (en) | 1983-02-24 |
ATA62073A (en) | 1978-09-15 |
SE359749B (en) | 1973-09-10 |
DE2303460A1 (en) | 1973-08-02 |
CH566855A5 (en) | 1975-09-30 |
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