• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    Summary The invention consists of a process according to which ADN can be produced from GUDN in one single process step. GUDN is reacted with an ammonium source (ammonium sulphamate, ammonium sulphate) whereby an ion exchange creates DNA from GUDN in a process step. The advantages are that the process gives pure ADN without potassium impurities and that a smaller amount of solvent is required. The GOD and the ammonium source are heated together with water until everything has gone into solution. Then an alcohol is added and the precipitate formed is filtered off. The filtrate is concentrated and the residue is slurried in an alcohol. The precipitate is filtered off and the DNA is obtained by concentrating the filtrate. An alternative is that after the alcohol addition partially concentrated then formed the mixture. Filtration of the particles from this mixture gives a single solution of ADN in alcohol. Evaporation of this solution gives pure ADN after only one filtration step. Ammonia can also be used as an ammonium source. GUDN is then dissolved in ammonia after which ammonium dinitramide and guanylurea formed are separated by separation on a column filled with activated carbon. The eluted solution is concentrated to dryness to give ADN. GUDN can also be reacted with ammonium sulphate in alcohol, whereby a precipitate is formed and filtered off. The filtrate is concentrated and the residue is slurried in alcohol. The undissolved particles are filtered off and the DNA is obtained by concentrating the filtrate.
    公开号:SE1400043A1
    申请号:SE1400043
    申请日:2014-01-30
    公开日:2015-07-31
    发明作者:Jonas Johansson；Stefan Ek；Martin Skarstind；Nikolaj Latypov；Henrik Skifs
    申请人:Totalförsvarets Forskningsinstitut；
    IPC主号:
    专利说明:

    Aqueous solution until the solution is homogeneous. Then the heat source is removed and alcohol, for example methanol, ethanol, propanols, butanols or the like is added, whereby guanyl urea sulphate (using ammonium sulphate) or guanyl urea sulphamate (when using ammonium sulphamate) precipitates from the solution and is filtered off. A filtrate is obtained, which contains, among other things, ADN and unreacted GU DN. The filtrate is concentrated and the residue from this step is slurried in one of the above-mentioned alcohols, whereby the DNA is dissolved. GOD remains unresolved and is removed by filtration. The filtrate is concentrated to dryness to give pure ADN. In a second described method, ammonia is used as the ammonium source. A solution is made of ammonia and GOD. Then an ion exchange takes place at which DNA and guanylurea are formed in the solution. The solution is passed through a column of activated carbon, which has been pretreated with dilute ammonia. Guanylurea then remained in the column and the DNA followed with the solvent out. Evaporation of this so-called eluted solution gives pure ADN.
    In a third method described, GUDN and ammonium sulfate are mixed in an alcohol, for example methanol, ethanol, propanols and butanols or the like. A mixture of alcohol, GU DN and ammonium sulphate is refluxed to make an ion exchange.
    The mixture is then allowed to cool and a precipitate forms. The precipitate is filtered off and a filtrate is obtained. The filtrate contains, among other things, ADN and unreacted GOD. The filtrate is concentrated to dryness and the residue from this step is slurried in one of the above-mentioned alcohols, whereby the DNA is dissolved. GOD remains unresolved and is removed by filtration. The filtrate then obtained is concentrated to dryness, giving pure ADN.
    In a fourth described method, GUDN and ammonium sulphate are mixed in a solution of water and alcohol, alcohols which can be used are, for example, propanols, butanols, pentanols or the like, so that a two-phase system is obtained. The mixture is heated until a homogeneous solution is obtained. Then the heat source is removed and the phases separate again. The organ phase is separated. The aqueous phase is extracted with one of the alcohols mentioned above. After separation, the organ phase from this extraction is mixed with the organ phase from the previous step. This mixture is concentrated to dryness to give pure ADN. Example 1 A mixture was made of GUDN (1 g, 4.78 mmol), ammonium sulfate (0.758 g, 5.74 mmol) and water (10 g). The mixture was heated to about 100 ° C with stirring until homogeneous, i.e. about 5 minutes. Then the heat source was removed and 2-propanol (100 ml) was added to give a precipitate. The precipitate was filtered off and washed with 2-propanol (50 ml). The filtrate and washings were mixed and then concentrated to dryness. The residue from this step was slurried in 2-propanol (100 ml) and the undissolved particles were filtered off. The filtrate from this step was concentrated to give ADN. The yield was 0.470 g (79.2%).
    Example 2 A mixture was made of GUDN (1 g, 4.78 mmol), ammonium sulfamate (0.0655 g, 5.74 mmol) and water (10 g). The mixture was heated to about 100 ° C with stirring until homogeneous, i.e. about 5 minutes. Then the heat source was removed and 2-propanol (100 ml) was added to give a precipitate. The precipitate was filtered off and washed with 2-propanol (50 ml). The filtrate and washings were mixed and then concentrated to dryness. The residue from this step was slurried in 2-propanol (100 ml) and the undissolved particles were filtered off. The filtrate from this step was concentrated to give ADN. The yield was 0.457 g (76.9%).
    Example 3 A mixture was made of GUDN (1 g, 4.78 mmol), ammonium sulfate (0.758 g, 5.74 mmol) and water (10 g). The mixture was heated to about 100 ° C with stirring until homogeneous, i.e. about 5 minutes. Then the heat source was removed and 2-propanol (200 ml) was added. About 150 ml of the solvent was removed from the mixture by roller evaporation in vacuo. The residue from this concentration was filtered. The filtered precipitate was washed with 2-propanol (50 ml). This washing liquid was mixed with the filtrate. The mixture was concentrated to give ADN. The yield was 0.327 g (55.1%). Example 4 A mixture was made of GUDN (1 g, 4.78 mmol) and ammonium sulfate (0.758 g, 5.74 mmol), water (5 mL) and 2-butanol (10 mL). The mixture was heated to about 100 ° C with stirring until homogeneous, i.e. about 5 minutes. Then the heat source was removed. The solution then separated into an organic phase and an aqueous phase. The organ phase and the aqueous phase were separated. The aqueous phase was extracted with 2-butanol (50 ml), the solution being separated into an organic phase and an aqueous phase.
    The organ phases from the two separations were combined and concentrated to give ADN. The yield was 0.160 g (26.9%).
    Example 5 A mixture was made of GUDN (1 g, 4.78 mmol), ammonium sulfate (0.758 g, 5.74 mmol) and methanol (50 mL). The mixture was refluxed for 2 hours, after which the heat source was removed. The undissolved particles were filtered off and washed with 2-propanol (50 ml). The filtered reaction solution was mixed with the washing liquid.
    This mixture was then concentrated to dryness. The residue from this step was slurried in 2-propanol (100 ml) and the undissolved particles were filtered off. The filtrate was concentrated to give pure ADN. The yield was 0.145 g (24.4%).
    Example gel 6 A column was filled with activated carbon (20 g). The carbon was rinsed with dilute ammonia (5% NH 4 q). A solution was made of GUDN (1.5 g, 7.17 mmol) and NH 3 (6 g, 25% aq.).
    The solution was applied to the column, which was then eluted with dilute ammonia (5% NH 3 aq). The resulting eluent was then concentrated to dryness to give ADN. The yield was 0.667 g (75%).
    权利要求:
    Claims (17)
    [1]
    Claims Method for producing ammonium dinitramide characterized in that guanylurea dininitramide is reacted with an ammonium source so that an ion exchange takes place and ammonium dinitramide is formed.
    [2]
    A process for preparing ammonium dinitramide according to claim 1, wherein the guanylurea dinitramide is reacted with an ammonium source in a solution of water and alcohol.
    [3]
    Process for producing ammonium dinitramide according to Claim 2, characterized in that the alcohol consists of methanol.
    [4]
    Process for the preparation of ammonium dinitramide according to Claim 2, characterized in that the alcohol consists of ethanol.
    [5]
    Process for producing ammonium dinitramide according to Claim 2, characterized in that the alcohol consists of a propanol.
    [6]
    Process for producing ammonium dinitramide according to Claim 2, characterized in that the alcohol consists of a butanol.
    [7]
    Process for producing ammonium dinitramide according to Claim 2, characterized in that the ammonium source consists of ammonium sulphamate.
    [8]
    Method of producing ammonium dinitramide according to claim 2, characterized in that the ammonium source consists of ammonium sulphate.
    [9]
    A process for producing ammonium dinitramide according to claim 1, characterized in that guanylurea dininitramide is reacted with an ammonium source in a solution of alcohol.
    [10]
    10 15 20 25 30 10.
    [11]
    11.
    [12]
    12.
    [13]
    13.
    [14]
    14.
    [15]
    15.
    [16]
    16.
    [17]
    17. A process for producing ammonium dinitramide according to claim 9, characterized in that the ammonium source is ammonium sulphate. Method of producing ammonium dinitramide according to claim 9, characterized in that the ammonium source consists of ammonium sulphamate. Process for producing ammonium dinitramide according to Claim 9, characterized in that the alcohol consists of methanol. Process for the preparation of ammonium dinitramide according to Claim 9, characterized in that the alcohol consists of ethanol. Process for the preparation of ammonium dinitramide according to Claim 9, characterized in that the alcohol consists of a propanol. A process for producing ammonium dinitramide according to claim 9, characterized in that the alcohol consists of a butanol. Process for producing ammonium dinitramide according to Claim 1, characterized in Process for preparing ammonium dinitramide according to Claim 16, characterized in that ammonium dinitramide is isolated by separation on a carbon column. a v that the ammonium source consists of ammonia.
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    同族专利:
    公开号 | 公开日
    US10112834B2|2018-10-30|
    SE537747C2|2015-10-13|
    US20170008768A1|2017-01-12|
    EP3099652A1|2016-12-07|
    WO2015115962A1|2015-08-06|
    EP3099652A4|2017-07-26|
    EP3099652B1|2018-12-26|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    US5316749A|1991-07-30|1994-05-31|Sri International|Process for forming ammonium dinitramide salt by reaction between ammonia and a nitronium-containing compound|
    SE516719C2|1995-08-08|2002-02-19|Totalfoersvarets Forskningsins|Methods for preparing dinitramic acid and salts thereof|
    US6117255A|1998-07-28|2000-09-12|Trw Inc.|Gas generating composition comprising guanylurea dinitramide|
    SE526402C2|2004-01-21|2005-09-06|Foersvarets Materielverk|Methods for preparing salt of dinitramic acid|EP3853174A1|2018-09-17|2021-07-28|Totalförsvarets Forskningsinstitut|Synthesis of ammonium dinitramide |
    CN111228855A|2020-01-14|2020-06-05|无锡市疾病预防控制中心|Preparation method of pineapple pulp matrix biochar filler solid-phase extraction column|
    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    SE1400043A|SE537747C2|2014-01-30|2014-01-30|Synthesis of ammonium dinitramide, ADN|SE1400043A| SE537747C2|2014-01-30|2014-01-30|Synthesis of ammonium dinitramide, ADN|
    PCT/SE2015/000004| WO2015115962A1|2014-01-30|2015-01-29|Synthesis of amonnium dinitramide, adn|
    EP15743454.9A| EP3099652B1|2014-01-30|2015-01-29|Synthesis of amonnium dinitramide, adn|
    US15/115,743| US10112834B2|2014-01-30|2015-01-29|Synthesis of ammonium dinitramide, ADN|
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