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    • 4. 发明授权
    • Sodium percarbonate and process for producing sodium percarbonate
    • 过碳酸钠和生产过碳酸钠的方法
    • US06482385B2
    • 2002-11-19
    • US09794122
    • 2001-02-28
    • Alun P. JamesGraham R. HorneRichard RoeslerLido SignoriniRobert OwenSoraya ParvanehRomano PardiniStefano BiginiManfred MathesUwe DrostePier-Luigi Deli
    • Alun P. JamesGraham R. HorneRichard RoeslerLido SignoriniRobert OwenSoraya ParvanehRomano PardiniStefano BiginiManfred MathesUwe DrostePier-Luigi Deli
    • C01B1510
    • C11D3/3942C01B15/103C11D3/128
    • Sodium percarbonate is traditionally made in a crystallization process from aqueous hydrogen peroxide and sodium carbonate with recycle of mother liquor in the presence of a substantial concentration of a salting out agent, conventionally sodium chloride. The invention provides a process intended to be conducted without addition of chloride salting-out agent in which the dissolution step is controlled to restrict the sodium carbonate concentration to below 95%, preferably 60 to 90% of its saturated concentration at a temperature preferably controlled to at most 35C. and the mole ratio of hydrogen peroxide:sodium carbonate in the reaction vessel is controlled to between 0.7 to 1.2:1, and preferably about 1:1. In some embodiments at least a fraction of the mother liquor introduced into the dissolution tank is obtained by extraction from the reaction vessel and in other embodiments a fraction of the sodium percarbonate is introduced in solution in the mother liquor and a fraction is introduced in particulate form directly into the reaction vessel. Large particle sodium percarbonate is provided which has a 7 day aged heat emission at 40C. of not more than 3 &mgr;W/g measured in a microcalorimeter over 16 hours that is lower than the heat emission from conventionally produced sodium percarbonate employing a chloride salting-out agent.
    • 传统上,过碳酸钠通过过氧化氢水溶液和碳酸钠的结晶过程进行,在过量的盐析剂(常规氯化钠)存在下,再循环母液。 本发明提供一种在不加入氯化物盐析剂的情况下进行的方法,其中控制溶解步骤以将碳酸钠浓度限制在其饱和浓度的95%以下,优选60%至90%,优选控制在 最多35℃。 并且将反应容器中过氧化氢:碳酸钠的摩尔比控制在0.7至1.2:1之间,优选约1:1。 在一些实施方案中,通过从反应容器中萃取而获得引入溶解槽的至少一部分母液,在其它实施方案中,将过碳酸钠的一部分引入母液中的溶液中,并将一部分以颗粒形式 直接进入反应容器。 提供了大颗粒过碳酸钠,其在40℃下具有7天的发热。 在微量热计中在16小时内测量的,不超过3微瓦/克,低于使用氯化物盐析剂的常规生产的过碳酸钠的散热。
    • 5. 发明授权
    • Process for producing sodium percarbonate
    • 生产过碳酸钠的方法
    • US06231828B1
    • 2001-05-15
    • US09142940
    • 1998-12-23
    • Alun P. JamesGraham R. HorneRichard RoeslerLido SignoriniRobert OwenSoraya ParvanehRomano PardiniStefano BiginiManfred MathesUwe DrostePier-Luigi Deli
    • Alun P. JamesGraham R. HorneRichard RoeslerLido SignoriniRobert OwenSoraya ParvanehRomano PardiniStefano BiginiManfred MathesUwe DrostePier-Luigi Deli
    • C01B1510
    • C11D3/3942C01B15/103C11D3/128
    • Sodium percarbonate is traditionally made in a crystallization process from aqueous hydrogen peroxide and sodium carbonate with recycle of mother liquor in the presence of a substantial concentration of a salting-out agent, conventionally sodium chloride. The invention provides a process intended to be conducted without addition of chloride salting-out agent in which the dissolution step (1) is controlled to restrict the sodium carbonate concentration to below 95%; preferably 60 to 90% of its saturated concentration at a temperature preferably controlled to at most 35° C. and the mole ratio of hydrogen peroxide: sodium carbonate in the reaction vessel is controlled to between 0.7 to 1.2:1, and preferably about 1:1. In some embodiments at least a fraction of the mother liquor introduced into the dissolution tank (1) is obtained by extraction from the reaction vessel (6) and in other embodiments a fraction of the sodium percarbonate (2) is introduced in solution in the mother liquor (4) and a fraction is introduced in particulate form (8) directly into the reaction vessel (6). Large particle sodium percarbonate is provided which has a 7 day aged heat emission at 40° C. of not more than 3 &mgr;W/g measured in a microcalorimeter over 16 hours that is lower than the heat emission from conventionally produced sodium percarbonate employing a chloride salting-out agent.
    • 传统上,过碳酸钠通过过氧化氢和碳酸钠水溶液的结晶过程在母液中,在大量浓度的盐析剂,常规氯化钠存在下进行。 本发明提供了一种在不加入氯化物盐析剂的情况下进行的方法,其中控制溶解步骤(1)以将碳酸钠浓度限制在95%以下; 优选其饱和浓度的60至90%,优选控制在至多35℃,反应容器中过氧化氢:碳酸钠的摩尔比控制在0.7至1.2:1之间,优选约1: 1。 在一些实施方案中,通过从反应容器(6)中提取,获得引入溶解槽(1)的至少一部分母液,在其它实施方案中,将过量碳酸钠(2)的一部分引入母体溶液中 液体(4)和一部分颗粒形式(8)直接引入反应容器(6)。 提供大颗粒过碳酸钠,其在40℃下具有7天以上的热释放度,其在微量热计中在16小时内测量的不超过3μW/ g,低于常规制备的过碳酸钠使用氯化物盐析 -out代理。
    • 8. 发明授权
    • Method for producing sodium percarbonate
    • 生产过碳酸钠的方法
    • US06248707B1
    • 2001-06-19
    • US09331010
    • 1999-08-13
    • Werner DoetschManfred MathesHelmut HonigGabriele Wasem
    • Werner DoetschManfred MathesHelmut HonigGabriele Wasem
    • C11D3395
    • C11D3/3942B01J2/00C01B15/103C11D1/04C11D3/128C11D17/065
    • A method for the “dry” production of sodium percarbonate (dry process), in which monohydrate crystals of sodium carbonate are reacted with a quasi-stoichiometric quantity of concentrated aqueous hydrogen peroxide solution, relative to the quantity of active oxygen required in the sodium percarbonate to be produced. This method can be combined to great advantage with subsequent compaction of the sodium percarbonate obtained. Sodium percarbonate products containing varying concentrations of active oxygen of at least 10 weight percent, particularly high active oxygen concentrations of above 14.5 weight percent, can be produced. The resulting sodium percarbonate products are distinguished in that they have remarkably advantageous dissolution rates, stabilities and compatibility with detergent bases, and are superior to conventional sodium percarbonates obtained, for example, by a crystallization process. The invention also relates to the sodium percarbonate products obtained and to detergent compositions containing such sodium percarbonate products.
    • 相对于过碳酸钠中所需的活性氧的量,将碳酸钠的一水合物晶体与准化学计算量的浓缩的过氧化氢水溶液进行“干”生产过碳酸钠(干法)的方法 要生产。 所得到的过碳酸钠随后的压实可以将该方法组合起来具有很大的优势。 可以生产含有至少10重量%的不同浓度的活性氧的过碳酸钠产物,特别是高于14.5重量%的特别高的活性氧浓度。 所得到的过碳酸钠产物的特征在于它们具有非常有利的溶解速率,稳定性和与洗涤剂碱的相容性,并且优于例如通过结晶方法获得的常规过碳酸钠。 本发明还涉及所得的过碳酸钠产品和含有过碳酸钠产品的洗涤剂组合物。
    • 9. 发明授权
    • Process for the production of sodium percarbonate
    • 过碳酸钠生产工艺
    • US06228342B1
    • 2001-05-08
    • US09011043
    • 1998-02-06
    • Manfred MathesWerner Doetsch
    • Manfred MathesWerner Doetsch
    • C01B1510
    • C01B15/103
    • A flexible process for production of homogeneous sodium precarbonate particles or granules according to which a reaction slurry with an average to high solids content is prepared initially from an aqueous hydrogen peroxide solution of up to maximum 50% by weight and solid soda, this reaction slurry, which optionally may be finely ground by wet comminution, being subsequently subjected immediately to short-term drying, preferably spray drying, and, optionally, granulation. The process enables production, in an efficient manner, of essentially homogeneous sodium percarbonate particles or granules with variable active oxygen contents of 10 to 14.5% by weight and grain sizes and bulk densities which are variable within wide ranges.
    • 用于生产均匀的预碳酸钠颗粒或颗粒的柔性方法,根据该方法,具有平均至高固体含量的反应浆料最初由最高达50重量%的过氧化氢水溶液和固体苏打制备,该反应浆料, 任选地可以通过湿粉碎精细研磨,随后立即进行短时干燥,优选喷雾干燥,和任选地制粒。 该方法能够以有效的方式生产基本均匀的过碳酸钠颗粒或具有10至14.5重量%的可变活性氧含量的颗粒,并且在宽范围内可变的颗粒尺寸和体积密度。