公开(公告)号：US06482385B2

公开(公告)日：2002-11-19

申请号：US09794122

申请日：2001-02-28

申请人： Alun P. James ,  Graham R. Horne ,  Richard Roesler ,  Lido Signorini ,  Robert Owen ,  Soraya Parvaneh ,  Romano Pardini ,  Stefano Bigini ,  Manfred Mathes ,  Uwe Droste ,  Pier-Luigi Deli

发明人： Alun P. James ,  Graham R. Horne ,  Richard Roesler ,  Lido Signorini ,  Robert Owen ,  Soraya Parvaneh ,  Romano Pardini ,  Stefano Bigini ,  Manfred Mathes ,  Uwe Droste ,  Pier-Luigi Deli

IPC分类号： C01B1510

CPC分类号： C11D3/3942 ,  C01B15/103 ,  C11D3/128

摘要： 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.

摘要翻译： 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。

公开(公告)号：US06306811B1

公开(公告)日：2001-10-23

申请号：US09142941

申请日：1999-03-30

申请人： Alun P. James ,  Graham R. Horne ,  Richard Roesler ,  Soraya Parvaneh ,  Romano Pardini ,  Pier-Luigi Deli

发明人： Alun P. James ,  Graham R. Horne ,  Richard Roesler ,  Soraya Parvaneh ,  Romano Pardini ,  Pier-Luigi Deli

IPC分类号： C11D300

CPC分类号： C11D3/128 ,  C01B15/103 ,  C11D3/3942

摘要： Sodium percarbonate exhibits a tendency to decompose in built compositions and particularly detergent compositions built with zeolites. The tendency can be ameliorated by selecting sodium percarbonate which intrinsically has a mean particle size of from 500 to 1000 microns and not more than 20% by weight of below 350 microns and has a moisture pick-up when measured in a test at 80% relative humidity and 32° C. after 24 hours of not greater than 30 g/1000 g sample. A suitable sodium percarbonate can be made most conveniently by crystallisation from a bulk saturated solution of sodium percarbonate in a crystalliser/classifier that does not employ a conventional chloride salting-out agent.

摘要翻译： 过碳酸钠表现出在内置组合物中分解的倾向，特别是用沸石构成的洗涤剂组合物。 通过选择过碳酸钠，其本质上具有500至1000微米且不大于20重量％低于350微米的平均粒度可以改善倾向，并且在80％相对的测试中测量时具有吸湿性 湿度为32℃，24小时后不大于30g / 1000g样品。 通过在不使用常规氯化物盐析剂的结晶器/分选机中从过饱碳酸钠的大量饱和溶液中结晶，可以最方便地制备合适的过碳酸钠。

公开(公告)号：US06231828B1

公开(公告)日：2001-05-15

申请号：US09142940

申请日：1998-12-23

申请人： Alun P. James ,  Graham R. Horne ,  Richard Roesler ,  Lido Signorini ,  Robert Owen ,  Soraya Parvaneh ,  Romano Pardini ,  Stefano Bigini ,  Manfred Mathes ,  Uwe Droste ,  Pier-Luigi Deli

发明人： Alun P. James ,  Graham R. Horne ,  Richard Roesler ,  Lido Signorini ,  Robert Owen ,  Soraya Parvaneh ,  Romano Pardini ,  Stefano Bigini ,  Manfred Mathes ,  Uwe Droste ,  Pier-Luigi Deli

IPC分类号： C01B1510

CPC分类号： C11D3/3942 ,  C01B15/103 ,  C11D3/128

摘要： 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.

摘要翻译： 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。