CN1160342C - 生产纯三聚氰胺的方法 - Google Patents
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 5
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- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 63
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- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D251/00—Heterocyclic compounds containing 1,3,5-triazine rings
- C07D251/02—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings
- C07D251/12—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings having three double bonds between ring members or between ring members and non-ring members
- C07D251/26—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings having three double bonds between ring members or between ring members and non-ring members with only hetero atoms directly attached to ring carbon atoms
- C07D251/40—Nitrogen atoms
- C07D251/54—Three nitrogen atoms
- C07D251/56—Preparation of melamine
- C07D251/60—Preparation of melamine from urea or from carbon dioxide and ammonia
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D251/00—Heterocyclic compounds containing 1,3,5-triazine rings
- C07D251/02—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings
- C07D251/12—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings having three double bonds between ring members or between ring members and non-ring members
- C07D251/26—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings having three double bonds between ring members or between ring members and non-ring members with only hetero atoms directly attached to ring carbon atoms
- C07D251/40—Nitrogen atoms
- C07D251/54—Three nitrogen atoms
- C07D251/62—Purification of melamine
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Abstract
本发明涉及生产纯三聚氰胺的方法。根据该方法，将在高压法中由脲制备的三聚氰胺熔体冷却，再加入氨，直至达到根据相应的氨压在三聚氰胺的熔点之上约1至50℃的温度，然后a)用水或含氨和/或三聚氰胺的水溶液或悬浮液进行骤冷，并将三聚氰胺固化，或b)用冷的液态或气态氨进行骤冷，三聚氰胺固化，然后在第二步骤中用水或含氨和/或三聚氰胺的水溶液或悬浮液进一步冷却，和c)然后分离三聚氰胺。
Description
本发明涉及在高压下生产纯三聚氰胺的方法，在该方法中，在固化前，通过提供氨来冷却三聚氰胺熔体，然后在含水介质中精制。通过脲热解生产三聚氰胺是已知的，例如参见“工业化学乌尔曼百科全(Ullmann’s Encyclopedia of Industrial Chemistry)”，卷A16，第5版(1990)，第171-185页。在其中例举的Montedison方法中，将脲在370℃和70巴下与氨一起在20分钟内在反应器中分解。然后在骤冷器内将主要包括三聚氰胺熔体、氨和CO2的反应混合物减压至25巴并在160℃下用NH3/CO2水溶液进行处理，沉淀固体三聚氰胺。为分解任何未转化的脲或副产物，非必需地将获得的粗三聚氰胺悬浮液放在骤冷器内一段时间。之后，非必需地在汽提塔中除去三聚氰胺悬浮液中的NH3和CO2并加入母液来稀释，使三聚氰胺溶解。加入氢氧化钠溶液并用活性碳处理后，三聚氰胺结晶。
在另一种三聚氰胺法(Nissan法)中，脲分解在100巴和400℃下进行，在三聚氰胺合成前使用所用的脲熔体从三聚氰胺反应器的尾气中将三聚氰胺和脲洗涤出来。将获得的三聚氰胺熔体用氨水溶液骤冷，非必需地在老化步骤后溶解并在180℃下静置以分解杂质。氨汽提和溶液过滤后，三聚氰胺结晶。根椐US3,637,686，在用氨水溶液骤冷前，将三聚氰胺熔体在第一步骤中用冷的液态或气态氨在5-100巴的压力下、200-270℃的温度下骤冷，使三聚氰胺固化。
然而，在三聚氰胺合成中初始获得的粗三聚氰胺(根椐生产方法含有约94-97％重量的三聚氰胺和特别地作为主要杂质的蜜白胺、蜜勒胺、氰尿酰胺、脲基三聚氰胺、三聚氰酸二酰胺和三聚氰酸一酰胺)，由于其可生产树脂的质量不高，不适宜于或仅不足以适用于大多数用途。为了获得纯三聚氰胺，必须进行另外的工艺步骤，如重结晶。
因此，本发明的一个目的是提供一种可获得更高纯度三聚氰胺并具有高产率的更简单的方法。根椐本发明，若将从三聚氰胺反应器获得的粗三聚氰胺熔体冷却到刚好高于固化前的熔点并加入另外的氨进行水精制，则可实现本发明目的。
因此，本发明涉及一种生产纯三聚氰胺的方法，其特征在于将在高压法中由脲制备的三聚氰胺熔体，非必需地在尾气汽提后和非必需地在老化容器中停留后，根椐相应的氨压，冷却至三聚氰胺的熔点之上约1-50℃的温度，并同时加入氨，然后：
a)用水或含氨和/或三聚氰胺的水溶液或悬浮液进行骤冷，并将三聚氰胺固化，或
b)用冷的液态或气态氨进行骤冷，三聚氰胺固化，然后在第二步骤中用水或含氨和/或三聚氰胺的水溶液或悬浮液进一步冷却，和
c)然后分离三聚氰胺。
在三聚氰胺高压法中，在约70-800巴和至少约370℃的温度下，获得作为熔体的液体三聚氰胺。在三聚氰胺合成中形成的并具体含有NH3和CO2的尾气可在熔体冷却之前或之后分离掉。有利地是，将尾气通过脲熔体进行洗涤，特别是三聚氰胺颗粒或未转换的脲的颗粒被正在冲洗的尾气夹带。脲熔体通过热尾气加热并有利地通入三聚氰胺反应器中以合成三聚氰胺，同时将纯化后的尾气有利地通入脲反应器中。尾气可直接通入脲反应器中，或将尾气例如借助例如在三聚氰胺装置或脲装置中获得的碳酸铵或氨基甲酸铵溶液冷凝。生成的热可用来例如预热脲装置中所用的氨或用来产生蒸汽。
在尾气被分离掉后，可有利地例如用NH3汽提三聚氰胺熔体，结果是特别地除去残余的CO2。另外有利的是使三聚氰胺熔体在老化容器中停留，如WO96/23778或WO96/20182中所述。可根椐相应的氨压，按本发明冷却至三聚氰胺的熔点之上约1-50℃的温度可通过如下方式进行：通过借助热交换器或通过加入冷的液态、气态或超临界NH3至熔体上方的气相，或优选通入熔体中或通过组合这些冷却措施，彻底混合，例如通入氨气，可通过另外的搅拌装置，如搅拌器、静态混合器等是优选的。理想的是，获得用NH3饱和的三聚氰胺熔体。然而，根椐本发明，根椐工艺条件和加入的NH3的量，在相应压力和温度下，可获得用NH3超饱和或亚饱和的三聚氰胺熔体。将熔体优选根椐相应的氨压，冷却至三聚氰胺的熔点之上约1-30℃的温度。若冷却到尽可能接近三聚氰胺的熔点之上(取决于相应的氨压)，则证明是特别有利的。优选冷却进行约1分钟至10小时，特别优选约1分钟至1小时。在该温度范围内的停留时间为约1分钟至10小时，优选约1分钟至1小时。在冷却期间氨压优选为约50至1000巴，特别优选的压力为约50至400巴。通过加入氨同时提高压力是有利的。
例如可在老化容器中或在单独的适当容器或在热交换器中冷却熔体。熔体冷却后，通过将冷却的三聚氰胺熔体与水或水溶液或悬浮液(根椐步骤a)，或与氨然后与水或水溶液或悬浮液(根椐步骤b)混合，进行骤冷。通过喷雾或将各物质通入，或通过喷雾或将熔体通入，初始加入的溶液或悬浮液中并同时压力降低，来特别有利地和彻底地进行混合。为在步骤a)中骤冷三聚氰胺，可特别有利地和经济地将在三聚氰胺固化或结晶和分离中获得的母液回收和再使用。根椐步骤a)，用水或用含氨和/或三聚氰胺的溶液或悬浮液骤冷三聚氰胺熔体期间的温度优选为25至300℃，特别优选约50至200℃，压力为约1至100巴，特别优选约1至50巴。温度取决于骤冷器中的操作条件，特别是取决于压力、浓度和流速。根椐步骤b)用氨骤冷优选在约200至270℃和在约1至100巴、特别优选在约1至50巴下进行，接着在第二冷却步骤中，用水或含氨和/或三聚氰胺的溶液或悬浮液进行进一步冷却至优选约50至200℃。然后将冷却期间获得的结晶或固化的三聚氰胺通过例如过滤或离心从母液中分离出来，然后干燥，获得的三聚氰胺具有高产率和约99％高的纯度，这主要归于省掉了另外的纯化步骤。
骤冷有利地在熔体冷却下游的骤冷容器中连续进行。例如，液体三聚氰胺在从刚好高于熔点(取决于相应的氨压)的温度至约370℃温度和约100至400巴下，进入骤冷容器的上部，并用水和用固体三聚氰胺在来自骤冷容器的三聚氰胺水溶液中的或在再循环母液中的再循环水悬浮液骤冷，这些骤冷液同样可喷入骤冷器的顶部。喷入的水具有温度例如约25至90℃，喷入的悬浮液或母液具有温度约25至150℃，和压力约1至10巴。根椐该实施例，将骤冷器中的温度保持约恒定，有利地搅拌骤冷器中的三聚氰胺悬浮液，从骤冷器的下部连续取出不循环并且除固体三聚氰胺外还包括溶解的三聚氰胺和氨的部分三聚氰胺悬浮液，通过过滤或离心分离三聚氰胺并干燥，并将母液部分再循环和部分除去。
为获得较高和非常高的纯度，可将三聚氰胺重结晶。也可以将根椐a)或b)获得的三聚氰胺不预先分离而是通过加入到氨水溶液中直接溶入该悬浮液中，特别优选和经济地是将三聚氰胺固化或结晶期间获得的母液再循环并用于溶解。由水解形成的任何副产物、尤其是羟氨三嗪如三聚氰酸二酰胺和三聚氰酸一酰胺，非必需地可通过加入碱如NaOH保留在溶液中。非必需地让溶液停留，非必需地溶解的NH3也被汽提掉，非必需地用活性碳处理。接着过滤，三聚氰胺通过例如进一步冷却和/或降低压力或施加真空来结晶，并从母液中分离和干燥。
本发明获得的三聚氰胺相对于常规三聚氰胺在用水骤冷后具有更高的纯度，且在重结晶后产率更高。
干燥后，可将三聚氰胺老化以进一步提高质量。将分离的、非必要再结晶的三聚氰胺优选在NH3压力约5至约600巴，优选约5-100巴下、在温度约100℃至低于三聚氰胺的的熔点(取决于相应的氨压)下停留(调和)约5分钟至10小时，优选约5分钟至5小时。
实施例1
将具有2％重量蜜白胺和1％重量蜜勒胺的20g三聚氰胺加入容积100ml的高压釜中，将高压釜在NH3压力250巴下加入氨的同时升至温度370℃，并在该温度和压力下保持2小时。在1小时内在加入NH3下冷却至320℃，保持压力250巴，保持该温度30分钟，然后将三聚氰胺熔体喷入第二高压釜(1000ml容积)中，在该高压釜中存在温度159℃和压力12巴的氨水溶液。三聚氰胺固化，第二高压釜中温度升至168℃和压力升至24巴。高压釜冷却后，过滤并干燥，获得纯度99.1％的三聚氰胺。
实施例2
将具有2％重量蜜白胺和1％重量蜜勒胺的20g三聚氰胺加入容积100ml的高压釜中，将高压釜在NH3压力250巴下加入氨的同时升至温度370℃，并在该温度和压力下保持2小时。在1小时内在加入NH3下冷却至330℃，保持压力250巴，保持该温度30分钟，然后将三聚氰胺熔体喷入第二高压釜(1000ml容积)中，在该高压釜中存在温度62℃和压力1巴的氨水溶液。三聚氰胺固化，第二高压釜中温度升至81℃和压力升至4巴。高压釜冷却后，过滤并干燥，获得纯度98.8％的三聚氰胺。
实施例3
将具有2％重量蜜白胺和1％重量蜜勒胺的20g三聚氰胺加入容积100ml的高压釜中，将高压釜在NH3压力250巴下加入氨的同时升至温度370℃，并在该温度和压力下保持2小时。在1小时内在加入NH3下冷却至350℃，保持压力250巴，保持该温度30分钟，然后将三聚氰胺熔体喷入第二高压釜(1000ml容积)中，在该高压釜中存在温度63℃和压力1巴的氨水溶液。三聚氰胺固化，第二高压釜中温度升至88℃和压力升至4巴。高压釜冷却后，过滤并干燥，获得纯度98.6％的三聚氰胺。
比较例1
将具有2％重量蜜白胺和1％重量蜜勒胺的20g三聚氰胺加入容积100ml的高压釜中，将高压釜在NH3压力250巴下加入氨的同时升至温度370℃，并在该温度和压力下保持2小时。将三聚氰胺熔体喷入第二高压釜(1000ml容积)中，在该高压釜中存在温度62℃和压力1巴的氨水溶液。三聚氰胺固化，第二高压釜中温度升至94℃和压力升至5巴。高压釜冷却后，过滤并干燥，获得纯度97.5％的三聚氰胺。
Claims (12)
1.一种生产纯三聚氰胺的方法，其特征在于将在高压法中由脲制备的三聚氰胺熔体，非必需地在尾气汽提后和非必需地在老化容器中停留后，根椐相应的氨压，冷却至三聚氰胺的熔点之上1-50℃的温度，并同时加入氨，然后：
用水或含氨和/或三聚氰胺的水溶液或悬浮液进行骤冷，并将三聚氰胺固化和然后分离。
2.根据权利要求1的方法，其特征在于通过将三聚氰胺熔体通入冷的液态或气态氨中使其冷却至三聚氰胺熔点之上1至50℃的温度。
3.根椐权利要求1的方法，其特征在于将骤冷并固化后获得的并以悬浮液形式存在的三聚氰胺通过加入含氨水溶液中使其溶解，将该溶液非必需地与NaOH混合，非必需地让其停留和非必需地汽提溶解的氨，然后过滤，并将三聚氰胺结晶和分离。
4.根据权利要求3的方法，其特征在于将骤冷并固化后获得的并以悬浮液形式存在的三聚氰胺通过加入在结晶中获得的再循环母液中使其溶解。
5.根椐权利要求1-4中任一项的方法，其特征在于将三聚氰胺熔体借助在结晶中获得的循环母液骤冷。
6.根椐权利要求1-4中任一项的方法，其特征在于将三聚氰胺熔体在加入氨的同时在氨压50至1000巴下冷却至三聚氰胺熔点之上1至50℃的温度。
7.根椐权利要求1-4中任一项的方法，其特征在于将三聚氰胺熔体冷却至三聚氰胺熔点之上1至30℃的温度。
8.根椐权利要求1-4中任一项的方法，其特征在于通过通入氨1分钟至10小时将三聚氰胺熔体冷却至三聚氰胺熔点之上1至50℃的温度。
9.根椐权利要求1-4中任一项的方法，其特征在于在温度25至300℃和压力1至100巴下进行骤冷。
10.根据权利要求9的方法，其特征在于所述温度为50-200℃，所述压力为1-50巴。
11.根椐权利要求1-4中任一项的方法，其特征在于借助同时加热的脲熔体从三聚氰胺反应器的尾气中将三聚氰胺和脲洗出，然后将该脲熔体加入三聚氰胺反应器中合成三聚氰胺，将尾气加入脲反应器中。
12.根椐权利要求11的方法，其特征在于将不含三聚氰胺和脲的尾气冷凝，非必需地借助于在三聚氰胺装置或脲装置中获得的碳酸铵和/或氨基甲酸铵溶液，并将生成的热用于预热脲装置所用的液态氨或用于生产蒸汽。
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| ATA1894/1998 | 1998-11-13 | ||
| AT189498 | 1998-11-13 |
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| US (1) | US6790956B1 (zh) |
| EP (1) | EP1129080B1 (zh) |
| JP (1) | JP2002529539A (zh) |
| KR (1) | KR100643552B1 (zh) |
| CN (1) | CN1160342C (zh) |
| AR (1) | AR021254A1 (zh) |
| AT (1) | ATE247648T1 (zh) |
| AU (1) | AU767818B2 (zh) |
| BR (1) | BR9915040A (zh) |
| CA (1) | CA2350777A1 (zh) |
| CZ (1) | CZ20011625A3 (zh) |
| DE (1) | DE59906703D1 (zh) |
| EA (1) | EA003233B1 (zh) |
| EE (1) | EE200100262A (zh) |
| ES (1) | ES2209560T3 (zh) |
| HU (1) | HUP0104769A2 (zh) |
| NO (1) | NO20012285L (zh) |
| PL (1) | PL198432B1 (zh) |
| RO (1) | RO119717B1 (zh) |
| SK (1) | SK6192001A3 (zh) |
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| WO (1) | WO2000029393A1 (zh) |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| AT410210B (de) * | 2000-08-07 | 2003-03-25 | Agrolinz Melamin Gmbh | Verfahren zur herstellung von melamin |
| US20030028020A1 (en) * | 2001-07-27 | 2003-02-06 | Gupta Ram B. | Process for the synthesis of high purity melamine |
| NL1018936C2 (nl) * | 2001-09-12 | 2003-03-13 | Dsm Nv | Werkwijze voor het verkrijgen van kristallijn melamine uit een melaminesmelt. |
| AT410795B (de) * | 2001-11-16 | 2003-07-25 | Agrolinz Melamin Gmbh | Verfahren zur herstellung von melemfreiem melamin |
| CN1315812C (zh) | 2001-11-16 | 2007-05-16 | Ami－阿格罗林茨三聚氰胺有限公司 | 制备不含蜜勒胺的三聚氰胺的方法及骤冷器 |
| ITMI20021026A1 (it) * | 2002-05-14 | 2003-11-14 | Eurotecnica Dev & Licensing S | Processo di produzione di melammina da urea e particolarmente per ottenere off-gas privi di melammina nello stadio di prima separazione |
| ITMI20021422A1 (it) * | 2002-06-27 | 2003-12-29 | Eurotecnica Dev & Licensing S | Procedimento e dispositivo per il recupero della melammina per espansione dalle sue miscele grezze prodotte nel processo di pirolisi dell'ur |
| DE102004018784A1 (de) * | 2004-04-14 | 2005-11-03 | Ami-Agrolinz Melamine International Gmbh | Verfahren zur Herstellung von reinem Melamin |
| CN1872842B (zh) * | 2006-06-27 | 2010-05-12 | 山东联合化工股份有限公司 | 常压两步法碳铵联产三聚氰胺工艺 |
| DE102006055571B4 (de) | 2006-11-20 | 2018-09-27 | Urea Casale S.A. | Verfahren und Vorrichtung zur Aufarbeitung einer Melaminschmelze |
| WO2009080176A2 (en) * | 2007-12-20 | 2009-07-02 | Dsm Ip Assets B.V. | Process for the preparation of melamine |
| EP2098516A1 (en) * | 2008-03-04 | 2009-09-09 | Urea Casale S.A. | Process for the production of high purity melamine from urea |
| RU2495876C1 (ru) | 2012-09-10 | 2013-10-20 | Открытое Акционерное Общество "Научно-Исследовательский И Проектный Институт Карбамида И Продуктов Органического Синтеза" (Оао Ниик) | Способ очистки меламина |
| RU2495875C1 (ru) * | 2012-10-11 | 2013-10-20 | Открытое Акционерное Общество "Научно-Исследовательский И Проектный Институт Карбамида И Продуктов Органического Синтеза" (Оао Ниик) | Способ охлаждения расплава меламина |
| EP3208264A1 (en) * | 2016-02-19 | 2017-08-23 | Casale SA | Method for revamping a high pressure melamine plant |
| EP3272743A1 (en) | 2016-07-22 | 2018-01-24 | Casale SA | Process for melamine purification |
| CA3084310A1 (en) * | 2018-01-26 | 2019-08-01 | Casale Sa | Plant for the synthesis of melamine with offgas recovery in a tied-in urea plant |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US3386999A (en) * | 1966-02-10 | 1968-06-04 | Chemical Construction Corp | Synthesis of melamine |
| US3637686A (en) * | 1969-02-10 | 1972-01-25 | Nissan Chemical Ind Ltd | Process for recovering purified melamine |
| NL8201479A (nl) * | 1982-04-07 | 1983-11-01 | Stamicarbon | Werkwijze voor het bereiden van melamine. |
| AT402294B (de) | 1994-12-23 | 1997-03-25 | Agrolinz Melamin Gmbh | Verfahren zur herstellung von hochreinem melamin |
| AT402296B (de) | 1995-02-03 | 1997-03-25 | Agrolinz Melamin Gmbh | Verfahren zur reinigung von melamin |
| AT403579B (de) * | 1995-12-07 | 1998-03-25 | Agrolinz Melamin Gmbh | Verfahren zur herstellung von hochreinem melamin |
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Also Published As
| Publication number | Publication date |
|---|---|
| DE59906703D1 (de) | 2003-09-25 |
| ATE247648T1 (de) | 2003-09-15 |
| HUP0104769A2 (hu) | 2002-03-28 |
| EA003233B1 (ru) | 2003-02-27 |
| JP2002529539A (ja) | 2002-09-10 |
| EE200100262A (et) | 2002-08-15 |
| EP1129080B1 (de) | 2003-08-20 |
| US6790956B1 (en) | 2004-09-14 |
| SK6192001A3 (en) | 2001-12-03 |
| KR100643552B1 (ko) | 2006-11-10 |
| EA200100537A1 (ru) | 2001-12-24 |
| EP1129080A1 (de) | 2001-09-05 |
| CN1326448A (zh) | 2001-12-12 |
| NO20012285D0 (no) | 2001-05-09 |
| PL347724A1 (en) | 2002-04-22 |
| ES2209560T3 (es) | 2004-06-16 |
| NO20012285L (no) | 2001-05-09 |
| BR9915040A (pt) | 2001-07-17 |
| AU1160400A (en) | 2000-06-05 |
| KR20010073230A (ko) | 2001-07-31 |
| TR200101341T2 (tr) | 2001-11-21 |
| PL198432B1 (pl) | 2008-06-30 |
| AU767818B2 (en) | 2003-11-27 |
| CZ20011625A3 (cs) | 2001-08-15 |
| WO2000029393A1 (de) | 2000-05-25 |
| CA2350777A1 (en) | 2000-05-25 |
| AR021254A1 (es) | 2002-07-03 |
| RO119717B1 (ro) | 2005-02-28 |
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