CN1171103A - 蜜胺的提纯方法 - Google Patents
蜜胺的提纯方法 Download PDFInfo
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- CN1171103A CN1171103A CN95197017.8A CN95197017A CN1171103A CN 1171103 A CN1171103 A CN 1171103A CN 95197017 A CN95197017 A CN 95197017A CN 1171103 A CN1171103 A CN 1171103A
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- melamine
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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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- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Phenolic Resins Or Amino Resins (AREA)
- Separation Of Suspended Particles By Flocculating Agents (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
- Distillation Of Fermentation Liquor, Processing Of Alcohols, Vinegar And Beer (AREA)
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Abstract
提出一种蜜胺的提纯方法,该法包括:将含杂质的蜜胺置于200℃~蜜胺熔点温度(具体取决于相应的氨分压)下,并在该温度范围及5~350bar压力下以固态形式保持1分钟~20小时,其间,蜜胺为固态,然后,按任何期望的顺序将反应混合物减压并冷却至室温,则得粉末状的纯蜜胺。
Description
目前,已有许多蜜胺生产方法见诸文献,其中,多以尿素为优选原料,再于高压、非催化条件下或低压且使用催化剂条件下将其转化为蜜胺、氨及CO2。如所周知,在这些方法尤其是高压法中,会生成各种副产物或杂质,如蜜勒胺、蜜白胺、氰尿二酰胺、氰尿一酰胺或脲基蜜胺,因此降低蜜胺的纯度。
然而,目前常规的提纯方法如重结晶却存在不足,这尤其在重结晶时表现为杂质在母液中的积累,因而尚含蜜胺的大量母液要被弃去或经后处理。而且,CH345.894提到,诸如蜜勒胺、蜜白胺或脲基蜜胺等杂质几乎不溶于或微溶于水及碱性水溶液,故欲以重结晶除去这些化合物有很大困难和待纯化蜜胺的部分损失。
故此,本发明试图找到一种大幅度降低待纯化蜜胺中的杂质又可避免蜜胺大量损失的方法,其中杂质尤其包括几不溶于或微溶于水及碱性水溶液的蜜勒胺和脲基蜜胺。
出乎意料地,可达到该目的的一种新方法是,在含氨介质中于升至低于蜜胺熔点的温度下,使含杂质的蜜胺静置一段时间。
因而,本发明涉及蜜胺的提纯方法,该法包括:将含杂质的蜜胺置于200℃~蜜胺熔点温度下,并在该温度及5~350bar下保持1分钟~20小时,然后,按任何期望顺序将反应混合物减压并冷却至室温,则得粉末状的纯蜜胺。
本发明方法适用由任何先有技术中已知方法所得蜜胺的提纯,特别是当蜜胺含蜜勒胺和脲基蜜胺等杂质时。业已发现,通过加热晶态或粉末状蜜胺,并在有氨参与、低于蜜胺熔点温度下,使其静置一段时间(回火),则蜜勒胺和脲基蜜胺含量可得以降低。但也可将原有温度高于所述范围的蜜胺冷却至该范围某一温度。此处,回火温度高于200℃,但低于蜜胺熔点。作为优选,该温度介于240℃~蜜胺熔点间,更优选为250℃~蜜胺熔点。蜜胺的初始温度应处于所述范围。在回火过程中,温度可保持常数,但也可在所述温度范围内变化。故此,在所限定温度范围内,温度可连续也可间断地增高或降低。
在所述温度范围内,蜜胺的静置时间可在大范围内变化。这主要取决于蜜勒胺和脲基蜜胺的预期终值以及特定的氨分压和经济考虑,一般为1分钟~20小时,优选值10分钟~10小时,更优选为0.5~3小时。氨分压同样可在大范围内变化,一般为5~350bar,优选值10~100bar。
回火毕,在相应操作条件下将反应混合物冷却并减压,或反之,先减压后冷却。如可能,在另一反应设备中进行上述步骤,并将其中蜜胺冷却至室温,例如,使用热交换器直接移除加热工质,或是与冷气体相混。
本发明方法所得蜜胺为晶体或粉末,其特点是蜜勒胺和脲基蜜胺含量大幅降低,有时甚至在可检出限以下。
本发明方法可以连续和间歇两种方式进行。
本发明方法也可与先有技术中任何已知蜜胺制法配合。一种最佳实施方案是,本发明方法与先有技术中已知任一高压法联用,后者见述于Ullmann s Encyclopedia of Industrial Chemistry,第5版,卷A-16,页174~179。尤为优选的是,本发明方法接续在高压法的已知后处理步骤之后进行,这些后处理步骤包括:
a)自液态蜜胺中分离出尿素转化时生成的NH3/CO2气体混合物;
b)通入NH3减少溶于蜜胺的CO2;
c)使液态蜜胺存留于氨介质中;且
d)冷却蜜胺,如以冷水或液氨骤冷,或是与冷气相混。上述后处理步骤在诸如美国专利第3116294号中有述。
此时,本发明方法接续在后处理步骤d)之后进行,前述后处理步骤a)~c)各步变化视具体条件而定。故此,以高压法自尿素生成蜜胺时,直至冷却阶段d)的后处理步骤中包括a)~c)各步,以及这些步骤之一或是其中两步的任一组合。
实施例1~20
取定量(SW)蜜胺,其蜜勒胺初含量18300ppm,脲基蜜胺初含量10600ppm,以及保持一定压力p所需量的氨,一并加入体积10mL的微压热釜中。其后,加热该釜至温度T并于该温度下保持t分钟。再将该釜迅即浸于冷水,随后减压。如此则蜜胺得以提纯,分析其中蜜勒胺及脲基蜜胺含量,后者含量一般在检出限100ppm以下。操作参数,如蜜胺样品初重(SW)、压力p、时间t、温度T、蜜勒胺终含量(MA),见表1所示。
表1实施 SW p T t MA例 (mg) (bar) (℃) (min) (ppm)1 22.03 10 250 10 50002 22.03 10 250 100 38003 22.03 10 250 1000 11004 67.93 30 250 10 30005 67.93 30 250 100 25006 67.93 30 250 1000 8207 21.19 10 270 10 61008 21.19 10 270 100 45009 21.19 10 270 1000 19010 65.16 30 270 10 300011 65.16 30 270 100 250012 65.16 30 270 1000 28013 20.42 10 290 10 310014 20.42 10 290 100 190015 20.42 10 290 1000 25016 62.61 30 290 10 370017 62.61 30 290 100 100018 62.61 30 290 1000 12019 286.57 350 290 10 32020 280.57 350 290 100 40实施例21~26
取定量(SW)蜜胺,其蜜勒胺初含量MAO,脲基蜜胺初含量UMO,以及保持一定压力p所需量的氨,一并加入体积2L的压热釜中。其后,加热该釜至温度T并于该温度下保持t分钟。再将该釜冷却并减压。如此则蜜胺得以提纯,分析其中蜜勒胺含量(MA)及脲基蜜胺含量(UM)。操作参数,如蜜胺样品初重(SW)、压力p、时间t、温度T、蜜勒胺终含量(MA),见表2所示。
表2实施 SW p T t 终值 初值例 MA UM MAO UMO
(g) (bar) (℃) (h)21 300 20 250 2 1200 600 <300 <5022 300 40 300 1.5 1200 600 <300 <5023 300 56 250 2 1200 600 <300 <5024 300 70 300 4 1200 600 <300 <5025 300 125 296 3 1200 1300 <300 <5026 51.1 139 250 3 2500 <500 <300 <50
Claims (5)
1 蜜胺的提纯方法,该法包括:将含杂质的蜜胺置于高于200℃但低于蜜胺熔点温度下,具体取决于相应的占优氨分压,并在该温度范围及5~350bar压力下保持1分钟~20小时,其间,蜜胺为固态,然后,按任何期望的顺序将反应混合物减压并冷却至室温,则得粉末状的纯蜜胺。
2 权利要求1的方法,其中,固态蜜胺所处温度介于240℃~蜜胺熔点间,具体取决于相应的占优氨分压。
3 权利要求1的方法,其中,氨分压介于10~100bar间。
4 权利要求1的方法,其中,本发明方法接续在某一蜜胺生产方法之后进行。
5 权利要求1的方法,其中,本发明方法接续在以高压法自尿素生产蜜胺之后进行。
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
ATA2393/1994 | 1994-12-23 | ||
AT0239394A AT402295B (de) | 1994-12-23 | 1994-12-23 | Verfahren zur reinigung von melamin |
ATA2393/94 | 1994-12-23 |
Publications (2)
Publication Number | Publication Date |
---|---|
CN1171103A true CN1171103A (zh) | 1998-01-21 |
CN1068315C CN1068315C (zh) | 2001-07-11 |
Family
ID=3533533
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN95197017A Expired - Fee Related CN1068315C (zh) | 1994-12-23 | 1995-12-13 | 蜜胺的提纯方法 |
Country Status (17)
Country | Link |
---|---|
EP (1) | EP0799213B1 (zh) |
JP (1) | JPH10511369A (zh) |
KR (1) | KR100374731B1 (zh) |
CN (1) | CN1068315C (zh) |
AT (2) | AT402295B (zh) |
BR (1) | BR9510606A (zh) |
DE (1) | DE59504292D1 (zh) |
DK (1) | DK0799213T3 (zh) |
ES (1) | ES2124034T3 (zh) |
HR (1) | HRP950605B1 (zh) |
IL (1) | IL116516A (zh) |
NZ (1) | NZ298044A (zh) |
PL (1) | PL187434B1 (zh) |
RO (1) | RO115521B1 (zh) |
RU (1) | RU2161610C2 (zh) |
TW (1) | TW299324B (zh) |
WO (1) | WO1996020183A1 (zh) |
Families Citing this family (16)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5514797A (en) * | 1995-06-07 | 1996-05-07 | Melamine Chemicals, Inc. | Method for increasing purity of melamine |
NL1003328C2 (nl) | 1996-06-13 | 1997-12-17 | Dsm Nv | Werkwijze voor het bereiden van melamine. |
NL1003709C2 (nl) * | 1996-07-30 | 1998-02-05 | Dsm Nv | Werkwijze voor het bereiden van melamine. |
ES2197470T3 (es) | 1997-05-21 | 2004-01-01 | Dsm Ip Assets B.V. | Metodo para preparar melamina. |
NL1006095C2 (nl) * | 1997-05-21 | 1998-11-25 | Dsm Nv | Werkwijze voor het bereiden van melamine. |
KR100495264B1 (ko) | 1997-05-28 | 2005-06-14 | 코닌클리즈케 디에스엠 엔.브이. | 멜라민의 제조방법 |
NL1006147C2 (nl) * | 1997-05-28 | 1998-12-01 | Dsm Nv | Werkwijze voor het bereiden van melamine. |
DE69837432T2 (de) * | 1997-06-02 | 2007-12-13 | Dsm Ip Assets B.V. | Kristallines melamin |
NL1006192C2 (nl) * | 1997-06-02 | 1998-12-03 | Dsm Nv | Werkwijze voor het bereiden van melamine. |
NL1006191C2 (nl) * | 1997-06-02 | 1998-12-03 | Dsm Nv | Kristallijn melamine. |
WO1998055466A1 (en) * | 1997-06-02 | 1998-12-10 | Dsm N.V. | Method for preparing melamine |
US6355797B2 (en) | 1998-01-30 | 2002-03-12 | Agrolinz Melamin Gmbh | Process for cooling melamine |
NL1008571C2 (nl) * | 1998-03-12 | 1999-07-28 | Dsm Nv | Kristallijn melamine. |
KR100575020B1 (ko) * | 1998-12-23 | 2006-05-02 | 아엠이-아그로린츠 멜라민 인터내셔날 게엠베하 | 멜라민의 정제방법 |
AU6697600A (en) * | 1999-07-27 | 2001-02-13 | Agrolinz Melamin Gmbh | Method for producing solid melamine |
RU2417992C2 (ru) * | 2009-07-20 | 2011-05-10 | Открытое акционерное общество "Научно-исследовательский и проектный институт карбамида и продуктов органического синтеза" (ОАО "НИИК") | Способ получения меламина и способ удаления растворенных газов из водного раствора неочищенного меламина |
Family Cites Families (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3116294A (en) * | 1963-12-31 | Process- for preparing high-purity melamine from urea | ||
GB1003277A (en) * | 1963-07-10 | 1965-09-02 | Nissan Chemical Ind Ltd | Process and apparatus for the production and separation of melamine |
DE2522233A1 (de) * | 1975-05-20 | 1976-12-02 | Bollmann L Kg | Maschine zum stapeln von flaechigen gegenstaenden, insbesondere brettern |
-
1994
- 1994-12-23 AT AT0239394A patent/AT402295B/de not_active IP Right Cessation
-
1995
- 1995-11-27 TW TW084112620A patent/TW299324B/zh active
- 1995-12-13 WO PCT/EP1995/004921 patent/WO1996020183A1/de active IP Right Grant
- 1995-12-13 RU RU97112395/04A patent/RU2161610C2/ru not_active IP Right Cessation
- 1995-12-13 KR KR1019970704111A patent/KR100374731B1/ko not_active IP Right Cessation
- 1995-12-13 DE DE59504292T patent/DE59504292D1/de not_active Expired - Fee Related
- 1995-12-13 PL PL95320790A patent/PL187434B1/pl not_active IP Right Cessation
- 1995-12-13 EP EP95942138A patent/EP0799213B1/de not_active Expired - Lifetime
- 1995-12-13 BR BR9510606A patent/BR9510606A/pt not_active IP Right Cessation
- 1995-12-13 DK DK95942138T patent/DK0799213T3/da active
- 1995-12-13 RO RO97-01138A patent/RO115521B1/ro unknown
- 1995-12-13 AT AT95942138T patent/ATE173474T1/de not_active IP Right Cessation
- 1995-12-13 JP JP8520160A patent/JPH10511369A/ja active Pending
- 1995-12-13 CN CN95197017A patent/CN1068315C/zh not_active Expired - Fee Related
- 1995-12-13 NZ NZ298044A patent/NZ298044A/xx unknown
- 1995-12-13 ES ES95942138T patent/ES2124034T3/es not_active Expired - Lifetime
- 1995-12-19 HR HRA2393/94A patent/HRP950605B1/xx not_active IP Right Cessation
- 1995-12-22 IL IL11651695A patent/IL116516A/xx not_active IP Right Cessation
Also Published As
Publication number | Publication date |
---|---|
HRP950605A2 (en) | 1997-10-31 |
WO1996020183A1 (de) | 1996-07-04 |
IL116516A (en) | 2000-07-16 |
PL320790A1 (en) | 1997-10-27 |
DK0799213T3 (da) | 1999-08-02 |
DE59504292D1 (de) | 1998-12-24 |
IL116516A0 (en) | 1996-03-31 |
ATE173474T1 (de) | 1998-12-15 |
HRP950605B1 (en) | 1999-12-31 |
EP0799213B1 (de) | 1998-11-18 |
BR9510606A (pt) | 1999-02-23 |
ATA239394A (de) | 1996-08-15 |
RO115521B1 (ro) | 2000-03-30 |
AT402295B (de) | 1997-03-25 |
EP0799213A1 (de) | 1997-10-08 |
RU2161610C2 (ru) | 2001-01-10 |
TW299324B (zh) | 1997-03-01 |
PL187434B1 (pl) | 2004-07-30 |
ES2124034T3 (es) | 1999-01-16 |
CN1068315C (zh) | 2001-07-11 |
NZ298044A (en) | 1999-07-29 |
JPH10511369A (ja) | 1998-11-04 |
KR100374731B1 (ko) | 2003-06-09 |
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