CN104080765A - 用于生产高纯度结晶尿素的方法 - Google Patents
用于生产高纯度结晶尿素的方法 Download PDFInfo
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- CN104080765A CN104080765A CN201280055878.4A CN201280055878A CN104080765A CN 104080765 A CN104080765 A CN 104080765A CN 201280055878 A CN201280055878 A CN 201280055878A CN 104080765 A CN104080765 A CN 104080765A
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- urea
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C273/00—Preparation of urea or its derivatives, i.e. compounds containing any of the groups, the nitrogen atoms not being part of nitro or nitroso groups
- C07C273/02—Preparation of urea or its derivatives, i.e. compounds containing any of the groups, the nitrogen atoms not being part of nitro or nitroso groups of urea, its salts, complexes or addition compounds
- C07C273/14—Separation; Purification; Stabilisation; Use of additives
- C07C273/16—Separation; Purification
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/42—Electrodialysis; Electro-osmosis ; Electro-ultrafiltration; Membrane capacitive deionization
- B01D61/422—Electrodialysis
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C237/00—Carboxylic acid amides, the carbon skeleton of the acid part being further substituted by amino groups
- C07C237/02—Carboxylic acid amides, the carbon skeleton of the acid part being further substituted by amino groups having the carbon atoms of the carboxamide groups bound to acyclic carbon atoms of the carbon skeleton
- C07C237/16—Carboxylic acid amides, the carbon skeleton of the acid part being further substituted by amino groups having the carbon atoms of the carboxamide groups bound to acyclic carbon atoms of the carbon skeleton the carbon skeleton being acyclic and unsaturated
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/58—Multistep processes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/02—Crystallisation from solutions
- B01D9/04—Crystallisation from solutions concentrating solutions by removing frozen solvent therefrom
Abstract
本发明涉及用于生产高纯度结晶尿素的方法。该方法包括尿素的结晶和干燥，其中，将水性尿素溶液从+30℃预热至+130℃，然后，将溶液在400V-600V范围内的电压下通过电渗析而被提纯。技术结果是，生产可作为食品工业中的添加剂和作为实验室分析中的试剂使用的高纯度结晶尿素。
Description
本发明涉及尿素生产领域，具体涉及用于生产高纯度结晶尿素的方法。
目前，有很多广为人知的方法来制备粒状和结晶尿素。生产尿素的工业方法是基于从二氧化碳和氨获得的水性尿素溶液的结晶。然而，通过已知方法获得的尿素不具有足够的纯度以用于食品工业和用作实验室分析的试剂。
作为原型选择的最接近的技术方案是一种用于生产在二氧化碳和氨的基础上所获得的结晶尿素的方法(专利RU2041202)。该方法包括在过饱和溶液的整个体积中进行尿素的结晶，从晶体除去水以获得致密块状体，随后通过过滤除去尿素晶体并进行其干燥。然而，所获得的尿素也不具有足够的纯度以用于食品工业和用作实验室分析的试剂。
所要求保护的本发明的目的是提供一种高纯度结晶尿素。
该目的通过一种从水性尿素溶液生产高纯度结晶尿素的方法实现，根据本发明，该方法包括尿素结晶和干燥，将水性尿素溶液的温度从+30℃加热至+130℃，之后将溶液在400V-600V范围内的电压下通过电渗析提纯，其中，溶液在30％的浓度下被加热至+30℃，在50％的浓度下被加热至+40-50℃，在70％的浓度下被加热至+70-80℃，在90％和更高的浓度下被加热至+90-130℃。
图1中示出了用于实施本发明方法的装置。该装置包括用于原始尿素溶液的储存容器1、电渗析单元2、用于将该溶液从容器1供应到电渗析单元2的泵3、用于纯化的尿素溶液的容器4、用于将纯化的尿素溶液供应到容器4的泵5、蒸发和结晶单元6、用于将净化的尿素从容器4供应到该蒸发和结晶单元6的泵7。
该方法执行如下。将位于储存容器1中的未加工的(crude)水性尿素溶液从+30℃加热到+130℃的操作温度，以避免尿素的早期结晶，其中，溶液在30％的浓度下被加热至+30℃，在50％的浓度下被加热至+40-50℃，在70％的浓度下被加热至+70-80℃，在90％和更高的浓度下被加热至+100-120℃。溶液的浓度与其加热温度之间的关系根据经验确定并在表1中示出。
表1
从表1可见，尿素在尿素溶液的温度低于30℃时被部分地转换成结晶状态。当加热该溶液高于130℃时，发生尿素的部分水解并且它被二聚化成缩二脲，缩二脲的含量在纯化的尿素中是严格标准化的。
然后，通过泵3将该溶液供应至电渗析单元2。在电渗析单元2中，通过400V-600V的电流从溶液中去掉盐形成离子。这个范围提供了该过程的最佳性能：数量/质量比率。当电压高于600V时，所得到的产品不满足实验室分析过程中和食品工业中应用的纯化尿素的要求。当电压低于400V时，电渗析纯化过程很慢，使得该过程的效率降低。在去离子处理之后，纯化溶液被泵5供应到储存容器4，然后被泵7供应到该蒸发和结晶单元6，在该蒸发和结晶单元中，溶液被分离成纯化的结晶尿素(尿素结晶)和去离子水。通过在大气压下或在50-80℃的50-10mmHg的真空压力下将溶液从110℃加热至150℃的温度，执行尿素结晶以及与其同时进行的干燥。
表2中示出了通过所要求保护的方法获得的尿素的质量参数。
因此，所获得的结晶尿素的纯度允许其作为食品工业中的添加剂(食品添加剂E927b)和作为实验室分析中的试剂使用。
此外，所得到的高纯度结晶尿素被包装在聚丙烯袋或其他类似容器中。所得到的去离子水是以下目标应用的副产物：用作挡风玻璃清洗装置的防冻溶液和不冻溶液的一种成分。
Claims (2)
1.一种用于从水性尿素溶液生产高纯度结晶尿素的方法，包括尿素结晶和干燥，其特征在于，将所述水性尿素溶液从+30℃加热至+130℃的温度，之后，将所述溶液在400V-600V范围内的电压下通过电渗析而被提纯。
2.根据权利要求1所述的方法，其特征在于，所述水性尿素溶液在30％的浓度下被加热至20-30℃，在50％的浓度下被加热至50-60℃，在70％的浓度下被加热至70-80℃，在90％和更高的浓度下被加热至90-130℃。
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| RU2011147680/04A RU2472777C1 (ru) | 2011-11-23 | 2011-11-23 | Способ получения кристаллического карбамида высокой очистки |
| PCT/RU2012/001014 WO2013077775A2 (ru) | 2011-11-23 | 2012-12-03 | Способ получения кристаллического карбамида высокой очистки |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104080765A true CN104080765A (zh) | 2014-10-01 |
| CN104080765B CN104080765B (zh) | 2016-08-17 |
Family
ID=48470397
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201280055878.4A Expired - Fee Related CN104080765B (zh) | 2011-11-23 | 2012-12-03 | 用于生产高纯度结晶尿素的方法 |
Country Status (25)
| Country | Link |
|---|---|
| US (1) | US9192893B2 (zh) |
| EP (1) | EP2784060B1 (zh) |
| CN (1) | CN104080765B (zh) |
| AT (1) | AT515241B1 (zh) |
| AU (1) | AU2012341102B9 (zh) |
| BG (1) | BG66591B1 (zh) |
| BR (1) | BR112014011817B1 (zh) |
| CA (1) | CA2856276C (zh) |
| CZ (1) | CZ305573B6 (zh) |
| DE (1) | DE112012004881T5 (zh) |
| DK (1) | DK178065B1 (zh) |
| ES (1) | ES2486640B1 (zh) |
| FI (1) | FI126352B (zh) |
| GB (1) | GB2538483A (zh) |
| HU (1) | HUP1400301A2 (zh) |
| MX (1) | MX2014006222A (zh) |
| NO (1) | NO20140641A1 (zh) |
| PL (1) | PL222478B1 (zh) |
| PT (1) | PT2013077775B (zh) |
| RO (1) | RO131559A2 (zh) |
| RU (1) | RU2472777C1 (zh) |
| SE (1) | SE537706C2 (zh) |
| SG (1) | SG11201402507YA (zh) |
| UA (1) | UA111241C2 (zh) |
| WO (1) | WO2013077775A2 (zh) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110357284A (zh) * | 2019-06-27 | 2019-10-22 | 福建中源新能源股份有限公司 | 一种船用尿素溶液的制备方法及其应用 |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110548403A (zh) * | 2018-05-31 | 2019-12-10 | 河南仁华生物科技有限公司 | 一种医药中间体的脱盐及浓缩方法 |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3903158A (en) * | 1973-05-16 | 1975-09-02 | Mexico Guanos | Process for reducing the biuret content in urea |
| WO1989001468A1 (en) * | 1987-08-13 | 1989-02-23 | Austral-Pacific Fertilizers Ltd. | Process for enhanced urea production |
| RU2041202C1 (ru) * | 1992-12-09 | 1995-08-09 | Научно-инженерный центр "Инфомир" | Способ получения кристаллического карбамида |
| CN102584635A (zh) * | 2012-01-09 | 2012-07-18 | 四川泸天化股份有限公司 | 一种车用尿素的制备方法 |
Family Cites Families (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3124612A (en) * | 1964-03-10 | Urea crystallization | ||
| GB690594A (en) * | 1950-04-06 | 1953-04-22 | Basf Ag | Improvements in the production of urea |
| US2892870A (en) * | 1955-11-21 | 1959-06-30 | Lonza Electric & Chem Works | Process for purifying and crystallizing urea |
| NL285601A (zh) * | 1961-11-28 | |||
| GB1148572A (en) * | 1966-02-05 | 1969-04-16 | Power Gas Ltd | Process for the production of coarse crystals of urea |
| FR2036413A5 (zh) * | 1969-03-13 | 1970-12-24 | Thomson Csf | |
| GB1404098A (en) * | 1973-05-16 | 1975-08-28 | Mexico Guanos | Process for reducing the biuret content in urea |
| US5645703A (en) * | 1995-12-20 | 1997-07-08 | University Of Chicago | Electrodialysis-based separation process for salt recovery and recycling from waste water |
| NZ503576A (en) * | 1999-03-26 | 2002-10-25 | Snow Brand Milk Products Co Ltd | Method of isolating urea from an urea containing solution using a nanofiltration membrane or reverse osmotic membrane |
| WO2006061082A1 (en) * | 2004-12-08 | 2006-06-15 | Dsm Ip Assets B.V. | Process for the removal of ammonia from an ammonia-containing gas stream |
| EP1857439A1 (en) * | 2006-05-17 | 2007-11-21 | Kemira GrowHow Oyj | Method for purifying aqueous urea solution |
| JP2008280263A (ja) * | 2007-05-09 | 2008-11-20 | Mitsui Chemicals Inc | 高純度尿素水の製造方法 |
| ITMI20072206A1 (it) * | 2007-11-21 | 2009-05-22 | Snam Progetti | Metodo per il recupero di ammoniaca da una corrente gassosa in un processo di sintesi di urea |
-
2011
- 2011-11-23 RU RU2011147680/04A patent/RU2472777C1/ru not_active IP Right Cessation
- 2011-11-23 RO ROA201400380A patent/RO131559A2/ro unknown
-
2012
- 2012-03-12 UA UAA201405505A patent/UA111241C2/uk unknown
- 2012-12-03 CA CA2856276A patent/CA2856276C/en not_active Expired - Fee Related
- 2012-12-03 CZ CZ2014-354A patent/CZ305573B6/cs not_active IP Right Cessation
- 2012-12-03 GB GB1408531.0A patent/GB2538483A/en not_active Withdrawn
- 2012-12-03 SG SG11201402507YA patent/SG11201402507YA/en unknown
- 2012-12-03 AU AU2012341102A patent/AU2012341102B9/en not_active Ceased
- 2012-12-03 BR BR112014011817-5A patent/BR112014011817B1/pt not_active IP Right Cessation
- 2012-12-03 DE DE112012004881.4T patent/DE112012004881T5/de not_active Withdrawn
- 2012-12-03 ES ES201490054A patent/ES2486640B1/es active Active
- 2012-12-03 AT ATA9437/2012A patent/AT515241B1/de not_active IP Right Cessation
- 2012-12-03 PT PT2012001014A patent/PT2013077775B/pt active IP Right Grant
- 2012-12-03 WO PCT/RU2012/001014 patent/WO2013077775A2/ru active Application Filing
- 2012-12-03 MX MX2014006222A patent/MX2014006222A/es unknown
- 2012-12-03 SE SE1450590A patent/SE537706C2/sv not_active IP Right Cessation
- 2012-12-03 HU HU1400301A patent/HUP1400301A2/hu unknown
- 2012-12-03 CN CN201280055878.4A patent/CN104080765B/zh not_active Expired - Fee Related
- 2012-12-03 PL PL408264A patent/PL222478B1/pl unknown
- 2012-12-03 US US14/360,347 patent/US9192893B2/en not_active Expired - Fee Related
- 2012-12-03 EP EP12850929.6A patent/EP2784060B1/en not_active Not-in-force
- 2012-12-03 BG BG111761A patent/BG66591B1/bg unknown
-
2014
- 2014-05-05 FI FI20145406A patent/FI126352B/en not_active IP Right Cessation
- 2014-05-15 DK DK201470284A patent/DK178065B1/da not_active IP Right Cessation
- 2014-05-22 NO NO20140641A patent/NO20140641A1/no not_active Application Discontinuation
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3903158A (en) * | 1973-05-16 | 1975-09-02 | Mexico Guanos | Process for reducing the biuret content in urea |
| US3903158B1 (zh) * | 1973-05-16 | 1984-02-21 | ||
| WO1989001468A1 (en) * | 1987-08-13 | 1989-02-23 | Austral-Pacific Fertilizers Ltd. | Process for enhanced urea production |
| RU2041202C1 (ru) * | 1992-12-09 | 1995-08-09 | Научно-инженерный центр "Инфомир" | Способ получения кристаллического карбамида |
| CN102584635A (zh) * | 2012-01-09 | 2012-07-18 | 四川泸天化股份有限公司 | 一种车用尿素的制备方法 |
Non-Patent Citations (1)
| Title |
|---|
| 周永益: "硫脲溶液净化除铜的电渗析法", 《有色矿冶》, no. 3, 30 June 1995 (1995-06-30), pages 59 - 60 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110357284A (zh) * | 2019-06-27 | 2019-10-22 | 福建中源新能源股份有限公司 | 一种船用尿素溶液的制备方法及其应用 |
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