NZ625024B2 - Method for producing high-purity crystalline carbamide - Google Patents
Method for producing high-purity crystalline carbamide Download PDFInfo
- Publication number
- NZ625024B2 NZ625024B2 NZ625024A NZ62502412A NZ625024B2 NZ 625024 B2 NZ625024 B2 NZ 625024B2 NZ 625024 A NZ625024 A NZ 625024A NZ 62502412 A NZ62502412 A NZ 62502412A NZ 625024 B2 NZ625024 B2 NZ 625024B2
- Authority
- NZ
- New Zealand
- Prior art keywords
- carbamide
- solution
- concentration
- purity crystalline
- producing high
- Prior art date
Links
- XSQUKJJJFZCRTK-UHFFFAOYSA-N urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 title claims abstract description 50
- 229960000539 carbamide Drugs 0.000 title claims abstract description 49
- 235000013877 carbamide Nutrition 0.000 title claims abstract description 49
- 239000004202 carbamide Substances 0.000 title claims abstract description 49
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 12
- 238000002425 crystallisation Methods 0.000 claims abstract description 12
- 230000005712 crystallization Effects 0.000 claims abstract description 12
- 238000000909 electrodialysis Methods 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 6
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 5
- 239000000654 additive Substances 0.000 abstract description 3
- 230000000996 additive Effects 0.000 abstract description 3
- 238000004458 analytical method Methods 0.000 abstract 2
- 238000004450 types of analysis Methods 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- OHJMTUPIZMNBFR-UHFFFAOYSA-N biuret Chemical compound NC(=O)NC(N)=O OHJMTUPIZMNBFR-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 239000004743 Polypropylene Substances 0.000 description 1
- 230000002528 anti-freeze Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 150000001805 chlorine compounds Chemical class 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 235000013373 food additive Nutrition 0.000 description 1
- 239000002778 food additive Substances 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- -1 polypropylene Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
Classifications
-
- 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
-
- 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
-
- 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
-
- 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
Abstract
Disclosed herein is a method for producing high-purity crystalline carbamide. The method comprises the crystallization and drying of carbamide, wherein an aqueous carbamide solution is preheated from +30°C to +130°C, and thereafter the solution is purified by electrodialysis at a voltage in the range of 400 V - 600 V. The result is the production of high-purity crystalline carbamide that can be used as an additive in the food industry and as a reagent in laboratory analysis. e of 400 V - 600 V. The result is the production of high-purity crystalline carbamide that can be used as an additive in the food industry and as a reagent in laboratory analysis.
Description
METHOD FOR PRODUCING HIGH-PURITY CRYSTALLINE CARBAMIDE
Description:
The invention relates to the field of carbamide production, particularly to the method for
producing high purity crystalline carbamide.
At the present time there are widely known methods for preparing granulated and crystalline
carbamide. Industrial methods for producing carbamide are based on the crystallization of
aqueous carbamide solution obtained from carbon dioxide and ammonia. However, carbamide
obtained by known methods does not have sufficient degree of purity for use in the food
industry and for use as a reagent for laboratory analyses.
The closest technical solution chosen as a prototype is a method for producing crystalline
carbamide obtained on the basis of carbon dioxide and ammonia (Patent RU 2041202). The
method comprises crystallization of carbamide in the whole volume of the supersaturated
solution, water removal from crystals to obtain compact mass, followed by removal of
carbamide crystals by filtration and their drying. However, the obtained carbamide also does
not have sufficient degree of purity for use in the food industry and for use as a reagent for
laboratory analyses.
The object of the claimed invention is to provide a high purity crystalline carbamide.
The object is achieved by a method for producing high purity crystalline carbamide from an
aqueous carbamide solution, comprising carbamide crystallization and drying according to the
invention, the aqueous carbamide solution is heated to the temperature from +30°C to +130°C,
and thereafter the solution is purified by electrodialysis at a voltage in the range of 400 V - 600
V, wherein the solution is heated to +30°C at a concentration of 30%, to +40-50°C at a
concentration of 50%, to +70-80°C at a concentration of 70%, to +90-130°C at a concentration
of 90% and higher.
A definition of a specific embodiment of the invention claimed herein follows.
In a broad format, the invention provides a method for producing high purity crystalline
carbamide from an aqueous carbamide solution, comprising carbamide crystallization and
drying, characterized in that the aqueous carbamide solution is heated to a temperature from
+30°C to +130°C, whereupon the solution is purified by electrodialysis at a voltage in the range
of 400V - 600V.
Device for implementing the inventive method is shown in Figure 1. The device comprises a
storage container 1 for the initial carbamide solution, electrodialysis unit 2, a pump 3 for
supplying the solution from the container 1 to electrodialysis unit 2, a container 4 for the
purified carbamide solution, a pump 5 for supplying the purified carbamide solution to the
container 4, evaporation and crystallization unit 6, a pump 7 for supplying the purified
carbamide from the container 4 to the evaporation and crystallization unit 6.
The method is performed as follows. The crude aqueous carbamide solution located in the
storage container 1 is heated to the operating temperature from +30°C to +130°C to avoid early
crystallisation of carbamide, wherein the solution is heated to +30°C at a concentration of 30%,
to +40-50°C at a concentration of 50%, to +70-80°C at a concentration of 70%, to +100-120°C
at a concentration of 90% and above. The relation between the concentration of the solution
and the heating temperature thereof is determined empirically and is shown in Figure 2.
As seen from Figure 2, carbamide is partially converted to crystalline state at the temperature of
the carbamide solution less than 30°C. Upon heating the solution above 130°C, a partial
hydrolysis of urea occurs and it is dimerized to biuret, which content in the purified carbamide
is strictly normalized.
Then the solution is supplied by the pump 3 to the electrodialysis unit 2. In the electrodialysis
unit 2, salt-forming ions are removed from the solution by the electric current of 400V-600V.
This range provides the optimal performance of the process: the amount/quality ratio. When the
voltage is above 600V, the resulting product does not meet the requirements of the purified
carbamide, applicable during laboratory analyses and in the food industry. When the voltage is
below 400V, electrodialysis purification process is slow, so that the efficiency of the process is
reduced. After deionization process, purified solution is supplied by the pump 5 to the storage
container 4, and then is supplied by the pump 7 to the evaporation and crystallization unit 6,
where the solution is separated to purified crystalline carbamide (carbamide crystallization) and
deionized water. Carbamide crystallization with its simultaneous drying is performed by
heating the solution to the temperature from 110°C to 150°C under atmospheric pressure or
under vacuum pressure of 50 - 10 mm Hg. 50-80°C.
Quality parameters of carbamide obtained by the claimed method is shown in the Table 1.
Table 1
Parameter name Value
1. Mass fraction of carbamide (CH ON ), %, not less 99.8
2. Melting temperature, °C 132.7±1
3. Mass fraction of water-insoluble components, %, up to 0.003
4. Mass fraction of residues after baking (in the form of sulphates), %, up to 0.01
6. Mass fraction of sulphates (SO ), %, up to 0.001
7. Mass fraction of chlorides (Cl), %, up to 0.0005
8. Mass fraction of ferrum (Fe), %, up to 0.0001
9. Mass fraction of heavy metals (Pb), %, up to 0.0002
. Mass fraction of free ammonia (NH ), %, up to 0.005
11. Mass fraction of biuret, %, up to 0.1
Thus, the degree of purity of the obtained crystalline carbamide allows its use as an additive in
the food industry (food additive Е927b) and as a reagent for laboratory analyses.
Further, the obtained high purity crystalline carbamide is packaged in polypropylene bags or
other similar containers. The obtained de-ionized water is a by-product with a target
application: the use as a component of anti-freeze and non-freezing solution for windshields
washer.
Claims (2)
1. A method for producing high purity crystalline carbamide from an aqueous carbamide solution, comprising carbamide crystallization and drying, characterized in that the aqueous carbamide solution is heated to a temperature from +30°C to +130°C, whereupon the solution is purified by electrodialysis at a voltage in the range of 400V - 600V.
2. The method according to claim 1, characterized in that the aqueous carbamide solution is heated to: 30°C at a concentration of 30%; 50-60°C at a concentration of 50%; 70-80°C at a concentration of 70%; or 90-130°C at a concentration of 90% and higher. Farid Alekovich Batullin & Andrei Vladimirovich Andreev By the patent attorneys for the applicants CULLENS
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| RU2011147680/04A RU2472777C1 (en) | 2011-11-23 | 2011-11-23 | Method of producing high-purity crystalline carbamide |
| RU2011147680 | 2011-11-23 | ||
| PCT/RU2012/001014 WO2013077775A2 (en) | 2011-11-23 | 2012-12-03 | Method for producing high-purity crystalline carbamide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| NZ625024A NZ625024A (en) | 2016-09-30 |
| NZ625024B2 true NZ625024B2 (en) | 2017-01-05 |
Family
ID=
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102806011A (en) | Method for preparing automobile urea liquid reducing agent | |
| CA2856276C (en) | Method for producing high-purity crystalline carbamide | |
| CN104004926A (en) | Method for preparing high-purity vanadium pentoxide through sodium polyvanadate | |
| CN101219946B (en) | Method for recycling waste liquor of ammonium hexanedioic acid and recycling system thereof | |
| CN108840354B (en) | Deep impurity removal method for battery-grade lithium chloride | |
| NZ625024B2 (en) | Method for producing high-purity crystalline carbamide | |
| CN104925844A (en) | Method for refining high-purity cerium carbonate | |
| CN104129811A (en) | Process for preparing zinc sulfate | |
| JP6067736B2 (en) | Method for producing high purity crystalline carbamide | |
| CN110885357B (en) | Method for separating and purifying glutamine dipeptide by nanofiltration membrane | |
| CN104399448A (en) | Catalyst zinc oxide and preparation method thereof | |
| WO2009054618A3 (en) | Method for achieving high purity separation and refinement by controlling morphology and particle size of 2,6-dimethylnaphthalene crystals | |
| CN104045071A (en) | Efficient impurity-removing production method for industrial monoammonium phosphate extracted in ammonium phosphate production process | |
| CN104447287A (en) | Preparation method of diammonium hydrogen citrate |