CN104557616A - Method of synthesizing urea solution - Google Patents
Method of synthesizing urea solution Download PDFInfo
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- CN104557616A CN104557616A CN201410805818.0A CN201410805818A CN104557616A CN 104557616 A CN104557616 A CN 104557616A CN 201410805818 A CN201410805818 A CN 201410805818A CN 104557616 A CN104557616 A CN 104557616A
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- Prior art keywords
- ammonia
- high pressure
- carbon dioxide
- pressure
- water
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- 239000004202 carbamide Substances 0.000 title claims abstract description 31
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 28
- 230000002194 synthesizing effect Effects 0.000 title abstract 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 115
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 105
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 51
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 47
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 43
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 16
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 16
- 238000009833 condensation Methods 0.000 claims abstract description 11
- 230000005494 condensation Effects 0.000 claims abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 45
- 235000011089 carbon dioxide Nutrition 0.000 claims description 27
- 230000006835 compression Effects 0.000 claims description 10
- 238000007906 compression Methods 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 10
- 238000006356 dehydrogenation reaction Methods 0.000 claims description 8
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 7
- 239000003921 oil Substances 0.000 claims description 7
- 238000003860 storage Methods 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 6
- 238000006477 desulfuration reaction Methods 0.000 claims description 4
- 230000023556 desulfurization Effects 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000012535 impurity Substances 0.000 claims description 3
- 238000010791 quenching Methods 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 238000000354 decomposition reaction Methods 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 238000004880 explosion Methods 0.000 abstract description 3
- 230000003247 decreasing effect Effects 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 238000009434 installation Methods 0.000 abstract description 2
- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 abstract 4
- 238000012423 maintenance Methods 0.000 abstract 1
- 238000011084 recovery Methods 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 5
- 238000005260 corrosion Methods 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- PPBAJDRXASKAGH-UHFFFAOYSA-N azane;urea Chemical compound N.NC(N)=O PPBAJDRXASKAGH-UHFFFAOYSA-N 0.000 description 2
- 230000001351 cycling effect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- 235000009508 confectionery Nutrition 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
Abstract
The invention discloses a method of synthesizing a urea solution. The method comprises the following specific steps: (1) compressing carbon dioxide, and purifying the compressed carbon dioxide; (2) purifying ammonia, and delivering the purified ammonia; and (3) synthesizing urea solution. The decomposition rate of methylamine can be increased due to the self-stripping effect of ammonia, the low and medium-pressure decomposition and recovery load can be reduced, the power consumption be decreased accordingly, the heat from the condensation of methylamine separated under high temperature and high pressure can be utilized effectively, and the total energy consumption can be lowered. In addition, the production process has the advantages of high operating flexibility, high operating rate, low risk of explosion, convenience in installation and maintenance, secondary use of a condensate and no pollution. Furthermore, carbon dioxide and ammonia can be highly converted during the synthesis of the urea solution, the left unreacted carbon dioxide and ammonia can be recycled fully, nearly all the raw materials can be used, and the cost can be reduced greatly.
Description
Technical field
The present invention relates to a kind of method of urea synthesis solution, belong to chemical field.
Background technology
Urea is a kind of Chemicals of basis, and China is large agricultural country, and amount of urea is huge, and the relationship between productivity of urea is to National agricultural food safety.The production technique that current big-and-middle-sized urea plant adopts has: water solution total cycling method, middle pressure integrated ammonia urea process, carbon dioxide stripping process, ammonia stripping process.
Water solution total cycling method: the most of middle-size and small-size urea plant of this Fa Shi China produces the method adopted, mature production technology, convenient and reliable operation, pump and non-standard equipment all domesticize, be characterized in that in synthetic tower, transformation efficiency is higher, unreacted reactant adopts two sections of decomposition of reducing pressure, and power consumption is larger, tail gas pressure, temperature are all lower, and the danger of blast is little.
Carbon dioxide stripping process: from the seventies, China successively introduces tens cover carbon dioxide stripping process urea plants, mostly be large-scale plant, be characterized in that technical process is short, synthesis pressure is low, and power consumption is few, but operational condition is harsh, corrosion is comparatively serious, and tail gas fires danger, and turndown ratio is little.Modified version CO
2vaporizing extract process, unstripped gas has set up desulfurization dehydrogenation unit, alleviates corrosion, reduces explosion hazard, and meanwhile, one-time investment is also larger.
Middle pressure integrated ammonia urea process: this method is applicable to take Sweet natural gas as the synthesis ammonia plant of raw material, and be characterized in that thermal utilization is good, rate of decomposition is high, eliminates low pressure decomposition, simplifies flow process, because first ammonium temperature is higher, HO
2/ CO
2lower.The corrosion of first ammonium pump is comparatively serious, and the material requirements of pump is harsh.
All there is distinct disadvantage and limitation in visible above-mentioned main flow urea production process.
Summary of the invention
For prior art Problems existing, the invention provides a kind of method of urea synthesis solution, concrete steps comprise:
(1) carbonic acid gas, transported from carbon dioxide storage tank is first by a carbonic acid gas drop separator with water seal, by the water removing in carbon dioxide, then carbonic acid gas five sections of compressors are entered, carbon dioxide is after one, two, three section of compression, pressure is about 2.4MPa, temperature is 40 DEG C, after entering the desulfurization of oil removing desulfurizer, enter middle pressure CO2 heater steam heating, temperature rises to more than 150 DEG C, enter dehydrogenation reactor, the H in dehydrogenation reactor in carbon dioxide
2with other inflammable gass burned fall, then carbon dioxide enters middle pressure carbon dioxide cooler, gas-liquid separator is entered with after water quench, carbon dioxide after separation is back to carbon dioxide compressor four sections of entrances, again through four, five sections of compressions, final absolute pressure 14.6MPa;
(2), raw materials ammonia is sent here from ammonia storehouse, synthetic ammonia workshop, enter entrained solid impurity and oils in liquid ammonia filter removing liquefied ammonia, then liquefied ammonia dashpot is entered, high-pressure ammonia pump is entered after flow metering, send into high-pressure injector after liquefied ammonia being pressurized to absolute pressure 18.34MPa with high-pressure ammonia pump, high-pressure injector connects high pressure condenser;
(3) carbonic acid gas, through five sections of compressions sends into high pressure condenser top, also the top of high pressure condenser is delivered to from the liquefied ammonia that high-pressure injector is next, above-mentioned two kinds of logistics mix mutually in high pressure condenser, control to enter the NH that flow makes to enter high pressure condenser
3/ CO
2mol ratio is 3 ~ 3.5, high pressure condenser is provided with vertical tube, the temperature at high pressure condenser top is about 180 ~ 183 DEG C, flow to into urea synthesis tower bottom by the first ammonium liquid, ammonia and the carbon dioxide mixture that come bottom high pressure condenser by upflow tube, synthetic tower liquid level to remain on above upflow tube funnel at least 1 meter, be provided with 11 pieces of sieve plates in synthetic tower, urea soln flows out from urea synthesis tower bottom;
(4), containing unconverted NH
3and CO
2and rare gas element sends into high pressure scrubber by synthetic tower, in high pressure scrubber, NH
3and CO
2obtain sufficient condensation, water cooler is provided with in high pressure scrubber bottom, water cooler adopts tempered water to cool, with high pressure scrubber water circulating pump, tempered water is successively flow through high pressure scrubber and high pressure scrubber water recirculator, tempered water removes the heat of condensation in high pressure scrubber, thus make the temperature of tempered water be heated to 95 DEG C by 80 DEG C, this heat is removed by high pressure scrubber water recirculator, tempered water is cooled to 80 DEG C from 95 DEG C again, in this closed circulation system, temperature crosses the flow of high pressure scrubber water recirculator with control flow check and automatically controls, the liquefied ammonia that condensation obtains returns to ammonia storehouse, carbonic acid gas returns carbon dioxide storage tank.
Step enters CO in the carbon dioxide of carbonic acid gas drop separator in (1)
2volumetric concentration is more than 96%, and pressure is 0.005MPa, temperature≤40 DEG C.
Carbonic acid gas five sections of compressors are four row five cylinder opposed balance compressors.
The temperature of raw materials ammonia is about 30 DEG C, and absolute pressure is about 2.5MPa.
The invention has the advantages that:
(1) this production technique due to ammonia from stripping effect, first ammonium rate of decomposition is increased, thus in decreasing, low pressure decomposition reclaim load, power consumption reduces thereupon, the first ammonium be separated under High Temperature High Pressure, heat during its condensation is effectively utilized, and total energy consumption reduces, turndown ratio is large in addition, operation factor is high, and explosion hazard is little, and installation and repairing is convenient, process condensate can second stage employ, pollution-free;
(2) in urea soln building-up process, the transformation efficiency of carbonic acid gas and ammonia is high, and remains unreacted carbonic acid gas and ammonia and can circulate and make full use of, and raw material availability, close to 100%, greatly reduces cost.
Accompanying drawing explanation
Fig. 1 is compression and the purification process schematic diagram of carbon dioxide.
Fig. 2 is purification and the conveying schematic flow sheet of ammonia.
Fig. 3 is urea soln synthesis flow schematic diagram.
1-carbon dioxide storage tank, 2-carbonic acid gas drop separator, 3-carbonic acid gas five sections of compressors, 31 to 35-, one to five section of compressor, 4-oil removing desulfurizer, CO2 heater is pressed in 5-, 6-dehydrogenation reactor, carbon dioxide cooler is pressed in 7-, 8-gas-liquid separator, 9-high pressure condenser, 10-liquid ammonia filter, 11-liquefied ammonia dashpot, 12-high-pressure ammonia pump, 13-high-pressure injector, 14-urea synthesizer, 15-upflow tube, 16-high pressure scrubber, 17-high pressure scrubber water recirculator.
Embodiment
In conjunction with Figure of description 1-3, the method for urea synthesis solution of the present invention is specifically introduced:
(1) carbonic acid gas, from carbon dioxide storage tank 1 transported first by a carbonic acid gas drop separator 2 with water seal, by the water removing in carbon dioxide, enters CO in the carbon dioxide of carbonic acid gas drop separator 2
2volumetric concentration is more than 96%, and pressure is 0.005MPa, temperature≤40 DEG C.Then carbonic acid gas five sections of compressors 3 are entered, carbonic acid gas five sections of compressors are four row five cylinder opposed balance compressors, carbon dioxide is after one, two, three section of compression, pressure is about 2.4MPa, and temperature is 40 DEG C, after entering oil removing desulfurizer 4 desulfurization, enter middle pressure CO2 heater 5 steam heating, temperature rises to more than 150 DEG C, enters dehydrogenation reactor 6, the H in dehydrogenation reactor 6 in carbon dioxide
2with other inflammable gass burned fall, then carbon dioxide enters middle pressure carbon dioxide cooler 7, with entering gas-liquid separator 8 after water quench, carbon dioxide after separation is back to carbon dioxide compressor four section of 34 entrance, again through four, five sections of compressions, final absolute pressure 14.6MPa;
(2), temperature is about 30 DEG C, the raw materials ammonia that absolute pressure is about 2.5MPa is sent here from ammonia storehouse, synthetic ammonia workshop, enter liquid ammonia filter 10 and remove entrained solid impurity and oils in liquefied ammonia, then liquefied ammonia dashpot 11 is entered, high-pressure ammonia pump 12 is entered after flow metering, send into high-pressure injector 13 after liquefied ammonia being pressurized to absolute pressure 18.34MPa with high-pressure ammonia pump 12, high-pressure injector 13 connects high pressure condenser 9;
(3) carbonic acid gas, through five sections of compressions sends into high pressure condenser 9 top, also the top of high pressure condenser 9 is delivered to from the liquefied ammonia that high-pressure injector is next, above-mentioned two kinds of logistics mix mutually in high pressure condenser, control to enter the NH that flow makes to enter high pressure condenser
3/ CO
2mol ratio is 3 ~ 3.5, high pressure condenser 9 is provided with vertical tube, the temperature at high pressure condenser 9 top is about 180 ~ 183 DEG C, flow to bottom urea synthesizer 14 by the first ammonium liquid, ammonia and the carbon dioxide mixture that come bottom high pressure condenser 9 by upflow tube, synthetic tower liquid level to remain on above upflow tube 15 funnel at least 1 meter, be provided with 11 pieces of sieve plates in synthetic tower, urea soln flows out bottom urea synthesizer 14;
(4), containing unconverted NH
3and CO
2and rare gas element sends into high pressure scrubber 16 by synthetic tower, in high pressure scrubber, NH
3and CO
2obtain sufficient condensation, water cooler 17 is provided with in high pressure scrubber bottom, water cooler adopts tempered water to cool, with high pressure scrubber water circulating pump, tempered water is successively flow through high pressure scrubber 16 and high pressure scrubber water recirculator 17, tempered water removes the heat of condensation in high pressure scrubber, thus make the temperature of tempered water be heated to 95 DEG C by 80 DEG C, this heat is removed by high pressure scrubber water recirculator, tempered water is cooled to 80 DEG C from 95 DEG C again, in this closed circulation system, temperature crosses the flow of high pressure scrubber water recirculator with control flow check and automatically controls, the liquefied ammonia that condensation obtains returns to ammonia storehouse, carbonic acid gas returns carbon dioxide storage tank 1.
Claims (4)
1. a method for urea synthesis solution, is characterized in that concrete steps comprise:
(1) carbonic acid gas, transported from carbon dioxide storage tank is first by a carbonic acid gas drop separator with water seal, by the water removing in carbon dioxide, then carbonic acid gas five sections of compressors are entered, carbon dioxide is after one, two, three section of compression, pressure is about 2.4MPa, temperature is 40 DEG C, after entering the desulfurization of oil removing desulfurizer, enter middle pressure CO2 heater steam heating, temperature rises to more than 150 DEG C, enter dehydrogenation reactor, the H in dehydrogenation reactor in carbon dioxide
2with other inflammable gass burned fall, then carbon dioxide enters middle pressure carbon dioxide cooler, gas-liquid separator is entered with after water quench, carbon dioxide after separation is back to carbon dioxide compressor four sections of entrances, again through four, five sections of compressions, final absolute pressure 14.6MPa;
(2), raw materials ammonia is sent here from ammonia storehouse, synthetic ammonia workshop, enter entrained solid impurity and oils in liquid ammonia filter removing liquefied ammonia, then liquefied ammonia dashpot is entered, high-pressure ammonia pump is entered after flow metering, send into high-pressure injector after liquefied ammonia being pressurized to absolute pressure 18.34MPa with high-pressure ammonia pump, high-pressure injector connects high pressure condenser;
(3) carbonic acid gas, through five sections of compressions sends into high pressure condenser top, also the top of high pressure condenser is delivered to from the liquefied ammonia that high-pressure injector is next, above-mentioned two kinds of logistics mix mutually in high pressure condenser, control to enter the NH that flow makes to enter high pressure condenser
3/ CO
2mol ratio is 3 ~ 3.5, high pressure condenser is provided with vertical tube, the temperature at high pressure condenser top is about 180 ~ 183 DEG C, flow to into urea synthesis tower bottom by the first ammonium liquid, ammonia and the carbon dioxide mixture that come bottom high pressure condenser by upflow tube, synthetic tower liquid level to remain on above upflow tube funnel at least 1 meter, be provided with 11 pieces of sieve plates in synthetic tower, urea soln flows out from urea synthesis tower bottom;
(4), containing unconverted NH
3and CO
2and rare gas element sends into high pressure scrubber by synthetic tower, in high pressure scrubber, NH
3and CO
2obtain sufficient condensation, water cooler is provided with in high pressure scrubber bottom, water cooler adopts tempered water to cool, with high pressure scrubber water circulating pump, tempered water is successively flow through high pressure scrubber and high pressure scrubber water recirculator, tempered water removes the heat of condensation in high pressure scrubber, thus make the temperature of tempered water be heated to 95 DEG C by 80 DEG C, this heat is removed by high pressure scrubber water recirculator, tempered water is cooled to 80 DEG C from 95 DEG C again, in this closed circulation system, temperature crosses the flow of high pressure scrubber water recirculator with control flow check and automatically controls, the liquefied ammonia that condensation obtains returns to ammonia storehouse, carbonic acid gas returns carbon dioxide storage tank.
2. the method for urea synthesis solution according to claim 1, is characterized in that, step enters CO in the carbon dioxide of carbonic acid gas drop separator in (1)
2volumetric concentration is more than 96%, and pressure is 0.005MPa, temperature≤40 DEG C.
3. the method for urea synthesis solution according to claim 1, is characterized in that, carbonic acid gas five sections of compressors are four row five cylinder opposed balance compressors.
4. the method for urea synthesis solution according to claim 1, is characterized in that, the temperature of raw materials ammonia is about 30 DEG C, and absolute pressure is about 2.5MPa.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410805818.0A CN104557616B (en) | 2014-12-22 | 2014-12-22 | A kind of method of urea synthesis solution |
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|---|---|---|---|
| CN201410805818.0A CN104557616B (en) | 2014-12-22 | 2014-12-22 | A kind of method of urea synthesis solution |
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| CN104557616A true CN104557616A (en) | 2015-04-29 |
| CN104557616B CN104557616B (en) | 2016-06-22 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109516931A (en) * | 2018-12-12 | 2019-03-26 | 河南心连心化肥有限公司 | The device and production technology of a kind of low biuret urea for vehicle solution of continuous production |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0504966A1 (en) * | 1991-03-22 | 1992-09-23 | SNAMPROGETTI S.p.A. | Urea production process of high energy efficiency |
| CN1074901A (en) * | 1992-12-23 | 1993-08-04 | 中国五环化学工程公司 | Producing urea with increased yield by stripping with CO 2 novel process and device |
| CN1086511A (en) * | 1993-08-02 | 1994-05-11 | 中国五环化学工程总公司 | Energy-conservation, joint money, safety type urea production process and device |
| US5849952A (en) * | 1989-09-15 | 1998-12-15 | Shamprogetti S.P.A. | Urea production process with high energy efficiency |
| CN1554643A (en) * | 2003-12-25 | 2004-12-15 | 黑龙江黑化集团有限公司 | Method and apparatus for improving industrial producing urea |
-
2014
- 2014-12-22 CN CN201410805818.0A patent/CN104557616B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5849952A (en) * | 1989-09-15 | 1998-12-15 | Shamprogetti S.P.A. | Urea production process with high energy efficiency |
| EP0504966A1 (en) * | 1991-03-22 | 1992-09-23 | SNAMPROGETTI S.p.A. | Urea production process of high energy efficiency |
| CN1074901A (en) * | 1992-12-23 | 1993-08-04 | 中国五环化学工程公司 | Producing urea with increased yield by stripping with CO 2 novel process and device |
| CN1086511A (en) * | 1993-08-02 | 1994-05-11 | 中国五环化学工程总公司 | Energy-conservation, joint money, safety type urea production process and device |
| CN1554643A (en) * | 2003-12-25 | 2004-12-15 | 黑龙江黑化集团有限公司 | Method and apparatus for improving industrial producing urea |
Non-Patent Citations (1)
| Title |
|---|
| 孙盛杰和杨树禹: "浅谈尿素的工艺流程及设计特点", 《黑龙江科技信息》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109516931A (en) * | 2018-12-12 | 2019-03-26 | 河南心连心化肥有限公司 | The device and production technology of a kind of low biuret urea for vehicle solution of continuous production |
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Effective date of registration: 20170317 Address after: 073099 Hebei City, North Street, the main street of the city of heaven and earth home, room 3, unit 502, room 6, room Patentee after: Du Jinzhi Patentee after: He Hui Address before: 312432 Zhejiang city of Shaoxing province Shengzhou City Lake Yan Street West Backstreet 66 Jinshan scenic garden room 908 Patentee before: SHENGZHOU PILOTAGE INFORMATION TECHNOLOGY CO., LTD. |
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