CN101928016A - Process for producing ammonium sulfate by adopting negative pressure double-countercurrent evaporation and crystallization mode - Google Patents
Process for producing ammonium sulfate by adopting negative pressure double-countercurrent evaporation and crystallization mode Download PDFInfo
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- CN101928016A CN101928016A CN2009100163718A CN200910016371A CN101928016A CN 101928016 A CN101928016 A CN 101928016A CN 2009100163718 A CN2009100163718 A CN 2009100163718A CN 200910016371 A CN200910016371 A CN 200910016371A CN 101928016 A CN101928016 A CN 101928016A
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Abstract
The invention relates to a process for producing ammonium sulfate by adopting a negative pressure double-countercurrent evaporation and crystallization mode. One-effect evaporation and crystallization equipment comprises an evaporator, a crystallizer circulating pump and a crystallization heater; two-effect condensation and evaporation equipment comprises a condensation evaporator, a condenser heater and a condenser circulating pump; and the evaporation of the one-effect evaporation and crystallization equipment and the two-effect condensation and evaporation equipment is carried out under negative pressure by using a vacuum pump and a communicating pipe between the one-effect evaporation and crystallization equipment and the two-effect condensation and evaporation equipment. The one-effect evaporation and crystallization equipment is heated by using medium pressure steam for crystallization and evaporation, then secondary steam evaporated by the one-effect evaporation and crystallization equipment is utilized to provide a heat source for the two-effect condensation and evaporation equipment for extracting a feed solution, and condensed materials enter the crystallization evaporator of the one-effect condensation and evaporation equipment to form a saturated ammonium sulfate crystal solution, and centrifugally separated to obtain a finished product of the ammonium sulfate. Steam evaporated by the two-effect condensation and evaporation equipment is condensed and cooled by the condenser and an emptying cooler, condensate enters a quenching water tank, and noncondensable gas is discharged through a water-ring vacuum pump. Heat value of secondary steam evaporated by the one-effect evaporation and crystallization equipment after reconstruction is utilized fully, which reduces the consumption of heating steam, and lowers the temperature of steam evaporated by the two-effect evaporation and crystallization equipment.
Description
Technical field
The invention belongs to sulphur ammonium production equipment, particularly a kind of processing method that adopts negative pressure double-countercurrent evaporation and crystallization mode to produce ammonium sulfate.
Background technology
Ammonia obtains ammonium sulfate products through centrifugation after blasting and making it reach supersaturation in the dilute sulphuric acid, but after introducing the large nitrogen fertilizer plant of producing urea certainly, the also urea of changing products of former middle nitrogen fertilizer production device more.At present, the sulphur ammonium mainly absorbs the ammonia in the coke(oven)gas by dilute sulphuric acid or carries out the neutral method with adding sulfuric acid and ammonia and remove the diluted thioamine liquid evaporative crystallization of (sulfur acid system propylhomoserin method vent gas treatment) in reactor unreacted ammonia and other production processes and get in acrylonitrile installation.
The main modes such as the crystallization of normal pressure single-effect evaporation, the crystallization of decompression single-effect evaporation, the crystallization of jet-type heat pump single-effect evaporation, double-effect evaporation crystallization that adopt in the diluted thioamine liquid evaporative process.
Present domestic most of producer adopts normal pressure or decompression single-effect evaporation crystallization processes, and systematic comparison is simple, but steam consumption is bigger, and evaporation is discharged a large amount of secondary steams and do not added utilization, and gas phase pollution is serious; And double-effect evaporation can make full use of secondary steam, reduces the consumption of water coolant, can compare the heat of reasonable use system, adopts the double-effect evaporation crystallization processes to mainly contain following a few family:
What the ammonium sulfate device of Ba Ling branch office of China Petrochemical Corp. adopted is simple double-effect evaporation flow process, one is imitated the 0.5MPa that thermal source adopted, 150 ℃ low-pressure steam, mainly be by 0.9MPa from heat power plant's outsourcing, 250 ℃ of middle pressure steam pressure and temperature reducings cause great process crushing to lose for this reason; Two effects then adopt the cold cycle heat medium water to make thermal source, and a secondary steam of imitating is not utilized effectively, and need from external world's introducing thermal source, overall system process more complicated.
What the nitrate device of Xiangfan City, Hubei nitrogen fertilizer plant adopted is flow-reversing dual-purpose evaporation flow process, with solution in steam heating first single-effect evaporator that comes from boiler, the secondary steam that is produced feeds in second single-effect evaporator as termite, continues solution in this vaporizer of evaporation.Second imitates evaporation adopts negative-pressure operation, and the secondary steam that is produced is drained after extracting out in the water-jet exhauster after separating.Solution is added by header tank in second single-effect evaporator, and under the effect of secondary steam, concentration is increased to about 42% by about 30%, is pumped in first single-effect evaporator with moving material again, is evaporated to terminal point concentration with Boiler Steam, puts into the crystallization of crystallizer internal cooling then.The main deficiency of this technology is the pumped vacuum systems instability, easily causes environmental pollution, and the solution header tank causes and produces fluctuation in case the pressure that nothing material two is imitated rise rapidly in addition.
The advection double-effect evaporation flow process that the L-Phenylglycine device of Gongda Chemical Equipment Co., Ltd., Shijiazhuang adopts, be to feed the thermal source that an effect external circulation evaporator shell side is made an effect external circulation evaporator after a part of and continuous heating steam that feeds of secondary steam that an effect evaporation crystallization equipment steams is pressurizeed by heat pump, the thermals source of the steam work two effect external circulation evaporators that the water of condensation feeding two effect external circulation evaporator shell sides that a secondary steam that a remaining effect evaporation crystallization equipment steams and an effect external circulation evaporator are discharged flash off are produced, and two imitate the mode of employing while charging while dischargings.The shortcoming of this method is that the heat of high-temperature material is not fully utilized.
Summary of the invention
Technical problem to be solved by this invention provides a kind of technology that adopts negative pressure double-countercurrent evaporation and crystallization mode to produce ammonium sulfate, make full use of a heat of imitating the secondary steam that steams and provide thermal source for two effect concentration and evaporations, reduce the heating steam consumption, reduce by two and imitate the temperature that steams vapour, reduce the recirculated cooling water consumption.
The present invention adopts negative pressure double-countercurrent evaporation and crystallization mode to produce the technology of ammonium sulfate, wherein one imitate by crystallizing evaporator, crystallizer recycle pump and crystallization well heater are formed evaporation crystallization equipment, two imitate by concentration evaporator, thickener well heater and thickener recycle pump are formed concentration and evaporation equipment, it is characterized in that utilizing middle pressure steam to carry out crystallization and evaporation by the ammonium sulfate solution of carrying after dense through concentration evaporator in the crystallization well heater pump circulation heating crystallizing evaporator, the secondary steam that the raw material diluted thioamine liquid is discharged by the crystallizing evaporator top in concentration evaporator is by the thickener heater heats, carry out reduction vaporization, send into after concentration promotes and continue evaporative crystallization in the crystallizing evaporator, the water vapour that steams from the concentration evaporator top cools off through condenser, lime set is advanced the chilling tank, non-condensable gas is discharged by water-ring vacuum pump, and utilize this pump to form system's negative pressure, add communicating pipe between concentration heater and condenser, the sulfur-bearing ammonium crystalline sulphur ammonium supersaturated solution that comes out in crystallizing evaporator bottom obtains finished product sulphur ammonium after by centrifugation.
Wherein optimized technical scheme is:
Utilize vacuum pump to imitate the concentration evaporator vacuum degree control at 0.07～0.08Mpa with two, temperature is controlled at 60 ± 5 ℃, makes material obtain carrying dense, and solid-liquid ratio weighs 1.15～1.20.
The vacuum tightness that crystallizing evaporator is imitated in control one is 0.03～0.04Mpa, and temperature is controlled at 85～90 ℃, makes concentration liquid form supersaturation sulphur ammonium crystalloid solution therein, and its feed liquid proportion is 0.88～1.88.
Add communicating pipe two between imitating, regulate valve on this pipe and can control two pressure reduction between imitating between 0.03～0.05Mpa, utilize to keep vacuum pump and communicating pipe two to imitate and under different pressure, carry out negative pressure evaporation.
The mass concentration of the rare sulphur ammonium of described stock liquid is preferably 16～24%.
The present invention is a kind of technology that adopts negative pressure double-countercurrent evaporation and crystallization mode to produce ammonium sulfate, two effects are made up of evaporative crystallization and evaporation and concentrating two complete equipments respectively, utilize the two-effect evaporation that keeps communicating pipe between vacuum pump and two effects all to move under negative pressure, the pressure reduction that the valve on adjusting communicating pipe can be controlled between two effects is making two effects carry out negative pressure evaporation under different pressure between 0.03～0.05Mpa.Utilize middle pressure steam heating one to imitate and carry out crystallization and evaporation, the secondary steam that utilizes an effect to steam then is dense for two effects provide thermal source that stock liquid is carried, one calorific value of imitating the secondary steam that steams is fully used, not only reduced the heating steam consumption, imitate the temperature that steams vapour and reduced the recirculated cooling water consumption thereby also reduced by two, reduced heat-energy losses.
Description of drawings
Fig. 1 is a process flow diagram of the present invention.
Among the figure: 1 crystallizing evaporator, 2 concentration evaporators, 3 crystallizer well heaters, 4 thickener well heaters, 5 crystallizer recycle pumps, 6 thickener recycle pumps, 7 condensers, 8 water coolers, 9 vacuum pumps, 10 coagulate water pot, 11 chilling tanks, 12 mother liquor tanks, 13 feedstock pumps, 14 whizzers, 15 middle pressure steams, 16 secondary steams, 17 communicating pipe
Embodiment
Present embodiment adopts negative pressure double-countercurrent evaporation and crystallization mode to handle acrylonitrile installation by product diluted thioamine liquid, and it mainly is made up of evaporative crystallization and evaporation and concentrating two complete equipments.One applies mechanically crystallizing evaporator 1, crystallizer recycle pump 5 and crystallizer well heater 3 forms, and does one and imitates evaporation crystallization equipment; One applies mechanically concentration evaporator 2, thickener well heater 4 and thickener recycle pump 6 forms, and does two and imitates concentration and evaporation equipment.Utilize middle pressure steam 15 to imitate by crystallization well heater 3 pump circulation heating one and carry out crystallization and evaporation, the secondary steam 16 that utilizes an effect to steam then is dense for two effects provide thermal source by the circulation of concentration heater semi-finals system stock liquid to be carried, the design technology parameter:
Rare sulphur ammonium inlet amount: 0～6600kg/h
Rare sulphur ammonium charging mass concentration: 18～20%
Diluted thioamine liquid temperature: 80+5 ℃
Crystallizing evaporator 1 liquid level: 50～80%
Crystallizing evaporator 1 head temperature: 85～90 ℃
Crystallizing evaporator 1 top pressure: vacuum tightness 0.03～0.04Mpa
Feed liquid proportion in the crystallizing evaporator 1: 1.38
Concentration evaporator 2 liquid levels: 20～80%
Concentration evaporator 2 head temperature: 60 ± 5 ℃
Concentration evaporator 2 top pressures: vacuum tightness 0.07～0.08Mpa
Feed liquid proportion in the concentration evaporator 2: 1.15～1.20
Condenser 7, water cooler 8 cooling water outlet temperatures: 35～40 ℃
Crystallizer recycle pump 5, thickener recycle pump 6 top hole pressures: 0.2～0.3Mpa
Supply mains's temperature in the circulation: 30～40 ℃
Pipe network saturation steam 15 pressure: 0.6～0.8MpaG
With reference to accompanying drawing 1, the main flow process that the embodiment of the invention adopted uses pump 13 separately to concentration evaporator 2 continuously feedings for being that 18%～20% diluted thioamine liquid is fed to 50～80% of liquid level separately to crystallizing evaporator 1 and concentration evaporator 2 respectively by feedstock pump 13 with mass concentration at first then.Utilize middle pressure steam to carry out crystallization and evaporation by crystallization well heater 3 pump circulation heating evaporation crystallizers 1, the secondary steam heating that stock liquid in the concentration evaporator 2 is extracted out by crystallizing evaporator 1 top by thickener well heater 4, carry out reduction vaporization, send in the evaporative crystallizer 1 after concentration promotes and continue evaporative crystallization.The water vapour that steams from thickener 2 tops flow to quenched water groove 11 respectively certainly through the lime set condenser 7, water cooler 8 condensations cooling back and the thickener well heater 4, non-condensable gas is discharged by vacuum pump 9, and utilize this pump with the two concentration evaporator vacuum degree control of imitating at 0.07～0.08Mpa, temperature is controlled at 60 ± 5 ℃, makes material obtain carrying dense.Between thickener well heater 4 and condenser 7, add communicating pipe 17 and communicate with crystallizing evaporator 1, the vacuum tightness of regulating the crystallizing evaporator of valve control one effect on communicating pipe is 0.03～0.04Mpa, temperature is controlled at 85～90 ℃, makes concentration liquid form supersaturation sulphur ammonium crystalloid solution therein.Lime set in the crystallization well heater 3 is from flowing to water pot 10 with fixed attention.The sulfur-bearing ammonium crystalline sulphur ammonium supersaturated solution that comes out in crystallizing evaporator bottom obtains finished product sulphur ammonium and rarer mother liquor after by whizzer 14 centrifugations, mother liquor enters mother liquor tank 12 and pumps in the concentration evaporator 2 through carrying out oily water separation lower floor mother liquor again, and upper strata tar is delivered to incinerator and burnt.More reasonable through transforming back ammonium sulfate device technical process, usefulness is had been further upgraded, and quality product is qualified.
The embodiment of the invention is after 5700 tons of/year ammonium sulfate devices are on probation, the recirculated cooling water unit consumption drops to 94.8t/t, the heating steam unit consumption drops to 2.58t/t, do not use that the recirculated cooling water unit consumption is that 110.8t/t, heating steam unit consumption position are 4.5t/t before the present invention, economized cycle water coolant 16.0t/t, save heating steam 1.92t/t.
Claims (5)
1. technology that adopts negative pressure double-countercurrent evaporation and crystallization mode to produce ammonium sulfate, wherein one imitate by crystallizing evaporator, crystallizer recycle pump and crystallization well heater are formed evaporation crystallization equipment, two imitate by concentration evaporator, concentration heater and thickener recycle pump are formed concentration and evaporation equipment, it is characterized in that utilizing middle pressure steam to carry out crystallization and evaporation by the ammonium sulfate solution of carrying after dense through concentration evaporator in the crystallization well heater pump circulation heating crystallizing evaporator, the secondary steam that the raw material diluted thioamine liquid is discharged by the crystallizing evaporator top in concentration evaporator is by the thickener heater heats, carry out reduction vaporization, send into after concentration promotes and continue evaporative crystallization in the crystallizing evaporator, the water vapour that steams from the concentration evaporator top cools off through condenser, lime set is advanced the chilling tank, non-condensable gas is discharged by water-ring vacuum pump, and utilize this pump to form system's negative pressure, add communicating pipe between concentration heater and condenser, the sulfur-bearing ammonium crystalline sulphur ammonium supersaturated solution that comes out in crystallizing evaporator bottom obtains finished product sulphur ammonium after by centrifugation.
2. technology according to claim 1 is characterized in that utilizing vacuum pump to imitate the concentration evaporator vacuum degree control at 0.07～0.08Mpa with two, and temperature is controlled at 60 ± 5 ℃, makes material obtain carrying dense, and solid-liquid ratio weighs 1.15～1.20.
3. technology according to claim 1 is characterized in that a vacuum tightness of imitating crystallizing evaporator is 0.03～0.04Mpa, and temperature is controlled at 85～90 ℃, makes concentration liquid form supersaturation sulphur ammonium crystalloid solution therein, and its feed liquid proportion is 0.88～1.88.
4. technology according to claim 1 is characterized in that being added with communicating pipe two between imitating, and regulates valve control two on this pipe pressure reduction between imitating between 0.03～0.05Mpa.
5. technology according to claim 1, the mass concentration that it is characterized in that the rare sulphur ammonium of described stock liquid is 16～24%.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102951657A (en) * | 2012-12-10 | 2013-03-06 | 张卫东 | Process and equipment for producing ammonium sulfate by taking sulfur pulp and ammonia water as raw materials |
| CN103910617A (en) * | 2012-12-28 | 2014-07-09 | 帝斯曼知识产权资产管理有限公司 | Continuous method for purification of cyclohexanone by using mild water-based heat transfer medium as cryogen |
| CN104619642A (en) * | 2012-09-11 | 2015-05-13 | 帝斯曼知识产权资产管理有限公司 | Process for initiating an ammonium sulfate crystallization process |
| CN106075943A (en) * | 2016-07-04 | 2016-11-09 | 江苏斯尔邦石化有限公司 | A kind of sulfur ammonium enrichment facility and the sulfur ammonium method for concentration of this device |
| CN106132516A (en) * | 2014-07-29 | 2016-11-16 | 奥加诺株式会社 | Organic solvent purifying system and method |
| CN111530119A (en) * | 2020-04-14 | 2020-08-14 | 中石化南京工程有限公司 | Tandem ammonium sulfate crystallization method and device thereof |
| CN113044856A (en) * | 2021-03-23 | 2021-06-29 | 李文娟 | Method for preparing ammonium sulfate by using coke oven gas |
| CN117861250A (en) * | 2024-03-12 | 2024-04-12 | 江苏嘉泰蒸发设备股份有限公司 | Double-effect evaporation crystallization performance enhancement equipment and method |
Family Cites Families (2)
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| CN201088872Y (en) * | 2007-06-19 | 2008-07-23 | 项公浩 | Multifunctional multiple-effect automatic continuous-evaporation crystallizer |
| CN101306260B (en) * | 2007-07-12 | 2012-02-22 | 项公浩 | Multifunctional multiple-effect automatic continuous evaporative crystallization technique and crystallization device |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US10369493B2 (en) | 2012-09-11 | 2019-08-06 | Cap Iii B.V. | Process for initiating an ammonium sulfate crystallization process |
| CN104619642A (en) * | 2012-09-11 | 2015-05-13 | 帝斯曼知识产权资产管理有限公司 | Process for initiating an ammonium sulfate crystallization process |
| CN102951657A (en) * | 2012-12-10 | 2013-03-06 | 张卫东 | Process and equipment for producing ammonium sulfate by taking sulfur pulp and ammonia water as raw materials |
| CN102951657B (en) * | 2012-12-10 | 2014-06-04 | 张卫东 | Process and equipment for producing ammonium sulfate by taking sulfur pulp and ammonia water as raw materials |
| CN103910617B (en) * | 2012-12-28 | 2018-03-06 | Cap Iii 有限公司 | Continuation method by the use of gentle water-based heat transfer medium as refrigerant purification cyclohexanone |
| CN103910617A (en) * | 2012-12-28 | 2014-07-09 | 帝斯曼知识产权资产管理有限公司 | Continuous method for purification of cyclohexanone by using mild water-based heat transfer medium as cryogen |
| CN106132516A (en) * | 2014-07-29 | 2016-11-16 | 奥加诺株式会社 | Organic solvent purifying system and method |
| CN106132516B (en) * | 2014-07-29 | 2021-09-24 | 奥加诺株式会社 | Organic solvent purification system and method |
| CN106075943A (en) * | 2016-07-04 | 2016-11-09 | 江苏斯尔邦石化有限公司 | A kind of sulfur ammonium enrichment facility and the sulfur ammonium method for concentration of this device |
| CN111530119A (en) * | 2020-04-14 | 2020-08-14 | 中石化南京工程有限公司 | Tandem ammonium sulfate crystallization method and device thereof |
| CN113044856A (en) * | 2021-03-23 | 2021-06-29 | 李文娟 | Method for preparing ammonium sulfate by using coke oven gas |
| CN117861250A (en) * | 2024-03-12 | 2024-04-12 | 江苏嘉泰蒸发设备股份有限公司 | Double-effect evaporation crystallization performance enhancement equipment and method |
| CN117861250B (en) * | 2024-03-12 | 2024-05-17 | 江苏嘉泰蒸发设备股份有限公司 | Double-effect evaporation crystallization performance enhancement equipment and method |
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