CN105582810B - A kind of preparation method and system of high-purity urea for vehicle solution - Google Patents

A kind of preparation method and system of high-purity urea for vehicle solution Download PDF

Info

Publication number
CN105582810B
CN105582810B CN201610005408.7A CN201610005408A CN105582810B CN 105582810 B CN105582810 B CN 105582810B CN 201610005408 A CN201610005408 A CN 201610005408A CN 105582810 B CN105582810 B CN 105582810B
Authority
CN
China
Prior art keywords
urea
storage tank
vehicle
solution
liquid
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201610005408.7A
Other languages
Chinese (zh)
Other versions
CN105582810A (en
Inventor
姜晓滨
贺高红
王君山
李盼
唐治钫
任继炎
卢大鹏
肖武
李祥村
吴雪梅
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Dalian University of Technology
North Huajin Chemical Industries Group Co Ltd
Original Assignee
Dalian University of Technology
North Huajin Chemical Industries Group Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Dalian University of Technology, North Huajin Chemical Industries Group Co Ltd filed Critical Dalian University of Technology
Priority to CN201610005408.7A priority Critical patent/CN105582810B/en
Publication of CN105582810A publication Critical patent/CN105582810A/en
Application granted granted Critical
Publication of CN105582810B publication Critical patent/CN105582810B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34Chemical or biological purification of waste gases
    • B01D53/92Chemical or biological purification of waste gases of engine exhaust gases
    • B01D53/94Chemical or biological purification of waste gases of engine exhaust gases by catalytic processes
    • B01D53/9404Removing only nitrogen compounds
    • B01D53/9409Nitrogen oxides
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2251/00Reactants
    • B01D2251/20Reductants
    • B01D2251/206Ammonium compounds
    • B01D2251/2067Urea
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2258/00Sources of waste gases
    • B01D2258/01Engine exhaust gases
    • B01D2258/012Diesel engines and lean burn gasoline engines

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Combustion & Propulsion (AREA)
  • Health & Medical Sciences (AREA)
  • Biomedical Technology (AREA)
  • Environmental & Geological Engineering (AREA)
  • Analytical Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)

Abstract

The present invention relates to diesel exhaust gas after-treatment system field, and in particular to a kind of new urea for vehicle production method and system.Using technical grade urea solid or saturated solution, with reference to liquid membrane crystal crystal growth rate is fast and the big advantage of suspension crystallization phase separation area, the urea saturated solution prepared or directly used is passed through the relatively low liquid membrane crystal section of temperature, formation coarse-grain;The higher suspension crystallization section of temperature is passed into again, is purified;Last simple filtration separation, obtains high-purity urea solid, then fills ultra-pure water, obtains urea for vehicle solution.The method of the production urea for vehicle of the present invention intermittently can continuously be designed and operating flexibility is big, and in the absence of mother liquor discharge and pollution problem, product quality stabilization produces facility.

Description

A kind of preparation method and system of high-purity urea for vehicle solution
Technical field
The present invention relates to Diesel engine post-processing technology field, and in particular to a kind of new high-purity urea for vehicle production Method and system.
Background technology
Nitrogen oxides (the NO of emission of diesel enginex) and harm of the particulate matter (PM) to human health and atmospheric environment caused The concern of height.Countries in the world are devoted to reduce net in the research of this two emissions, including raising fuel qualities, implementation machine The outside purification technology of change technology and exhaust aftertreatment.China urban have been carried out " state's V " discharge standards mean car The discharge of tail gas must use more advanced technology.
Catalytic reduction technique (SCR) is to be best suitable for diesel vehicle " state V " discharge solutions, and the use of this technology at present Reducing agent urea solution carries out SCR to nitrogen oxides, reduces NOxDischarge, so as to meet " state's V " Abgasgesetzs For PM and NOxLimitation.
But the purity requirement of urea for vehicle is very high, such as the content of the element such as Na, Mg, Al, K, Ca, Fe is not more than 0.5ppm, Cr, Ni, Cu, Zn constituent content are not more than 0.2ppm.Common urea can not meet urea for vehicle and high-cleanness, high wanted Ask.Obviously, how to purify urea liquid to meet automobile-used technical requirements, be the unavoidable problem of research worker in the industry.
Is being carried out always on the research of urea for vehicle technology at present, mainly there is crystallisation, ion-exchange, micro-filtration/surpass Filter/counter-infiltration/electrodialysis coupling membrane separation process etc..Wherein, ion exchange needs step less, can pointedly eliminate miscellaneous Matter, but need regular desalination and change separating medium, complex operation increases extra consumption.Coupling membrane separation process is typically all related to And more than ten separating steps are, it is necessary to regularly replace film, operate too complicated and extremely easy introducing impurity, scale application difficulty compared with Greatly.The crystallisation reported at present is divided into evaporative crystallization and crystallisation by cooling, and crystallization technique need not introduce other separating mediums, behaviour Make comparisons simple, but crystallisation by cooling reaches required purity, it is necessary to which multistage cooling, consumes energy higher;Evaporative crystallization was difficult to control Saturation degree, temperature is high, and urea is unstable, consumes energy also larger.
Publication No. CN104258730A Chinese patent employs yin, yang secondary ion exchange resin column to urea liquid Purification process is carried out, although this method can preferably realize the purifying of urea liquid, is periodically required to carry out desalination and more Separating medium is changed, is expended higher.And Publication No. CN204073982U Chinese patent uses ultrafiltration/counter-infiltration/electrodialysis coupling Legal, Publication No. CN204111628U Chinese patent uses ultrafiltration/cation and anion exchange coupled method, Publication No. CN204185305U Chinese patent uses ultrafiltration/nanofiltration/counter-infiltration coupled method, and Publication No. CN203955038U China is specially Profit uses ion exchange/micro-filtration/ultrafiltration/counter-infiltration/electrodialysis coupled method, and Publication No. CN204097153U Chinese patent is adopted With two-stage ultrafiltering, though these technologies reach required purity, operating procedures more than ten steps even ten steps is required for, is operated too multiple It is miscellaneous, it is difficult to control, consumes energy higher, and be easily introduced impurity.Publication No. CN104289106A uses urea one-level crystallisation by cooling, though Required purity is reached, but higher is required to material purity, the urea production factory of preferable preconditioning technique is only applicable to, is applicable Scope is narrower, it is impossible to generally applicable.Publication No. CN104557617A is to having deviate from the urea synthesis reaction of ammonia and carbon dioxide Liquid carries out vacuum flashing crystallization, it is necessary to which extra vacuum equipment, expends larger.Publication No. 102584635A Chinese patent is adopted Purified, consumed energy higher with the method for three-level crystallisation by cooling.Publication No. 103657498A Chinese patent, devises one kind Urea liquid device for formulating, can be continuously produced, and product directly dissolving is configured to liquid, but the technology is without purification effect, It is not suitable for technical grade urea.
The content of the invention
It is an object of the invention to:A kind of method of purification of urea for vehicle solution is provided, this method can utilize technical grade urine Plain solid or saturated solution, large-scale industrial production, its product quality are stable, with low cost.In addition, in the inventive method not Need activated carbon or ion exchange resin to be handled, also excluded without harmful mother liquor, it is simple to operate, it is a kind of environment-friendly type, warp Ji type technology.
Piece-rate system of the present invention, is characterized in utilizing technical grade urea solid or saturated solution, with reference to liquid film Crystallographic growth rate is fast and the big advantage of suspension crystallization phase separation area, will preparation or the urea saturated solution that directly uses The relatively low liquid membrane crystal section of temperature is passed through, coarse-grain is formed;The higher suspension crystallization section of temperature is passed into again, is purified;Finally Simple filtration is separated, and obtains high-purity urea solid, then fills distilled water, obtains urea for vehicle solution.
System used in a kind of preparation method of high-purity urea for vehicle solution of present invention offer, including raw material urea storage tank, First distillation water storage tank, saturation urea liquid storage tank, feed pump, cooling device, liquid membrane crystal tower, suspension crystallization kettle, stirring are set Standby, firing equipment, discharging pump, filter plant, filtrate recycling can, after-fractionating water storage tank and urea for vehicle product solution storage tank; Described raw material urea storage tank and the first distillation water storage tank connection saturation urea liquid storage tank, saturation urea liquid storage tank, charging Pump, liquid membrane crystal tower, suspension crystallization kettle, discharging pump and filter plant are sequentially connected, and cooling device is carried on liquid membrane crystal tower, are hanged Floating crystallization kettle is provided with firing equipment and mixing plant, filter plant connection filtrate recycling can and the storage of urea for vehicle product solution Tank, after-fractionating water storage tank connection urea for vehicle product solution storage tank.
A kind of preparation method of urea for vehicle solution, step is as follows:
Step one:It is molten that urea saturation is prepared with the distilled water in the urea in raw material urea storage tank and the first distillation water storage tank Liquid, is led to the urea saturated solution in saturation urea liquid storage tank by feed pump at 20-70 DEG C from liquid membrane crystal top of tower Enter in liquid membrane crystal tower apparatus, flow super cooled sect, it is 30~50 DEG C to keep urea saturated solution and cold section of the temperature difference, is crystallized;
Step 2:The crystallized product that step one is obtained flows through hot arc, keep hot arc and the urea saturated solution temperature difference be 5~ 10 DEG C, purification processes are carried out under mixing plant;
Step 3:Product in step 2 is separated from the device afterbody of suspension crystallization kettle by filter plant simple filtration Afterwards, high-purity urea solid product is obtained;
Step 4:High-purity urea solid product that step 3 is obtained, fills distilled water, obtains urea for vehicle solution product.
Described cold section is liquid membrane crystal section, and temperature is -10~30 DEG C, and described hot arc is suspension crystallization section, and temperature is 25~80 DEG C.
Compared with prior art, the advantage of the invention is that:
(1) present invention is simple to operate, and cold section interconnects with hot arc, and urea for vehicle product is produced therefore, it is possible to continuous, from And improve production efficiency;
(2) temperature simple of cold section of the present invention and hot arc is controllable, easy to operate;
(3) whole device is closed, it is to avoid influence of the external environment to product quality;
(4) present invention in, the mother liquor isolated, can make industrial urea and agricultural production is used, in the absence of mother liquor discharge and Pollution problem, is a kind of environment-friendly type, economical technology;
(5) production method of the invention has steady quality, the advantages of production is convenient;
(6) intermittently it can continuously design and operating flexibility is big.
Brief description of the drawings
Fig. 1 is the schematic diagram of preparation method system for use in carrying of the present invention.
Fig. 2 is urea liquid temperature variation curve schematic diagram in a device.
In figure:1 raw material urea storage tank;2 first distillation water storage tanks;3 saturation urea liquid storage tanks;4 feed pumps;5 coolings are set It is standby;6 liquid membrane crystal towers;7 suspension crystallization kettles;8 mixing plants;9 firing equipments;10 discharging pumps;11 filter plants;12 filtrates are reclaimed Tank;13 after-fractionating water storage tanks;14 urea for vehicle product solution storage tanks.
Embodiment
Below in conjunction with accompanying drawing and technical scheme, the specific embodiment of the present invention is further illustrated.
Embodiment 1
Urea solid in raw material storage tank is configured to saturated solution with the distilled water in the first distillation water storage tank, prepared Urea saturated solution (20 DEG C) by feed pump, sequentially enter in liquid membrane crystal tower and suspension crystallization kettle, cooling device maintain Cold section of temperature is -10 DEG C, and firing equipment maintains hot arc temperature to be 25 DEG C.Product passes through discharging pump from bottom, by filter plant, The solid of filtering is to obtain high-purity urea solid, the material liquid that the non-crystalline mother solution being filtrated to get can be produced as industrial urea Recycle.Urea for vehicle solution product is configured to distilled water.
Embodiment 2
Urea solid in raw material storage tank is configured to saturated solution with the distilled water in the first distillation water storage tank, prepared Urea saturated solution (50 DEG C) by feed pump, sequentially enter in liquid membrane crystal tower and suspension crystallization kettle, cooling device maintain Cold section of temperature is 10 DEG C, and firing equipment maintains hot arc temperature to be 55 DEG C.Product passes through discharging pump from bottom, by filter plant, The solid of filtering is to obtain high-purity urea solid, the material liquid that the non-crystalline mother solution being filtrated to get can be produced as industrial urea Recycle.Urea for vehicle solution product is configured to distilled water.
Embodiment 3
Urea saturated solution (70 DEG C), by feed pump, disposably adds liquid membrane crystal tower by saturation urea liquid storage tank In suspension crystallization kettle, cooling device maintains cold section of temperature to be 20 DEG C, and firing equipment maintains hot arc temperature to be 80 DEG C.Product is the bottom of from Discharging pump is passed through in portion, by filter plant, and the solid of filtering is to obtain high-purity urea solid, the non-crystalline mother solution being filtrated to get The material liquid that can be produced as industrial urea is recycled.Urea for vehicle solution product is configured to distilled water.

Claims (2)

1. the system used in a kind of preparation method of high-purity urea for vehicle solution, it is characterised in that the system includes raw material urea Storage tank, the first distillation water storage tank, saturation urea liquid storage tank, feed pump, cooling device, liquid membrane crystal tower, suspension crystallization kettle, stir Mixing equipment, firing equipment, discharging pump, filter plant, filtrate recycling can, after-fractionating water storage tank and the storage of urea for vehicle product solution Tank;Described raw material urea storage tank and the first distillation water storage tank connection saturation urea liquid storage tank, saturation urea liquid storage tank, enter Material pump, liquid membrane crystal tower, suspension crystallization kettle, discharging pump and filter plant are sequentially connected, and cooling device is carried on liquid membrane crystal tower, Suspension crystallization kettle is provided with firing equipment and mixing plant, filter plant connection filtrate recycling can and the storage of urea for vehicle product solution Tank, after-fractionating water storage tank connection urea for vehicle product solution storage tank.
2. a kind of system with described in claim 1 carries out the preparation method of urea for vehicle solution, it is characterised in that step is such as Under:
Step one:Urea saturated solution is prepared with the distilled water in the urea in raw material urea storage tank and the first distillation water storage tank, The urea saturated solution in saturation urea liquid storage tank is passed through liquid by feed pump from liquid membrane crystal top of tower at 20-70 DEG C In membrane crystallization tower apparatus, super cooled sect is flowed, it is 30~50 DEG C to keep urea saturated solution and cold section of the temperature difference, is crystallized;
Step 2:The crystallized product that step one is obtained flows through hot arc, and it is 5~10 with the urea saturated solution temperature difference to keep hot arc DEG C, purification processes are carried out under mixing plant;
Step 3:Product in step 2 after the separation of filter plant simple filtration, is obtained from the device afterbody of suspension crystallization kettle To high-purity urea solid product;
Step 4:High-purity urea solid product that step 3 is obtained, fills distilled water, obtains urea for vehicle solution;
Described cold section is liquid membrane crystal section, and temperature is -10~30 DEG C, and described hot arc is suspension crystallization section, temperature is 25~ 80℃。
CN201610005408.7A 2016-01-06 2016-01-06 A kind of preparation method and system of high-purity urea for vehicle solution Active CN105582810B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201610005408.7A CN105582810B (en) 2016-01-06 2016-01-06 A kind of preparation method and system of high-purity urea for vehicle solution

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610005408.7A CN105582810B (en) 2016-01-06 2016-01-06 A kind of preparation method and system of high-purity urea for vehicle solution

Publications (2)

Publication Number Publication Date
CN105582810A CN105582810A (en) 2016-05-18
CN105582810B true CN105582810B (en) 2017-10-20

Family

ID=55922933

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201610005408.7A Active CN105582810B (en) 2016-01-06 2016-01-06 A kind of preparation method and system of high-purity urea for vehicle solution

Country Status (1)

Country Link
CN (1) CN105582810B (en)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107774183A (en) * 2016-08-31 2018-03-09 衡水卡力洁环保科技有限公司 A kind of urea for vehicle production equipment and process
CN112094207A (en) * 2020-09-30 2020-12-18 河南弘康环保科技有限公司 Preparation method of low-formaldehyde automobile urea solution

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101774555A (en) * 2010-02-02 2010-07-14 天津大学 Method for preparing electronic grade phosphoric acid through liquid membrane crystallization
CN102198937A (en) * 2011-04-18 2011-09-28 天津大学 Static multistage melting crystallization method for preparing electronic grade phosphoric acid
CN102442928A (en) * 2012-01-09 2012-05-09 四川泸天化股份有限公司 Purification method for urea
CN102584635A (en) * 2012-01-09 2012-07-18 四川泸天化股份有限公司 Preparation method for urea for vehicle
CN104289106A (en) * 2014-09-23 2015-01-21 河南弘康环保科技有限公司 Method for preparing vehicle urea solution

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101774555A (en) * 2010-02-02 2010-07-14 天津大学 Method for preparing electronic grade phosphoric acid through liquid membrane crystallization
CN102198937A (en) * 2011-04-18 2011-09-28 天津大学 Static multistage melting crystallization method for preparing electronic grade phosphoric acid
CN102442928A (en) * 2012-01-09 2012-05-09 四川泸天化股份有限公司 Purification method for urea
CN102584635A (en) * 2012-01-09 2012-07-18 四川泸天化股份有限公司 Preparation method for urea for vehicle
CN104289106A (en) * 2014-09-23 2015-01-21 河南弘康环保科技有限公司 Method for preparing vehicle urea solution

Also Published As

Publication number Publication date
CN105582810A (en) 2016-05-18

Similar Documents

Publication Publication Date Title
CN102806011A (en) Method for preparing automobile urea liquid reducing agent
EP1857439A1 (en) Method for purifying aqueous urea solution
CN104557617B (en) Diesel exhaust fluid production method
CN110526839B (en) Improved process for preparing taurine by ethylene oxide method
CN110272461A (en) A method of purifying beta-thymidine from fermentation liquid
CN105582810B (en) A kind of preparation method and system of high-purity urea for vehicle solution
CN102442928B (en) Purification method for urea
CN103523758A (en) Method for continuously preparing sodium azide
CN103305286B (en) Coke oven gas purifying system for efficiently recycling coking plant heat source and desulfurated liquid waste treatment method
CN211497025U (en) Forward osmosis and combined soda production process co-production combined system
CN205773845U (en) A kind of processing system of N-(phosphonomethyl) iminodiacetic acid wastewater recycling
CN113563215B (en) Glycine production process
CN213231531U (en) Continuous nitric oxide production device
CN101492369B (en) Separation purification method for benzoic anhydride sour water and production process for allomaleic acid
CN106621867A (en) A preparing method of a urea solution used for vehicles
CN113788770A (en) Method for producing taurine by using ethylene oxide
KR101073726B1 (en) Economical manufacturing process of xylose from biomass hydrolysate using electrodialysis and direct recovery method
CN110902919A (en) Method for treating wastewater generated in production of thiosemicarbazide
CN217127205U (en) Contain salt organic wastewater treatment system
CN110960978A (en) Preparation method of diesel vehicle tail gas treatment liquid
CN219272164U (en) System for recycling and purifying dibasic acid in adipic acid production waste liquid
CN215855847U (en) Cyclohexane purifying device in cyclohexanone oxime solvent rearrangement process
CN103172099B (en) Method for producing high purity aluminum ammonium sulfate by using industrial aluminum sulfate and industrial ammonium sulfate
CN219423925U (en) Continuous sulfur melting and closed oxidation thiocyanate extracting system
CN112551548B (en) Recycling system for organic wastewater rich in sodium sulfate and ammonium sulfate

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant