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WO2016200027A1 - Appareil de préparation d'une solution d'urée de grande pureté, et procédé de préparation d'une solution d'urée de grande pureté au moyen de l'appareil - Google Patents

Appareil de préparation d'une solution d'urée de grande pureté, et procédé de préparation d'une solution d'urée de grande pureté au moyen de l'appareil Download PDF

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Publication number
WO2016200027A1
WO2016200027A1 PCT/KR2016/002904 KR2016002904W WO2016200027A1 WO 2016200027 A1 WO2016200027 A1 WO 2016200027A1 KR 2016002904 W KR2016002904 W KR 2016002904W WO 2016200027 A1 WO2016200027 A1 WO 2016200027A1
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Prior art keywords
unit
pure water
urea
dissolving
solid
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Ceased
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PCT/KR2016/002904
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English (en)
Korean (ko)
Inventor
권용철
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Kyeongminwatercom Inc
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Kyeongminwatercom Inc
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D24/00—Filters comprising loose filtering material, i.e. filtering material without any binder between the individual particles or fibres thereof
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D35/00—Filtering devices having features not specifically covered by groups B01D24/00 - B01D33/00, or for applications not specifically covered by groups B01D24/00 - B01D33/00; Auxiliary devices for filtration; Filter housing constructions
    • B01D35/02—Filters adapted for location in special places, e.g. pipe-lines, pumps, stop-cocks
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/50—Mixing liquids with solids
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/26—Nozzle-type reactors, i.e. the distribution of the initial reactants within the reactor is effected by their introduction or injection through nozzles
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07B—GENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
    • C07B61/00—Other general methods
    • 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
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
    • F01N—GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR MACHINES OR ENGINES IN GENERAL; GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR INTERNAL-COMBUSTION ENGINES
    • F01N3/00—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust
    • F01N3/08—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous
    • F01N3/10—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by thermal or catalytic conversion of noxious components of exhaust
    • F01N3/18—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by thermal or catalytic conversion of noxious components of exhaust characterised by methods of operation; Control
    • F01N3/20—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by thermal or catalytic conversion of noxious components of exhaust characterised by methods of operation; Control specially adapted for catalytic conversion

Definitions

  • the present invention relates to a high-purity urea water producing apparatus and a high-purity urea water producing apparatus for producing an expensive high-quality urea water by subjecting low-cost urea water containing impurity ions to high stagnation treatment.
  • Urea is a liquid chemical substance, which is a chemical substance with an element content of 32.5%, which is a mixture of Urea and pure water, which is a raw material of urea fertilizer commonly known to us.
  • This urea is used to purify nitrogen oxides in diesel engine cars. Nitrogen oxides cause various respiratory diseases such as bronchitis and pneumonia, and are known to be a major cause of optical smog and acid rain. Research has shown that more than twice the number of traffic accident deaths is attributed to automobile exhaust, which has a great impact on our everyday lives. So, as a part of the reduction of greenhouse gas emissions, which has been raised steadily since long ago, especially in the developed countries, regulation of vehicle exhaust gas has become increasingly strict. Korea is following the European standards for 'diesel emission regulation'.
  • the SCR catalyst system can achieve DeNOx performance of 90% or more by using ammonia as a reducing agent.
  • ammonia since ammonia is in a gaseous state, it is hard to store and adversely affects the human body due to leakage.
  • the Urea-SCR system is a way to secure the disadvantages of SCR systems using such ammonia catalysts.
  • Urea-SCR The technique of purifying nitrogen oxides by using urea water is called Urea-SCR, which is called DEF (Diesel Exhaust Fluid) in the US and AdBlue in Europe.
  • DEF Diesel Exhaust Fluid
  • the number of ellipsis changes very much with freezing point. Since the freezing point is the lowest at -11 °C when the concentration is 32.5%, the concentration of the urea water for automobile is set at 32.5% when the standard is set.
  • the SCR improves fuel economy by an average of 3 to 5% over the EGR + DPF system in systems that respond to enhanced emissions regulations. Therefore, Urea-SCR is economical because of the fuel cost.
  • the Urea-SCR system purifies the nitrogen oxides in the exhaust gas by injecting urea water through the urea water injector during the passage of the exhaust gas from the diesel engine through the SCR catalytic device.
  • the urea water production and refining technology by the water circulation system used overseas has a disadvantage in that the dissolution of the urea is not properly performed and the dissolution time is longer than 30 minutes, which is very inefficient in view of productivity. As the time increases, CO 2 in the atmosphere continues to be injected causing salt formation.
  • the present invention aims at providing a high purity urea water by using a low-grade element by solving the problems of conventional dissolution method by heat and dissolution method by water circulation, and it is an object of the present invention to provide a method of minimizing equipment size and miniaturization by a forced dissolution method
  • the present invention relates to a high purity urea water producing apparatus capable of effectively producing urea water even at low temperatures in winter and minimizing the heavy metal content and impurity content to provide a high purity urea water, For the purpose of the invention.
  • the present invention relates to a pure water supply unit for supplying pure water
  • An element dissolving unit for receiving pure water supplied from the pure water supply unit and a solid element Urea injected from the outside through a urea inlet port to undergo a dissolution process
  • a solid transfer pump for injecting the solid element and pure water together at the lower portion of the urea dissolving unit together with the strong suction at the upper portion of the element dissolution unit and strongly dissolving the solid element by the vortex generated at this time;
  • a precise metering section including a pre-sorter which is located at the lower end of the urea dissolution section and precisely measures the supply amount of pure water, a level gauge installed on the side wall of the urea dissolution section, and a flow meter;
  • the high-purity urea water producing apparatus includes:
  • the solid-phase component immersed in the lower portion of the urea-dissolving portion is strongly suctioned together with pure water, then is strongly sprayed from the upper portion of the urea dissolving portion, and the solid-phase component is forcedly dissolved (S40)
  • the number of urea generated through the step S40 is transferred to the refining unit, the impurity ions contained in the urea water are removed by ion exchange through the first polymer filter material unit, and then the ammonium polymer, And a high purity filtration step (S50) of laminating, removing and finally filtering the composite metal salt.
  • the high purity urea water producing apparatus and the high purity urea water producing method according to the present invention have the following effects.
  • Superior productivity and quality stability Easy to use and excellent controllability due to combined control Excellent productivity due to superior element melting time.
  • FIG. 1 is a perspective view showing the entire configuration of a high-purity urea water producing apparatus according to the present invention.
  • FIG. 2 is a front view showing the entire configuration of the high-purity urea water producing apparatus of the present invention.
  • a totalizer 401 positioned at the lower end of the element dissolving unit 20 for precisely measuring the supply amount of pure water and a level gauge 402 and a flow meter 403 installed on the side wall of the element dissolving unit 20 A precision measuring unit 40;
  • a transfer pump 501 for supplying the number of urea generated in the element dissolving unit 20 to the first polymer filter material part and an ion exchange unit for transferring impurity ions contained in the urea water supplied through the transfer pump 501 by ion exchange
  • a first polymeric filter material 502 which receives the urea water treated first in the first polymeric material filter 502 and a second polymeric filter material 502 which is laminated and removed from the urea water,
  • a filter unit (504) for finally filtering the urea water treated in the second polymer filter unit (503) by a filter unit (504).
  • High purity urea water production equipment for supplying the number of urea generated in the element dissolving unit 20 to the first polymer filter material part and an ion exchange unit for transferring impurity ions contained in the urea water supplied through the transfer pump 501 by ion exchange
  • a first polymeric filter material 502 which receives the urea water treated first in the first polymeric material filter 502 and
  • a high purity urea water producing apparatus 1 includes a pure water supplying unit 10 for supplying purified water;
  • a totalizer 401 positioned at the lower end of the element dissolving unit 20 for precisely measuring the supply amount of pure water and a level gauge 402 and a flow meter 403 installed on the side wall of the element dissolving unit 20 A precision measuring unit 40;
  • a transfer pump 501 for supplying the number of urea generated in the element dissolving unit 20 to the first polymer filter material part and an ion exchange unit for transferring impurity ions contained in the urea water supplied through the transfer pump 501 by ion exchange
  • a first polymeric filter material 502 which receives the urea water treated first in the first polymeric material filter 502 and a second polymeric filter material 502 which is laminated and removed from the urea water, And a filter unit 504 for finally filtering the urea water that has been secondarily treated in the second polymer filter unit 503.
  • the pure water supply unit 10 is not particularly limited in its selection, and any apparatus capable of supplying pure water can be used.
  • the ionic material contained in the pure water is removed and the resistivity of the ionic material is not less than 10 M ⁇ .cm.
  • An electronic balance 401 is installed at the lower end of the element dissolving unit 20 so as to accurately measure a pure water supply amount while supporting a lower front surface of the element dissolving unit 20 for accurate measurement of the pure water supply amount,
  • a level gauge 402 installed on the side wall of the element dissolving unit 20 for checking the amount of pure water in the dissolving unit 20 and a pure water supply pipe 100 for connecting the pure water supplying unit 10 and the element dissolving unit 20
  • a flow meter 403 provided on one side of the flow meter 40.
  • the precision measuring unit 40 is configured to increase the accuracy of the pure water supply amount according to the water temperature.
  • the accurate pure water supply amount is achieved through the precision measurement by the combined measurement of the electronic balance, level gauge, and flow meter.
  • the purpose of precise control of the pure feed rate is to dissolve the element with a weight fraction to precisely control the concentration of the element.
  • the elliptic point has the lowest value when the concentration is 32.5%, and therefore, the convenience of use is excellent.
  • concentration of the urea water In order to make the concentration of the urea water to be 32.5%, 325 kg of the element should be accurately placed in 675 kg of water. Therefore, the supply amount by precision measurement should be controlled accurately.
  • An element input port 202 for inputting a solid element is provided on one side of the body 201 of the element dissolving portion 20 and a gas discharge pipe 203 is formed on the other side of the upper portion, , And the gas generated in the urea dissolving unit 20 is discharged to the outside through the gas discharge pipe 203 which is opened and closed by a valve.
  • the solid element injected into the element dissolving unit 20 dissolves by a forced dissolution method by vortex unlike the conventional method.
  • the advantage of such a dissolution method is that it does not need to supply heat for dissolution, so that it is possible to miniaturize the entire apparatus because there is no additional equipment, and it can be used in a low temperature environment such as in winter. Compared with the existing water circulation system used in foreign countries, it is possible to shorten urea water production and purification time to less than 10 minutes and to increase the dissolution rate, which is very effective in producing urea water.
  • the water circulation system In the conventional water circulation system, it takes 30 minutes or more to complete the complete dissolution. Therefore, the water circulation system has many disadvantages to produce a high purity urea water. In the forced circulation system according to the present invention, It is possible to achieve complete dissolution of the element in time.
  • the urea water produced through the forced dissolution method in the element dissolution part 20 contains impurity ions such as phosphorus, potassium, iron, copper, zinc, chromium, nickel, magnesium, sodium and potassium. In order to remove the impurities, the urea water is transferred to the urea-hardenable section 50 and highly purified.
  • the urea-hardenable part 50 is a place to remove impurity ions using a styrene-based polymer filter material and an acrylic-based polymer filter material, and is removed by ion exchange and chelating.
  • the pelletizing unit 50 includes a feed pump 501 for feeding urea water to the first polymer filter unit 502 and an impurity contained in the urea water supplied through the feed pump 501, A first polymer material filter 502 for removing ions by ion exchange and a second polymer material filter 502 for receiving the first urea-treated urea water in the first polymer material filter 502, And a filter unit 504 for finally filtering the urea water that has been secondarily treated in the second polymer filter medium unit 503 are provided in the second polymeric filter unit 503.
  • the number of urea produced in the element dissolving unit 20 is first introduced into the first polymer filter unit 502 through a pump.
  • the ion exchange is a mixed ion exchange resin of ion type H and OH type, but a mixed resin having a chemical equivalent, that is, H equivalent and OH equivalent of 1: 1 is used.
  • a mixed resin of Stylrene and divinylbenzene sulfonated copolymers which are strongly acidic cation exchange resins and styrrene and divinylbenzene quaternary amine copolymers as strongly basic anion exchange resins are used.
  • a second polymer filter material portion 503 is disposed adjacent to the first polymer filter material portion 502.
  • the second polymer filter portion 503 is formed by laminating an ammonium salt and a composite metal salt by chelating.
  • the chelating uses a chelating resin with an amino phosphonic group and an iminodiacetic group group.
  • the second polymer filter portion 503 is for laminating and removing the salt precipitated during the ion exchange process in the first polymer filter portion 502 in the filtering material in the chelating step.
  • pH should be kept below 7.1 by proper adjustment of pH and washing. This is to minimize the amount of Na ion impurities by removing NaOH remained in the chelating resin.
  • the chelating resin is a polymer having ligands by covalent bonding, and is generally characterized by multi-functional ligands in one part, or with two or more ligands in a crosslinked polymer network,
  • the metal-polymer which forms a molecular chelate functional group with a linear polymer having a substituted ligand, or a polymer-chelate complex through a metal ion between a monomer or oligomer ligand, Of the inactive polymer.
  • Iminodiacetic acid and aminophosphoric acid chelating resins show selectivity to heavy metals such as Pb (II), Cu (II) and Zn (II) and the removal of hard substances [Ca (II) and Mg .
  • the high-purity urea water producing apparatus (1) comprises a device including a solid feed pump, a feed pump, a first polymer filter material part, and a second polymer filter material part in order to prevent salt from being precipitated through reaction between a metal and urea Instead of metal, plastic materials are used.
  • the supply amount of the pure water supplied from the pure water supplying unit 10 to the element dissolving unit 20 is precisely measured through the precise measuring unit 40 including the entire author 401, the level gauge 402, and the flow meter 403 Step S20,
  • Solid-state elements immersed in the lower portion of the element dissolving unit 20 are strongly suctioned together with pure water and then strongly ejected from the upper portion of the element dissolving unit 20 by using the solid transfer pump 30, A step (S40) of forcibly dissolving the solid phase element by the step
  • the number of urea generated through the step S40 is transferred to the urea stage topology unit 50 to remove impurity ions contained in urea water through the first polymer filter medium unit 502 by ion exchange, 2 high-purity filtration step (S50) of laminating and removing the ammonium salt and the composite metal salt in the polymer filter medium portion 503 and finally filtering the same.
  • the high purity urea water ultimately produced through the urea-free extruder 50 is used as a catalyst additive for a vehicle, and it meets the criteria for manufacturing a urea-free catalyst as shown in Table 1 below as a condition for use as a catalyst additive.
  • Criteria for urea-based catalyst preparation Item unit standard Minimum standard Maximum standard Urea content % (m / m) 31.8 33.2 Density @ 20 °C kg / m3 1087 1093 Refraction index @ 20 °C - 1.3814 1.3843 Alkalinity (NH 3 ) % (m / m) - 0.2 burette % (m / m) - 0.3 Aldehyde mg / kg - 5 Insoluble substance mg / kg - 20 Phosphorus (PO 4 ) mg / kg - 0.5 Calcium (Ca) mg / kg - 0.5 Iron (Fe) mg / kg - 0.5 Copper (Cu) mg / kg - 0.2 Zinc (Zn) mg / kg - 0.2 Chromium (Cr) mg / kg - 0.2 Nickel (Ni) mg / kg - 0.2 Aluminum (Al) mg / kg - 0.5 Magnesium (Mg) mg / kg - 0.5
  • the high-purity urea water produced through such a process has the advantage that it can be utilized in various places such as gas stations, bus terminals, cargo terminals, heavy equipment companies, charter bus operators, cargo / buses, and the like.
  • the urea water purifying apparatus effectively removes impurity ions and heavy metal ions in urea water to produce high-quality urea water using a low-grade element, and dissolves the element in a forced dissolution system using a strong vortex, The dissolution by the heat of the system is unnecessary, and the effect is great in terms of cost reduction, which is highly likely to be used industrially.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Health & Medical Sciences (AREA)
  • Toxicology (AREA)
  • Combustion & Propulsion (AREA)
  • Mechanical Engineering (AREA)
  • General Engineering & Computer Science (AREA)
  • Dispersion Chemistry (AREA)
  • Treatment Of Water By Ion Exchange (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

La présente invention concerne : un appareil de préparation d'une solution d'urée de grande pureté permettant de préparer et de fournir une solution d'urée de grande qualité et onéreuse en purifiant de manière élevée une solution d'urée de faible qualité et peu onéreuse contenant des ions d'impureté; et un procédé de préparation d'une solution d'urée de grande pureté à l'aide de l'appareil.
PCT/KR2016/002904 2015-06-12 2016-03-23 Appareil de préparation d'une solution d'urée de grande pureté, et procédé de préparation d'une solution d'urée de grande pureté au moyen de l'appareil Ceased WO2016200027A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
KR1020150083589A KR101544503B1 (ko) 2015-06-12 2015-06-12 고순도 요소수 제조장치 및 이를 이용한 고순도 요소수 제조방법
KR10-2015-0083589 2015-06-12

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WO2016200027A1 true WO2016200027A1 (fr) 2016-12-15

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WO (1) WO2016200027A1 (fr)

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IT201600131605A1 (it) * 2016-12-28 2018-06-28 Ama Spa Impianto di piccole dimensioni e procedimento ottimizzato per la preparazione di una soluzione acquosa di urea

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KR101640401B1 (ko) 2016-05-25 2016-07-18 경민워터컴(주) 고상 요소와 물의 동시 흡입·강제이송 용해방식에 따른 배관시스템을 포함하여 이루어진 자동차·선박·산업용 고순도 요소수 제조장치 및 이를 이용한 고순도 요소수 제조방법
CA3028550C (fr) * 2016-07-15 2021-06-15 Thyssenkrupp Fertilizer Technology Gmbh Utilisation d'une composition a base d'uree pour la production d'un fluide d'echappement diesel
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KR102137054B1 (ko) 2018-07-26 2020-07-29 김기원 요소수 자동화 제조 시스템
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KR102442953B1 (ko) 2022-05-13 2022-09-14 대산철강공업 주식회사 요소수 제조장치
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JPH08252429A (ja) * 1995-03-20 1996-10-01 Mitsubishi Heavy Ind Ltd 尿素水吹き込み脱硝装置
JP2005118705A (ja) * 2003-10-17 2005-05-12 Nissan Diesel Motor Co Ltd 尿素水溶液製造装置
KR100500325B1 (ko) * 2003-07-09 2005-07-12 한모기술주식회사 요소 수용액 조제장치
WO2014114306A1 (fr) * 2013-01-25 2014-07-31 Kautex Textron Gmbh & Co. Kg Appareil de filtration pour récipient de liquide, en particulier pour solution aqueuse d'urée

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JPH0711147Y2 (ja) * 1990-04-27 1995-03-15 株式会社新潟鐵工所 尿素水溶液製造装置
JPH08252429A (ja) * 1995-03-20 1996-10-01 Mitsubishi Heavy Ind Ltd 尿素水吹き込み脱硝装置
KR100500325B1 (ko) * 2003-07-09 2005-07-12 한모기술주식회사 요소 수용액 조제장치
JP2005118705A (ja) * 2003-10-17 2005-05-12 Nissan Diesel Motor Co Ltd 尿素水溶液製造装置
WO2014114306A1 (fr) * 2013-01-25 2014-07-31 Kautex Textron Gmbh & Co. Kg Appareil de filtration pour récipient de liquide, en particulier pour solution aqueuse d'urée

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WO2018122717A1 (fr) * 2016-12-28 2018-07-05 Ama S.P.A. Installation compacte et procédé optimisé pour la production d'une solution aqueuse d'urée

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