EP3160634A1 - Commande d'alimentation en ammoniac et/ou en air d'un réacteur d'ammoxydation - Google Patents

Commande d'alimentation en ammoniac et/ou en air d'un réacteur d'ammoxydation

Info

Publication number
EP3160634A1
EP3160634A1 EP15731470.9A EP15731470A EP3160634A1 EP 3160634 A1 EP3160634 A1 EP 3160634A1 EP 15731470 A EP15731470 A EP 15731470A EP 3160634 A1 EP3160634 A1 EP 3160634A1
Authority
EP
European Patent Office
Prior art keywords
reactor
ammonia
oxygen
quench
amount
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.)
Withdrawn
Application number
EP15731470.9A
Other languages
German (de)
English (en)
Inventor
Timothy Robert Mcdonel
Jay Robert COUCH
David Rudolph Wagner
Paul Trigg Wachtendorf
Thomas George TRAVERS
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.)
Ineos Europe AG
Original Assignee
Ineos Europe AG
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 Ineos Europe AG filed Critical Ineos Europe AG
Publication of EP3160634A1 publication Critical patent/EP3160634A1/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • 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
    • B01J4/00—Feed or outlet devices; Feed or outlet control devices
    • B01J4/008—Feed or outlet control devices
    • 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
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
    • B01J8/1809—Controlling processes
    • 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
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
    • B01J8/1818—Feeding of the fluidising gas
    • 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
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
    • B01J8/1818—Feeding of the fluidising gas
    • B01J8/1827—Feeding of the fluidising gas the fluidising gas being a reactant
    • 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
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
    • B01J8/1836—Heating and cooling the reactor
    • 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
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
    • B01J8/24—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles according to "fluidised-bed" technique
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C253/00—Preparation of carboxylic acid nitriles
    • C07C253/18—Preparation of carboxylic acid nitriles by reaction of ammonia or amines with compounds containing carbon-to-carbon multiple bonds other than in six-membered aromatic rings
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C253/00—Preparation of carboxylic acid nitriles
    • C07C253/24—Preparation of carboxylic acid nitriles by ammoxidation of hydrocarbons or substituted hydrocarbons
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C255/00—Carboxylic acid nitriles
    • C07C255/01—Carboxylic acid nitriles having cyano groups bound to acyclic carbon atoms
    • C07C255/06—Carboxylic acid nitriles having cyano groups bound to acyclic carbon atoms of an acyclic and unsaturated carbon skeleton
    • C07C255/07—Mononitriles
    • C07C255/08—Acrylonitrile; Methacrylonitrile
    • 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
    • B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00008—Controlling the process
    • B01J2208/00017—Controlling the temperature
    • B01J2208/00106—Controlling the temperature by indirect heat exchange
    • B01J2208/00115—Controlling the temperature by indirect heat exchange with heat exchange elements inside the bed of solid particles
    • B01J2208/00141—Coils
    • 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
    • B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00008—Controlling the process
    • B01J2208/00592—Controlling the pH
    • 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
    • B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00008—Controlling the process
    • B01J2208/00628—Controlling the composition of the reactive mixture
    • 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
    • B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00796—Details of the reactor or of the particulate material
    • B01J2208/00893—Feeding means for the reactants
    • 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
    • B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00796—Details of the reactor or of the particulate material
    • B01J2208/00893—Feeding means for the reactants
    • B01J2208/00911—Sparger-type feeding elements
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00191—Control algorithm
    • B01J2219/00193—Sensing a parameter
    • B01J2219/00195—Sensing a parameter of the reaction system
    • B01J2219/00202—Sensing a parameter of the reaction system at the reactor outlet
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00191—Control algorithm
    • B01J2219/00222—Control algorithm taking actions
    • B01J2219/00227—Control algorithm taking actions modifying the operating conditions
    • B01J2219/00229—Control algorithm taking actions modifying the operating conditions of the reaction system
    • B01J2219/00231—Control algorithm taking actions modifying the operating conditions of the reaction system at the reactor inlet

Definitions

  • a process for controlling an amount of ammonia and/or air provided to an ammoxidation reactor. More specifically, the process includes maintaining a pH of a quench water bottoms and adjusting an amount of ammonia in a reactor feed to provide an ammonia to hydrocarbon ratio of about 1 to about 2 in the reactor feed. Further, the process may include adjusting an amount of air the reactor feed to provide an air to hydrocarbon ratio of about 9 to about 10 in the reactor feed.
  • This process which is commonly referred to as ammoxidation, is carried out in the gas phase at elevated temperature (e.g. , 350° to 480° C) in the presence of a suitable fluid bed ammoxidation catalyst.
  • Fig. 1 illustrates a typical acrylonitrile reactor used to carry out this process.
  • reactor 10 comprises reactor shell 12, air grid 14, feed sparger 16, cooling coils 18 and cyclones 20.
  • process air is charged into reactor 10 through air inlet 22, while a mixture of propylene and ammonia from propylene inlet 34 and ammonia inlet 36 is charged into reactor 10 through feed sparger 16.
  • the flow rates of these incoming gases are high enough to fluidize a bed 24 of ammoxidation catalyst in the reactor interior, where the catalytic ammoxidation of the propylene and ammonia to acrylonitrile occurs.
  • reaction gases exit reactor 10 through reactor effluent outlet 26. Before doing so, they pass through cyclones 20, which remove any ammoxidation catalyst these gases may have entrained for return to catalyst bed 24 through diplegs 25. Ammoxidation is highly exothermic, and cooling coils 18 are used to withdraw excess heat and thereby keep the reaction temperature at an appropriate level.
  • the first step in recovering acrylonitrile and other byproducts from the hot reaction gases passing out of a typical acrylonitrile reactor 10 is to cool them down by spraying them with quench water in quench column 30. These reaction gases contain unreacted ammonia, which are removed before these gases are further processed. For this purpose, sulfuric acid is added to the quench water, which reacts with this unreacted ammonia to produce ammonium sulfate in accordance with the following reaction:
  • the amount of ammonia being fed to the reactor at any particular time should be a slight molar excess of the amount needed to completely convert all of the propylene being fed to the reactor at that same time into acrylonitrile. Since the flowrate of incoming propylene can vary over time for a number of reasons, it is normal practice to continuously monitor this flowrate F and to continuously adjust the flowrate of incoming ammonia by means of ammonia control valve 32 and controller 38 in response to this measured propylene flowrate.
  • the NH 3 /C 3 ⁇ ratio setpoint programmed into controller 38 is increased slightly so that a slightly greater amount of ammonia is fed to the reactor relative to the propylene being fed on a continuous basis.
  • Periodic determination of the concentration of unreacted ammonia in reactor effluent outlet 26 is normally done on a routine basis, for example, several times per week. Accordingly, precise adjustment of the target NH 3 /C 3 ⁇ ratio in controller 38 in response to the concentration of unreacted ammonia in reactor effluent outlet 26 is inherently limited due to the inability to obtain data on this concentration on a more frequent basis.
  • a process for controlling an amount of ammonia provided to an ammoxidation reaction includes, providing a reactor feed to a reactor, the reactor feed including ammonia, oxygen, and a hydrocarbon selected from the group consisting of propane, propylene, isobutane and isobutylene, and combinations thereof; reacting the reactor feed in the presence of a catalyst to provide a reactor effluent stream; providing the reactor effluent stream to a quench vessel; providing a quench liquid to the quench vessel;
  • a process for controlling an amount of air provided to an ammoxidation reaction includes providing a reactor feed to a reactor, the reactor feed including ammonia, oxygen, and a hydrocarbon selected from the group consisting of propane, propylene, isobutane and isobutylene, and combinations thereof; reacting the reactor feed in the presence of a catalyst to provide a reactor effluent stream; monitoring an amount of oxygen in the reactor effluent; and adjusting an amount of air in the reactor feed to provide an air to hydrocarbon ratio of about 9 to about 10 in the reactor feed.
  • An ammoxidation process includes providing a reactor feed to a reactor, the reactor feed including ammonia, oxygen, and a hydrocarbon selected from the group consisting of propane, propylene, isobutane and isobutylene, and combinations thereof; reacting the reactor feed in the presence of a catalyst to provide a reactor effluent stream; providing a quench liquid to the quench vessel; contacting the gaseous stream with the quench liquid; monitoring a pH of quench water bottoms, monitoring an amount of oxygen in the reactor effluent stream; adjusting an amount of ammonia in the reactor feed to provide an ammonia to hydrocarbon ratio of about 1 to about 2 in the reactor feed; and adjusting an amount of air in the reactor feed to provide an air to hydrocarbon ratio of about 9 to about 10 in the reactor feed.
  • a reactor feed including ammonia, oxygen, and a hydrocarbon selected from the group consisting of propane, propylene, isobutane and isobutylene, and combinations thereof.
  • a system for ammonia control in an ammoxidation reactor includes an ammoxidation reactor configured to supply a reactor effluent to a quench column; a pH sensor for monitoring pH of a quench water bottoms from the quench column; and a controller electronically connected to the pH sensor and to an ammonia control valve.
  • the ammonia control valve configured to control ammonia flow to the ammoxidation reactor and the controller is configured to increase or decrease ammonia flow through the ammonia control valve.
  • Figure 1 is a schematic view illustrating fine control of the amount of ammonia being fed to a commercial acrylonitrile reactor.
  • Figure 2 is a schematic view illustrating another aspect for fine control of the amount of ammonia being fed to a commercial acrylonitrile reactor
  • Fine control of the amount of ammonia being fed to a commercial acrylonitrile reactor is accomplished in accordance with this invention by adjusting the NH 3 /C3 ⁇ ratio setpoint in controller 38 for controlling the operation of ammonia control valve 32 in response to the measured pH of the quench water bottoms in quench column 30.
  • pH sensor 37 continuously monitors the pH of the quench water column bottoms in quench column 30.
  • Sensor 37 is electronically connected to controller 38.
  • controller 38 is programmed so that its predetermined NH 3 /C 3 ⁇ ratio setpoint, which is used for controlling ammonia control valve 32 in response to the measured flowrate of incoming propylene, F 1; is modified so that this predetermined set point is adjusted in response to the measured pH of the quench water bottoms in quench column 30.
  • the measured pH of these quench water column bottoms provides an accurate indication of the concentration of unreacted ammonia in the hot reaction gases in reactor effluent line 26. Accordingly, the present invention takes advantage of this phenomenon by changing the NH 3 /C 3 ⁇ ratio setpoint of controller 38 in response to this measured pH. So, for example, if this measured pH becomes too low, which indicates that more sulfuric acid is being fed to quench column 30 than is necessary which, in turn, indicates that the amount of unreacted ammonia in reactor effluent line 26 has decreased, the NH 3 /C 3 ⁇ ratio setpoint of controller 38 is automatically increased by a corresponding amount.
  • This set point decrease causes a decrease in the relative amount of propylene fed to the reactor, and hence a corresponding increase in the relative amount of ammonia fed to the reactor, which in turn causes the amount of unreacted ammonia in the hot reaction gases in reactor effluent line 26 to increase back to its desired value.
  • a quench liquid is provided to the quench vessel through line 45.
  • the quench liquid may include an acid to maintain a pH of the quench liquid of about 3 to about 6, and in another aspect, about 4.5 to about 6.
  • the acid utilized may be sulfuric acid.
  • the process includes adjusting an amount of ammonia in the reactor feed to provide an ammonia to hydrocarbon molar ratio of about 1 to about 2, in another aspect, about 1.25 to about 1.75, in another aspect, about 1.4 to about 1.6, and in another aspect, about 1.25 to about 1.3.
  • a significant advantage is that reliance on the NH 3 /C3 ⁇ ratio setpoint of controller 38 to insure that a proper amount of ammonia is always maintained in the acrylonitrile reactor occurs both automatically and continuously and hence is no longer dependent on a manual analytical test that occurs discontinuously.
  • the system is configured such that a pH change resulting from increasing or decreasing ammonia flow through the ammonia control valve is detected by the pH sensor within a lag time of one hour or less.
  • the lag time may be about 10 seconds to about 60 minutes, in another aspect, about 30 seconds to about 45 minutes, in another aspect, about 1 minute to about 30 minutes, in another aspect, about 1 minute to about 10 minutes, in another aspect, about 1 minute to about 5 minutes, and in another aspect, about 2 minutes to about 4 minutes.
  • a process for controlling an amount of air provided to an ammoxidation reaction includes monitoring an amount of oxygen in the reactor effluent and adjusting an amount of air in the reactor feed to provide an air to hydrocarbon ratio of about 9 to about 12 in the reactor feed, in another aspect, a ratio of about 9 to about 11, in another aspect, a ratio of about 9 to about 10, in another aspect, a ratio of about 10.5 to about 11, in another aspect, a ratio of about 9.25 to about 9.75, and in another aspect, a ratio of about 9.4 to about 9.6.
  • the reactor effluent stream includes about 0.5 to about 1 weight % oxygen.
  • the process may further include continuously measuring the amount of oxygen in the reactor effluent and continuously adjusting the molar ratio of air to hydrocarbon in response.
  • Oxygen may be measured at any location downstream of the reactor, such as for example, between the reactor and quench column or downstream of the quench column.
  • the oxygen monitor is electronically connected to controller 38. Controller 38 may be configured to increase or decrease air flow to the reactor. The system is configured such that an oxygen change resulting from increased or decrease oxygen flow is detected by the oxygen monitor within a lag time of one hour or less.
  • the lag time may be about 10 seconds to about 60 minutes, in another aspect, about 30 seconds to about 45 minutes, in another aspect, about 1 minute to about 30 minutes, in another aspect, about 1 minute to about 10 minutes, in another aspect, about 1 minute to about 5 minutes, and in another aspect, about 2 minutes to about 4 minutes.
  • Ammonia control and air control may be utilized individually or may both be included in an ammoxidation process.
  • the technology of this invention requires that no new equipment or structure be added to an existing acrylonitrile plant, since it can be implemented using only the equipment already in the plant, in particular controller 38, ammonia control valve 32 and pH sensor 37 for sensing the pH of the quench column water bottoms. All that is necessary to implement this invention is to electronically connect pH sensor 37 with controller 38 and reprogram this controller to adjust its NH 3 /C3 ⁇ ratio setpoint in response the signal generated by this sensor in accordance with the teachings of this invention, which are easy and inexpensive to do.
  • the process and systems described herein may be utilized with multiple size reactors and quench columns, including reactors having large diameters, such as for example, about 9 to about 12 meters, in another aspect, about 10 to about 12 meters, in another aspect, about 10 to about 11 meters, in another aspect about 9.4 meters and above, in another aspect, about 9.5 meters, and in another aspect, about 10.7 meters.
  • a ratio of cross-sectional area of the ammoxidation reactor to a cross- sectional area of the quench column is about 1 to about 3, in another aspect, about 1.5 to about 2.5, and in another aspect, about 1.6 to about 1.9.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Combustion & Propulsion (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)

Abstract

La présente invention concerne un procédé et un système de commande d'une quantité d'ammoniac et/ou d'air fournie à un réacteur d'ammoxydation. Le procédé consiste à maintenir un pH de résidus d'eau de trempe et à ajuster une quantité d'ammoniac dans une charge d'alimentation de réacteur afin de fournir un rapport entre l'ammoniac et les hydrocarbures d'environ 1 à environ 2 dans la charge d'alimentation du réacteur. De plus, le procédé peut consister à ajuster une quantité d'air dans la charge d'alimentation du réacteur pour fournir un rapport entre l'air et les hydrocarbures d'environ 9 à environ 10 dans la charge d'alimentation du réacteur.
EP15731470.9A 2014-06-27 2015-06-15 Commande d'alimentation en ammoniac et/ou en air d'un réacteur d'ammoxydation Withdrawn EP3160634A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CN201410295420.7A CN104028172B (zh) 2014-06-27 2014-06-27 用于氨氧化反应器的氨进料的控制
PCT/US2015/035791 WO2015200022A1 (fr) 2014-06-27 2015-06-15 Commande d'alimentation en ammoniac et/ou en air d'un réacteur d'ammoxydation

Publications (1)

Publication Number Publication Date
EP3160634A1 true EP3160634A1 (fr) 2017-05-03

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EP15731470.9A Withdrawn EP3160634A1 (fr) 2014-06-27 2015-06-15 Commande d'alimentation en ammoniac et/ou en air d'un réacteur d'ammoxydation

Country Status (7)

Country Link
EP (1) EP3160634A1 (fr)
JP (1) JP2017520579A (fr)
KR (1) KR20170023847A (fr)
CN (2) CN107252663A (fr)
EA (1) EA201692340A1 (fr)
TW (1) TW201605772A (fr)
WO (1) WO2015200022A1 (fr)

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CN107420917A (zh) * 2016-05-24 2017-12-01 英尼奥斯欧洲股份公司 废气焚烧炉控制
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KR102404282B1 (ko) * 2019-09-24 2022-05-30 주식회사 엘지화학 유동층 반응기

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Also Published As

Publication number Publication date
WO2015200022A1 (fr) 2015-12-30
CN104028172B (zh) 2018-05-25
JP2017520579A (ja) 2017-07-27
CN107252663A (zh) 2017-10-17
CN104028172A (zh) 2014-09-10
TW201605772A (zh) 2016-02-16
EA201692340A1 (ru) 2017-08-31
KR20170023847A (ko) 2017-03-06

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