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WO2018168641A1 - Fluide de nettoyage, détergent, et procédé de nettoyage d'élément en contact avec l'eau - Google Patents

Fluide de nettoyage, détergent, et procédé de nettoyage d'élément en contact avec l'eau Download PDF

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Publication number
WO2018168641A1
WO2018168641A1 PCT/JP2018/008978 JP2018008978W WO2018168641A1 WO 2018168641 A1 WO2018168641 A1 WO 2018168641A1 JP 2018008978 W JP2018008978 W JP 2018008978W WO 2018168641 A1 WO2018168641 A1 WO 2018168641A1
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WO
WIPO (PCT)
Prior art keywords
cleaning
chlorine
membrane
compound
water
Prior art date
Application number
PCT/JP2018/008978
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English (en)
Japanese (ja)
Inventor
貴子 岩見
孝博 川勝
愛理 田中
Original Assignee
栗田工業株式会社
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 栗田工業株式会社 filed Critical 栗田工業株式会社
Priority to JP2018513034A priority Critical patent/JP6610776B2/ja
Priority to CN201880010367.8A priority patent/CN110248723B/zh
Publication of WO2018168641A1 publication Critical patent/WO2018168641A1/fr

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D65/00—Accessories or auxiliary operations, in general, for separation processes or apparatus using semi-permeable membranes
    • B01D65/02—Membrane cleaning or sterilisation ; Membrane regeneration
    • B01D65/06—Membrane cleaning or sterilisation ; Membrane regeneration with special washing compositions
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
    • C11D17/08—Liquid soap, e.g. for dispensers; capsuled
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
    • C11D7/02—Inorganic compounds
    • C11D7/04—Water-soluble compounds
    • C11D7/08—Acids
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
    • C11D7/02—Inorganic compounds
    • C11D7/04—Water-soluble compounds
    • C11D7/10—Salts

Definitions

  • the present invention relates to a cleaning liquid, a cleaning agent, and a cleaning method for cleaning a wetted member such as a UF membrane (ultrafiltration membrane), an MF membrane (microfiltration membrane), a filter, a pipe, a pressure gauge, and a flow meter.
  • a wetted member such as a UF membrane (ultrafiltration membrane), an MF membrane (microfiltration membrane), a filter, a pipe, a pressure gauge, and a flow meter.
  • Patent Document 1 describes that a film that is susceptible to oxidative degradation is washed with a combined chlorine agent.
  • the concentration of the chloramine compound is 0.005 to 0.5 M, and the molar ratio (Cl 2 / N) of effective chlorine (Cl 2 ) to nitrogen atom N derived from the chloramine compound is 0.00.
  • the membrane is cleaned under conditions where almost no free chlorine exists.
  • Patent Document 2 describes that a cooling water system, a wastewater treatment water system, and a paper pulp water system are sterilized by using a combined chlorine agent having Cl 2 / N larger than 1. Patent Document 2 describes that the free chlorine concentration during the sterilization treatment is 0.05 mg / L or more. Patent Document 2 does not describe the use of the cleaning agent for the selective permeable membrane.
  • An object of the present invention is to provide a cleaning liquid, a cleaning agent, and a cleaning method having a high cleaning effect.
  • the gist of the present invention is as follows.
  • the cleaning solution for a water contact member of the present invention is a cleaning solution containing free chlorine and a chloramine compound, and the molar ratio (Cl 2 / N) of nitrogen atoms N derived from total chlorine and the chloramine compound is 1 or more, and the pH is 9 That's it.
  • the chloramine compound includes at least one sulfamic acid compound selected from bound chlorine type sulfamic acid and a salt thereof.
  • the water contact member is at least one of an MF membrane, a UF membrane, a filter, a pipe, a pressure gauge, and a flow meter.
  • the pH of the cleaning liquid is 11 or more.
  • the combined chlorine concentration of the chloramine compound and chlorine is 100 mg / L or more, and the free chlorine concentration is 20 mg / L or more.
  • the cleaning agent for a water contact member of the present invention is a cleaning agent containing free chlorine and a chloramine compound, and the molar ratio (Cl 2 / N) of nitrogen atoms N derived from total chlorine and the chloramine compound is 1 or more. , PH 12 or more.
  • the chloramine compound includes at least one sulfamic acid compound selected from bound chlorine type sulfamic acid and a salt thereof.
  • the cleaning agent of the present invention it is obtained by mixing sulfamic acid and an alkali agent and then adding a chlorine agent to form a combined chlorine compound.
  • the concentration of sulfamic acid relative to the final cleaning agent weight is 5% by mass or less.
  • the water contact member is at least one of an MF membrane, a UF membrane, a filter, a pipe, a pressure gauge, and a flow meter.
  • the cleaning solution for the water contact member of the present invention is obtained by diluting the above-described cleaning agent of the present invention with water.
  • the water contact member cleaning method of the present invention cleans the water contact member using the cleaning liquid of the present invention.
  • the cleaning solution, cleaning agent, and cleaning method for the water contact member of the present invention have both the oxidizing power of the free chlorine agent and the strength of penetration of the bound chlorine agent (chloramine compound) into the water contact member. Therefore, it is more effective than the combined chlorine agent and has a higher cleaning effect than the free chlorine agent. Moreover, the cleaning liquid and the cleaning agent of the present invention also have an excellent sterilizing effect.
  • the present invention relates to a cleaning liquid, a cleaning agent, and a cleaning method.
  • cleaning liquid and “cleaning agent” are distinguished as follows.
  • the cleaning liquid is a liquid used during cleaning.
  • the cleaning agent in the present invention is a product used for distribution.
  • the cleaning agent may be used as it is as a cleaning solution, but usually the cleaning agent is diluted with water or the like and used as a cleaning solution for cleaning.
  • the cleaning liquid of the present invention contains free chlorine and a combined chlorine compound.
  • the cleaning liquid of the present invention has a molar ratio (Cl 2 / N) of nitrogen atoms N derived from total chlorine (Cl 2 ) and combined chlorine compounds of 1 or more and a pH of 9 or more.
  • Cleaning solution of the present invention preferably, the total chlorine concentration 5,000mg-Cl 2 / L or less, more preferably 200 ⁇ 5,000mg-Cl 2 / L , particularly preferably 1,000 ⁇ 2,000mg-Cl 2 / L, bound chlorine concentration of 100 mg-Cl 2 / L or more, more preferably 100 to 4,980 mg-Cl 2 / L, particularly preferably 300 to 1,980 mg-Cl 2 / L, free chlorine concentration of 20 mg-Cl 2 / L or more, more preferably 20 to 4,900 mg-Cl 2 / L, particularly preferably 20 to 1,700 mg-Cl 2 / L.
  • the cleaning agent of the present invention is a cleaning agent containing free chlorine and a chloramine compound, and the molar ratio (Cl 2 / N) of total chlorine (Cl 2 ) to nitrogen atom N derived from the chloramine compound is 1 or more. , PH 12 or more.
  • the cleaning agent of the present invention preferably has a total chlorine concentration (Cl 2 equivalent concentration) of 10% by mass or less, more preferably 1 to 8% by mass, particularly preferably 3 to 8% by mass.
  • the combined chlorine concentration (Cl 2 equivalent concentration) is 0.1% by mass or more, more preferably 0.5 to 3% by mass, particularly preferably 1 to 2.8% by mass, and the free chlorine concentration (Cl 2 equivalent concentration) is 0. 0.02% by mass or more, more preferably 0.1 to 10% by mass, particularly preferably 1 to 5% by mass.
  • the total chlorine concentration and the free chlorine concentration are measured by the DPD method defined in JIS K 0400-33-10: 1999.
  • the bound chlorine concentration is determined by subtracting the free chlorine concentration from the total chlorine concentration determined above.
  • the present invention makes it possible to apply a chlorine-based cleaning liquid and a cleaning agent to a water contact member under alkaline conditions.
  • the organic substance decomposing action by the combined chlorine compound and the immediate sterilizing and washing effect by free chlorine are synergistically added to the organic substance peeling action and hydrolysis action by washing under alkaline conditions. For this reason, according to this invention, the effect of alkali washing
  • the water contact member examples include, but are not limited to, a UF membrane, an MF membrane, a filter, a pipe, a pressure gauge, and a flow meter.
  • the filter examples include those using granular filter media such as sand and anthracite.
  • the selective permeable membrane is not limited to these, and the present invention can be applied to other selective permeable membranes, and the membrane material is not limited.
  • hypochlorous acid and / or hypochlorite is used.
  • hypochlorite alkali metal salts of hypochlorous acid such as sodium hypochlorite, alkaline earth metal salts of hypochlorous acid such as calcium hypochlorite, and the like can be used. These may be used alone or in combination of two or more.
  • the bound chlorine compound is obtained by reacting hypochlorous acid (HOCl) with a compound having a primary amino group (XNH 2 ) by the reaction shown in the following reaction formulas (1) and (2).
  • a compound (XNHCl) in which a hydrogen atom of an amino group is substituted with a chlorine atom is preferred. Since this compound has a weak oxidizing action, it can be used as a cleaning liquid and a cleaning agent even for aromatic polyamide RO membranes with low chlorine resistance. Also penetrates and exerts a decomposing action inside.
  • the bonded chlorine compound is any one of a compound having a primary amino group, ammonia, and an ammonium salt (hereinafter referred to as “NH 2 -based compound”), hypochlorous acid and / or the following. It is preferable to produce by mixing with chlorite.
  • NH 2 -based compound an ammonium salt
  • the compound having a primary amino group include aliphatic amines, aromatic amines, sulfamic acids, sulfanilic acids, sulfamoylbenzoic acids, and amino acids.
  • ammonium salts include ammonium chloride and ammonium sulfate. These may be used alone or in combination of two or more.
  • sulfamic acid (NH 2 SO 2 OH) is preferable.
  • a stable bound chlorine compound is obtained. Since sulfamic acid does not contain carbon, it does not increase the TOC value of the cleaning agent.
  • sulfamic acid and an alkaline agent in combination, a very effective cleaning solution and cleaning agent are obtained.
  • Hypochlorite to be reacted with NH 2 compounds includes alkali metal salts of hypochlorous acid such as sodium hypochlorite, alkaline earth metal salts of hypochlorous acid such as calcium hypochlorite, etc. Can be used. These may be used alone or in combination of two or more.
  • the weight concentration of sulfamic acid used is preferably 5% by mass or less based on the weight of the final cleaning agent. If the concentration of sulfamic acid is higher than 5% by mass, chlorine may be easily decomposed.
  • the Cl 2 / N molar ratio which is the molar ratio of available chlorine derived from free chlorine (Cl 2 ) and nitrogen atom N derived from the combined chlorine compound, is 1 or more, preferably 1 to 10, particularly preferably 1 to 5. By setting it within this range, an immediate cleaning action of free chlorine and an osmotic cleaning action of the combined chlorine compound can be obtained in a balanced manner.
  • the cleaning liquid of the present invention comprises an aqueous alkaline solution containing free chlorine and a combined chlorine compound, and has a pH of 9 or more. If the pH of the cleaning liquid is less than 9, sufficient cleaning properties cannot be obtained. The higher the pH of the cleaning solution is, the better the cleaning effect is. However, when the cleaning solution is too high, the handling property as the cleaning solution is deteriorated, and the film to be cleaned is deteriorated or the risk of corrosion of the metal is increased.
  • the pH of the cleaning liquid is preferably 11 or more and 13 or less.
  • the alkali agent used to adjust the cleaning liquid of the present invention to pH 9 or more, particularly 12 or more, is preferably an alkali metal hydroxide such as sodium hydroxide or potassium hydroxide.
  • the cleaning agent of the present invention comprises an aqueous alkaline solution containing free chlorine and bound chlorine, and has a pH of 12 or more.
  • the pH of the cleaning agent is preferably 13 or more. If the pH of the cleaning agent is too high, the total chlorine concentration becomes low, and the balance with the pH when diluted is poor.
  • the upper limit of the pH of the cleaning agent of the present invention is 14.
  • the cleaning liquid and cleaning agent of the present invention are prepared by adding and dissolving an NH 2 -based compound such as sulfamic acid in the aqueous solution of the alkali agent described above, and adding hypochlorous acid and / or hypochlorous acid to the resulting NH 2 -based compound aqueous solution.
  • a combined chlorine compound aqueous solution can be prepared by adding and mixing chlorate, and hypochlorous acid and / or hypochlorite can be added to and mixed with this combined chlorine compound aqueous solution. .
  • a compound having a primary amino group such as sulfamic acid may be added in the form of a salt.
  • a salt sodium sulfamate, potassium sulfamate, ammonium sulfamate, etc. can be used.
  • the cleaning liquid of the present invention may be obtained by diluting the cleaning agent produced as described above with water, preferably with pure water as necessary.
  • surfactants and chelating agents such as EDTA (ethylenediaminetetraacetic acid), EGTA (ethyleneglycolbis (aminoethylether) tetraacetic acid), IDA (iminodiacetic acid), etc. to enhance the peeling effect of membrane contaminants You may add 1 type, or 2 or more types of the other washing
  • EDTA ethylenediaminetetraacetic acid
  • EGTA ethyleneglycolbis (aminoethylether) tetraacetic acid
  • IDA iminodiacetic acid
  • the water contact member is brought into contact with the cleaning liquid.
  • the cleaning liquid is introduced into the membrane device.
  • the cleaning liquid may be introduced from the raw water inlet of the membrane device, or may be introduced from the treated water outlet and pushed out to the raw water side.
  • the membrane is immersed in the cleaning liquid or the cleaning liquid is circulated. When the cleaning liquid is circulated, air may be blown into the cleaning liquid.
  • the contact time between the cleaning solution and the selective permeable membrane is preferably about 1 to 24 hours, particularly about 1 to 18 hours. Also in the case of a water contact member other than a membrane, the contact time between the cleaning liquid and the water contact member is preferably about 1 to 24 hours, particularly about 1 to 18 hours.
  • Example 1 Using a membrane (effective membrane length 100 mm) obtained from a UF hollow fiber membrane module (HFU-2008, membrane material PVDF, pore diameter 0.01 ⁇ m) manufactured by Toray Industries, Inc., a single membrane module (single yarn module) was created. . Thereafter, the membrane was contaminated by passing water for industrial use (hereinafter referred to as “Yamakura Kosui”) in the Hara area of Goi City, Chiba Prefecture with the single-thread module water flow device shown in FIG.
  • Yamakura Kosui contaminated by passing water for industrial use
  • the membrane 1 is arranged in the column 2 with its upper and lower ends held by holding members 3a and 3b made of a potting material.
  • the upper end of the film 1 is embedded in the holding member 3a.
  • the lower end of the membrane 1 passes through the holding member 3b and communicates with the chamber 4 below the column 2.
  • Yamakura industrial water is supplied to the lower part of the column 2 (above the holding member 3b) via the pipe 5, the pump 6 and the valve 7, and the permeated water passes through the valve 8 and the pipe 9 from the chamber 4 at the lower end of the column 2. Leaked.
  • the concentrated water flows out from the upper part of the column 2 (just below the holding member 3a) through the pipe 10 and the valve 11.
  • the backwash water is introduced into the chamber 4 at the lower end of the column 2 through the pipe 12, the pump 13 and the valve 14 and flows into the membrane 2.
  • the backwash drainage flows out through the pipe 15 and the valve 16 branched from the pipe 10.
  • Process 1 Water filling (30 seconds)
  • Step 2 Filtration (permeation flux 2-4 m 3 / m 2 / d, 28 minutes)
  • Step 3 Backwash (water volume 0.6-1.4 mL / min, 30 seconds)
  • Process 4 Drainage (30 seconds)
  • the measurement result of the transmembrane pressure value (relation between the immersion time and the transmembrane pressure value) is shown in FIG.
  • Each cleaning solution has a pH of 12 and a total chlorine concentration of about 1200 mg. Free chlorine concentration was measured by the DPD method.
  • Fig. 4 shows the relationship between cleaning time and differential pressure. It can be seen that the cleaning liquid prepared by diluting the cleaning agent of Example 5 has the fastest difference pressure drop and the lowest ultimate pressure difference. In Comparative Example 6, the ultimate differential pressure remains high. In Comparative Examples 7 and 8, the ultimate differential pressure is close to that of Example 5, but the method of decreasing the differential pressure is slow.
  • FIG. 7 shows the relationship between the molar concentration of sulfamic acid and the residual effective molar concentration of chlorine in the detergents obtained by the formulations (i) to (iv), and the decomposition rate of chlorine. As shown in FIG. 7, the higher the weight concentration of sulfamic acid, the greater the decomposition rate of chlorine.
  • the weight concentration of sulfamic acid is 5.0 mass%
  • the ratio of (effective chlorine molar concentration) / (sulfamic acid molar concentration) is 1.01, which is slightly over 1. Accordingly, the weight concentration of sulfamic acid is preferably 5.0% by mass or less. The reason why the decomposition rate of chlorine increases is presumably because unstable dichlorosulfamic acid is easily formed.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)
  • Detergent Compositions (AREA)

Abstract

L'invention concerne un fluide de nettoyage et un détergent destinés à des éléments en contact avec l'eau, contenant tous les deux du chlore libre et un composé de chlore combiné, le rapport molaire du chlore total (Cl2) aux atomes d'azote N dérivés du composé de chlore combiné, Cl2/N, étant égal ou supérieur à 1, le fluide de nettoyage ayant un pH égale ou supérieur à 9 et le détergent ayant un pH égale ou supérieur à 12. Le fluide de nettoyage peut être préparé par dilution du détergent avec de l'eau. L'invention concerne également un procédé de nettoyage destiné à des éléments en contact avec l'eau, le procédé consistant à utiliser le fluide de nettoyage pour nettoyer un élément en contact avec l'eau.
PCT/JP2018/008978 2017-03-15 2018-03-08 Fluide de nettoyage, détergent, et procédé de nettoyage d'élément en contact avec l'eau WO2018168641A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
JP2018513034A JP6610776B2 (ja) 2017-03-15 2018-03-08 接水部材の洗浄液および洗浄方法
CN201880010367.8A CN110248723B (zh) 2017-03-15 2018-03-08 水接触构件的洗涤液、洗涤剂及洗涤方法

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2017050165 2017-03-15
JP2017-050165 2017-03-15

Publications (1)

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WO2018168641A1 true WO2018168641A1 (fr) 2018-09-20

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PCT/JP2018/008978 WO2018168641A1 (fr) 2017-03-15 2018-03-08 Fluide de nettoyage, détergent, et procédé de nettoyage d'élément en contact avec l'eau

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JP (1) JP6610776B2 (fr)
CN (1) CN110248723B (fr)
TW (1) TWI734898B (fr)
WO (1) WO2018168641A1 (fr)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110449033A (zh) * 2019-08-27 2019-11-15 湖北中泉环保技术有限公司 超滤膜表面有机沉积物的清洗方法
CN114940906A (zh) * 2022-05-13 2022-08-26 武汉汉烯科技有限公司 一种适用于多相金属矿物的高效腐蚀剂及制备方法

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JPH07124559A (ja) * 1993-11-08 1995-05-16 Toyobo Co Ltd 海水淡水化プロセスにおける被処理水の殺菌方法
JP2009195823A (ja) * 2008-02-21 2009-09-03 Kurita Water Ind Ltd 水系処理剤の濃度制御方法
JP2013010718A (ja) * 2011-06-29 2013-01-17 Hakuto Co Ltd スライム剥離剤およびスライム剥離方法
WO2013179775A1 (fr) * 2012-05-30 2013-12-05 栗田工業株式会社 Agent de nettoyage de film de perméation et procédé de nettoyage
JP2015097991A (ja) * 2013-11-19 2015-05-28 栗田工業株式会社 透過膜の洗浄剤及び洗浄方法
JP2016215125A (ja) * 2015-05-20 2016-12-22 栗田工業株式会社 ポリアミド系逆浸透膜の洗浄液、および洗浄方法

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JP3832399B2 (ja) * 2001-08-28 2006-10-11 栗田工業株式会社 殺菌殺藻剤組成物及び水系の殺菌殺藻方法
SG184357A1 (en) * 2010-03-31 2012-11-29 Kurita Water Ind Ltd Combined chlorine agent, and manufacturing method and method of use for same
TWI537046B (zh) * 2011-07-06 2016-06-11 栗田工業股份有限公司 膜分離方法
JP6299595B2 (ja) * 2013-06-28 2018-03-28 三菱ケミカル株式会社 濾過膜の洗浄方法
JP5892136B2 (ja) * 2013-09-24 2016-03-23 栗田工業株式会社 冷却水系の殺藻方法

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH07124559A (ja) * 1993-11-08 1995-05-16 Toyobo Co Ltd 海水淡水化プロセスにおける被処理水の殺菌方法
JP2009195823A (ja) * 2008-02-21 2009-09-03 Kurita Water Ind Ltd 水系処理剤の濃度制御方法
JP2013010718A (ja) * 2011-06-29 2013-01-17 Hakuto Co Ltd スライム剥離剤およびスライム剥離方法
WO2013179775A1 (fr) * 2012-05-30 2013-12-05 栗田工業株式会社 Agent de nettoyage de film de perméation et procédé de nettoyage
JP2015097991A (ja) * 2013-11-19 2015-05-28 栗田工業株式会社 透過膜の洗浄剤及び洗浄方法
JP2016215125A (ja) * 2015-05-20 2016-12-22 栗田工業株式会社 ポリアミド系逆浸透膜の洗浄液、および洗浄方法

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110449033A (zh) * 2019-08-27 2019-11-15 湖北中泉环保技术有限公司 超滤膜表面有机沉积物的清洗方法
CN114940906A (zh) * 2022-05-13 2022-08-26 武汉汉烯科技有限公司 一种适用于多相金属矿物的高效腐蚀剂及制备方法
CN114940906B (zh) * 2022-05-13 2023-10-10 武汉汉烯科技有限公司 一种适用于多相金属矿物的高效腐蚀剂及制备方法

Also Published As

Publication number Publication date
TWI734898B (zh) 2021-08-01
TW201902563A (zh) 2019-01-16
JPWO2018168641A1 (ja) 2019-03-28
JP6610776B2 (ja) 2019-11-27
CN110248723A (zh) 2019-09-17
CN110248723B (zh) 2020-09-11

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