JP7275618B2 - Method for treating slurry containing heavy metals - Google Patents

Method for treating slurry containing heavy metals Download PDF

Info

Publication number
JP7275618B2
JP7275618B2 JP2019020862A JP2019020862A JP7275618B2 JP 7275618 B2 JP7275618 B2 JP 7275618B2 JP 2019020862 A JP2019020862 A JP 2019020862A JP 2019020862 A JP2019020862 A JP 2019020862A JP 7275618 B2 JP7275618 B2 JP 7275618B2
Authority
JP
Japan
Prior art keywords
heavy metal
slurry
magnesium oxide
sludge
containing slurry
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
JP2019020862A
Other languages
Japanese (ja)
Other versions
JP2020127911A (en
Inventor
崇 原口
隆明 篠原
健一 藪中
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.)
Kurita Water Industries Ltd
Original Assignee
Kurita Water Industries 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 Kurita Water Industries Ltd filed Critical Kurita Water Industries Ltd
Priority to JP2019020862A priority Critical patent/JP7275618B2/en
Publication of JP2020127911A publication Critical patent/JP2020127911A/en
Application granted granted Critical
Publication of JP7275618B2 publication Critical patent/JP7275618B2/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Landscapes

  • Treatment Of Sludge (AREA)

Description

本発明は、排煙脱硫排水などの処理により生じた重金属含有スラリーの処理方法に係り、特に重金属として少なくともカドミウムを含む重金属含有スラリーの処理方法に関する。 TECHNICAL FIELD The present invention relates to a method for treating heavy metal-containing slurry produced by treating flue gas desulfurization effluent, and more particularly to a method for treating heavy metal-containing slurry containing at least cadmium as a heavy metal.

工場等に発生する重金属含有排水を処理した際に発生する汚泥からの重金属の溶出を防止する薬剤として、特許文献1には、鉄、マンガン及びアルミニウムから選ばれる少なくも1種の金属の水溶性酸性金属塩と、アルカリ金属及び又はアルカリ土類金属の水難溶性塩基性化合物と、水とを含む材料を粉体混合して得られる混合物からなる薬剤が記載されている。 As an agent for preventing the elution of heavy metals from sludge generated when wastewater containing heavy metals generated in factories, etc. is treated, Patent Document 1 discloses at least one kind of water-soluble metal selected from iron, manganese and aluminum. A drug comprising a mixture obtained by powder-mixing a material containing an acid metal salt, a poorly water-soluble basic compound of an alkali metal and/or an alkaline earth metal, and water is described.

この水溶性酸性金属塩は、塩化鉄、硝酸鉄、硫酸鉄、塩化マンガン、硫酸マンガン、塩化アルミニウム及び硫酸アルミニウムから選ばれる少なくとも1種であり、水難溶性塩基性化合物は、酸化カルシウム、水酸化カルシウム、珪酸カルシウム、酸化マグネシウム、水酸化マグネシウム、珪酸ナトリウム、珪酸カリウム、珪酸塩ガラス、製鉄スラグ及びセメントから選ばれる少なくとも1種である。 The water-soluble acidic metal salt is at least one selected from iron chloride, iron nitrate, iron sulfate, manganese chloride, manganese sulfate, aluminum chloride and aluminum sulfate, and the poorly water-soluble basic compound is calcium oxide and calcium hydroxide. , calcium silicate, magnesium oxide, magnesium hydroxide, sodium silicate, potassium silicate, silicate glass, steelmaking slag and cement.

特開2015-81270号公報JP 2015-81270 A

特許文献1の重金属不溶化薬剤は、複数の金属塩などを混合した粉体混合物であり製造に手間がかかる。また、脱水した汚泥に不溶化剤を添加する場合、脱水汚泥と不溶化剤を均一に混合するための混合装置が必要である。 The heavy metal insolubilizing agent of Patent Document 1 is a powder mixture in which a plurality of metal salts and the like are mixed, and thus production is troublesome. Moreover, when adding an insolubilizing agent to the dehydrated sludge, a mixing device is required to uniformly mix the dehydrated sludge and the insolubilizing agent.

本発明は、重金属含有汚泥からのカドミウム溶出を防止することができ、かつ容易に実施することができる重金属含有スラリーの処理方法を提供することを目的とする。 An object of the present invention is to provide a method for treating a heavy metal-containing slurry that can prevent cadmium elution from the heavy metal-containing sludge and can be easily carried out.

本発明の重金属含有スラリーの処理方法は、カドミウムを含む重金属含有スラリーに対し酸化マグネシウムを添加する工程を有する。 A method for treating a heavy metal-containing slurry of the present invention has a step of adding magnesium oxide to a heavy metal-containing slurry containing cadmium.

本発明の一態様では、前記重金属含有スラリーは、火力発電所の排煙脱硫排水を凝集処理し、さらに沈殿処理することにより生じたスラリーである。 In one aspect of the present invention, the heavy metal-containing slurry is a slurry produced by subjecting flue gas desulfurization effluent from a thermal power plant to flocculation treatment and further to precipitation treatment.

本発明の一態様では、前記酸化マグネシウムをスラリーの沈殿槽又は濃縮槽で混合する。 In one aspect of the invention, the magnesium oxide is mixed in a slurry settler or thickener.

本発明の一態様では、前記重金属含有スラリーに対する酸化マグネシウムの添加量が固形分重量比で0.1~10%特に0.2~3%である。 In one aspect of the present invention, the amount of magnesium oxide added to the heavy metal-containing slurry is 0.1 to 10%, particularly 0.2 to 3% in terms of solid content weight ratio.

本発明では、不溶化剤として酸化マグネシウムを重金属含有スラリーに添加することにより、汚泥からのカドミウムの溶出を防止する。酸化マグネシウムの添加により汚泥からのカドミウムの溶出が防止される機構については、酸化マグネシウムのpH緩衝作用によるものと推察される。 In the present invention, leaching of cadmium from sludge is prevented by adding magnesium oxide as an insolubilizing agent to the heavy metal-containing slurry. The mechanism by which the addition of magnesium oxide prevents cadmium from eluting from the sludge is presumed to be due to the pH buffering action of magnesium oxide.

本発明の一態様では、酸化マグネシウムと重金属含有スラリーとを、沈殿槽又は濃縮槽で混合する。例えば、酸化マグネシウムを重金属含有スラリーの沈殿槽又は濃縮槽に添加して混合する。これにより、汚泥と不溶化剤との混合専用の装置が不要となる。 In one aspect of the invention, the magnesium oxide and heavy metal-containing slurry are mixed in a settling tank or a thickening tank. For example, magnesium oxide is added to and mixed with the settling tank or thickening tank of the heavy metal-containing slurry. This eliminates the need for a dedicated device for mixing the sludge and the insolubilizer.

本発明方法の一例を示す説明図である。BRIEF DESCRIPTION OF THE DRAWINGS It is explanatory drawing which shows an example of this invention method.

本発明では、重金属として少なくともカドミウムを含む重金属含有スラリーを処理する。このような重金属含有スラリーとしては、火力発電所排煙脱硫排水を無機凝集剤及びポリマー凝集剤を用いて凝集処理することにより生じたスラリーのほか、化学工場、鉱山、製錬所、製鉄所、鍍金工場、焼却処分場等から排出される重金属含有排水を凝集処理することにより生じた重金属含有スラリーなどが例示される。 In the present invention, a heavy metal-containing slurry containing at least cadmium as a heavy metal is treated. Examples of such heavy metal-containing slurries include slurries produced by flocculating flue gas desulfurization effluent from thermal power plants using inorganic flocculants and polymer flocculants; Heavy metal-containing slurries produced by flocculating waste water containing heavy metals discharged from plating plants, incineration disposal sites, etc. are exemplified.

なお、火力発電所排煙脱硫排水には、石炭の種類にもよるが、0.01~2mg/L程度のカドミウムが含有されていることが多い。この火力発電所排煙脱硫排水を凝集処理した場合、カドミウム含有汚泥を含んだ凝集処理水が生成する。 It should be noted that flue gas desulfurization effluent from thermal power plants often contains about 0.01 to 2 mg/L of cadmium, depending on the type of coal. When this thermal power plant flue gas desulfurization effluent is coagulated, coagulated water containing cadmium-containing sludge is produced.

この汚泥を含んだ凝集処理水は、沈殿槽で沈殿分離され、さらに必要に応じて濃縮槽で濃縮される。本発明は、酸化マグネシウムの添加によって、このような沈殿汚泥あるいは濃縮汚泥からのカドミウム溶出を防止するものである。 The coagulated water containing this sludge is sedimented and separated in a sedimentation tank, and further concentrated in a thickening tank as necessary. The present invention prevents the elution of cadmium from such precipitated sludge or thickened sludge by adding magnesium oxide.

本発明では、カドミウム含有スラリーに添加されるカドミウム不溶化剤として酸化マグネシウムが用いられる。酸化マグネシウムとしては平均粒径(JIS篩による。以下、同様)が200μm以下、例えば5~200μm程度の粉末状のものが好ましい。 In the present invention, magnesium oxide is used as a cadmium-insolubilizing agent added to the cadmium-containing slurry. Magnesium oxide is preferably in the form of powder having an average particle size (according to JIS sieve, hereinafter the same) of 200 μm or less, for example, about 5 to 200 μm.

カドミウム含有スラリーに対し、酸化マグネシウムのみを添加してもよく、酸化マグネシウムの他に生石灰、消石灰、炭酸カルシウム、炭酸マグネシウム、水酸化マグネシウムなどを含む不溶化剤を添加してもよい。 Only magnesium oxide may be added to the cadmium-containing slurry, or an insolubilizer containing quick lime, slaked lime, calcium carbonate, magnesium carbonate, magnesium hydroxide, etc. may be added in addition to magnesium oxide.

酸化マグネシウムの重金属含有スラリーへの添加量は、重金属含有スラリー中の固形分(乾燥重量)100重量部に対し0.1~10重量部特に0.2~3重量部(固形分重量比で0.1~10%特に0.2~3%)程度が好ましい。 The amount of magnesium oxide added to the heavy metal-containing slurry is 0.1 to 10 parts by weight, particularly 0.2 to 3 parts by weight (0.2 to 3 parts by weight in solid content weight ratio) per 100 parts by weight of the solid content (dry weight) in the heavy metal-containing slurry. 0.1 to 10%, particularly 0.2 to 3%) is preferred.

本発明では、酸化マグネシウムを沈殿槽又は濃縮槽に添加し、好ましくは、沈殿槽又は濃縮槽の流入時に添加する。このように不溶化剤を沈殿槽又は濃縮槽に添加すると、添加された酸化マグネシウムは沈殿槽又は濃縮槽内に滞留する間に汚泥と十分に混合されるようになるので、酸化マグネシウムと汚泥とを混合するための専用の混合手段が不要である。 In the present invention magnesium oxide is added to the clarifier or thickener, preferably at the inflow of the clarifier or thickener. When the insolubilizing agent is added to the sedimentation tank or thickening tank in this way, the added magnesium oxide is sufficiently mixed with the sludge while staying in the sedimentation tank or thickening tank. A dedicated mixing means for mixing is not required.

図1は、濃縮槽(シックナー)に酸化マグネシウムを添加する場合の一例を示している。 FIG. 1 shows an example of adding magnesium oxide to a thickener (thickener).

濃縮槽1は、槽体2と、該槽体2の中央部に上下方向に設けられた筒状のフィードウェル3と、該フィードウェル3の下端に対峙するバッフル板4と、槽体2の底面に沿って旋回するレーキ5と、該レーキ5の回転装置6と、上澄水オーバーフロー用の越流堰7と、槽体2の底部中央から沈殿汚泥を抜き出すためのピット8等を有する。槽体2の底面は、ピット8に向って下り勾配となっている。 The thickening tank 1 includes a tank body 2, a cylindrical feedwell 3 vertically provided in the center of the tank body 2, a baffle plate 4 facing the lower end of the feedwell 3, and the tank body 2. It has a rake 5 rotating along the bottom surface, a rotating device 6 for the rake 5, an overflow weir 7 for overflowing supernatant water, a pit 8 for extracting settled sludge from the center of the bottom of the tank body 2, and the like. The bottom surface of the tank body 2 slopes downward toward the pit 8 .

排煙脱硫排水を凝集処理し、沈殿槽で沈殿処理されたスラリーがフィードウェル3に供給される。このフィードウェル3に流入するスラリーに対して(又はフィードウェル3に流入したスラリーに対してフィードウェル3内において)、酸化マグネシウムが添加される。酸化マグネシウムが添加されたスラリーは、濃縮槽1内に滞留する間に沈降濃縮され、上澄水は越流堰7をオーバーフローして取り出される。沈降濃縮された汚泥はピット8から配管9を介して取り出され、汚泥ポンプ10及び配管11を介して脱水機12に送られ、脱水処理される。 Flue gas desulfurization effluent is subjected to coagulation treatment, and a slurry obtained by precipitation treatment in a sedimentation tank is supplied to the feed well 3 . Magnesium oxide is added to the slurry flowing into this feedwell 3 (or within the feedwell 3 to the slurry flowing into the feedwell 3). The slurry to which magnesium oxide has been added is sedimented and concentrated while staying in the concentration tank 1, and the supernatant water overflows the overflow weir 7 and is taken out. The sedimented and thickened sludge is taken out from the pit 8 through the pipe 9, sent to the dehydrator 12 through the sludge pump 10 and the pipe 11, and dewatered.

脱水された汚泥は、コンベア13及びケーキホッパ14を介してトラック15等へ移送される。脱水機12で生じた脱水濾液は、一般排水貯槽又は排煙脱硫排水処理装置(図示略)へ送水される。 The dewatered sludge is transferred to the truck 15 or the like via the conveyor 13 and the cake hopper 14 . The dehydrated filtrate produced by the dehydrator 12 is sent to a general wastewater storage tank or a flue gas desulfurization wastewater treatment device (not shown).

なお、配管11から分岐した配管16によって汚泥の一部が濃縮槽1へ返送可能とされている。 A part of the sludge can be returned to the thickening tank 1 by a pipe 16 branched from the pipe 11 .

なお、図1は本発明方法の一例を示すものであり、本発明はこれに限定されない。 Note that FIG. 1 shows an example of the method of the present invention, and the present invention is not limited to this.

<処理対象スラリー>
火力発電所の排煙脱硫排水に無機凝集剤及びポリマー凝集剤を添加し、沈殿槽に導入して沈殿させた。この沈殿槽の底部から取り出された重金属含有スラリーの固形分(乾燥重量)含有量は50g/Lであった。
<Slurry to be processed>
An inorganic flocculant and a polymer flocculant were added to flue gas desulfurization effluent from a thermal power plant, and the mixture was introduced into a sedimentation tank and precipitated. The solids (dry weight) content of the heavy metal-containing slurry taken out from the bottom of this sedimentation tank was 50 g/L.

[実施例1~6]
上記の重金属含有スラリーを図1の濃縮槽1のフィードウェル3に流入させると共に、このスラリーに対し、酸化マグネシウム含有不溶化剤として、栗田工業株式会社製クリミックスM-5(酸化マグネシウム含有率90wt%)をフィードウェル3において、濃縮槽1内のスラリー中の酸化マグネシウム濃度が次の濃度となるように添加した(固形分重量比は、スラリー中のSS(懸濁物質)の乾燥重量に対する酸化マグネシウムの重量%を表わす。)。
[Examples 1 to 6]
The above heavy metal-containing slurry is flowed into the feed well 3 of the concentration tank 1 in FIG. ) was added to the feedwell 3 so that the magnesium oxide concentration in the slurry in the thickening tank 1 was the following concentration (the solid content weight ratio was magnesium oxide to the dry weight of SS (suspended solids) in the slurry represents the weight percent of ).

実施例1:150mg/L(固形分重量比0.25%)
実施例2:300mg/L(固形分重量比0.5%)
実施例3:600mg/L(固形分重量比1%)
実施例4:1800mg/L(固形分重量比3%)
実施例5:3000mg/L(固形分重量比5%)
実施例6:6000mg/L(固形分重量10%)
Example 1: 150 mg / L (solid content weight ratio 0.25%)
Example 2: 300 mg / L (solid content weight ratio 0.5%)
Example 3: 600 mg / L (solid content weight ratio 1%)
Example 4: 1800 mg / L (solid content weight ratio 3%)
Example 5: 3000 mg / L (solid content weight ratio 5%)
Example 6: 6000 mg / L (solid content weight 10%)

脱水機12で脱水して得られた脱水汚泥中のカドミウム等の各重金属の溶出値を昭和48年環境庁告示第13号に準拠して測定した。結果を表1に示す。 The elution value of each heavy metal such as cadmium in the dehydrated sludge obtained by dehydration by the dehydrator 12 was measured according to Environmental Agency Notification No. 13 of 1973. Table 1 shows the results.

また、脱水汚泥の含水率と、脱水濾液のCd濃度及びpHとを測定し、結果を表1に示した。 In addition, the moisture content of the dewatered sludge and the Cd concentration and pH of the dewatered filtrate were measured, and the results are shown in Table 1.

[比較例1]
不溶化剤を添加しなかったこと以外は実施例と同様の測定を行い、結果を表1に示した。
[Comparative Example 1]
Measurements were carried out in the same manner as in Examples except that no insolubilizing agent was added, and the results are shown in Table 1.

Figure 0007275618000001
Figure 0007275618000001

表1の通り、不溶化剤を300mg/L以上添加することにより、カドミウムが十分に不溶化されることが認められた。なお、脱水汚泥の含水率は60~65%とほぼ同じで不溶化剤の添加濃度の影響は認められない。 As shown in Table 1, it was confirmed that cadmium was sufficiently insolubilized by adding 300 mg/L or more of the insolubilizing agent. The water content of the dehydrated sludge is almost the same at 60 to 65%, and no effect of the added concentration of the insolubilizing agent is observed.

1 濃縮槽
2 槽体
3 フィードウェル
5 レーキ
7 越流堰
8 ピット
12 脱水機
1 thickening tank 2 tank body 3 feed well 5 rake 7 overflow weir 8 pit 12 dehydrator

Claims (1)

カドミウムを含む重金属含有スラリーに対し酸化マグネシウムを添加する工程を有する重金属含有スラリーの処理方法であって、
前記重金属含有スラリーは、火力発電所の排煙脱硫排水を凝集処理し、さらに沈殿処理することにより生じたスラリーであること、
前記酸化マグネシウムをスラリーの沈殿槽又は濃縮槽で混合すること、及び
前記重金属含有スラリーに対する酸化マグネシウムの添加量が固形分重量比で0.5~3%であり、
前記スラリーの脱水濾液のpHが7.8~8.4であることを特徴とする重金属含有スラリーの処理方法。
A method for treating a heavy metal-containing slurry comprising adding magnesium oxide to a heavy metal-containing slurry containing cadmium,
The heavy metal-containing slurry is a slurry produced by flocculating flue gas desulfurization wastewater from a thermal power plant and then precipitating it.
The magnesium oxide is mixed in a slurry sedimentation tank or thickening tank, and the amount of magnesium oxide added to the heavy metal-containing slurry is 0.5 to 3 % in solid content weight ratio ,
A method for treating a heavy metal-containing slurry , wherein the dehydrated filtrate of the slurry has a pH of 7.8 to 8.4 .
JP2019020862A 2019-02-07 2019-02-07 Method for treating slurry containing heavy metals Active JP7275618B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP2019020862A JP7275618B2 (en) 2019-02-07 2019-02-07 Method for treating slurry containing heavy metals

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP2019020862A JP7275618B2 (en) 2019-02-07 2019-02-07 Method for treating slurry containing heavy metals

Publications (2)

Publication Number Publication Date
JP2020127911A JP2020127911A (en) 2020-08-27
JP7275618B2 true JP7275618B2 (en) 2023-05-18

Family

ID=72175227

Family Applications (1)

Application Number Title Priority Date Filing Date
JP2019020862A Active JP7275618B2 (en) 2019-02-07 2019-02-07 Method for treating slurry containing heavy metals

Country Status (1)

Country Link
JP (1) JP7275618B2 (en)

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2003230897A (en) 2002-02-08 2003-08-19 Babcock Hitachi Kk Waste treatment method and waste treatment apparatus
JP2007105549A (en) 2005-08-19 2007-04-26 Ube Ind Ltd Treatment composition for heavy metal contaminated soil and treatment method
JP2015081270A (en) 2013-10-21 2015-04-27 日鉄住金環境株式会社 Harmful substance treating agent

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH1190169A (en) * 1997-09-18 1999-04-06 Chiyoda Corp Treatment of fly ash-containing waste gas and its treating device

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2003230897A (en) 2002-02-08 2003-08-19 Babcock Hitachi Kk Waste treatment method and waste treatment apparatus
JP2007105549A (en) 2005-08-19 2007-04-26 Ube Ind Ltd Treatment composition for heavy metal contaminated soil and treatment method
JP2015081270A (en) 2013-10-21 2015-04-27 日鉄住金環境株式会社 Harmful substance treating agent

Also Published As

Publication number Publication date
JP2020127911A (en) 2020-08-27

Similar Documents

Publication Publication Date Title
JP4515273B2 (en) Condensation separation purification agent and purification method of polluted waste water
JP6793014B2 (en) Wastewater treatment method and wastewater treatment equipment
JP2007061718A (en) Composite flocculant
JP6935924B2 (en) Wastewater and sludge treatment system containing high concentration of suspended solids
CN103951114A (en) Heavy metal wastewater tertiary treatment and deep purification recycling process
CN104496139A (en) Pretreatment method of heavy metal sludge
US3226319A (en) Process of consolidating a voluminous, low solids content sludge
JP2011101830A (en) Water treatment agent and water treatment method
JP6060320B1 (en) System for recovering phosphorus in treated water and method for collecting phosphorus in treated water
CN110040880A (en) The processing method of desulfurization wastewater
JP4272122B2 (en) Coagulated water treatment method and apparatus
JP7275618B2 (en) Method for treating slurry containing heavy metals
CN112158896A (en) Efficient wet desulphurization wastewater treatment water purifying agent and application thereof
JP4723624B2 (en) Disposal of chlorine-containing fine powder waste
JP2001347104A (en) Powdery decontaminant and method of decontaminating clean water and waste water
JP2006000837A (en) Inorganic powdered water treatment coagulant and processing method for various sludge and polluted waste water
JP2019155216A (en) Water treatment method and water treatment equipment
JP7117101B2 (en) Water treatment method and device
JP2010253424A (en) Muddy water purification system
JP2001129309A (en) Powder type flocculating and precipitating agent
JP6197095B1 (en) Method for recovering phosphorus in treated water
JP2007061749A (en) Method for treating cement-containing waste liquid
JP5154898B2 (en) Flocculant
AU2016277790B2 (en) Water softening treatment using in-situ ballasted flocculation system
JPH0732000A (en) Low concentration sludge slurry flock-settling agent, inorganic flocculant, organic high polymer flocculant and surplus soil making method of sludge

Legal Events

Date Code Title Description
A621 Written request for application examination

Free format text: JAPANESE INTERMEDIATE CODE: A621

Effective date: 20211203

A977 Report on retrieval

Free format text: JAPANESE INTERMEDIATE CODE: A971007

Effective date: 20220930

A131 Notification of reasons for refusal

Free format text: JAPANESE INTERMEDIATE CODE: A131

Effective date: 20221004

A521 Request for written amendment filed

Free format text: JAPANESE INTERMEDIATE CODE: A523

Effective date: 20221124

A131 Notification of reasons for refusal

Free format text: JAPANESE INTERMEDIATE CODE: A131

Effective date: 20230117

A521 Request for written amendment filed

Free format text: JAPANESE INTERMEDIATE CODE: A523

Effective date: 20230316

TRDD Decision of grant or rejection written
A01 Written decision to grant a patent or to grant a registration (utility model)

Free format text: JAPANESE INTERMEDIATE CODE: A01

Effective date: 20230404

A61 First payment of annual fees (during grant procedure)

Free format text: JAPANESE INTERMEDIATE CODE: A61

Effective date: 20230417

R150 Certificate of patent or registration of utility model

Ref document number: 7275618

Country of ref document: JP

Free format text: JAPANESE INTERMEDIATE CODE: R150