JP6610913B2 - Mixed grease - Google Patents
Mixed grease Download PDFInfo
- Publication number
- JP6610913B2 JP6610913B2 JP2018533992A JP2018533992A JP6610913B2 JP 6610913 B2 JP6610913 B2 JP 6610913B2 JP 2018533992 A JP2018533992 A JP 2018533992A JP 2018533992 A JP2018533992 A JP 2018533992A JP 6610913 B2 JP6610913 B2 JP 6610913B2
- Authority
- JP
- Japan
- Prior art keywords
- polyurea
- lithium
- occupies
- service life
- accounts
- 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
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
- C10M169/06—Mixtures of thickeners and additives
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Chemistry (AREA)
- Lubricants (AREA)
Description
本発明はグリースの技術分野に属し、具体的には、混合グリースに関する。 The present invention belongs to the technical field of grease, and specifically relates to a mixed grease.
近年、グリース技術の持続的な発展に伴い、リチウムグリースは繊維構造が柔らかくて、長さが制御可能であることから、低ノイズ分野に幅広く適用されており、特別な処理をしたリチウムグリースを密封軸受内に適用すると、軸受の振動を短時間で安定した値にすることができ、優れた低ノイズ性能を有する。しかし、工業技術の発展に伴い、軸受の作動条件への要求が高まり、たとえば、低ノイズ、耐高温、長耐用年数、高回転数、低トルク等が求められている。リチウムグリースは、150℃以上で長時間する場合に制限があり、ポリウレアグリースは150℃以上で使用可能であるが、低ノイズ性能が悪く、両方の利点を組み合わせた新規な混合グリースの研究には注目が集められている。 In recent years, along with the continuous development of grease technology, lithium grease has been widely applied in low noise fields because its fiber structure is soft and its length is controllable, and specially treated lithium grease is sealed When applied in a bearing, the vibration of the bearing can be stabilized in a short time, and has excellent low noise performance. However, with the development of industrial technology, demands for operating conditions of bearings are increasing, and for example, low noise, high temperature resistance, long service life, high rotation speed, low torque, etc. are required. Lithium grease has limitations when it is used at 150 ° C or higher for a long time, and polyurea grease can be used at 150 ° C or higher, but low noise performance is poor, and research on new mixed grease combining both advantages Attention has been gathered.
本発明の目的は、耐用年数が長く、低ノイズ性能に優れて、150℃以上でも使用可能であり、応用の将来性が期待できる混合グリースを提供することである。 An object of the present invention is to provide a mixed grease that has a long service life, is excellent in low noise performance, can be used at 150 ° C. or higher, and can be expected to have a future application.
上記目的を達成させるために、本発明は下記技術案を用いる。 In order to achieve the above object, the present invention uses the following technical solution.
混合グリースであって、リチウム石鹸とポリウレアの重量比率が7〜9:1〜3の増ちょう剤が10〜15wt.%を占める。 A mixed grease, wherein a thickener having a weight ratio of lithium soap to polyurea of 7 to 9: 1 to 3 is 10 to 15 wt. %.
さらに、基油70〜90wt%と添加剤0〜10wt.%を含む。 Furthermore, 70-90 wt% of base oil and 0-10 wt. %including.
前記リチウム石鹸は、ステアリン酸リチウム石鹸、12−ヒドロキシステアリン酸リチウム石鹸のうちの1種又は2種である。 The lithium soap is one or two of lithium stearate soap and 12-hydroxy lithium stearate soap.
前記ポリウレアは、脂肪族ポリウレア、脂環族ポリウレア、芳香族ポリウレアのうちの1種であり、前記ポリウレアはジウレア、ポリウレアのうちの1種又は複数種である。 The polyurea is one of aliphatic polyurea, alicyclic polyurea, and aromatic polyurea, and the polyurea is one or more of diurea and polyurea.
前記脂肪族ポリウレアは、C8アミン〜C22アミンのうちの1種とジフェニルメタン−4,4´−ジイソシアネート又はトリレンジイソシアネートとを反応させて得るものであり、前記脂環族ポリウレアは、シクロヘキシルアミンとMDI又はTDIとを反応させて得るものであり、前記芳香族ポリウレアはp−トルイジンとMDI又はTDIとを反応させて得るものである。 The aliphatic polyurea is obtained by reacting one of C8 amine to C22 amine with diphenylmethane-4,4′-diisocyanate or tolylene diisocyanate, and the alicyclic polyurea includes cyclohexylamine and MDI. Alternatively, the aromatic polyurea is obtained by reacting p-toluidine with MDI or TDI.
前記基油は鉱物油、エステル系油、合成炭化水素油、エーテル系油のうちの1種又は複数種である。 The base oil is one or more of mineral oil, ester oil, synthetic hydrocarbon oil, and ether oil.
前記添加剤は酸化防止剤、防錆剤及び耐摩耗剤である。 The additives are antioxidants, rust inhibitors and antiwear agents.
前記防錆剤は、石油スルホン酸カルシウム、石油スルホン酸バリウム、スパン80のうちの1種又は複数種である。 The rust preventive is one or more of petroleum calcium sulfonate, petroleum barium sulfonate, and span 80.
前記酸化防止剤は、オクチル/ブチルジフェニルアミン、ジイソオクチルジフェニルアミン、フェノールエステル、アルキルフェニルアミンのうちの1種又は複数種である。 The antioxidant is one or more of octyl / butyldiphenylamine, diisooctyldiphenylamine, phenol ester, and alkylphenylamine.
前記耐摩耗剤は、ジアルキルジチオリン酸亜鉛と、ジアルキルジチオカルバミン酸モリブデンのうちの1種又は複数種である。 The antiwear agent is one or more of zinc dialkyldithiophosphate and molybdenum dialkyldithiocarbamate.
本発明の顕著な利点は以下のとおりである。該混合グリースは、耐用年数が長く、低ノイズ性能に優れて、150℃以上でも使用可能であり、応用の将来性が期待できる。 The significant advantages of the present invention are as follows. The mixed grease has a long service life, is excellent in low noise performance, can be used at 150 ° C. or higher, and is expected to have a future application.
混合グリースであって、リチウム石鹸とポリウレアの重量比率が7〜9:1〜3の増ちょう剤が10〜15wt.%を占める。 A mixed grease, wherein a thickener having a weight ratio of lithium soap to polyurea of 7 to 9: 1 to 3 is 10 to 15 wt. %.
さらに、基油70〜90wt%と添加剤0〜10wt.%を含む。 Furthermore, 70-90 wt% of base oil and 0-10 wt. %including.
前記リチウム石鹸は、ステアリン酸リチウム石鹸、12−ヒドロキシステアリン酸リチウム石鹸のうちの1種又は2種である。 The lithium soap is one or two of lithium stearate soap and 12-hydroxy lithium stearate soap.
前記ポリウレアは、脂肪族ポリウレア、脂環族ポリウレア、芳香族ポリウレアのうちの1種であり、前記ポリウレアはジウレア、ポリウレアのうちの1種又は複数種である。 The polyurea is one of aliphatic polyurea, alicyclic polyurea, and aromatic polyurea, and the polyurea is one or more of diurea and polyurea.
前記脂肪族ポリウレアは、C8アミン〜C22アミンのうちの1種とジフェニルメタン−4,4´−ジイソシアネート又はトリレンジイソシアネートとを反応させて得るものであり、前記脂環族ポリウレアは、シクロヘキシルアミンとMDI又はTDIとを反応させて得るものであり、前記芳香族ポリウレアはp−トルイジンとMDI又はTDIとを反応させて得るものである。 The aliphatic polyurea is obtained by reacting one of C8 amine to C22 amine with diphenylmethane-4,4′-diisocyanate or tolylene diisocyanate, and the alicyclic polyurea includes cyclohexylamine and MDI. Alternatively, the aromatic polyurea is obtained by reacting p-toluidine with MDI or TDI.
前記基油は鉱物油、エステル系油、合成炭化水素油、エーテル系油のうちの1種又は複数種である。 The base oil is one or more of mineral oil, ester oil, synthetic hydrocarbon oil, and ether oil.
前記添加剤は酸化防止剤、防錆剤及び耐摩耗剤である。 The additives are antioxidants, rust inhibitors and antiwear agents.
前記防錆剤は、石油スルホン酸カルシウム、石油スルホン酸バリウム、スパン80のうちの1種又は複数種である。 The rust preventive is one or more of petroleum calcium sulfonate, petroleum barium sulfonate, and span 80.
前記酸化防止剤は、オクチル/ブチルジフェニルアミン、ジイソオクチルジフェニルアミン、フェノールエステル、アルキルフェニルアミンのうちの1種又は複数種である。 The antioxidant is one or more of octyl / butyldiphenylamine, diisooctyldiphenylamine, phenol ester, and alkylphenylamine.
前記耐摩耗剤は、ジアルキルジチオリン酸亜鉛と、ジアルキルジチオカルバミン酸モリブデンのうちの1種又は複数種である。 The antiwear agent is one or more of zinc dialkyldithiophosphate and molybdenum dialkyldithiocarbamate.
製造プロセス
1、リチウムクリーズの製造
Manufacturing process 1. Lithium crease manufacturing
1.1反応原理:
C17H35COOH+LiOH
→C17H35COOLi+H2O
CH3(CH2)5CH(OH)(CH2)10COOH+LiOH
→CH3(CH2)5CH(OH)(CH2)10COOLi+H2O
1.1 Reaction principle:
C 17 H 35 COOH + LiOH
→ C 17 H 35 COOLi + H 2 O
CH 3 (CH 2) 5 CH (OH) (CH 2) 10 COOH + LiOH
→ CH 3 (CH 2 ) 5 CH (OH) (CH 2 ) 10 COOLi + H 2 O
1.2、プロセス
予め製造されたブリチウム石鹸粉末と基油を正確に秤量して、混合して溶解釜に投入し、加熱してリチウム石鹸粉末が完全に溶解する。すなわち約220℃の温度にあるまで昇温し、室温に高速冷却させて、三本ロールミルで粉砕し、必要に応じて添加剤を加え、均一に撹拌して、濾過と脱気を行った。
1.2, Process Pre-manufactured britium soap powder and base oil are accurately weighed, mixed, put into a melting pot, and heated to completely dissolve the lithium soap powder. That is, the temperature was raised to about 220 ° C., rapidly cooled to room temperature, pulverized with a three-roll mill, added with additives as needed, and stirred uniformly to perform filtration and deaeration.
2、ポリウレアの製造
2.1反応原理
2RNH2+MDI
→R−NH−CO−NH−(C6H4)−CH2−(C6H4)−NH−CO−NH−R
2. Production of polyurea 2.1 Reaction principle 2RNH 2 + MDI
→ R—NH—CO—NH— (C 6 H 4 ) —CH 2 — (C 6 H 4 ) —NH—CO—NH—R
2.2プロセス
イソシアネートとアミンをそれぞれ基油に溶解して、80〜100℃で反応させ、反応終了後、150〜160℃に昇温した。
80℃に冷却させて、さらに室温に冷却させ、粉砕して、必要に応じて添加剤を加え、均一に撹拌して、濾過、脱気を行った。
2.2 Process Each of isocyanate and amine was dissolved in a base oil and reacted at 80 to 100 ° C. After the reaction was completed, the temperature was raised to 150 to 160 ° C.
The mixture was cooled to 80 ° C., further cooled to room temperature, pulverized, added with additives as necessary, stirred uniformly, filtered and deaerated.
3、混合クリーズの製造
リチウムクリーズとポリウレアを所定の割合で秤量して、室温条件において三本ロールミルで均一に混合し、最後に濾過、脱気を行った。
3. Production of mixed crease Lithium crease and polyurea were weighed at a predetermined ratio, and uniformly mixed with a three-roll mill at room temperature, and finally filtered and degassed.
評価
1、低ノイズ性能のテスト
1.1テスト条件
BVT−1A軸受振動試験機、6201軸受、クリーズ注入量0.45g、荷重40N、回転数1800min−1。
Evaluation 1. Low noise performance test 1.1 Test conditions BVT-1A bearing vibration tester, 6201 bearing, crease injection amount 0.45 g, load 40 N, rotation speed 1800 min −1 .
1.2テスト過程
各軸受について正面と裏面をテストし、一面ごとに3点テストした。
1.2 Test process The front and back surfaces of each bearing were tested, and three points were tested for each surface.
1.3テスト結果
テスト結果として、中間周波数値と高周波数値の平均値を取る。
1.3 Test result The average value of the intermediate frequency value and the high frequency value is taken as the test result.
2、グリースの耐用年数のテスト
2.1テスト条件
ASTMD 3336参照、6204−2ZZ軸受、クリーズ注入量1.45g。アキシャル荷重22N、ラジアル荷重67N、回転数10000min−1。
2. Grease life test 2.1 Test conditions See ASTM D 3336, 6204-2ZZ bearing, crease injection amount 1.45g. Axial load 22N, radial load 67N, rotation speed 10000 min −1 .
2.2テスト過程
温度150℃、165℃条件において、テストを行った。
テスト結果は表1、2に示される。
2.2 Test process The test was performed under conditions of temperatures of 150 ° C and 165 ° C.
The test results are shown in Tables 1 and 2.
注:
低ノイズ性能:◎6〜8μm/s、○6〜9μm/s、×6〜10μm/s、××6〜14μm/s
150℃での耐用年数:◎耐用年数1500h超、○耐用年数1000h超、△耐用年数600h−800h、×耐用年数500h未満。
165℃での耐用年数:◎耐用年数1000h超、○耐用年数700h超、×耐用年数500h未満。
note:
Low noise performance: ◎ 6-8 μm / s, ○ 6-9 μm / s, x6-10 μm / s, xx6-14 μm / s
Service life at 150 ° C .: ◎ service life more than 1500h, ○ service life more than 1000h, △ service life 600h-800h, x service life less than 500h.
Service life at 165 ° C .: ◎ service life more than 1000h, ○ service life more than 700h, x service life less than 500h.
注:
低ノイズ性能:◎6〜8μm/s、○6〜9μm/s、×6〜10μm/s、××6〜14μm/s
150℃での耐用年数:◎耐用年数1500h超、○耐用年数1000h超、△耐用年数600h−800h、×耐用年数500h未満。
165℃での耐用年数:◎耐用年数1000h超、○耐用年数700h超、×耐用年数500h未満。
note:
Low noise performance: ◎ 6-8 μm / s, ○ 6-9 μm / s, x6-10 μm / s, xx6-14 μm / s
Service life at 150 ° C .: ◎ service life more than 1500h, ○ service life more than 1000h, △ service life 600h-800h, x service life less than 500h.
Service life at 165 ° C .: ◎ service life more than 1000h, ○ service life more than 700h, x service life less than 500h.
以上は本発明の好適実施例に過ぎず、本発明の出願特許範囲を逸脱することなく行う同等変化や修飾はいずれも本発明の保護範囲に属する。 The above are only preferred embodiments of the present invention, and any equivalent changes and modifications made without departing from the scope of the patent application for the present invention belong to the protection scope of the present invention.
Claims (4)
ことを特徴とする混合グリース。 A thickener with a weight ratio of lithium soap to polyurea of 7.5: 2.5 occupies 13 wt.% ; Further includes 82 wt.% Base oil and 5 wt.% Additive; Lithium lithium stearate soap; lithium stearate soap accounts for 7.8 wt.%; 12-hydroxy lithium stearate soap accounts for 1.95 wt.%; Said polyurea is an aliphatic polyaliphatic and an alicyclic polyurea; Aliphatic polyurea occupies 1.63 wt.% And alicyclic polyurea occupies 1.62 wt.%; The polyurea is one or more of diurea and polyurea; the base oil is an ester oil Yes; the additive is an antioxidant, an antirust agent and an antiwear agent, the antioxidant accounts for 1.5 wt.%, The antirust agent accounts for 2.5 wt.%, And the antiwear agent characterized in that occupies 1 wt.% If grease.
請求項1に記載の混合グリース。 The rust inhibitor is one or more of calcium calcium sulfonate, barium petroleum sulfonate, and span 80.
The mixed grease according to claim 1 .
請求項1に記載の混合グリース。 The antioxidant is one or more of octyl / butyldiphenylamine, diisooctyldiphenylamine, phenol ester, and alkylphenylamine.
The mixed grease according to claim 1 .
請求項1に記載の混合グリース。 The antiwear agent is one or more of zinc dialkyldithiophosphate and molybdenum dialkyldithiocarbamate.
The mixed grease according to claim 1 .
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201510604753.8 | 2015-09-22 | ||
CN201510604753.8A CN105112143B (en) | 2015-09-22 | 2015-09-22 | A kind of mixed grease |
PCT/CN2016/098415 WO2017050135A1 (en) | 2015-09-22 | 2016-09-08 | Mixed lubricating grease |
Publications (2)
Publication Number | Publication Date |
---|---|
JP2018527452A JP2018527452A (en) | 2018-09-20 |
JP6610913B2 true JP6610913B2 (en) | 2019-11-27 |
Family
ID=54660264
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP2018533992A Active JP6610913B2 (en) | 2015-09-22 | 2016-09-08 | Mixed grease |
Country Status (3)
Country | Link |
---|---|
JP (1) | JP6610913B2 (en) |
CN (1) | CN105112143B (en) |
WO (1) | WO2017050135A1 (en) |
Families Citing this family (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105112143B (en) * | 2015-09-22 | 2018-04-17 | 福建优立盛油脂有限公司 | A kind of mixed grease |
CN106497660A (en) * | 2016-10-05 | 2017-03-15 | 中国石油化工股份有限公司 | A kind of polyureas slaine composite bearing lubricant composition and preparation method |
CN106590846A (en) * | 2016-12-13 | 2017-04-26 | 天津箭牌石油化工有限公司 | Industrial robot joint speed reducer lubricating grease and preparation method thereof |
CN106854486A (en) * | 2016-12-14 | 2017-06-16 | 钦州学院 | A kind of functional urea-based lubricating grease and preparation method thereof |
CN107338095B (en) * | 2017-06-23 | 2020-08-07 | 辽宁海华科技股份有限公司 | Low-noise lubricating grease and preparation method thereof |
CN112080328B (en) * | 2020-08-13 | 2022-06-21 | 长沙众城石油化工有限责任公司 | Organic lithium soap composite carbamido lubricating grease and preparation method thereof |
CN115651736A (en) * | 2022-10-24 | 2023-01-31 | 东莞市欧迪斯润滑剂科技有限公司 | Composite soap-based lubricating grease for high-temperature demolding and preparation process thereof |
CN115786018B (en) * | 2022-12-28 | 2024-01-26 | 洛阳精一新材料科技有限公司 | Lubricating grease for harmonic reducer and preparation method thereof |
Family Cites Families (11)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS62209199A (en) * | 1986-02-05 | 1987-09-14 | Nippon Kokan Kk <Nkk> | Lubricant composition for hot rolling of steel |
JP2002265970A (en) * | 2001-03-14 | 2002-09-18 | Koyo Seiko Co Ltd | Grease composition and rolling bearing lubricated with the grease composition |
JP3982364B2 (en) * | 2002-08-28 | 2007-09-26 | 日本精工株式会社 | Grease composition and rolling device |
JP2004083798A (en) * | 2002-08-28 | 2004-03-18 | Nsk Ltd | Grease composition and rolling apparatus |
JP2004250481A (en) * | 2003-02-18 | 2004-09-09 | Nsk Ltd | Lubricating grease composition for reduction gear and electric power steering apparatus |
CN1253524C (en) * | 2003-09-05 | 2006-04-26 | 中国科学院兰州化学物理研究所 | Composite gelatinizer for liquid seal agent and its preparation method |
CN101177645B (en) * | 2006-11-10 | 2011-07-20 | 协同油脂株式会社 | Lubricating grease as well as bearing and gear using the same |
JP2009046625A (en) * | 2007-08-22 | 2009-03-05 | Cosmo Sekiyu Lubricants Kk | Grease composition |
CN101353606B (en) * | 2007-09-11 | 2011-04-20 | 威海旺润来润滑科技有限公司 | Complex grease additive |
JP2011001398A (en) * | 2009-06-16 | 2011-01-06 | Toyota Motor Corp | Grease composition |
CN105112143B (en) * | 2015-09-22 | 2018-04-17 | 福建优立盛油脂有限公司 | A kind of mixed grease |
-
2015
- 2015-09-22 CN CN201510604753.8A patent/CN105112143B/en active Active
-
2016
- 2016-09-08 JP JP2018533992A patent/JP6610913B2/en active Active
- 2016-09-08 WO PCT/CN2016/098415 patent/WO2017050135A1/en active Application Filing
Also Published As
Publication number | Publication date |
---|---|
WO2017050135A1 (en) | 2017-03-30 |
CN105112143B (en) | 2018-04-17 |
JP2018527452A (en) | 2018-09-20 |
CN105112143A (en) | 2015-12-02 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
JP6610913B2 (en) | Mixed grease | |
JP5496087B2 (en) | Grease composition | |
JP5943479B2 (en) | Grease composition | |
CN103254976B (en) | A kind of Grease composition and method of making the same | |
JP6448801B2 (en) | High temperature lubricant | |
CN107406793B (en) | Grease composition | |
JP2013035882A (en) | Grease composition | |
JP2016089040A (en) | Biodegradable grease composition for wind power generator | |
JP2017036385A (en) | Grease composition and grease encapsulated rolling shaft bearing | |
WO2012115141A1 (en) | Grease composition | |
JP2012229334A (en) | Grease and rolling bearing | |
JP5087989B2 (en) | Lubricant composition, method for producing the same, and rolling bearing | |
JP2020204016A (en) | Grease composition and rolling bearing | |
JP6534816B2 (en) | Rolling bearing | |
JP2009209180A (en) | Grease composition and method for producing the same | |
DE112018004265T5 (en) | LUBRICATING GREASE COMPOSITION | |
JP5765806B2 (en) | Grease composition | |
JP2013253257A (en) | Grease composition and bearing | |
JP2014228059A (en) | Rolling bearing | |
WO2018025981A1 (en) | Grease composition | |
JP6919848B2 (en) | Grease composition | |
JP6480785B2 (en) | Grease composition | |
JP2008285574A (en) | Roller bearing | |
JP2014108997A (en) | Grease composition and rolling bearing | |
JP2015021566A (en) | Rolling bearing |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
A621 | Written request for application examination |
Free format text: JAPANESE INTERMEDIATE CODE: A621 Effective date: 20180320 |
|
A977 | Report on retrieval |
Free format text: JAPANESE INTERMEDIATE CODE: A971007 Effective date: 20181212 |
|
A131 | Notification of reasons for refusal |
Free format text: JAPANESE INTERMEDIATE CODE: A131 Effective date: 20190122 |
|
A521 | Request for written amendment filed |
Free format text: JAPANESE INTERMEDIATE CODE: A523 Effective date: 20190422 |
|
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: 20190917 |
|
A521 | Request for written amendment filed |
Free format text: JAPANESE INTERMEDIATE CODE: A523 Effective date: 20190930 |
|
A711 | Notification of change in applicant |
Free format text: JAPANESE INTERMEDIATE CODE: A711 Effective date: 20190930 |
|
A521 | Request for written amendment filed |
Free format text: JAPANESE INTERMEDIATE CODE: A821 Effective date: 20191001 |
|
A61 | First payment of annual fees (during grant procedure) |
Free format text: JAPANESE INTERMEDIATE CODE: A61 Effective date: 20191015 |
|
R150 | Certificate of patent or registration of utility model |
Ref document number: 6610913 Country of ref document: JP Free format text: JAPANESE INTERMEDIATE CODE: R150 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |