CN1041532C - Lubricant for metal wiredrawing and its preparation - Google Patents

Lubricant for metal wiredrawing and its preparation Download PDF

Info

Publication number
CN1041532C
CN1041532C CN 92102823 CN92102823A CN1041532C CN 1041532 C CN1041532 C CN 1041532C CN 92102823 CN92102823 CN 92102823 CN 92102823 A CN92102823 A CN 92102823A CN 1041532 C CN1041532 C CN 1041532C
Authority
CN
China
Prior art keywords
lubricant
oxidic polyethylene
blending emulsifiers
water
acid
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.)
Expired - Fee Related
Application number
CN 92102823
Other languages
Chinese (zh)
Other versions
CN1065288A (en
Inventor
余宪虎
芮斌
鲍筠
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.)
CHEMICAL INDUSTRY DESIGN INST HUBEI PROV
Original Assignee
CHEMICAL INDUSTRY DESIGN INST HUBEI PROV
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 CHEMICAL INDUSTRY DESIGN INST HUBEI PROV filed Critical CHEMICAL INDUSTRY DESIGN INST HUBEI PROV
Priority to CN 92102823 priority Critical patent/CN1041532C/en
Publication of CN1065288A publication Critical patent/CN1065288A/en
Application granted granted Critical
Publication of CN1041532C publication Critical patent/CN1041532C/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

Links

Landscapes

  • Lubricants (AREA)
  • Metal Extraction Processes (AREA)

Abstract

The present invention relates to a metallic drawing lubricant and a preparation method thereof. The lubricant does not contain mineral oil but containing water, oxidic polyethylene and emulsifiers whose HLB acid is not smaller than 8, or is a composition that is matched with additives, such as extreme pressure antiwear agents, chelating agents, mildew inhibitors, auxiliary emulsifiers, metallic antirust agents antiseptics, etc. In the preparation method of the composition, oxidic polyethylene is matched with other additives after being dispersed in water by way of dispersion, and the concentrates of a high water base lubricant are prepared. The solid content of the concentrates is from 20 to 40%, the oxidic polyethylene accounts for 18 to 80% in the solid content. When the solid content is diluted with water to be from 0.5 to 10%, the concentrates are used for drawing metals on tungsten carbide dies at a speed of 700 to 900 meters per minute. Therefore, the metallic drawing lubricant is especially suitable for drawing brass-plated steel wires at high speed.

Description

Lubricant for metal wiredrawing and compound method thereof
The present invention relates to the oxidic polyethylene is the water base lubricant technology of major ingredient, and what particularly relate to metal forming processing usefulness is the water-based mixture lubricant and the compound method thereof of major ingredient with the oxidic polyethylene.
As everyone knows, the lubricant that is used for metal wire-drawing in field of metallurgy is to serve as basic lubricated constituent with fatty acid soaps, vegetable and animals oils, mineral oil, and such lubricant lubricity is poor, can not adapt to the lubricated requirement of high-speed wire-drawing.
Soviet Union SU1122686 has introduced a kind of lubricant that is used for metal wire-drawing, is the oil lubricant that contains oxidic polyethylene, and its weight percent composition is:
Oxidic polyethylene 0.5-1.0
Mineral oil 3.6-7.1
Monoethanolamine C 10-16Synthetic
Aliphatic acid polyethenoxy ether 0.1-0.15
Trolamine 0.1-0.15
Sodium sulfonate 0.8-1.6
Water surplus
Obviously, this lubricant is the lubricant that contains mineral oil, and its mineral oil content is 70.5% of total solid content, and oxidic polyethylene content is 10% of total solid content.This lubricant can make metal wire-drawing speed 2 times for the drawing speed when lubricated with common fats acid soap class, but its wortle be artificial diamond and natural diamond mould under working concentration 10% condition, this mould involves great expense, and can make the production cost increase.In addition, this lubricant product concentration only is 5-10%, and working concentration causes the packed and transported expense higher up to 10% like this, and the wire drawing production cost is increased.
China is used for steel wire stringy mould and is all the carbon tungsten alloy mould, uses this mould with common fats acid soap series lubricant agent lubrication wiredrawing, and drawing speed can only reach 300 meters/minute, can not satisfy drawing speed far away) 700 meters/minute requirement.
The present invention's purpose is a kind of excellent property of preparation, can satisfies and use the wc die drawing speed) lubricant concentrate of 700 meters/minute requirements, solid content is higher in this enriched material, working concentration can be lower, thereby reduce the Transport Package expense, reduces the wire drawing production cost.
In order to realize goal of the invention, develop a kind of oil-water emulsion lubricant enriched material, its ground mass percentage composition is:
As better
Oxidic polyethylene 5-20 8-15
The emulsifying agent 5-22.5 7.5-15 of HLB value 〉=8
Other additives 0-15 0-15
The water surplus surplus
Above-mentioned enriched material added promptly form a kind of fuel-water emulsion in the entry.Be applied to metal drawing lubricating, solid content 0.5%-10% in using lubricating fluid, preferably 1-3%, i.e. water-content 90-99.5%, preferably 97-99%.
The oxidic polyethylene that uses in the lubricant of the present invention, molecular weight ranges 500-10000, is by high-pressure polyethylene or low pressure polyethylene at acid number scope 10-60mgKOH/g, or its corresponding by product catalyzed oxidation and getting, can buy in market, also can make by oneself.The consumption of oxidic polyethylene is the 18-80% of solid content total amount in the enriched material in this lubricant concentrate, and the best is 33-50%.
The emulsifying agent that uses in the lubricant of the present invention can be ionic, non-ionic type or theirs is compound.Used a kind of blending emulsifiers among the present invention, wherein ionic emulsifying agent is RA rosin acid and C 10-18The mixture of acid soap, its weight ratio is RA rosin acid: C 10-18Acid soap=2.2~3.5: 1 is more preferred from 2.5~3.0: 1, and nonionic emulsifier is by C 10-18The derivative of fatty acid alcohol acid amides and OP-10 is formed, its weight ratio is C 10-16The fatty acid alcohol acid amides: OP-10 derivative=1: 2~8.5, be more preferred from 1: 3~5.The mixed emulsion weight ratio of using among the present invention is the ionic blending emulsifiers: non-ionic type blending emulsifiers=1: 1.5~3.5, be more preferred from 1: 1.8~and 3.5.Blending emulsifiers weight is 5-22.5% in this lubricant concentrate, is more preferred from 7.5-15%.
Other additives have abrasion resistant extreme-pressure additive, sequestrant, mould inhibitor, assistant for emulsifying agent in this lubricant concentrate, also need add metal antirusting agent, sanitas sometimes, and indicator, defoamer, also add a little other compounds in order to increase solid content.
Described abrasion resistant extreme-pressure additive be the phosphoric acid ester of alkyl or/and phosphorous acid ester, thiophosphatephosphorothioate, thiophosphatephosphorothioate molybdate.Its alkyl can be C 10-18Straight chained alkyl, C 10-18Band branched-chain alkyl or aralkyl also can be C 7-18Alkyl alcohol polyoxyethylene 4-125 ether, C 7-10Alkylphenol-polyethenoxy 4-15 ether, C 7-18Alkyl acid polyoxyethylene 4-25 ether etc.
The sequestrant of selecting for use is one or more a mixture in the sodium salt of HEDP, ATMP, EDTA, morpholine, nitrilotriacetic acid and above-claimed cpd or the amine salt.
The mould inhibitor of selecting for use is formaldehyde derivatives or salicylic acid and derivative thereof, Sodium Benzoate.
The assistant for emulsifying agent of selecting for use is Macrogol 200-600 or glycol ether, ethanol, trolamine.
When processing iron and iron alloy thereof, need add ferrous metal rust-preventive agent, select phosphoric acid salt for use, phosphite, metaphosphate, silicate, nitrate, nitrite, molybdate, borate, benzoate, C 5-10Alkylphosphonic, C 5-10Alkyl borate, C 2-10Alkanol phosphoric acid salt, C 3-10One or more mixture in the alkanol borate.
When worked copper and Cu alloy material, need add the copper and copper alloy sanitas in this lubricant concentrate, as benzotriazole and derivative thereof, methyl benzotriazazole, nitro benzotriazole, mercaptobenzothiazole, mercaptobenzimidazole, and one or more mixture in the sodium salt of these compounds, sylvite, amine salt.
Indicator can be selected for use in tropeolin-D, phenolphthalein, thymol blue, murexide, the malachite green a kind of as required.
In preparation or application process, if stir to impact severely, foam then need add defoamer for a long time, as the silicone emulsion, or the multistage segmented copolymer of ethylene oxide-propylene oxide, or is no more than the low-viscosity (mobile) liquid paraffin wax of enriched material content 5%.
When increasing solid content, can add sulfuration grease, fatty acid ester, C 10-18Lipid acid C 2-9Alkyl alcohol amine salt, C 10-18One or more mixture in the amine or derivatives thereof.
Above-mentioned all additives total consumption in lubricant concentrate of the present invention is the 0-15% of its total amount, and this needs to select to use according to user's requirement.
The lubricant difference that lubricant of the present invention and SU1122686 describe is that this lubricant is a kind of high-water base lubricant.Do not contain mineral oil in the solid content, the lubricant concentrate solid content is 20-40%, and the oxidic polyethylene amount accounts for the 18-80% of solid content, can be applicable to metal high speed drawing on wc die, is specially adapted to the brass-plated steel wire high speed drawing.Also can be used for processing and lubrication such as rolling metal, rolling, ironing.
The lubricant solid content that SU1122686 describes is 5-10% only, and the solid content mineral oil in fluid accounts for 70%, and this lubricant is adapted to diamond mould, incompatibility wc die high-speed wire-drawing.
This lubricant concentrate is compared with the lubricant that SU1122686 describes, and its advantage is that solid content improves 2-8 doubly, can minimize transport costs, and working concentration reduces 3-5 doubly, thereby can reduce the wire drawing production cost, can adapt to the wire drawing of carbon tungsten alloy mold high speed.Compare with common fats acid soap series lubricant agent, can make and draw (pulling out) silk speed to improve 2.5-3 doubly.
The method for preparing this lubricant concentrate be will metering oxidic polyethylene and zero amount to the blending emulsifiers of metering mixes after, be warmed up to 80-160 ℃, be preferably 90-140 ℃, under continuous stirring.Once or gradation add the blending emulsifiers of zero remaining amount to metering, after adding, once or gradation add 90-100 ℃ water of metering.Be cooled to promptly get below 40 ℃ product then.Also can be as required with after aforementioned other additives meterings once or gradation undertaken by top preparation manipulation again after joining the oxidic polyethylene mixture, perhaps treat oxidic polyethylene and emulsifying agent, water mix reaction well, be cooled to below 40 ℃ after, the abrasion resistant extreme-pressure additive, sequestrant, mould inhibitor, assistant for emulsifying agent, the rust-preventive agent that add metering more as required, the compounds of sanitas, indicator, defoamer and other increase solid contents etc. stir and promptly get needed product.
Further specifying this lubricant below in conjunction with example forms and compound method:
Embodiment 1-9 according to the preparation method of aforementioned lubricants enriched material, adopts L 9(4 3) the orthogonal experiment prescription, result such as table 1.
Table 1 quadrature prescription and analytical results
Example number Essentially consist Press 1: 14 dilution back test-results with tap water
Oxidic polyethylene wt Blending emulsifiers wt Thanomin wt Water wt Outward appearance PH value Surface tension (dynes per centimeter) Frictional coefficient u
1 7.5 7.5 1.0 84 Translucent 7.0 29.69 0.0573
2 10.5 7.5 1.5 80.5 Translucent 7.7 29.21 0.0573
3 15 7.5 2.0 75.5 Translucent 8.0 29.69 0.0602
4 7.5 15 1.5 76 Translucent 7.7 28.73 0.0520
5 0.5 5 2.0 72.5 Translucent 7.7 28.73 0.0505
6 15 15 1.0 69 Milky white 7.0 29.69 0.0405
7 7.5 22.5 2.0 68 Translucent 7.7 29.69 0.0749
8 10.5 22.5 1.0 66 Translucent 7.0 28.73 0.0500
9 15 22.5 1.5 61 Milky white 7.2 28.73 0.0487
Annotate: 1, pH value is checked with the 6.4-8.0 special pH test paper,
2, surface tension is compiled " physico-chemical test " (People's Press's publication) maximum bubble determining by Fudan University.
3, frictional coefficient is tested by the SY2685-82 method with MHK-500 ring block abrasion tester, is provided by the Wuhan Institute of Technology tribology research.
4, blending emulsifiers is formed
A, ionic blending emulsifiers weight: non-ionic type blending emulsifiers weight=1: 2.75
B, ionic blending emulsifiers are formed RA rosin acid weight: C 10-18Acid soap weight=3: 1
C, non-ionic type blending emulsifiers are formed C 10-16Ester fat acid alcohol acid amides weight: OP-10 derivative weight=this lubricant was the lubricating system of a kind of low surface tension, low-friction coefficient by experimental example 1-9 as can be seen in 1: 4.5.Best group by quadrature analysis, this lubricant becomes:
Composition weight percent %
Oxidic polyethylene 8-15
Blending emulsifiers 7.5-15
Thanomin 12
Water surplus
Embodiment 10: this lubricant system and other additive compounds, make a kind of brass-plating steel wire wire drawing lubricant enriched material that is used for, and its composition is:
The composition weight percent
Oxidic polyethylene 10
Blending emulsifiers 13.5
Trolamine phosphoric acid salt (extreme pressure agent, rust-preventive agent) 2.5
Sulfonation grease (anti-wear agent) 4
Benzotriazole (sanitas, sequestrant) 0.5
Water surplus
This constituent is used for the brass-plated steel wire high speed drawing, and its application result is as follows:
Drawing wire rod: high pressure copper facing braided steel wire
Inlet wire diameter: 1.35mm
Finished silk diameter: 0.3 ± 0.01mm
Core rod material: carbon tungsten alloy
Project Lubricant of the present invention Fatty acid soaps class (commercially available)
Working concentration % 1.5~3 3~4
Drawing speed rice/minute 600 720 900 300
The drawing situation Normally Normally Normally Generally
Die life (hour) ≥10 ≥10 ≥10 <5
Lubricant consumes kilogram/ton silk ~3 36
Be several compound method examples below.
Embodiment 11, with the oxidic polyethylene of metering once or gradation with after the blending emulsifiers of metering mixes, be warmed up to 80-160 ℃, be preferably 90-140 ℃, under constantly stirring, add 90-100 ℃ water of metering, be cooled to then below 40 ℃, promptly get lubricant concentrate of the present invention.
Embodiment 12, the oxidic polyethylene of metering with after 1/3 blending emulsifiers of metering mixes, is warming up to 80-160 ℃, is preferably 90-140 ℃, under constantly stirring, add remaining blending emulsifiers, and make it mixing, continue to stir 1-30 minute preferably 2-15 minute, 90-100 ℃ the water that adds metering then, and be cooled to below 40 ℃, promptly making lubricant concentrate of the present invention, this method product is very stable.
Embodiment 13, with the oxidic polyethylene of metering with after 1/5~2/5 blending emulsifiers of metering mixes, be warming up to 80-160 ℃, be preferably 90-140 ℃, under constantly stirring, add 1/5~2/5 blending emulsifiers of metering again and make it mixing, continue to stir 1-30 minute, preferably 2-15 minute, add 90-100 ℃ water of metering then, and be cooled to below 40 ℃, add remaining blending emulsifiers again, promptly make this lubricant concentrate.
Embodiment 14, this law is roughly with the method for embodiment 11-13, just with twice adding of moisture of measuring, promptly earlier the 15-30% of 90-100 ℃ of water of metering is joined in 90-140 ℃ the mixture, make its temperature reduce to 90-98 ℃, 90-98 ℃ mixture is joined in the water of remaining 70-85% then, and make it to be cooled to below 40 ℃, promptly make lubricant concentrate of the present invention.
Embodiment 15, and this method is to join in the mixture of oxidic polyethylene after other additive meterings, to operate by arbitrary method steps among the embodiment 11-14 and produce lubricant concentrate.
Embodiment 16, other additives metering rear sections are joined in the mixture of oxidic polyethylene, operate by implementing among the 11-14 arbitrary method steps again, treat that material is cooled to below 40 ℃ after, add other remaining additives, produce the lubricant concentrate product.
Embodiment 17, earlier get material by any method among the embodiment 11-14, operations such as mixing, treat that it is cooled to below 40 ℃ after, add other additives, stir, promptly get the lubricant concentrate product that needs.

Claims (8)

1, a kind of lubricant that is used for metal drawing is characterized in that it is blending emulsifiers and other additive of moisture, oxidic polyethylene, ionic and non-ionic type blended LHR 〉=8, and the weight percent of said composition is formed and is:
Oxidic polyethylene 7.5-15
Blending emulsifiers 7.5-22.5
Water surplus
Other additive 1-7
2, the lubricant that is used for metal drawing according to claim 1 is characterized in that weight percent consists of oxidic polyethylene 7.5-15, blending emulsifiers 7.5-15, and other additive 1-7, surplus is a water.
3, the lubricant that is used for metal drawing according to claim 1 is characterized in that other additives have the assistant for emulsifying agent thanomin, and its addition is the 1-2% of lubricant concentrate weight.
4, the lubricant that is used for metal drawing according to claim 1 is characterized in that the weight % of other additives in lubricant concentrate is extreme pressure agent, rust-preventive agent trolamine phosphoric acid salt 2.5%, anti-wear agent sulfonation grease 4%, sanitas sequestrant benzotriazole 0.5%.
5, the lubricant that is used for metal drawing according to claim 1 and 2 is characterized in that oxidic polyethylene is that molecular weight is 500-10000, and acid number is the oxidic polyethylene of 10-60mg KOH/g.
6, the lubricant that is used for metal drawing according to claim 1 is characterized in that blending emulsifiers is RA rosin acid and C 10-18Acid soap blended ionic emulsifying agent and C 10-16The derivative of fatty acid alcohol acid amides and OP-10 is formed the non-ionic type blending emulsifiers, and its ratio of components is:
Ionic mixture RA rosin acid: C 10-18Acid soap=3: 1
The non-ionic type mixture C 10-16The derivative of fatty acid alcohol acid amides: OP-10=1: 2.0-8.5 ionic blending emulsifiers: non-ionic type blending emulsifiers=1: 2.7.
7, prepare metal drawing method with lubricator, after it is characterized in that measuring oxidic polyethylene and the blending emulsifiers of 1/5-1 metering mixing, be warmed up to 80-160 ℃, under constantly stirring, once or gradation add the remaining blending emulsifiers of metering, after adding, once or gradation add 90-100 ℃ water of metering, be cooled to below 40 ℃.The additive that adds other meterings stirs and promptly gets product.
8, according to the described metal drawing of claim 7 method with lubricator, after it is characterized in that measuring oxidic polyethylene and the blending emulsifiers of 1/5-1 metering mixing, be warmed up to 90-140 ℃, under constantly stirring, once or gradation add remaining blending emulsifiers, then once or gradation add 90-100 ℃ water of metering, be cooled to 40 ℃, add other additives.
CN 92102823 1992-04-16 1992-04-16 Lubricant for metal wiredrawing and its preparation Expired - Fee Related CN1041532C (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN 92102823 CN1041532C (en) 1992-04-16 1992-04-16 Lubricant for metal wiredrawing and its preparation

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN 92102823 CN1041532C (en) 1992-04-16 1992-04-16 Lubricant for metal wiredrawing and its preparation

Publications (2)

Publication Number Publication Date
CN1065288A CN1065288A (en) 1992-10-14
CN1041532C true CN1041532C (en) 1999-01-06

Family

ID=4939868

Family Applications (1)

Application Number Title Priority Date Filing Date
CN 92102823 Expired - Fee Related CN1041532C (en) 1992-04-16 1992-04-16 Lubricant for metal wiredrawing and its preparation

Country Status (1)

Country Link
CN (1) CN1041532C (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101892117A (en) * 2010-07-30 2010-11-24 湖北恒鑫化工有限公司 Water-based lubricant for drawing processing of brass-plated steel wire and preparation method thereof

Families Citing this family (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1088100C (en) * 1999-09-29 2002-07-24 中国石油化工集团公司 Water-series wax-base lubricant and its preparing process
CN101993770B (en) * 2010-11-18 2013-08-21 江南大学 Lubricating agent for high-speed wire drawing and preparation method thereof
CN103436888B (en) * 2013-08-23 2015-07-01 南京理工大学 High temperature copper corrosion inhibitor containing benzimidazole and preparation method of high temperature copper corrosion inhibitor
CN103952690B (en) * 2014-03-23 2018-03-09 汕头市联达包装材料有限公司 A kind of water-soluble powder metal antirust agent composition
CN105925344B (en) * 2016-04-29 2019-10-11 湖北洪乐电缆股份有限公司 A kind of oil for drawing copper wire additive
CN111534361A (en) * 2020-04-23 2020-08-14 梧州市同润铜业有限公司 Copper micro-drawing oil
CN112023452B (en) * 2020-08-19 2022-02-11 肇庆领誉环保实业有限公司 Defoaming agent for domestic sewage treatment and preparation method thereof
CN114874835A (en) * 2022-06-01 2022-08-09 武汉工商学院 Water-based lubricant for high-speed drawing of galvanized filaments and preparation method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101892117A (en) * 2010-07-30 2010-11-24 湖北恒鑫化工有限公司 Water-based lubricant for drawing processing of brass-plated steel wire and preparation method thereof
CN101892117B (en) * 2010-07-30 2013-04-03 湖北恒鑫化工有限公司 Water-based lubricant for drawing processing of brass-plated steel wire and preparation method thereof

Also Published As

Publication number Publication date
CN1065288A (en) 1992-10-14

Similar Documents

Publication Publication Date Title
CN102220183B (en) Vegetable oil-based water-soluble cutting fluid
CN101613634B (en) High-property water-based emulsion cutting fluid composite
WO2018032853A1 (en) Micro-emulsion cutting fluid and preparation process therefor
CN101191099B (en) Total synthesis water-base cutting fluid for sintering neodymium-iron-boron and preparation method thereof
CN106318586A (en) Multifunctional semi-synthetic metal processing liquid and preparation method thereof
CN102585986B (en) Water-soluble grinding fluid
CN1041532C (en) Lubricant for metal wiredrawing and its preparation
CN104164283A (en) Microemulsion metal cutting fluid
CN108034485A (en) A kind of semi-synthetic cutting fluid of low-phosphorous no chlorine non-formaldehyde aluminium alloy machining
JP5224251B2 (en) Lubricant composition for aqueous plastic processing of metallic materials
CN102295975B (en) Water-soluble cutting oil and preparation method thereof
CN104450120A (en) Semi-synthetic metal wire drawing lubricant liquid and preparation method thereof
CN1730634A (en) Extreme pressure cutting fuild microemulsion free of chlorine and its preparation method and uses
CN102559351B (en) Automobile radial tire steel cord wet-pulling lubricating agent
CN105524688A (en) Extreme pressure cutting oil used for achieving performance stability in metal processing and preparation method thereof
CN106164040A (en) The high-performance water dilution type oiliness additive applied for polymetallic intermetallic composite coating
CN104073321A (en) Microemulsion cutting fluid, cutting diluent and preparation and application methods of microemulsion cutting fluid
CN104073328A (en) Microemulsion cutting fluid, cutting diluent and preparation and application methods of microemulsion cutting fluid
CN106675698A (en) Metal cutting fluid and preparation method thereof
CN104403769A (en) Multifunctional cutting fluid and preparation method thereof
JPS6112791A (en) Grease containing solid lubricant
CN103555392A (en) Ionic liquid-containing micro-emulsified metal cutting fluid, and preparation method and application thereof
CN107353995A (en) A kind of environment-friendly type fully synthetic cutting fluid and preparation method thereof
CN101948711B (en) Water-soluble cutting fluid and preparation method thereof
WO2006128119A2 (en) Emulsions and products thereof

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant
C19 Lapse of patent right due to non-payment of the annual fee
CF01 Termination of patent right due to non-payment of annual fee