CN1069694C - Aqueous cleaning agent composite - Google Patents

Aqueous cleaning agent composite Download PDF

Info

Publication number
CN1069694C
CN1069694C CN98110031A CN98110031A CN1069694C CN 1069694 C CN1069694 C CN 1069694C CN 98110031 A CN98110031 A CN 98110031A CN 98110031 A CN98110031 A CN 98110031A CN 1069694 C CN1069694 C CN 1069694C
Authority
CN
China
Prior art keywords
cleaning agent
cleaning
ether
composition according
agent composition
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
CN98110031A
Other languages
Chinese (zh)
Other versions
CN1188795A (en
Inventor
李玉香
于新好
马洪磊
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.)
Shandong University
Original Assignee
Shandong University
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 Shandong University filed Critical Shandong University
Priority to CN98110031A priority Critical patent/CN1069694C/en
Publication of CN1188795A publication Critical patent/CN1188795A/en
Application granted granted Critical
Publication of CN1069694C publication Critical patent/CN1069694C/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

Links

Landscapes

  • Detergent Compositions (AREA)

Abstract

本发明涉及一种电子工业用清洗剂。其组成为:5-10%脂肪醇聚氧乙烯醚硫酸钠,10-20%壬基酚聚氧乙烯醚,10-15%椰子油酰二乙醇胺或烷基醇酰胺磷酸酯,1-10%乙二醇烷基醚,5-10%直链或支链低级脂肪醇,0.1-0.2%络合剂,1-4%聚醚及余量去离子水。本发明的清洗剂能代替氟里昂清洗剂,无毒无腐蚀性,不污染环境,不破坏高空臭氧层,不引起温室效应,并可降低清洗成本。The invention relates to a cleaning agent for electronic industry. Its composition is: 5-10% fatty alcohol polyoxyethylene ether sodium sulfate, 10-20% nonylphenol polyoxyethylene ether, 10-15% coconut oil diethanolamine or alkyl alcohol amide phosphate, 1-10% Ethylene glycol alkyl ether, 5-10% straight chain or branched lower fatty alcohol, 0.1-0.2% complexing agent, 1-4% polyether and the balance deionized water. The cleaning agent of the invention can replace Freon cleaning agent, is non-toxic and non-corrosive, does not pollute the environment, does not destroy the high-altitude ozone layer, does not cause greenhouse effect, and can reduce cleaning cost.

Description

A kind of aqueous cleaning agent composite
The present invention relates to the cleansing composition and the purging method of semi-conductor or metal, liquid crystal cleaning usefulness, be specifically related to the used in electronic industry aqueous cleaning agent.
Hard disc of computer parts such as hard disk drive suspension mechanism and disk drive element HGA, matrix all is stainless material, in the course of processing, various impurity can be stain in its surface, and the liquid dirt is arranged, as the lubricating oil that uses in the processing; The solid dirt is also arranged,, in transmission course, also can stain finger mark simultaneously as dust, abrasive material, metal oxide and carbon deposit etc.These dirts generally all are to be adsorbed on the metallic surface by electrostatic attraction and Van der Waals force.For the liquid dirt, generally be on the metallic surface, to adhere to into the thin even or uneven oil lamella of one deck, and the solid dirt, typically refer to the very little discrete particles of three-dimensional space, they are rare on more uniform and bigger region surface in the adhesion of metallic surface, and often only contact and adhere to the surface on some less points.Because dirt difference, its scavenging mechanism are also different, generally are that the solid dirt is removed than liquid dirt difficulty.
Fluorine Lyons (being CFC) is the fluorochlorohydrocarbon kind solvent, because it is good that it has chemical stability, toxicity is little, do not burn, and surface tension is less, does not damage to be cleaned material and can to keep many advantageous characteristic such as strong perviousness, rapid-drying properties, is widely used as the refrigeration agent of air-cooling system, refrigerator etc. so far, the propellant of atomizer, the clean-out system of the whipping agent of lagging materials such as urethane foam and film, audiotape, electrical equipment, electronic component, precision optical machinery etc.But the ozonosphere in these material havoc earth high-altitudes, the harm humans ecotope, so fluorine Lyons 11, fluorine Lyons 12, fluorine Lyons 113, fluorine Lyons 114, fluorine Lyons 115 and the mixture that contains them all are the materials of time limit production in the world and use.In recent years, also developed some short-term surrogates, as Hydrochlorofluorocarbons (HCFC), perfluoroparaffin (PFC) and other halogenated solvents etc.HCFC is that the part halogen atom in fluorine Lyons is replaced by hydrogen atom, makes the ozone-depleting of CFC value (ODP value) reduction of diving, but it still can damage the ozone layer, and also will be eliminated to the year two thousand twenty, is no more than the year two thousand forty the latest.Some organic solvent also can be used as the surrogate of CFC, but cleaning performance is good not as the CFC cleaning performance, and flash-point is low, inflammable, explosive, and some is also toxic simultaneously, and operating environment is had relatively high expectations.Therefore people's expectation develop can substitute CFC high performance non-halogen be clean-out system, but do not have such clean-out system openly to report up to now as yet with excellent cleaning performance.
The objective of the invention is to overcome the shortcoming of prior art, a kind of nontoxic non-corrosiveness is provided, the cleaning hard disc of computer parts of readily biodegradable or the aqueous cleaning agent composite of liquid crystal.
Cleansing composition of the present invention basic composition is:
Weight percentages (%)
A. polyoxyethylenated alcohol sodium sulfate 5-10
B. polyoxyethylene nonylphenol ether 10-20
C. coconut oleoyl diethanolamine or 10-15
The alkylol amide phosphoric acid ester
D. ethylene glycol alkyl oxide 1-10
E. straight or branched alkyl alcohol 5-10
F. contain nitronic acid or hydroxycarboxylic acid complexing agent 0.1-0.2
G. polyethers GP 1-4
H. deionized water surplus
The complexing agent F that the present invention uses is organic chelate and agent, as ethylenediamine tetraacetic acid (EDTA) (EDTA) and sodium salt, Trisodium Citrate etc.
Described ethylene glycol alkyl oxide D can be an alkyl oxide, also can be dialkyl ether, can be ethyl, propyl group or butyl ether.
Straight or branched alkyl alcohol E of the present invention is side chain or straight chain low-grade alkane alcohol, as the mixing of ethanol, propyl alcohol, Virahol, butanols or its arbitrary proportion.
Described polyethers GP is a colourless transparent liquid, and molecular-weight average is 1000-2000.
The anti-soil dirt that 0.5-1.5% also can be arranged in the above-mentioned cleansing composition is deposition agent I again, and as Xylo-Mucine (CMC), polyvinyl alcohol or polyvinylpyrrolidone (PVP), the dirt under preventing to come off is again attached on the surface that cleans up.
In all raw materials, polyoxyethylenated alcohol sodium sulfate and polyoxyethylene nonylphenol ether are colourless to light yellow transparent liquid, coconut oleoyl diethanolamine or alkylol amide phosphoric acid ester are the reddish-brown transparent liquid, these tensio-active agents are water-soluble fully, do not fire, not quick-fried, readily biodegradable is the main component of clean-out system.The complexing agent that the present invention uses is organic chelate and agent, as ethylenediamine tetraacetic acid (EDTA) (EDTA) and sodium salt thereof, Trisodium Citrate, is white particle or Powdered, except can chelating Ca 2+, Mg 2+Outward, can also chelating Fe 3+, Cu 2+Etc. many other metal ions, thereby prevent the consumption of tensio-active agent, also overcome the overfertilization phenomenon of using the deterioration water quality that the phosphoric acid salt inorganic assistant agent causes simultaneously, environment is not produced pollution.Described ethylene glycol alkyl oxide can be an alkyl oxide, also can be dialkyl ether, can be ethyl, propyl group or butyl ether, is colourless transparent liquid, and dirts such as mineral oil, grease are had stronger dissolving power.Alkyl alcohol is generally side chain or straight chain low-grade alkane alcohol, as ethanol, propyl alcohol, Virahol, butanols etc., is colourless transparent liquid, can dissolve dirt, also can regulate the viscosity of clean-out system.Described polyethers GP is a colourless transparent liquid, molecular-weight average is 1000-2000, the froth breaking effect is arranged, too many as foam in the clean-out system, often bring difficulty to rinsing, waste time and energy and waste a large amount of water, therefore adding some nonionogenic tensides such as polyethers has the effect of the foamy of inhibition, makes that being cleaned parts is easy to flushing.
With above-mentioned raw materials heating for dissolving under 40-60 ℃ of temperature, add above-mentioned each component one by one, make its whole dissolvings, can obtain the light yellow liquid of homogeneous transparent, can be mixed with arbitrary proportion with water, and nontoxic, non-corrosiveness, free from environmental pollution, its key technical indexes is:
Outward appearance and yellow homogeneous transparent liquid of light color
PH value 9.5-11.5 (25 ℃)
Viscosity 10-50 centipoise (25 ℃)
Proportion 1.02-1.05
Surface-active substance content is greater than 30%
-10~+ 50 ℃ of stability are stable
Harmful metal ion content is less than 1ppm
The cleansing composition of preparation can substitute CFC be a clean-out system according to the present invention, and following advantage is arranged:
1, to be cleaned the substance dissolves of removing good to various, and clean range is wide;
2, safe owing to be aqua, do not fire not quick-fried, euosmia invariably;
3, use and can directly discharge, easy to use;
4, not phosphorous and halogen is free from environmental pollution, does not destroy the high-altitude ozonosphere;
5, because usage ratio is less, therefore can reduce cost;
6, cleaning performance reaches the CFC cleaning performance, and has no adverse effect to being cleaned thing.
When being applied to clean the hard disc of computer parts surface, can remove pollutents such as its lip-deep grease, dust, carbon deposit, when omitting liquid crystal outside when being applied to clean packaged liquid crystal display, can easier clean up, effect is suitable when cleaning with CFC-113.
When cleaning the hard disc of computer parts with this cleansing composition, said composition and the deionized water of available 5-10% are mixed with scavenging solution, soak or ultrasonic cleaning in the time of 40-60 ℃, rinse well with deionized water then to get final product.
The invention will be further described below in conjunction with embodiment.
100 kilograms of embodiment 1. clean-out systems
Weight percentages (%)
A. polyoxyethylenated alcohol sodium sulfate AES is 6 kilogram 6
(produce in Xi'an, light yellow transparent liquid)
B. polyoxyethylene nonylphenol ether TX-10 is 12 kilogram 12
(synthetic chemistry factory in Beijing produces, colourless transparent liquid)
C. coconut oleoyl diethanolamine is 6,501 15 kilogram 15
(synthetic chemistry factory in Beijing produces, the reddish-brown transparent liquid)
D. ethylene glycol monobutyl ether (analytical pure) is 2 kilogram 2
E. Virahol (analytical pure) is 5 kilogram 5
F. ethylenediamine tetraacetic acid (EDTA) (analytical pure) is 0.15 kilogram 0.15
G. polyethers GP (molecular weight 1400) is 2 kilogram 2
H. deionized water is 57.35 kilogram 57.35
I. Xylo-Mucine (CMC) is 0.5 kilogram 0.5
Above-mentioned clean-out system outward appearance is light yellow homogeneous transparent liquid, and proportion is 1.03, and viscosity is 27 centipoises, and pH value is that 10.46. cleans with Ultrasonic Cleaners, effectively pollutents such as the lip-deep grease of removing component, dust, carbon deposit.
Embodiment 2. is as described in the embodiment 1, and different is that component C is an alkylol amide phosphoric acid ester 6503, and component E is 95% ethanol, and I is a polyvinyl alcohol.
Embodiment 3. is as described in the embodiment 1, and different is that component F is a Trisodium Citrate, and component D is a glycol ethyl ether, and I is polyvinylpyrrolidone (PVP).
When using cleansing composition of the present invention to clean computer hard disc driver suspension mechanism parts,
Cleaning performance is compared with the CFC clean-out system, and the result is as follows:
Clean-out system cleans number of packages and cleans preceding workpiece surface situation cleaning back workpiece surface situation qualification rate
Embodiment 1 280 has 11 adularescent spots 96.1% of a large amount of grit greasy dirts
CFC113 163 has 9 of a large amount of grit greasy dirts that yellow spotting 94.5% is arranged
100 kilograms of embodiment 4. clean-out systems
Weight percentages (%)
A. polyoxyethylenated alcohol sodium sulfate AES is 5 kilogram 5
(produce in Xi'an, light yellow transparent liquid)
B. polyoxyethylene nonylphenol ether TX-10 is 15 kilogram 15
(synthetic chemistry factory in Beijing produces, colourless transparent liquid)
C. the alkylol amide phosphoric acid ester is 6,503 15 kilogram 15
(is produced from detergent factory, Beijing, the reddish-brown transparent liquid)
D. ethylene glycol monobutyl ether (analytical pure) is 1.5 kilogram 1.5
E.95% ethanol (analytical pure) is 5 kilogram 5
F. ethylenediamine tetraacetic acid (EDTA) (analytical pure) is 0.2 kilogram 0.2
G. polyethers GP (molecular weight 1400) is 1.5 kilogram 1.5
H. deionized water is 55.8 kilogram 55.8
I. polyvinylpyrrolidone (PVP) is 1 kilogram 1
Above-mentioned raw materials is dissolved at 50-70 ℃ of temperature range internal heating, stir,, also obtain yellow homogeneous transparent liquid through static froth breaking, precipitating extraction, press filtration, sterilization, concentrated.
Embodiment 5. is as described in the embodiment 4, and different is that component E is a propyl carbinol.
Embodiment 6. is as described in the embodiment 4, and different is that component F is EDTA2Na, and component E is Virahol and the 95% ethanol mixture with arbitrary proportion.
When using cleansing composition of the present invention to clean disk drive element HGA, cleaning performance compared with the prior art, the result is as follows:
The clean-out system cleaning temperature (℃) scavenging period (S) cleaning rate (%)
CFC-113 45-50 285 85
Embodiment 4 40-45 285 85
More than be good with embodiment 1 and embodiment 4.

Claims (6)

1、一种水剂清洗剂组合物,其特征在于,基本组成为:1. An aqueous cleaning composition, characterized in that the basic composition is:          组份                   重量百分比(%)Components Weight Percentage (%) A.脂肪醇聚氧乙烯醚硫酸钠            5-10A. Sodium fatty alcohol polyoxyethylene ether sulfate 5-10 B.壬基酚聚氧乙烯醚                 10-20B. Nonylphenol polyoxyethylene ether 10-20 C.椰子油酰二乙醇胺或               10-15C. Coconut Oleoyl Diethanolamine or 10-15    烷基醇酰胺磷酸酯Alkyl alcohol amidophosphate D.乙二醇烷基醚                      1-10D. Ethylene glycol alkyl ether 1-10 E.直链或支链低级烷基醇              5-10E. Straight chain or branched lower alkyl alcohol 5-10 F.含氮羧酸或羟基羧酸络合剂        0.1-0.2F. Nitrogen-containing carboxylic acid or hydroxycarboxylic acid complexing agent 0.1-0.2 G.聚醚GP,平均分子量为1000-2000     1-4G. Polyether GP, the average molecular weight is 1000-2000 1-4 H.去离子水                          余量。H. Deionized water The balance. 2、如权利要求1所述的清洗剂组合物,其特征在于,所述的络合剂选自乙二胺四乙酸(EDTA)及其钠盐、柠檬酸钠。2. The cleaning agent composition according to claim 1, wherein the complexing agent is selected from ethylenediaminetetraacetic acid (EDTA) and its sodium salt, and sodium citrate. 3、如权利要求1所述的清洗剂组合物,其特征在于,所述的乙二醇烷基醚D可以是一烷基醚,也可以是二烷基醚,可以是乙基、丙基或丁基醚。3. The cleaning agent composition according to claim 1, characterized in that, said ethylene glycol alkyl ether D can be monoalkyl ether or dialkyl ether, can be ethyl, propyl or butyl ether. 4、如权利要求1所述的清洗剂组合物,其特征在于,所述的直链或支链低级烷基醇选自乙醇、丙醇、异丙醇、丁醇。4. The cleaning agent composition according to claim 1, characterized in that, said straight chain or branched lower alkyl alcohol is selected from ethanol, propanol, isopropanol and butanol. 5、如权利要求1所述的清洗剂组合物,其特征在于,所述清洗剂组合物中还可有0.5-1.5%的抗污垢再沉积剂I,选自羧甲基纤维素钠(CMC)、聚乙烯醇或聚乙烯吡咯烷酮(PVP)。5. The cleaning agent composition according to claim 1, characterized in that, 0.5-1.5% of the anti-dirt redeposition agent I is selected from the group consisting of sodium carboxymethylcellulose (CMC) in the cleaning agent composition. ), polyvinyl alcohol or polyvinylpyrrolidone (PVP). 6、一种清洗计算机硬盘部件表面上的油脂、灰尘、积炭等污染物的方法,包括使用权利要求1所述的清洗剂组合物,用超声波清洗机清洗,然后用去离子水冲洗,热风或真空干燥即可。6. A method for cleaning grease, dust, carbon deposits and other pollutants on the surface of computer hard disk components, comprising using the cleaning agent composition according to claim 1, cleaning with an ultrasonic cleaner, then rinsing with deionized water, hot air Or vacuum dry.
CN98110031A 1998-01-20 1998-01-20 Aqueous cleaning agent composite Expired - Fee Related CN1069694C (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN98110031A CN1069694C (en) 1998-01-20 1998-01-20 Aqueous cleaning agent composite

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN98110031A CN1069694C (en) 1998-01-20 1998-01-20 Aqueous cleaning agent composite

Publications (2)

Publication Number Publication Date
CN1188795A CN1188795A (en) 1998-07-29
CN1069694C true CN1069694C (en) 2001-08-15

Family

ID=5220124

Family Applications (1)

Application Number Title Priority Date Filing Date
CN98110031A Expired - Fee Related CN1069694C (en) 1998-01-20 1998-01-20 Aqueous cleaning agent composite

Country Status (1)

Country Link
CN (1) CN1069694C (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101503804B (en) * 2008-12-15 2010-12-08 中国石油化工股份有限公司 Cleaning liquid composition and use thereof

Families Citing this family (19)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1080757C (en) * 1999-05-31 2002-03-13 江苏同大气雾剂股份有限公司 Detergent for mobile telephone
CN100393862C (en) * 2002-04-18 2008-06-11 狮王株式会社 Aqueous liquid detergent composition for liquid crystal panel
CN100351361C (en) * 2004-06-23 2007-11-28 比亚迪股份有限公司 Water-based liquid-crystal cleaning agent
CN100350030C (en) * 2005-09-15 2007-11-21 山东大学 Semi-water base detergent specially for liquid crystal and its prepn process
CN1995305B (en) * 2005-12-26 2010-06-23 比亚迪股份有限公司 Water-soluble liquid crystal cleaning agent composition and its preparing method
CN101434890B (en) * 2007-11-16 2011-03-02 比亚迪股份有限公司 Water-soluble washing agent composition
CN101463295B (en) * 2008-11-28 2011-08-17 江苏海迅实业集团股份有限公司 Cleaning agent for semiconductor industry
CN101985583B (en) * 2010-11-29 2013-01-23 陕西永泰生物工程有限责任公司 Oil fume detergent composition and preparation method thereof
CN102363739A (en) * 2010-12-14 2012-02-29 深圳车仆汽车用品发展有限公司 Carbon deposit scavenging agent for combustion chamber and spark plug, and preparation method of the same
CN103525577A (en) * 2013-10-30 2014-01-22 合肥市华美光电科技有限公司 Antirust antibacterial circuit board cleaning agent and preparation method thereof
CN104212658B (en) * 2014-09-03 2018-01-23 盐城交大能源有限公司 A kind of electrified cleaning agent of electric equipment and preparation method thereof
CN104293504A (en) * 2014-09-24 2015-01-21 中国海洋石油总公司 Descaling cleaning agent for poly-containing dirt on polymer flooding produced liquid treatment equipment
CN104774697A (en) * 2015-04-28 2015-07-15 苏州永创达电子有限公司 Liquid crystal cleaning agent
CN104804881A (en) * 2015-05-20 2015-07-29 龚灿锋 Cleaning liquid for display screen of computer
CN105002005A (en) * 2015-06-29 2015-10-28 广东月福汽车用品有限公司 Ultrasonic automobile carbon removal cleaning agent and preparation method thereof
CN106148978B (en) * 2016-07-03 2018-06-12 广州恒荣电子科技有限公司 A kind of preparation method of the aqueous metal cleaning agent of biomass
CN106701343B (en) * 2016-12-08 2019-08-09 深圳市合明科技有限公司 Neutral water-based cleaning agent, preparation method thereof, and semiconductor package cleaning method
CN106967520A (en) * 2017-02-24 2017-07-21 玉林博飞商贸有限公司 A kind of glass for vehicle window cleaning agent and preparation method thereof
CN109576067A (en) * 2018-12-14 2019-04-05 北京金冠恒科技发展有限公司 A kind of high-efficiency heavy oil dirt cleaning agent and preparation method thereof and heavy oil dirt cleaning method

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1111675A (en) * 1994-03-23 1995-11-15 安卫公司 Concentrated all-purpose light duty liquid cleaning composition and method of use
CN1114350A (en) * 1994-06-29 1996-01-03 首钢总公司 General-purpose hard surface detergent

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1111675A (en) * 1994-03-23 1995-11-15 安卫公司 Concentrated all-purpose light duty liquid cleaning composition and method of use
CN1114350A (en) * 1994-06-29 1996-01-03 首钢总公司 General-purpose hard surface detergent

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101503804B (en) * 2008-12-15 2010-12-08 中国石油化工股份有限公司 Cleaning liquid composition and use thereof

Also Published As

Publication number Publication date
CN1188795A (en) 1998-07-29

Similar Documents

Publication Publication Date Title
CN1069694C (en) Aqueous cleaning agent composite
CN1482223A (en) Glass cleaner composition for electronics industry
US5705472A (en) Neutral aqueous cleaning composition
CN106947979B (en) Magnesium-aluminum alloy cleaning agent
CN101684558A (en) Water-base cleaning agent composition for cleaning metal parts
CN108486587A (en) A kind of environmentally-friendly water-based metal cleaner and preparation method thereof
CN111705323A (en) Environment-friendly stainless steel cleaning agent and method for cleaning stainless steel parts
WO2007116669A1 (en) Cleaning composition
CN1316497A (en) Water-base composite detergent for metallic parts
JP2009511653A (en) Suctionable gel and its use for decontaminating surfaces
CN106567088A (en) Environmentally friendly industrial heavy oil cleaning agent
CN102296001B (en) Cleaning fluid for panel display and preparation method thereof
CN1162525C (en) A kind of water-based liquid crystal cleaning composition
CN1055721C (en) Detergent composition for hard surface
CN1162524C (en) A kind of water-based cleaning agent composition for printed circuit board
CN115058717A (en) Non-phosphorus neutral dedusting degreasing agent for metal coating pretreatment
CN114561252A (en) Low-residue efficient cleaning agent and preparation method thereof
CN1119456A (en) Method of manufacture of cleaning articles
KR101275549B1 (en) Inhibiting redeposition and low foaming aqueous cleaner composition
CN117821170A (en) A high-efficiency cleaning agent and preparation method thereof
CN109267074B (en) A metal parts cleaning agent
JP2015127382A (en) Remover for floor polish, and removal method of floor polish
JP4502474B2 (en) Cleaning composition for optical parts
CN120795997A (en) Glass cleaning agent with long-acting anti-fog function and preparation method thereof
TW202216976A (en) Cleaner for electronic device components

Legal Events

Date Code Title Description
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C06 Publication
PB01 Publication
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