CN1817795A - Production of aluminium hydrate from aluminium ash - Google Patents
Production of aluminium hydrate from aluminium ash Download PDFInfo
- Publication number
- CN1817795A CN1817795A CN 200610049387 CN200610049387A CN1817795A CN 1817795 A CN1817795 A CN 1817795A CN 200610049387 CN200610049387 CN 200610049387 CN 200610049387 A CN200610049387 A CN 200610049387A CN 1817795 A CN1817795 A CN 1817795A
- Authority
- CN
- China
- Prior art keywords
- aluminium
- sodium aluminate
- utilizing
- ash
- solid
- 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.)
- Granted
Links
Images
Abstract
Production of aluminum hydrate from aluminum ash is carried out by mixed agitating in proportion=100:80-120 of aluminum ash and solid sodium carbonate, melting solid mixture at 900-1500 degrees C for 1-5hrs, immersing melts in water above 10hrs, removing deposits to obtain sodium aluminate solution, adding sulfuric acid into sodium aluminate solution in proportion=2:0.9-1.1mol, solid-liquid separating by filter to obtain aluminum hydrate deposits and sodium sulfate solution, drying aluminum hydrate deposits at 20-80 degrees C and crushing to obtain final product. It is cheap and simple, has no environmental pollution and uses of regenerative resources fully.
Description
Technical field
The present invention relates to the preparation method of aluminium hydroxide, especially relate to a kind of method of utilizing the aluminium ash to prepare aluminium hydroxide.
Background technology
In the processing fusion process of aluminium, can produce partial oxidation and nitrogenize usually, generate aluminum oxide and aluminium nitride, these aluminum oxide and aluminium nitride and part metallic aluminium mix, and have just become the aluminium slag.For a long time, have many enterprises to utilize the aluminium slag to come processing regenerated aluminium, but the aluminium slag is through refining a great problem that remaining aluminium ash behind the secondary aluminum has but become to perplex for many years people.
The composition of aluminium ash is very complicated, based on aluminum oxide and aluminium nitride, a spot of metallic aluminium, iron, nickel, zinc, manganese, copper, silicon etc. are still arranged, pile up like a mountain everywhere for the aluminium ash that the processing regenerated aluminium industry of aluminium slag is produced, soil and ecotope have been caused very big pressure, can decomposite ammonia after aluminium nitride in the aluminium ash makes moist in air in addition, breath malodor is unpleasant and toxic, also can cause bigger pollution to atmosphere.Therefore, the problem of environmental pollution that caused of aluminium ash has restricted further developing of the processing regenerated aluminium industry of aluminium slag.
In fact, contain higher renewable resources in the aluminium ash, single with aluminum oxide calculating, alumina content reaches 60～80% approximately, if can be used, and turns waste into wealth, and not only has good economic benefit, and has good environment and ecological benefits.At present existing people attempts utilizing aluminium ash processing aluminium salt, and main method is to adopt hydrochloric acid to process aluminium chlorohydroxide.Because the aluminum oxide phase inversion becomes αYang Hualv under the high temperature, be insoluble to bronsted lowry acids and bases bronsted lowry, therefore this method has only been utilized a spot of metallic aluminium in the aluminium ash, and a large amount of aluminum oxide is not utilized well, not only cause the waste of resource, and employed hydrochloric acid also can cause secondary pollution to environment.
Summary of the invention
Technical problem to be solved by this invention provides a kind of method of utilizing the aluminium ash to prepare aluminium hydroxide, not only can effectively utilize aluminium ash preparation aluminium hydroxide, can also eliminate of the pollution of aluminium ash effectively, and avoid in the course of processing, environment being caused secondary pollution environment.
The present invention solves the problems of the technologies described above the technical scheme that is adopted: a kind of method of utilizing the aluminium ash to prepare aluminium hydroxide, and it may further comprise the steps: 1. the aluminium ash is mixed stirring with solid sodium carbonate by weight 100: 80～120; 2. with solid mixture fusion 1～5 hour under 900 ℃～1500 ℃ conditions; 3. melts is put into clear water and soaked more than 10 hours, remove remaining sodium aluminate solution behind the throw out; 4. sodium aluminate in molar ratio: sulfuric acid is 2: 0.9～1.1 to add sulfuric acid in sodium aluminate solution; 5. use strainer to carry out solid-liquid separation, obtain aluminum hydroxide precipitate and metabisulfite solution respectively; 6. aluminum hydroxide precipitate is promptly obtained the aluminium hydroxide finished product after dry under 20～80 ℃ the temperature and pulverizing.
1. add fusing assistant in step in, the aluminium ash is 100: 80～120: 10～20 with the weight ratio of solid sodium carbonate and fusing assistant; 2. with solid mixture fusion 1～5 hour under 900 ℃～1180 ℃ conditions.
Described fusing assistant can be a borax.
3. described step is melts to be cooled to put into water after the room temperature again and soak more than 10 hours, removes remaining sodium aluminate solution behind the throw out.
4. described step is sodium aluminate in molar ratio: sulfuric acid is 2: 0.9～1.1 to add sulfuric acid in sodium aluminate solution, and precipitation was carried out solid-liquid separation more than 2 hours.
Can obtain the industrial chemicals Sodium sulfate anhydrous.min(99) after the metabisulfite solution evaporation drying that 5. step is obtained.
Throw out behind the 3. middle extraction sodium aluminate solution of step is free of contamination red mud.
Compared with prior art, the invention has the advantages that the use solid phase method extracts the aluminium hydroxide in the aluminium ash, make aluminum oxide solid and the frit reaction at high temperature of yellow soda ash solid and generate sodium aluminate, the aqueous solution and sulfuric acid reaction with sodium aluminate generates aluminium hydroxide product and sodium sulfate byproduct then, not only method is simple, and with low cost, and the whole aluminium compositions in the aluminium ash all can be extracted, not only renewable resource can be utilized fully, and secondary pollution can not be produced; And remaining red mud composition is that iron, nickel, zinc, manganese, copper, silicon etc. are the natural composition in the soil, and back to nature can not cause any pollution to environment; The adding fusing assistant can reduce the melt temperature of aluminium ash and solid sodium carbonate; Be cooled to and put into water after the room temperature again and soak and to avoid forming immobilized particles and will add melts behind the fusing assistant; In sodium aluminate solution, add sulfuric acid and can make all resultant of reaction all obtain utilizing, thereby avoid remaining refuse that environment is caused secondary pollution.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Embodiment
Embodiment describes in further detail the present invention below in conjunction with accompanying drawing.
Embodiment one: a kind of method of utilizing the aluminium ash to prepare aluminium hydroxide, and it may further comprise the steps: 1. the aluminium ash is mixed to be incorporated in the stirrer by weight 100: 100 with solid sodium carbonate and stir; 2. solid mixture is put into High Temperature Furnaces Heating Apparatus fusion 3 hours under 1100 ℃ of conditions; 3. melts is put into the leaching groove and soaked 12 hours, remove remaining sodium aluminate solution behind the free of contamination red mud throw out with clear water; 4. sodium aluminate in molar ratio: sulfuric acid is sulfuric acid to be added in the sodium aluminate solution in the reactor in 2: 1; 5. use strainer that mixed solution is carried out solid-liquid separation, obtain aluminum hydroxide precipitate and metabisulfite solution respectively; 6. aluminum hydroxide precipitate is promptly obtained the aluminium hydroxide finished product after dry under 60 ℃ the temperature and pulverizing, and will can obtain the industrial chemicals Sodium sulfate anhydrous.min(99) after the metabisulfite solution evaporation drying.
Embodiment two: a kind of method of utilizing the aluminium ash to prepare aluminium hydroxide, and it may further comprise the steps: 1. the aluminium ash is mixed to be incorporated in the stirrer by weight 100: 80 with solid sodium carbonate and stir; 2. solid mixture is put into High Temperature Furnaces Heating Apparatus fusion 5 hours under 900 ℃ of conditions; 3. melts is put into the leaching groove and soaked 15 hours, remove remaining sodium aluminate solution behind the free of contamination red mud throw out with clear water; 4. sodium aluminate in molar ratio: sulfuric acid is sulfuric acid to be added in the sodium aluminate solution in the reactor in 2: 0.95; 5. use strainer that mixed solution is carried out solid-liquid separation, obtain aluminum hydroxide precipitate and metabisulfite solution respectively; 6. aluminum hydroxide precipitate is promptly obtained the aluminium hydroxide finished product after dry under 80 ℃ the temperature and pulverizing, and will can obtain the industrial chemicals Sodium sulfate anhydrous.min(99) after the metabisulfite solution evaporation drying.
Embodiment three: a kind of method of utilizing the aluminium ash to prepare aluminium hydroxide, and it may further comprise the steps: 1. the aluminium ash is mixed to be incorporated in the stirrer by weight 100: 120 with solid sodium carbonate and stir; 2. solid mixture is put into High Temperature Furnaces Heating Apparatus fusion 1 hour under 1500 ℃ of conditions; 3. melts is put into the leaching groove and soaked 10 hours, remove remaining sodium aluminate solution behind the free of contamination red mud throw out with clear water; 4. sodium aluminate in molar ratio: sulfuric acid is sulfuric acid to be added in the sodium aluminate solution in the reactor in 2: 1.05; 5. use strainer that mixed solution is carried out solid-liquid separation, obtain aluminum hydroxide precipitate and metabisulfite solution respectively; 6. aluminum hydroxide precipitate is promptly obtained the aluminium hydroxide finished product after dry under 40 ℃ the temperature and pulverizing, and will can obtain the industrial chemicals Sodium sulfate anhydrous.min(99) after the metabisulfite solution evaporation drying.
Embodiment four: a kind of method of utilizing the aluminium ash to prepare aluminium hydroxide, and it may further comprise the steps: 1. the aluminium ash is mixed to be incorporated in the stirrer by weight 100: 80: 10 with solid sodium carbonate and borax and stir; 2. solid mixture is put into High Temperature Furnaces Heating Apparatus fusion 4 hours under 900 ℃ of conditions; 3. melts is put into the leaching groove and soaked 13 hours, remove remaining sodium aluminate solution behind the free of contamination red mud throw out with clear water; 4. sodium aluminate in molar ratio: sulfuric acid is sulfuric acid to be added in the sodium aluminate solution in the reactor in 2: 0.9, precipitates 3 hours; 5. use strainer that mixed solution is carried out solid-liquid separation, obtain aluminum hydroxide precipitate and metabisulfite solution respectively; 6. aluminum hydroxide precipitate is promptly obtained the aluminium hydroxide finished product after dry under 20 ℃ the temperature and pulverizing, and will can obtain the industrial chemicals Sodium sulfate anhydrous.min(99) after the metabisulfite solution evaporation drying.
Embodiment five: a kind of method of utilizing the aluminium ash to prepare aluminium hydroxide, and it may further comprise the steps: 1. the aluminium ash is mixed to be incorporated in the stirrer by weight 100: 120: 20 with solid sodium carbonate and borax and stir; 2. solid mixture is put into High Temperature Furnaces Heating Apparatus fusion 1 hour under 1180 ℃ of conditions; 3. melts is put into the leaching groove and soaked 11 hours, remove remaining sodium aluminate solution behind the free of contamination red mud throw out with clear water; 4. sodium aluminate in molar ratio: sulfuric acid is sulfuric acid to be added in the sodium aluminate solution in the reactor in 2: 1.1, precipitates 2 hours; 5. use strainer that mixed solution is carried out solid-liquid separation, obtain aluminum hydroxide precipitate and metabisulfite solution respectively; 6. aluminum hydroxide precipitate is promptly obtained the aluminium hydroxide finished product after dry under 50 ℃ the temperature and pulverizing, and will can obtain the industrial chemicals Sodium sulfate anhydrous.min(99) after the metabisulfite solution evaporation drying.
Embodiment six: a kind of method of utilizing the aluminium ash to prepare aluminium hydroxide, and it may further comprise the steps: 1. the aluminium ash is mixed to be incorporated in the stirrer by weight 100: 105: 15 with solid sodium carbonate and borax and stir; 2. solid mixture is put into High Temperature Furnaces Heating Apparatus fusion 3 hours under 1000 ℃ of conditions; 3. melts is put into cement pit and soaked 14 hours, remove remaining sodium aluminate solution behind the free of contamination red mud throw out with clear water; 4. sodium aluminate in molar ratio: sulfuric acid is sulfuric acid to be added in the sodium aluminate solution in the reactor in 2: 1.02, precipitates 3 hours; 5. use strainer that mixed solution is carried out solid-liquid separation, obtain aluminum hydroxide precipitate and metabisulfite solution respectively; 6. aluminum hydroxide precipitate is promptly obtained the aluminium hydroxide finished product after dry under 70 ℃ the temperature and pulverizing, and will can obtain the industrial chemicals Sodium sulfate anhydrous.min(99) after the metabisulfite solution evaporation drying.
Embodiment seven: a kind of method of utilizing the aluminium ash to prepare aluminium hydroxide, and it may further comprise the steps: 1. the aluminium ash is mixed to be incorporated in the stirrer by weight 100: 105: 15 with solid sodium carbonate and borax and stir; 2. solid mixture is put into High Temperature Furnaces Heating Apparatus fusion 2 hours under 1100 ℃ of conditions; 3. melts is put into the leaching groove and soaked 16 hours, remove remaining sodium aluminate solution behind the free of contamination red mud throw out with clear water; 4. sodium aluminate in molar ratio: sulfuric acid is sulfuric acid to be added in the sodium aluminate solution in the reactor in 2: 1.02, precipitates 2 hours; 5. use strainer that mixed solution is carried out solid-liquid separation, obtain aluminum hydroxide precipitate and metabisulfite solution respectively; 6. aluminum hydroxide precipitate is promptly obtained the aluminium hydroxide finished product after dry under 30 ℃ the temperature and pulverizing, and will can obtain the industrial chemicals Sodium sulfate anhydrous.min(99) after the metabisulfite solution evaporation drying.
Claims (7)
1, a kind of method of utilizing the aluminium ash to prepare aluminium hydroxide is characterized in that it may further comprise the steps: 1. the aluminium ash is mixed stirring with solid sodium carbonate by weight 100: 80～120; 2. with solid mixture fusion 1～5 hour under 900 ℃～1500 ℃ conditions; 3. melts is put into clear water and soaked more than 10 hours, remove remaining sodium aluminate solution behind the throw out; 4. sodium aluminate in molar ratio: sulfuric acid is 2: 0.9～1.1 to add sulfuric acid in sodium aluminate solution; 5. use strainer to carry out solid-liquid separation, obtain aluminum hydroxide precipitate and metabisulfite solution respectively; 6. aluminum hydroxide precipitate is promptly obtained the aluminium hydroxide finished product after dry under 20～80 ℃ the temperature and pulverizing.
2, a kind of method of utilizing aluminium ash prepare aluminium hydroxide as claimed in claim 1 is characterized in that adding fusing assistant in step in 1., and aluminium weight ratio grey and solid sodium carbonate and fusing assistant is 100: 80～120: 10～20; 2. with solid mixture fusion 1～5 hour under 900 ℃～1180 ℃ conditions.
3, a kind of method of utilizing the aluminium ash to prepare aluminium hydroxide as claimed in claim 2 is characterized in that described fusing assistant is a borax.
4, a kind of method of utilizing aluminium ash prepare aluminium hydroxide as claimed in claim 2 is characterized in that 3. described step is melts to be cooled to put into water again after the room temperature and soak more than 10 hours, is left sodium aluminate solution after removing throw out.
5, as claim 1 or 2 or 4 described a kind of methods of utilizing the aluminium ash to prepare aluminium hydroxide, it is characterized in that 4. described step is sodium aluminate in molar ratio: sulfuric acid is 2: 0.9～1.1 to add sulfuric acid in sodium aluminate solution, precipitation was carried out solid-liquid separation more than 2 hours.
6, a kind of method of utilizing the aluminium ash to prepare aluminium hydroxide as claimed in claim 1 promptly obtains the industrial chemicals Sodium sulfate anhydrous.min(99) after the metabisulfite solution evaporation drying that it is characterized in that 5. step is obtained.
7, a kind of method of utilizing the aluminium ash to prepare aluminium hydroxide as claimed in claim 1 is characterized in that the throw out during step 3. is free of contamination red mud.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100493875A CN100349799C (en) | 2006-01-24 | 2006-01-24 | Production of aluminium hydrate from aluminium ash |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100493875A CN100349799C (en) | 2006-01-24 | 2006-01-24 | Production of aluminium hydrate from aluminium ash |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1817795A true CN1817795A (en) | 2006-08-16 |
| CN100349799C CN100349799C (en) | 2007-11-21 |
Family
ID=36918039
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2006100493875A Expired - Fee Related CN100349799C (en) | 2006-01-24 | 2006-01-24 | Production of aluminium hydrate from aluminium ash |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100349799C (en) |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100532268C (en) * | 2007-12-17 | 2009-08-26 | 中国铝业股份有限公司 | Production method of oxygen-containing beta aluminum fluoride for aluminum electrolysis bath by using aluminum scruff ash |
| CN101973565A (en) * | 2010-12-02 | 2011-02-16 | 中南大学 | Method for recovering aluminium in aluminium ash by low-temperature alkaline smelting |
| CN103060566A (en) * | 2011-10-21 | 2013-04-24 | 湖南创元铝业有限公司 | Method for recovering aluminum oxide, chlorine salt and villiaumite from aluminum ash |
| CN104445330A (en) * | 2014-12-10 | 2015-03-25 | 兴安宸亿工贸有限公司 | Method for producing aluminum ammonium sulfate crystal |
| CN106315640A (en) * | 2016-08-19 | 2017-01-11 | 云南文山铝业有限公司 | Method for treating high-evaporation mother liquid in alumina production |
| CN109437266A (en) * | 2018-12-25 | 2019-03-08 | 焦作大学 | It is a kind of to extract activity Al (OH) 3 Product Process using aluminium ash or rich-alumina residues |
| CN112830508A (en) * | 2021-01-29 | 2021-05-25 | 郑州大学 | Method for preparing aluminum hydroxide by using aluminum ash denitrification and fluorine fixation clinker |
| CN115304088A (en) * | 2022-01-21 | 2022-11-08 | 重庆龙健金属制造有限公司 | Method for preparing aluminum hydroxide by resource utilization of aluminum ash |
| CN115321568A (en) * | 2022-01-21 | 2022-11-11 | 重庆龙健金属制造有限公司 | Method for preparing sodium aluminate by resource utilization of aluminum ash |
| CN115321566A (en) * | 2022-01-21 | 2022-11-11 | 重庆龙健金属制造有限公司 | Method for preparing aluminum oxide by resource utilization of aluminum ash |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1291919C (en) * | 2004-12-03 | 2006-12-27 | 潘坤涛 | Process of producing alumina with waste aluminium ash |
-
2006
- 2006-01-24 CN CNB2006100493875A patent/CN100349799C/en not_active Expired - Fee Related
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100532268C (en) * | 2007-12-17 | 2009-08-26 | 中国铝业股份有限公司 | Production method of oxygen-containing beta aluminum fluoride for aluminum electrolysis bath by using aluminum scruff ash |
| CN101973565A (en) * | 2010-12-02 | 2011-02-16 | 中南大学 | Method for recovering aluminium in aluminium ash by low-temperature alkaline smelting |
| CN103060566A (en) * | 2011-10-21 | 2013-04-24 | 湖南创元铝业有限公司 | Method for recovering aluminum oxide, chlorine salt and villiaumite from aluminum ash |
| CN104445330A (en) * | 2014-12-10 | 2015-03-25 | 兴安宸亿工贸有限公司 | Method for producing aluminum ammonium sulfate crystal |
| CN104445330B (en) * | 2014-12-10 | 2016-05-18 | 兴安宸亿工贸有限公司 | A kind of production method of ammonia-alum |
| CN106315640A (en) * | 2016-08-19 | 2017-01-11 | 云南文山铝业有限公司 | Method for treating high-evaporation mother liquid in alumina production |
| CN106315640B (en) * | 2016-08-19 | 2018-06-19 | 云南文山铝业有限公司 | Handle the high method for steaming mother liquor in alumina producing |
| CN109437266A (en) * | 2018-12-25 | 2019-03-08 | 焦作大学 | It is a kind of to extract activity Al (OH) 3 Product Process using aluminium ash or rich-alumina residues |
| CN112830508A (en) * | 2021-01-29 | 2021-05-25 | 郑州大学 | Method for preparing aluminum hydroxide by using aluminum ash denitrification and fluorine fixation clinker |
| CN115304088A (en) * | 2022-01-21 | 2022-11-08 | 重庆龙健金属制造有限公司 | Method for preparing aluminum hydroxide by resource utilization of aluminum ash |
| CN115321568A (en) * | 2022-01-21 | 2022-11-11 | 重庆龙健金属制造有限公司 | Method for preparing sodium aluminate by resource utilization of aluminum ash |
| CN115321566A (en) * | 2022-01-21 | 2022-11-11 | 重庆龙健金属制造有限公司 | Method for preparing aluminum oxide by resource utilization of aluminum ash |
Also Published As
| Publication number | Publication date |
|---|---|
| CN100349799C (en) | 2007-11-21 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN100349799C (en) | Production of aluminium hydrate from aluminium ash | |
| CN110194474B (en) | Process for producing polyaluminium chloride and calcium aluminate by using aluminium ash | |
| CN106319218A (en) | Method for recovering rare earth, aluminum and silicon from rare earth-containing aluminum and silicon wastes | |
| CN1785537A (en) | Treatment method of aluminium electrolytic bath waste cathode carbon blook innocuousnes | |
| CN102923764B (en) | Method for preparing sodium stannate from stannic oxide and sodium salt in reduction roasting manner | |
| CN100417475C (en) | Production of metal zinc powder from zinc dust and zinc dross | |
| CN101054626A (en) | Stripping method for diasporite type bauxite | |
| CN102409177B (en) | Method for comprehensively recovering aluminum, silicon and titanium from pyrite tailings | |
| CN102586610A (en) | Cleaner production process for synchronously extracting vanadium and aluminum from aluminothermic vanadium iron slag | |
| JP5831914B2 (en) | Water treatment method | |
| JP5451323B2 (en) | Water treatment method | |
| CN102515280A (en) | Method for separation of aluminum and iron from acid leaching solution of coal gangue with high iron content | |
| CN111500864A (en) | Method for recycling electroplating sludge based on chromium recovery | |
| CN111592001A (en) | Method for preparing layered double hydroxide and white carbon black from fly ash | |
| CN103911517A (en) | Method of preparing vanadium-containing clinker by using TiCl4 refined tailings | |
| CN108178171A (en) | A kind of method that lithium carbonate is produced from lepidolite | |
| CN101302021A (en) | Method for extracting aluminum oxide from fly ash | |
| CN113648586A (en) | Wet harmless treatment method for electrolytic manganese slag | |
| CN102515234A (en) | Method for producing low-iron aluminum sulfate and polymeric aluminum ferric sulfate by using coal gangue | |
| CN102815728A (en) | Method for preparing nano-sized magnesium hydroxide and nano-silica by utilization of boron mud | |
| CN106755997B (en) | A kind of method of nickel-containing ore comprehensive utilization | |
| CN102849782B (en) | Method for producing high-purity zinc oxide by steel mill smoke dust ash ammonia method decarburization | |
| CN1899971B (en) | Method for extracting V2O5 from stone coal vanadium ore | |
| CN109280776B (en) | Method for recycling chromium in electroplating sludge by using sub-molten salt method | |
| CN1994881A (en) | Method for preparing polysilicate aluminium molten iron processing agent using bauxite gangue |
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 |