CN104386814A - Method for intensifying starting performance of anaerobic ammonia oxidation process by using ultrasonic wave - Google Patents
Method for intensifying starting performance of anaerobic ammonia oxidation process by using ultrasonic wave Download PDFInfo
- Publication number
- CN104386814A CN104386814A CN201410729076.8A CN201410729076A CN104386814A CN 104386814 A CN104386814 A CN 104386814A CN 201410729076 A CN201410729076 A CN 201410729076A CN 104386814 A CN104386814 A CN 104386814A
- Authority
- CN
- China
- Prior art keywords
- anaerobic ammonia
- ammonia oxidation
- oxidation process
- anaerobic
- reactor
- 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.)
- Pending
Links
Landscapes
- Purification Treatments By Anaerobic Or Anaerobic And Aerobic Bacteria Or Animals (AREA)
Abstract
The invention belongs to novel wastewater biological nitrogen removal processes, and discloses a method for intensifying the starting performance of an anaerobic ammonia oxidation process which takes ordinary activated sludge as an inoculum by using ultrasonic waves. An ultrasonic generator main machine is arranged outside an anaerobic ammonia oxidation starting reactor, and an ultrasonic wave vibrator is submerged below the liquid level inside the reactor. By irradiating culture sludge of the anaerobic ammonia oxidation process starting process by using low-intensity ultrasonic waves, the cytomembrane permeability, the electron transfer speed and the functional enzymatic activity of anaerobic ammonium oxidation bacteria are improved, so that the activity and flora competitive advantages of the anaerobic ammonium oxidation bacteria in the culture sludge are improved, and rapid starting of the process is achieved. By adopting the method, both the starting period of the anaerobic ammonia oxidation process is shortened, and the anaerobic ammonia oxidation bacteria can be domesticated in the activated sludge, and a technical support and stain reservation are provided for the industrialization process of the anaerobic ammonia oxidation process. The method has the advantages that the reaction condition is gentle and free of secondary pollution, the device is simple in structure and easy to operate, and the bacteria grow fast and are high in bioactivity, resistant to load impact and good in stability.
Description
Technical field
The invention belongs to Novel waste aquatic organism denitrification process.A kind of method utilizing ultrasonic irradiation to realize anaerobic ammonia oxidation process under being specifically related to precondition being inoculum with ordinary activated sludge to start fast.
Background technology
In recent years, the body eutrophication that nitrogen and phosphorus pollution causes is on the rise, and the environmental disaster such as wawter bloom, red tide frequently occurs.Ammonia nitrogen is the primary pollutant of water body polluted by nitrogen, and thus the process of nitrogen-containing wastewater is the important step of control body eutrophication.Conventional waste water biological denitrification process is when processing ammonia nitrogen in high density, and the denitrification stage need be dropped into a large amount of organic carbon and be served as electron donor, and the nitrated stage needs aeration aerating, causes running cost too high.Therefore, investigator proposes a kind of novel denitride technology-anaerobic ammonia oxidation process of applicable process high-concentration ammonia nitrogenous wastewater.
Anammox is a kind of novel denitrification process of applicable process high-concentration ammonia nitrogenous wastewater, can, under strictly anaerobic condition, using nitrite as electron acceptor(EA), be nitrogen by ammonium oxidation.Compared to traditional wastewater denitrification process, Anammox has the advantages such as efficiency is high, energy consumption is low, excess sludge production is few, do not produce greenhouse gases, running cost is low, and prospects for commercial application is wide.But anaerobic ammonia oxidizing bacteria poor growth, the multiplication cycle reaches 11 days, causes anaerobic ammonia oxidation process to start the cycle quite long, seriously constrains the industrial applications of anaerobic ammonia oxidation process.
At present, investigator proposes the method improving anaerobic ammonia oxidizing bacteria activity.The people such as Tsing-Hua University's left sword evil disclose a kind of mixing sludge that utilizes to cultivate the method for anaerobic ammonium oxidation granular sludge in the patent of invention of CN 1254440C: mix be seeded to upflow type anaerobic reactor with anaerobic grain sludge foster active sludge of becoming reconciled, adopt simulated wastewater (Anammox bacterium culture medium) water inlet, upflow liquid velocity controls at 1-2m/h, cultivates the good anaerobic ammonium oxidation granular sludge of availability energy through domestication.The people such as Beijing University of Technology Li Dong disclose a kind of quick start method being exclusively used in anaerobic ammonia oxidation process under the low matrix of normal temperature in the patent of invention that publication number is CN 102718314A: first adopt continuous aeration, control the method domestication nitrifiers such as dissolved oxygen, adopt the mode of intermittent aeration/anaerobism to carry out screening and the enrichment of anaerobic ammonia oxidizing bacteria again, finally reactor enter the anaerobism operation phase add certain anaerobic ammonia oxidizing bacteria accelerate anaerobic ammonia oxidation process start.At present, improved and operational process optimization by reactor configuration, anaerobic ammonia oxidation process toggle speed is improved to a certain extent, but, be that the anaerobic ammonia oxidation reactor start-up course of inoculum still needs 3 months or the longer time with active sludge.Rare and the anaerobic ammonia oxidation process of Anammox function bacterial classification starts excessive cycle and is still one of significant challenge that its course of industrialization faces.
Summary of the invention
In order to solve, anaerobic ammonia oxidizing bacteria growth velocity is low, environmental sensitivity is high and anaerobic ammonia oxidation process starts the problems such as excessive cycle in the present invention, aims to provide a kind of method that intensified by ultrasonic wave take ordinary activated sludge as the anaerobic ammonia oxidation process startup usefulness of inoculum.
The present invention both can shorten anaerobic ammonia oxidation process and start the cycle, can tame anaerobic ammonia oxidizing bacteria again, for process industry process provides some technical supports and bacterial classification deposit from active sludge.
Ultrasonic wave effectively can improve microorganism active, and reaction conditions is gentle, and non-secondary pollution belongs to environmentally friendly technology.Ultrasonic wave can be improved membrane passage, improves the activity of biological enzyme, accelerate electron transmission, the activity of promotion functions bacterium can improve and promote its competitive edge in mixed training thing flora.The present invention in anaerobic ammonia oxidation process start-up course with ul-trasonic irradiation, strengthens anaerobism ammonia oxygen bacterium activity and flora competitive edge, shortens its multiplication cycle, thus realize the quick startup of anaerobic ammonia oxidation process.
The present invention inoculates with ordinary activated sludge, and adopt ultrasonic wave interventional technique to accelerate anaerobic ammonia oxidation process and start, its concrete steps are as follows:
Step one reaction unit is built
The reactor started using fixed bed as anaerobic ammonia oxidation process.With cellular biologic packing material filling reactor.Ultrasonic generator is installed outward at reactor, makes ultrasonic oscillator insert in reactor under liquid level.Reactor is provided with outer tube sleeve, and constant-temperature hot water makes temperature of reaction maintain 35-37 DEG C in outer tube sleeve circulation.Constant-temperature hot water comes from constant temperature water tank, and this water tank realizes temperature by thermostatically heating rod and controls.Constant temperature water tank is also provided with thermometer, can show water tank temperature in real time, its benefit is: thermostatically heating rod breaks down, and thermometer can show abnormal water temperature, at this moment change heating rod in time, the disadvantageous effect that temperature variation is brought Anammox reactivity worth can be avoided.The pH of reaction system controls 7 ~ 8.Each interface of reactor and pipeline and junction seal intact, ensure the anaerobic environment of reaction, require wherein dissolved oxygen≤0.1mg/L.Meanwhile, device gobo wraps up, and avoids illumination to the restraining effect of function yeast.
Step 2 seed sludge
Adopt the active sludge of sewage work as inoculum.First rinsing is carried out to active sludge, remove the impurity of wherein dissolved organic matter and inactive, avoid it to the disadvantageous effect of technique start-up course.Again the active sludge after rinsing is seeded to fixed-bed reactor.
Step 3 operation process
Fixed-bed reactor adopt continuum micromeehanics.Water inlet, for not containing organic simulated wastewater, carries out artificial distribution according to Anammox bacterium culture medium.Simulated wastewater by peristaltic pump from the water inlet upper end water outlet of reactor lower end.The main component of described simulated wastewater is ammonia nitrogen and nitrite, in addition, also comprises appropriate KH
2pO
4, KHCO
3, CaCl
2and MgSO
4and liquid microelement (EDTA, ZnSO
4, CoCl
2, MnCl
2, CuSO
4, NaMoO
4, NiCl
2, NaSeO
4, H
3bO
4, NaWO
4and yeast extract paste).At the reactor start-up initial stage, also need to add a small amount of nitrate.Simulated wastewater exposes to the sun 95%Ar/5%CO in inlet chest
2gas mixture, to remove the dissolved oxygen in water, maintains the anaerobic condition of reaction.In reactor operational process, on the one hand, part microorganism apposition growth on filler forms microbial film; On the other hand, part microorganism is retained down formation floc sludge by the vesicular structure of honeycomb padding bed.The state that microbial film and floc sludge have concurrently can be formed in reactor.
Step 4 intensified by ultrasonic wave
In the reactor operational process of described step 3, every day carries out 1-3 ultrasonic irradiation to the culture sludge in reactor.Along with the oscillator be immersed in simulated wastewater sends ultrasonic wave, ultrasonic wave can be propagated in liquid phase and solid phase, makes the culture sludge comprising microbial film and cotton-shaped form all can be subject to irradiation.It is active that ultrasonic irradiation improves the cell-membrane permeable of anaerobic ammonia oxidizing bacteria, electron transmission speed and functional enzyme, thus improve anaerobic ammonia oxidizing bacteria growing multiplication speed and strengthen its competitive edge in culture sludge flora, and then effectively accelerate the startup process with the process of activated sludge acclimatization anaerobic ammonia oxidizing bacteria and anaerobic ammonia oxidation process.In the present invention, frequency that ultrasonic irradiation adopts is 20-50kHz, and intensity is 0.3-0.7w/cm
2, each irradiation time is 2-10min.
The invention provides method that anaerobic ammonia oxidation process under a kind of thermophilic (35-37 DEG C) condition starts fast and the method that anaerobic ammonia oxidizing bacteria is tamed fast.Application the present invention can efficiently remove ammonia nitrogen and cultured water, save a large amount of energy and material consumptions, thus working cost at least can cut down 70%, for the Sources controlling of body eutrophication provides technical support compared with traditional denitrification process.
The advantage of patent of the present invention is: 1) reaction conditions is gentle, non-secondary pollution; 2) device is simple and easy, simple to operate; 3) growth is fast, and biological activity is high; 4) resistance to overload shock, good stability.
Accompanying drawing explanation
Fig. 1 is the device schematic diagram of intensified by ultrasonic wave Anammox start-up course of the present invention
1. inlet chest 2. intake pump 3. fixed-bed reactor 4. honeycomb padding 5. outer tube sleeve 6. ultrasonic generator 7. water outlet 8. thermometer 9. temperature control heating rod 10. constant temperature water tank 11. water circulating pump 12. thermostat(t)ed water entrance
Embodiment
Below in conjunction with specific embodiment, the invention will be further described, but protection scope of the present invention is not limited in this.
Embodiment 1
Using the aerobic activated sludge in certain municipal sewage plant CASS pond as inoculum.Reactor is high is 1.5 with the ratio of internal diameter, and effective volume is 2.4L.First with cellular polypropylene (PP) filler filling fixed-bed reactor, selected PP honeycomb padding diameter is 2.5cm, and packing ratio is 85%.Again by collected aerobic activated sludge clear water rinsing 3 times.After rinsing, mud mixed liquid suspended sediment concentration (MLSS) is 1.86g/L, and mixed liquor volatile suspended solid, MLVSS concentration (MLVSS) is 1.53g/L.Get 2L mud mixed liquid and be seeded to reactor.Water inlet is simulated wastewater, and the main component according to Anammox bacterium culture medium is prepared, main containing ammonia nitrogen and cultured water, not containing organism.With 95%Ar/5%CO
2gas mixture, to simulated wastewater aeration 10min, is discharged the dissolved oxygen (DO) in water, is avoided DO to bring reactor into water inlet, the anaerobic environment of impact reaction.Simulated wastewater is flowed out from the water outlet close to top from the water-in inflow close to reactor bottom by peristaltic pump suction again.Reactor takes continuum micromeehanics mode.Reactor operating parameter: temperature 35 DEG C, pH value 7.3 ~ 8, DO≤0.1mg/L.Ammonia nitrogen concentration is 50 ~ 100mg/L, and the mol ratio of cultured water and ammonia nitrogen is (1 ~ 1.2): 1.In initial start stage, ammonia nitrogen concentration is 50mg/L, and hydraulic detention time (HRT) is 72h, and the mol ratio of cultured water and ammonia nitrogen is 1: 1, and the mol ratio of nitrate nitrogen and ammonia nitrogen is 0.3: 1.After this, along with the raising of anaerobic ammoxidation activity, progressively increase water inlet nitrogen load by improving influent ammonium concentration and shortening HRT.When anaerobic ammoxidation activity performance, in water inlet, just no longer add nitrate nitrogen.In reactor operational process, ultrasonic generator carries out 1 ultrasonic irradiation to the culture sludge in reactor every day.The oscillator be immersed in simulated wastewater sends ultrasonic wave, makes the culture sludge comprising microbial film and cotton-shaped form all be subject to irradiation.Frequency that each ultrasonic irradiation adopts is 30kHz, and intensity is 0.5w/cm
2, irradiation time is 5min.Ultrasonic irradiation improves anaerobic ammonia oxidizing bacteria growth velocity, shorten its generation cycle, make anaerobic ammonia oxidizing bacteria more competitive than other bacterial classifications in the flora of culture sludge, and then effectively accelerate the startup process of process that anaerobic ammonia oxidizing bacteria tames from active sludge and anaerobic ammonia oxidation process.Ran through 21 days, there is ammonia nitrogen and the synchronous removal effect of cultured water in reactor, namely occurs anaerobic ammoxidation activity.Ran through 56 days, influent ammonia nitrogen and cultured water concentration are respectively 100mg/L and 120mg/L, and HRT foreshortens to 12h, and reactor ammonia nitrogen, cultured water and nitrogen removal rate reach 95%, 98% and 90% respectively.Anaerobic ammoxidation activity significantly strengthens, and observing mud, to have grey to become light brown, and local, in brown, shows that anaerobic ammonium oxidation sludge domestication is ripe, illustrates that anaerobic ammonia oxidation process successfully starts.
Embodiment 2
To adopt certain aquiculture sewerage treatment plant nitrifying sludge of A/O technique as inoculum.Through 2 rinsings, inoculum mud MLSS and MLVSS is respectively 2.16g/L and 1.63g/L.Selected PP honeycomb padding diameter is 1.5cm.Temperature of reaction is 37 DEG C, and pH value is 7 ~ 7.8.Plant running process, every day carries out 2 ultrasound wave irradiations to culture sludge, and frequency that each ultrasonic irradiation adopts is 20kHz, and intensity is 0.3w/cm
2, irradiation time is 5min.All the other steps are identical with example 1, and after running 51 days continuously, anaerobic ammonium oxidation sludge domestication is ripe, and anaerobic ammonia oxidation process starts successfully.
Embodiment 3
Using the granule sludge of certain up-flow anaerobic sludge blanket (UASB) as inoculum.Through 1 rinsing, inoculum mud MLSS and MLVSS is respectively 2.85g/L and 2.13g/L.Selected PP honeycomb padding diameter is 1cm.Reactor mixed solution pH value is 7.5 ~ 8.Technique start-up course, every day carries out 1 ultrasound wave irradiation to culture sludge, and frequency that each ultrasonic irradiation adopts is 50kHz, and intensity is 0.7w/cm
2, irradiation time is 3min.All the other steps are identical with example 1, and run after 62 days, anaerobic ammonia oxidation process starts successfully, and anaerobic ammonium oxidation sludge domestication is ripe, and wherein anaerobic ammonia oxidizing bacteria is mud dominant bacteria.
Claims (4)
1. the method for an intensified by ultrasonic wave anaerobic ammonia oxidation process startup usefulness, it is characterized in that described method is: using active sludge as inoculum, use the culture sludge of ultrasonic irradiation anaerobic ammonia oxidation process start-up course again, shorten the multiplication cycle of anaerobic ammonia oxidizing bacteria, strengthen its competitive edge in flora, and then realize the quick startup of anaerobic ammonia oxidation process.
2. a kind of intensified by ultrasonic wave anaerobic ammonia oxidation process as claimed in claim 1 starts the method for usefulness, it is characterized in that ultrasonic generator is placed in outside reactor, ultrasonic oscillator is immersed in reactor under liquid level, makes culture sludge all can be subject to irradiation during work; In technique start-up course, every day carries out 1-3 ultrasonic irradiation to the culture sludge in reactor, active with strengthened anaerobic ammoxidation bacterium.
3. a kind of intensified by ultrasonic wave anaerobic ammonia oxidation process as claimed in claim 2 starts the method for usefulness, it is characterized in that:
(1) ultrasonic wave working parameter is: frequency 20-50kHz, intensity 0.3-0.7w/cm
2, each irradiation time 2-10min.
(2) reactor operating parameter: temperature 35-37 DEG C, pH 7 ~ 8, dissolved oxygen≤0.1mg/L.
4. a kind of intensified by ultrasonic wave anaerobic ammonia oxidation process as claimed in claim 3 starts the method for usefulness, it is characterized in that constant-temperature hot water makes temperature of reaction constant in outer tube sleeve circulation, constant-temperature hot water comes from constant temperature water tank, constant temperature water tank is provided with thermometer, can show water tank temperature in real time, when thermostatically heating rod breaks down, thermometer can show abnormal water temperature, be convenient to change heating rod in time, avoid the disadvantageous effect that temperature variation is brought Anammox reactivity worth.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201410729076.8A CN104386814A (en) | 2014-12-02 | 2014-12-02 | Method for intensifying starting performance of anaerobic ammonia oxidation process by using ultrasonic wave |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201410729076.8A CN104386814A (en) | 2014-12-02 | 2014-12-02 | Method for intensifying starting performance of anaerobic ammonia oxidation process by using ultrasonic wave |
Publications (1)
Publication Number | Publication Date |
---|---|
CN104386814A true CN104386814A (en) | 2015-03-04 |
Family
ID=52604796
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201410729076.8A Pending CN104386814A (en) | 2014-12-02 | 2014-12-02 | Method for intensifying starting performance of anaerobic ammonia oxidation process by using ultrasonic wave |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN104386814A (en) |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106011017A (en) * | 2016-06-28 | 2016-10-12 | 苏州科技大学 | Method for realizing rapid proliferation of anaerobic ammonium oxidation bacteria |
CN111974184A (en) * | 2020-08-12 | 2020-11-24 | 中石化南京化工研究院有限公司 | System and method for improving flue gas desulfurization effect of biological method |
CN115520962A (en) * | 2022-07-05 | 2022-12-27 | 济南大学 | With NO 3- Domestication culture method of electroactive anaerobic ammonium oxidation microorganisms serving as single nitrogen source |
Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103693749A (en) * | 2013-12-12 | 2014-04-02 | 大连理工大学 | Method for improving denitrification performance of anaerobic ammonium oxidation bacteria by using tourmaline |
-
2014
- 2014-12-02 CN CN201410729076.8A patent/CN104386814A/en active Pending
Patent Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103693749A (en) * | 2013-12-12 | 2014-04-02 | 大连理工大学 | Method for improving denitrification performance of anaerobic ammonium oxidation bacteria by using tourmaline |
Non-Patent Citations (1)
Title |
---|
汪涛: "厌氧氨氧化工艺快速启动及菌群特性研究", 《中国博士学位论文全文数据库 工程科技I辑》 * |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106011017A (en) * | 2016-06-28 | 2016-10-12 | 苏州科技大学 | Method for realizing rapid proliferation of anaerobic ammonium oxidation bacteria |
CN106011017B (en) * | 2016-06-28 | 2019-12-06 | 苏州科技大学 | method for realizing rapid proliferation of anaerobic ammonium oxidation bacteria |
CN111974184A (en) * | 2020-08-12 | 2020-11-24 | 中石化南京化工研究院有限公司 | System and method for improving flue gas desulfurization effect of biological method |
CN115520962A (en) * | 2022-07-05 | 2022-12-27 | 济南大学 | With NO 3- Domestication culture method of electroactive anaerobic ammonium oxidation microorganisms serving as single nitrogen source |
CN115520962B (en) * | 2022-07-05 | 2024-05-03 | 济南大学 | With NO3-Method for domesticating and culturing electroactive anaerobic ammonia oxidizing microorganism serving as single nitrogen source |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN107032506B (en) | Device and method for treating domestic sewage through sectional effluent shortcut nitrification-Anammox/denitrification | |
CN102718314B (en) | Method for quick starting of anaerobic ammonium oxidation technology at room temperature in low matrix | |
CN101759323B (en) | Treatment combined process for pig farm waste water with high nitrogen content | |
CN102583885B (en) | Technology and method for treating urban sewage by three-section short-cut nitrification/ anaerobic ammonia oxidation | |
CN106277315B (en) | A kind of denitrification microorganism nest and its cultural method based on basalt fibre filler | |
CN106430562B (en) | A kind of processing method of poultry discharged wastewater met the national standard | |
CN105540841B (en) | A kind of aerobic/anaerobic biofilter biological denitrification method and device | |
CN103787498B (en) | Rapid starting method of low-temperature low C/N sewage improvement A2/O process | |
CN110002697B (en) | Device and method for generating methane and performing IFAS A/O SPNAPD denitrification by UASB (upflow anaerobic sludge blanket) of landfill leachate | |
CN101007678A (en) | Temperature controlled USAB anaerobic ammoxidation strain denitrogenation method and its apparatus | |
CN104150716A (en) | Biology processing apparatus capable of processing sewage at low-temperature with low carbon-nitrogen-ratio in cold region and method for processing sewage at low-temperature with low carbon-nitrogen-ratio in cold region | |
CN104310580B (en) | Part denitrification series connection autotrophic denitrification realizes the apparatus and method of nitrate wastewater and city sewage deep denitrogenation | |
CN101817615A (en) | Anaerobic-sequencing batch biofilm reactor-artificial wetland method for treating piggery wastewater | |
CN102173504A (en) | Method for culturing shortcut nitrification granular sludge by combining dual inhibition of FA and FNA | |
CN110104774A (en) | Continuous flow segmental influent, sludge and fermented sludge segment reflux part denitrification/Anammox Treating Municipal Sewage device | |
CN107043197A (en) | A kind of method that blue-green algae joint CANON handles ammonia nitrogen waste water | |
CN102701442A (en) | Quick starting method of water source biological denitrification system | |
CN108862581A (en) | A kind of device and method that AO biomembrane+sludge fermentation coupling denitrification realizes sewage deep denitrogenation synchronous sludge decrement | |
CN104445619A (en) | Process and device for deeply removing nitrogen and phosphorus in waste water | |
CN113233592B (en) | Treatment device and method for realizing synchronous deep denitrification and decarbonization of advanced landfill leachate and domestic sewage | |
CN102503033A (en) | Technique for treating pig raising liquid waste by circular anaerobic reactor, sequencing batch biofilm, constructed wetland and facultative lagoon | |
CN102887589A (en) | Nano aeration biofilm reactor | |
CN105601025B (en) | A kind of breeding wastewater efficient degradation denitrogenation processing system and processing method | |
CN202542997U (en) | Half shortcut nitrification/ anaerobic ammonia oxidation nitrogen and phosphorus removal device for urban sewage | |
CN102060377B (en) | Method for enriched culture of nitrite-oxidizing bacterium granular sludge |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
C06 | Publication | ||
PB01 | Publication | ||
C10 | Entry into substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
RJ01 | Rejection of invention patent application after publication |
Application publication date: 20150304 |
|
RJ01 | Rejection of invention patent application after publication |