CN103449695B - Microbiological oil sludge treatment process - Google Patents

Microbiological oil sludge treatment process Download PDF

Info

Publication number
CN103449695B
CN103449695B CN201210180830.8A CN201210180830A CN103449695B CN 103449695 B CN103449695 B CN 103449695B CN 201210180830 A CN201210180830 A CN 201210180830A CN 103449695 B CN103449695 B CN 103449695B
Authority
CN
China
Prior art keywords
oil
greasy filth
cgmcc
sludge
biological
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201210180830.8A
Other languages
Chinese (zh)
Other versions
CN103449695A (en
Inventor
刘关平
王鹏
杜郭君
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.)
JIANGSU BODA ENVIRONMENTAL PROTECTION CO Ltd
Original Assignee
JIANGSU BODA ENVIRONMENTAL PROTECTION CO Ltd
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 JIANGSU BODA ENVIRONMENTAL PROTECTION CO Ltd filed Critical JIANGSU BODA ENVIRONMENTAL PROTECTION CO Ltd
Priority to CN201210180830.8A priority Critical patent/CN103449695B/en
Publication of CN103449695A publication Critical patent/CN103449695A/en
Application granted granted Critical
Publication of CN103449695B publication Critical patent/CN103449695B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02WCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W10/00Technologies for wastewater treatment
    • Y02W10/20Sludge processing

Landscapes

  • Micro-Organisms Or Cultivation Processes Thereof (AREA)
  • Purification Treatments By Anaerobic Or Anaerobic And Aerobic Bacteria Or Animals (AREA)
  • Preparation Of Compounds By Using Micro-Organisms (AREA)

Abstract

The invention belongs to the environment-friendly field and discloses a microbiological oil sludge treatment process. The microbiological oil sludge treatment process comprises four steps of oil sludge fluidization, biological treatment, sludge dehydration and biological induction, wherein the biological treatment step is to add candida lipolytica Y-57 with a preservation number of CGMCC (China General Microbiological Culture Collection Center) No.5790 and pseudomonas putida P-101 with the preservation number of CGMCC No.5801 into a biological reaction tank, wherein after aeration biological reaction, in terms of absolute dry mud, the oil content of the oil sludge is less than 2%, and the water contains less than 150mg/L of oil; floating oil on the upper part of water surface is recycled by an oil receiving device, fine sediment on the bottom is exhausted after reaching the standards, and the oil sludge enters the sludge dehydration step. According to the microbiological oil sludge treatment process disclosed by the invention, a microbiological treatment method, a biological induction method and a mechanical method are combined for application, so that the oil content of the sludge reaches 0.3%-standard to recover a sludge environment, thereby achieving a purpose of recycling and hazard-free treatment.

Description

A kind of Microbiological oil sludge treatment technique
Technical field
The invention belongs to field of Environment Protection, relate to a kind of Microbiological oil sludge treatment technique.
Background technology
Oily sludge is the oily solid sludge produced in oil production, transport, refining and oily water treatment process.Wherein containing a large amount of materials such as hydro carbons, benzene homologues, phenols, anthracene class, if do not processed, not only to contaminate environment, and it is the one waste of resource.
Each station of North China Oilfield has oil-sludge treatment to dispose difficult problem, and existing needs is processed the sedimentation greasy filth of slurry tank in each plant stand, makes it to discharge by safety compliance innoxiously.
And at present, the method for process greasy filth is varied, such as: the rotten method of landfill method, mechanical process, burning method, heap, till, bio-reactor method and plant method etc.On the whole, above method one-time investment is large, operation, management trouble, and working cost is high, the most important thing is that process is not thorough, easily causes secondary pollution, can not fundamentally solve greasy filth pollution problem.Although pile rotten method and plant method less investment and operational management is convenient, processing efficiency is very low.
Summary of the invention
The object of the invention is the above-mentioned defect for prior art, a kind of Microbiological oil sludge treatment technique is provided.
A kind of Microbiological oil sludge treatment technique, comprise greasy filth fluidization, biological treatment, sludge dewatering and biotic induce four steps, described biological treatment step is in biological reactor, add the pseudomonas putida P-101 that Candida lipolytica Y-57 that deposit number is CGMCC No.5790 and deposit number are CGMCC No.5801, after aeration and biological reaction, be less than 2% in over dry mud greasy filth oil-containing, water oil-containing is less than 150mg/L; On water surface top, oil slick is recycled by oil-collecting device, and bottom fine deposit standard discharge, greasy filth enters sludge dewatering step.
Described biological treatment step greasy filth is more than 8 hours in the biological reactor residence time; Water-gas ratio (volume ratio of water and air)=1: 4-5(liter in biological reactor: rise), hydraulic detention time 0.5-2 hour, control temperature 10 DEG C-40 DEG C, pH6-10.
To add Candida lipolytica Y-57 that deposit number is CGMCC No.5790 and deposit number in biological reactor be the mixed-culture medium dosage of the pseudomonas putida P-101 of CGMCC No.5801 is the 0.01%-1wt% of pending greasy filth quality.
The quantity of the deposit number added in biological reactor to be the Candida lipolytica Y-57 of CGMCC No.5790 and deposit number the be effective microbe of the pseudomonas putida P-101 mixed-culture medium of CGMCC No.5801 is greater than 10 11cfu/ gram.
Described greasy filth fluidization step adds water in greasy filth, makes the fluidization of thick shape greasy filth, and be greater than impurity, the waste material of 2mm by gravity settling sizing screening removal particle diameter.
Described sludge dewatering step be to biological treatment after greasy filth dewater, obtaining water ratio is 70% ~ 75%, the greasy filth being less than 2% in over dry mud greasy filth oil-containing.
The pseudomonas putida P-10 of described biotic induce to be that to access deposit number be CGMCC No.5790 Candida lipolytica Y-57 and deposit number in the greasy filth after dehydration be CGMCC No.5801, add simultaneously tensio-active agent 100-1000mg/Kg dewater after greasy filth, wood chip 5wt%-15wt%(is with greasy filth weighing scale) and nitrogenous nutrition 0-500mg/Kg dewater after greasy filth, greasy filth after phosphorous nutrition 0-100mg/Kg dehydration, stir, induce 80 ~ 100 days for 25 ~ 28 DEG C.
Described tensio-active agent is selected from one or more of tween, sapn, rhamnolipid, alkylaryl polyglycol ether, alkyl polyglycol ether or alkylaryl sulphonate.
Beneficial effect:
The present invention is by microorganism treatment and biotic induce method and mechanical process combined utilization, adopt machinery and biotechnology, to suffer petroleum products and polycyclic aromatic hydrocarbons, heavy oil, heavy metal Composite pollution environment greasy filth carry out purifying treatment, microorganism species is utilized to carry out biological degradation to oil pollutant (comprising heavy oil partial), mud oil length can be made to reach the standard of 0.3%, recover mud environment, reach resource utilization, innoxious object.The advantages such as it is low that the present invention also has cost, and power consumption is little.
Biomaterial preservation information
P-101, Classification And Nomenclature is pseudomonas putida (Pseudomonas putida), be preserved in China Committee for Culture Collection of Microorganisms's common micro-organisms center, preservation address is No. 3, Yard 1, BeiChen xi Road, Chaoyang District, Beijing City, Institute of Microorganism, Academia Sinica, preservation day is on February 24th, 2012, and deposit number is CGMCC No.5801.
Y-57, Classification And Nomenclature is Candida lipolytica (Candida lipolytica), be preserved in China Committee for Culture Collection of Microorganisms's common micro-organisms center, preservation address is No. 3, Yard 1, BeiChen xi Road, Chaoyang District, Beijing City, Institute of Microorganism, Academia Sinica, preservation day is on February 24th, 2012, and deposit number is CGMCC No.5790.
Embodiment
Embodiment 1
Choose trench greasy filth near Yixing City restaurant to screen by the following method:
1.1 bacterial classification enrichments
Add certain greasy filth (2%) in dextrose culture-medium in triangular flask and put into shaking table, cultivate 3 days, obtain bacterial classification pregnant solution for 30 DEG C.Dextrose culture-medium formula is: sodium-chlor 1g, calcium chloride 0.5g, dipotassium hydrogen phosphate 0.5g, potassium primary phosphate 0.5g, iron(ic) chloride 0.02g, ammonium nitrate 1g, magnesium sulfate heptahydrate, 1g yeast extract, 2g glucose, 1L water, PH 7.0-7.2; 110 DEG C of sterilizing 20min.
1.2 bacterial screening
By after the dilution of bacterial classification pregnant solution again dextrose solid medium flat board (adding 2% agar in dextrose culture-medium)) on to rule separation, cultivate 24 hours in 30 DEG C, picking in the good single bacterium colony streak inoculation of grow on plates on alkane flat board, cultivate 48 hours in 30 DEG C, choose maximum two single bacterium colonies called after Y-57, P-101 respectively.
Embodiment 2
Carry out biology and biochemical test to Y-57 bacterial strain, this yeast YPD Agar is incubated at flat board (30 DEG C) 3 days, and bacterium colony can grow to 1-2 millimeter, and white is to cream-colored.Initial stage bacterium colony is smooth shape, occurs gauffer through Extending culture bacterium colony.When solid or liquid nutrient medium grow, the rounded or oval of cellular form, cell also can elongate the false filamentous growth in class sometimes, and cell size is about 4-6 × 6-8 micron.
This yeast Biolog microbe auto-analysis instrument that Biolog company of the U.S. produces is identified, is accredited as Candida lipolytica.
Carry out biology and biochemical test to P-101 bacterial strain, the aerobic cultivation of this bacterium nutrient agar plate 24 hours, bacterial growth is vigorous, and bacterium colony is smooth, moistening, translucent faint yellow bacterium colony, produces strong smell, gramstaining is negative bacillus, and extremely raw many flagellums, most bacterial strain flagellum is more than three.This bacterium obligate aerobic, breathing pattern metabolism, decomposition glucose and wood sugar, utilize citritase, and Phenylalanine dehydrogenase reaction is feminine gender.Utilize inositol, oxydase and Terminal oxidase positive, arginine dihydrolase is positive, does not produce Polylevulosan, not gelatin hydrolysate, not hydrolyzed starch, hydrolysis polychrom, egg yellow reaction is negative, and Poly-β-hydroxybutyric Acid salt is negative, reduction nitrate, U.S. red negative, voges-Proskauer test is negative, and indole test is negative; 4 DEG C can grow, and 41 DEG C do not grow; Appropriate pH is 7-8.5.
This bacterium Biolog microbe auto-analysis instrument that Biolog company of the U.S. produces is identified, is accredited as pseudomonas putida.
Candida lipolytica Y-57 of the present invention and pseudomonas putida P-101 on February 24th, 2012 in the center preservation of China Committee for Culture Collection of Microorganisms's common micro-organisms, wherein, Candida lipolytica Y-57 deposit number is CGMCC NO.5790, and Classification And Nomenclature is: Candida lipolytica (Candida lipolytica); Pseudomonas putida P-101 deposit number is CGMCC NO.5801, and Classification And Nomenclature is: pseudomonas putida (Pseudomonas putida).
Embodiment 3
Candida lipolytica Y-57(CGMCC NO.5790) and pseudomonas putida P-10(CGMCC NO.5801) use LB substratum respectively, at 30 DEG C, 200rpm shaking table carries out cultivation 24 hours, fermention medium is seeded to again according to the inoculum size of 5%, in 30 DEG C, 200rpm stirs, air quantity 1:0.4-0.5, cultivates 36 hours to obtain the pseudomonas putida P-101 mixed-culture medium of deposit number to be the Candida lipolytica Y-57 of CGMCC No.5790 and deposit number be CGMCC No.5801 under tank pressure 0.05mpa.
Fermention medium (grams per liter): glucose 10, whiteruss 15, yeast extract paste 3.0, magnesium sulfate 0.2, Repone K 0.2, potassium primary phosphate 2.0, urea 1.0, ammonium nitrate 1.5, tween-80 0.5ml, Trace salts solution 1.0ml.PH nature.
Wherein: often liter of Trace salts solution contains 11.0 grams, zinc sulfate, manganous sulfate 6.0 grams, 1.0 grams, ferrous sulfate, EDTA-Na 27.3 grams, rose vitriol 0.3 gram, 40 milligrams, copper sulfate, boric acid 60 milligrams, potassiumiodide 1 milligram.
Embodiment 4
A, greasy filth fluidization
North China Oilfield slurry tank greasy filth oil length 9.6% drains into greasy filth collecting tank, by being pumped into fluidised form device, in device, being provided with whipping appts, adding the sewage of rear class dewatering part simultaneously, make the fluidization of thick shape greasy filth, be greater than impurity, the waste material of 2mm simultaneously by gravity settling sizing screening removal particle diameter.Through fluidization and sorting process, greasy filth is promoted to biological reactor by pump and carries out biochemical treatment.
B, biological treatment
The pseudomonas putida P-101 mixed-culture medium (prepared by embodiment 3) of the deposit number adding the 0.1wt% of greasy filth quality in biological reactor to be the Candida lipolytica Y-57 of CGMCC No.5790 and deposit number be CGMCC No.5801); Interpolation urea concentration is 100mg/L; When in oil-sludge treatment system, total phosphorus concentration is less than 25mg/L, interpolation potassium primary phosphate is 10mg/L.Under normal temperature, in water-gas ratio=1: 4, hydraulic detention time 2 hours, under the condition of pH6-10 after aeration and biological reacts 30 hours, obligate microorganism (Y-57 and P-101) degrades the oil pollutant in mud, water, greasy filth oil-containing is less than 2%(in over dry mud), water oil-containing is less than 150mg/L; On water surface top, oil slick is recycled by oil-collecting device, and bottom fine deposit is arranged outward, and greasy filth enters sludge dewatering system.
C, sludge dewatering
Greasy filth after biochemical treatment carries out centrifuge dehydration or adopts other dewatering type, makes mud-water separation, and the water after dehydration can arrive prime greasy filth fluidization equipment, and greasy filth water ratio about 75%, oil length is that 2%(is by over dry mud).
D, biotic induce
Water ratio is about 75%, oil length is that 2%(is by over dry mud) greasy filth carry out biotic induce process by adopting biotic induce pattern: in mud, introduce the deposit number being equivalent to 0.1% of dehydrated oil shale amount be CGMCC No.5790 Candida lipolytica Y-57 and deposit number is the pseudomonas putida P-10 mixed bacteria liquid of CGMCC No.5801, to improve rate of decomposition, add 500mg/Kg(by greasy filth weighing scale simultaneously) tween-80, wood chip 10%(presses greasy filth weighing scale) and urea 300mg/Kg(by greasy filth weighing scale), potassium primary phosphate 50mg/Kg(presses greasy filth weighing scale) etc. nutrition, stir, extraordinary bacterial strain normal temperature under this applicable environment provided decomposes the materials such as oils through 3 months induced reactions, mud oil length can be made to reach 0.27%(by over dry mud), lower than the standard of pollutant catabolic gene standard (GB4284-84) oleaginousness 0.3% in agricultural sludge.
Over dry mud described in the present invention is loaded in watch-glass by primary sludge sample, is placed in baking oven, and under the condition of 105 DEG C-108 DEG C, drying three hours, taking-up is weighed, and continues and puts into baking oven, similarity condition process 30min, and multiple taking-up is weighed, and so repeats twice.Relatively three secondary data, reach constant weight, are over dry mud.

Claims (1)

1. a Microbiological oil sludge treatment technique, it is characterized in that comprising greasy filth fluidization, biological treatment, sludge dewatering and biotic induce four steps, it is characterized in that described biological treatment step is in biological reactor, add the mixed-culture medium that Candida lipolytica Y-57 that deposit number is CGMCC No.5790 and deposit number are the pseudomonas putida P-101 of CGMCC No.5801, after aeration and biological reaction, be less than 2% in over dry mud greasy filth oil-containing, water oil-containing is less than 150mg/L; On water surface top, oil slick is recycled by oil-collecting device, bottom fine deposit standard discharge, and greasy filth enters sludge dewatering step; Described greasy filth fluidization step adds water in greasy filth, makes the fluidization of thick shape greasy filth, and be greater than impurity, the waste material of 2mm by gravity settling sizing screening removal particle diameter; The pseudomonas putida P-10 of described biotic induce to be that to access deposit number be CGMCC No.5790 Candida lipolytica Y-57 and deposit number in the greasy filth after dehydration be CGMCC No.5801, greasy filth after greasy filth after simultaneously adding tensio-active agent 100-1000mg/Kg dehydration after greasy filth, wood chip 5wt%-15wt%, nitrogenous nutrition 0-500 mg/Kg dehydration, phosphorous nutrition 0-100 mg/Kg dewater, stir, induce 80 ~ 100 days for 25 ~ 28 DEG C; Described over dry mud is loaded in watch-glass by primary sludge sample, is placed in baking oven, under the condition of 105 DEG C-108 DEG C, and drying three hours, taking-up is weighed, and continues and puts into baking oven, similarity condition process 30min, and multiple taking-up is weighed, repetition twice like this, compares three secondary data, reaches constant weight, is over dry mud.
2. Microbiological oil sludge treatment technique according to claim 1, is characterized in that biological treatment step greasy filth is more than 8 hours in the biological reactor residence time; Water-gas ratio=1 in biological reactor: 4-5, hydraulic detention time 0.5-2 hour, control temperature 10 DEG C-40 DEG C, pH6-10.
3. Microbiological oil sludge treatment technique according to claim 1, to it is characterized in that adding in biological reactor Candida lipolytica Y-57 that deposit number is CGMCC No.5790 and deposit number be the mixed-culture medium dosage of the pseudomonas putida P-101 of CGMCC No.5801 is the 0.01%-1wt% of pending greasy filth quality.
4. Microbiological oil sludge treatment technique according to claim 1, is characterized in that the deposit number added in biological reactor to be the Candida lipolytica Y-57 of CGMCC No.5790 and deposit number is that the quantity of the effective microbe of the pseudomonas putida P-101 mixed-culture medium of CGMCC No.5801 is greater than 10 11cfu/ gram.
5. Microbiological oil sludge treatment technique according to claim 1, it is characterized in that described sludge dewatering step be to biological treatment after greasy filth dewater, obtaining water ratio is 70% ~ 75%, the greasy filth being less than 2% in over dry mud oil-containing.
6. Microbiological oil sludge treatment technique according to claim 1, is characterized in that described tensio-active agent is selected from one or more of tween, sapn, rhamnolipid, alkylaryl polyglycol ether, alkyl polyglycol ether or alkylaryl sulphonate.
CN201210180830.8A 2012-06-04 2012-06-04 Microbiological oil sludge treatment process Active CN103449695B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201210180830.8A CN103449695B (en) 2012-06-04 2012-06-04 Microbiological oil sludge treatment process

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201210180830.8A CN103449695B (en) 2012-06-04 2012-06-04 Microbiological oil sludge treatment process

Publications (2)

Publication Number Publication Date
CN103449695A CN103449695A (en) 2013-12-18
CN103449695B true CN103449695B (en) 2014-12-17

Family

ID=49732597

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201210180830.8A Active CN103449695B (en) 2012-06-04 2012-06-04 Microbiological oil sludge treatment process

Country Status (1)

Country Link
CN (1) CN103449695B (en)

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103787508A (en) * 2014-01-16 2014-05-14 兰州石化职业技术学院 Application of microbial compound agent in treatment of petrochemical sewage and sludge
CN104276738B (en) * 2014-09-29 2016-06-22 西安建筑科技大学 A kind of fast and harmless biodegradation method for waxy oil mud
CN105819577A (en) * 2016-05-30 2016-08-03 青岛海之源智能技术有限公司 Method for quick environment-friendly treatment of littoral oil-spills
CN109020126B (en) * 2018-07-13 2021-09-07 山东宇尚节能环保科技有限公司 Construction process for bioremediation of oily sludge
CN113072258B (en) * 2021-04-16 2023-04-07 江苏博大环保股份有限公司 Enhanced biochemical treatment process for oilfield wastewater

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2826782B2 (en) * 1991-07-19 1998-11-18 エンザイム株式会社 Treatment of activated sludge from sewage and human waste by humus
CN101255227A (en) * 2008-04-14 2008-09-03 邵胜学 Method for synthesizing polyhydroxyalkanoates by employing oil-containing sludge
RU2394779C2 (en) * 2008-09-11 2010-07-20 Государственное учреждение Институт экологических проблем Севера Уральского отделения РАН Method for aerobic treatment of sewage sludge and active sludge
CN101935633B (en) * 2010-07-06 2011-10-19 中国科学院南京土壤研究所 Bacillus amyloliquefacien BZ6-1 strain for producing biosurfactant and application thereof in oil sludge elution

Also Published As

Publication number Publication date
CN103449695A (en) 2013-12-18

Similar Documents

Publication Publication Date Title
CN103449696B (en) Method for improving oil sludge separating and processing efficiency and bacterial strain used for method
Lee et al. Microbial flocculation, a potentially low-cost harvesting technique for marine microalgae for the production of biodiesel
CN105174476B (en) Activated sludge and microalgae coupling particle system and its structure and operation method for wastewater treatment
CN103449695B (en) Microbiological oil sludge treatment process
Ke et al. Bioremediation of oily sludge by solid complex bacterial agent with a combined two-step process
Farghaly et al. Inoculation of paperboard mill sludge versus mixed culture bacteria for hydrogen production from paperboard mill wastewater
CN102766579A (en) Yeast strain for generating surfactant and application thereof
CN111849821B (en) High-temperature-resistant kitchen waste grease degradation compound microbial inoculum and application thereof
Jiang et al. The condition optimization and mechanism of aerobic phosphorus removal by marine bacterium Shewanella sp.
CN102676424B (en) Obligate halophile for processing high-salt oily waste liquor in petroleum industry
CN104830942A (en) Biological alcohol production technique of organic sewage
CN111518715A (en) Sulfonamide antibiotic synergistic degradation bacteria and application thereof
CN110438033B (en) Grease degrading bacterium, application and grease degrading method
Yan et al. Effect of Fe (II) on nitrogen removal of anammox under organic matter inhibition
Liu et al. Characteristics for production of hydrogen and bioflocculant by Bacillus sp. XF-56 from marine intertidal sludge
CN108298701A (en) A kind of fermentation waste water processing method of low biodegradability after Anaerobic Treatment
CN105238843A (en) Microbial flocculant, preparation method and application thereof
CN102796778B (en) Method for removing kitchen grease by using calcium stearate generated through phase-split anaerase hydrolysis
CN102250776A (en) Acid-resistance heterotrophic bacterium strain Z3 used for bioleaching treatment of sludge and livestock and poultry manure
CN106865937B (en) A kind of method that red mud joint rumen fluid processing sludge promotes short chain fatty acids to generate
CN110157634B (en) Sphingomonas paucimobilis and application thereof
CN1169945C (en) Thiobacillus thiooxidans and biological eliminating method of chromium in tanning sludge
CN102766580B (en) Yeast strain for producing biosurfactant and application thereof
CN115058357A (en) Bacterial strain for biological drying of kitchen waste, screening method and application
CN105502868A (en) Harmless oil sludge treatment process

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