CN104803428B - Preparation method for coking wastewater treating agent - Google Patents

Preparation method for coking wastewater treating agent Download PDF

Info

Publication number
CN104803428B
CN104803428B CN201510247652.XA CN201510247652A CN104803428B CN 104803428 B CN104803428 B CN 104803428B CN 201510247652 A CN201510247652 A CN 201510247652A CN 104803428 B CN104803428 B CN 104803428B
Authority
CN
China
Prior art keywords
parts
temperature
stirring
stir
treating agent
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
CN201510247652.XA
Other languages
Chinese (zh)
Other versions
CN104803428A (en
Inventor
张启磊
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.)
Individual
Original Assignee
Individual
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 Individual filed Critical Individual
Priority to CN201510247652.XA priority Critical patent/CN104803428B/en
Publication of CN104803428A publication Critical patent/CN104803428A/en
Application granted granted Critical
Publication of CN104803428B publication Critical patent/CN104803428B/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Landscapes

  • Separation Of Suspended Particles By Flocculating Agents (AREA)
  • Treatment Of Sludge (AREA)

Abstract

The invention discloses a preparation method for a coking wastewater treating agent. The preparation method comprises the following steps: adding concentrated sulfuric acid and sodium silicate into water to uniformly mix in a stirring process, continuously adding calcium oxide, sodium ferrate, polyaluminum chloride and polyferric sulfate to continuously stir, and cooling to obtain pre-prepared materials; putting the pre-prepared materials into a reaction kettle, rising the temperature of the reaction kettle to stir, adding anionic polyacrylamide,an aluminum salt and a ferric salt to stir, and continuously rising the temperature until reacting completely; sequentially adding xanthan gum, sodium alginate, gelatin, modified starch, modified fibers, lignin and gum into the obtained materails to uniformly stir at a normal temperature, and rising the temperature to continuously stir; sequentially adding polyaluminum silicate chloride and boric acid into the obtained materials to stir, rising the temperature, adding potassium permanganate and isooctane to stir, and cooling to the room temperature to obtain the coking wastewater treating agent. The preparation method disclosed by the invention is simple, the effect of treating the coking wastewater by the coking wastewater treating agent is good, and emission standards can be reached without secondary pollution.

Description

A kind of preparation method of coking sewage treating agent
Technical field
A kind of the present invention relates to sewage-treating agent technical field, more particularly to preparation method of coking sewage treating agent.
Background technology
With the continuous improvement of people's living standard, environmental protection has become people's question of common concern, industrial wastewater Particularly it is important pollution sources for causing environmental pollution to the discharge of coking water, and country also takes compulsive measures, To not meeting the coking producer of discharge standard, the compulsory measure such as pass taken, stopped, turned, being thus badly in need of a kind of effective coking Water treatment agent.At present for municipal sewage is particularly coke-oven plant's sewage water treatment method of Cities with Coal Mines, the protochloride for generally adopting Iron or aluminum sulfate liquid are processed, and treatment effect is poor, some leading indicators, such as chemical oxygen consumption (COC)(COD), suspension(SS) Removal rate it is relatively low, be extremely difficult to specify discharge standard, the consumption of these inorganic agents is generally larger in addition, easily produces more Reluctant residue, easily causes secondary pollution.
The content of the invention
The present invention proposes a kind of preparation method of coking sewage treating agent, and method is simple, and sewage-treating agent processes coking Sewage effect is good, can reach discharge standard and will not cause secondary pollution.
A kind of preparation method of coking sewage treating agent proposed by the present invention, comprises the steps:
S1,30-50 part water is weighed by weight, add 2-4 part concentrated sulfuric acids, the mixing of 1-4 parts sodium metasilicate equal in whipping process It is even, continuously add 20-40 part calcium oxide, 10-15 part Na2Fe04s, 2-8 part aluminium polychlorides, 10-13 part bodied ferric sulfates and enter Row stirring, mixing time is 50-60min, is warming up to 60-65 DEG C and continues stirring 1-3h, and cooling obtains prefabricated material;
Be put in reactor in S2, the prefabricated material for obtaining S1, temperature of reaction kettle is raised to 40-50 DEG C of stirring 20-40min Afterwards, 1.5-1.9 part PAMAs, 0.1-0.2 part aluminium salts, 0.1-0.2 part molysite stirring reactions 10-15min is added, Continue liter high-temperature complete to fully reaction to 55-60 DEG C;
1-2 part xanthans, 1-2 part algins, 0.3-0.7 part gelatin, 1- is sequentially added in S3, the material obtained to S2 1.5 parts of modified starches, 1-1.5 part modified fibres, 0.6-1 part lignin, 0.6-1 parts natural gum stirring at normal temperature are uniform, by temperature liter Up to 40-50 DEG C is continued stirring 20-40min;
Sequentially add 1-4 part polysilicate aluminum chlorides, 1-3 part boric acid persistently to stir at 30-45 DEG C in S4, the material obtained to S3 3-5h, is warming up to 60-85 DEG C, adds 1-1.5 part potassium permanganate, 1-2 parts isooctane stirring 3-5h, is cooled to room temperature and obtains coking Sewage-treating agent.
Preferably, in S1,40-45 part water is weighed by weight, add 2.5-3 part concentrated sulfuric acids, 2-3 parts in whipping process Sodium metasilicate is well mixed, and continuously adds 30-35 part calcium oxide, 12-14 part Na2Fe04s, 3-5 part aluminium polychlorides, 11-12 parts Bodied ferric sulfate is stirred, and mixing time is 55-58min, is warming up to 62-64 DEG C and continues stirring 1.5-2.5h, and cooling is obtained Prefabricated material.
Preferably, in S1,42 parts of water are weighed by weight, add 2.8 parts of concentrated sulfuric acids, 2.5 parts of silicic acid in whipping process Sodium is well mixed, and continuously adding 32 parts of calcium oxide, 13 parts of Na2Fe04s, 4 parts of aluminium polychlorides, 11.5 parts of bodied ferric sulfates is carried out Stirring, mixing time is 56min, is warming up to 63 DEG C and continues stirring 2h, and cooling obtains prefabricated material.
Preferably, in S2, be put in reactor in the prefabricated material that S1 is obtained, temperature of reaction kettle is raised to 45-48 DEG C After stirring 30-36min, 1.6-1.8 part PAMAs, 0.14-0.18 part aluminium salts, 0.15-0.19 part molysite is added Stirring reaction 12-14min, continues liter high-temperature complete to fully reaction to 56-58 DEG C.
Preferably, in S2, it is put in reactor in the prefabricated material that S1 is obtained, raises temperature of reaction kettle and stir to 46 DEG C After 35min, 1.7 parts of PAMAs, 0.16 part of aluminium salt, 0.18 part of molysite stirring reaction 13min are added, continue to raise Temperature is complete to fully reaction to 57 DEG C.
Preferably, in S3,1.2-1.5 part xanthans, 1.5-1.8 part brown algas in the material obtained to S2, are sequentially added Glue, 0.4-0.6 part gelatin, 1.2-1.4 part modified starches, 1.1-1.3 part modified fibres, 0.6-0.8 part lignin, 0.8-0.96 The gummy stirring at normal temperature of part is uniform, temperature is increased to 42-46 DEG C and continues stirring 30-35min.
Preferably, in S3, sequentially add in the material obtained to S2 1.3 parts of xanthans, 1.6 parts of algins, 0.5 part it is bright Glue, 1.35 parts of modified starches, 1.25 parts of modified fibres, 0.75 part of lignin, 0.95 part of gummy stirring at normal temperature are uniform, by temperature liter Up to 45 DEG C are continued stirring 32min.
Preferably, in S4,2-3 part polysilicate aluminum chlorides, 2-2.5 part boric acid is sequentially added in the material obtained to S3 and is existed 40-42 DEG C is persistently stirred 4-4.5h, is warming up to 70-76 DEG C, adds 1.2-1.4 part potassium permanganate, 1.52-1.8 part isooctane to stir 4-5h is mixed, room temperature is cooled to and is obtained coking sewage treating agent.
Preferably, in S4,2.5 parts of polysilicate aluminum chlorides, 2.3 parts of boric acid are sequentially added in the material obtained to S3 at 41 DEG C 4.5h is persistently stirred, 73 DEG C are warming up to, is added 1.3 parts of potassium permanganate, 1.7 parts of isooctane to stir 4.5h, is cooled to room temperature and obtains Coking sewage treating agent.
This coking sewage treating agent composition of the present invention is simple, and it is easy to prepare, good for processing coked waste water effect, not only may be used To reach emission request, it is possible to by sewage disposal into purified water, reused with doing recirculated water, saved and used water;By inciting somebody to action It is of the invention to carry out Experimental comparison, Jing test of many times with similar sewage-treating agent, sewage-treating agent press dosage respectively by 500, 700th, 1000, the optimum results of 2000mg/L carry out long run test, verify that its effect is more stable, to coking sewage chemical oxygen consumption Amount, suspension removal rate it is higher, sewage drainage standard can be reached, and secondary pollution will not be produced.The present invention is to coking chemical waste water Middle and high concentration petroleum-type, suspension and coked waste water have the effect of uniqueness, and waste water treating agent by little, the technique using temperature limiting It is stable, low cost.
Description of the drawings
Fig. 1 is a kind of preparation technology flow chart of coking sewage treating agent proposed by the present invention.
Specific embodiment
As shown in figure 1, Fig. 1 is a kind of preparation technology flow chart of coking sewage treating agent proposed by the present invention.
Embodiment 1
With reference to Fig. 1, a kind of preparation method of coking sewage treating agent comprises the steps:
S1,30 parts of water are weighed by weight, add 4 parts of concentrated sulfuric acids, 1 part of sodium metasilicate to be well mixed, continue in whipping process 40 parts of calcium oxide, 10 parts of Na2Fe04s, 8 parts of aluminium polychlorides, 10 parts of bodied ferric sulfates are added to be stirred, mixing time is 60min, is warming up to 60 DEG C and continues stirring 3h, and cooling obtains prefabricated material;
Be put in reactor in S2, the prefabricated material for obtaining S1, temperature of reaction kettle is raised to 40 DEG C of stirring 40min, plus Enter 1.5 parts of PAMAs, 0.2 part of aluminium salt, 0.1 part of molysite stirring reaction 15min, continue to rise high-temperature to 55 DEG C extremely Fully reaction is complete;
Sequentially add in S3, the material obtained to S2 2 parts of xanthans, 1 part of algin, 0.7 part of gelatin, 1 portion of modified starch, 1.5 parts of modified fibres, 0.6 part of lignin, 1 part of gummy stirring at normal temperature are uniform, temperature is increased to 40 DEG C and continues stirring 40min;
1 part of polysilicate aluminum chloride, 3 parts of boric acid is sequentially added in S4, the material obtained to S3 and persistently stirs 5h at 30 DEG C, heat up To 60 DEG C, add 1.5 parts of potassium permanganate, 1 part of isooctane to stir 5h, be cooled to room temperature and obtain coking sewage treating agent.
Embodiment 2
A kind of preparation method of coking sewage treating agent, comprises the steps:
S1,50 parts of water are weighed by weight, add 2 parts of concentrated sulfuric acids, 4 parts of sodium metasilicate to be well mixed, continue in whipping process 20 parts of calcium oxide, 15 parts of Na2Fe04s, 2 parts of aluminium polychlorides, 13 parts of bodied ferric sulfates are added to be stirred, mixing time is 50min, is warming up to 65 DEG C and continues stirring 1h, and cooling obtains prefabricated material;
Be put in reactor in S2, the prefabricated material for obtaining S1, temperature of reaction kettle is raised to 50 DEG C of stirring 20min, plus Enter 1.9 parts of PAMAs, 0.1 part of aluminium salt, 0.2 part of molysite stirring reaction 10min, continue to rise high-temperature to 60 DEG C extremely Fully reaction is complete;
1 part of xanthans, 2 parts of algins, 0.3 part of gelatin, 1.5 parts of modified shallow lakes are sequentially added in S3, the material obtained to S2 Powder, 1 part of modified fibre, 1 part of lignin, 0.6 part of gummy stirring at normal temperature are uniform, temperature is increased to 50 DEG C and continues stirring 20min;
4 parts of polysilicate aluminum chlorides, 1 part of boric acid are sequentially added in S4, the material obtained to S3 and persistently stirs 3h at 45 DEG C, heat up To 85 DEG C, add 1 part of potassium permanganate, 2 parts of isooctane to stir 3h, be cooled to room temperature and obtain coking sewage treating agent.
Embodiment 5
A kind of preparation method of coking sewage treating agent, comprises the steps:
S1,42 parts of water are weighed by weight, add 2.8 parts of concentrated sulfuric acids, 2.5 parts of sodium metasilicate to be well mixed in whipping process, Continuously add 32 parts of calcium oxide, 13 parts of Na2Fe04s, 4 parts of aluminium polychlorides, 11.5 parts of bodied ferric sulfates to be stirred, during stirring Between be 56min, be warming up to 63 DEG C continue stirring 2h, cooling obtain prefabricated material;
Be put in reactor in S2, the prefabricated material for obtaining S1, temperature of reaction kettle is raised to 46 DEG C of stirring 35min, plus Enter 1.7 parts of PAMAs, 0.16 part of aluminium salt, 0.18 part of molysite stirring reaction 13min, continue to rise high-temperature to 57 DEG C It is complete to fully reaction;
Sequentially add in S3, the material obtained to S2 1.3 parts of xanthans, 1.6 parts of algins, 0.5 part of gelatin, 1.35 parts change Property starch, 1.25 parts of modified fibres, 0.75 part of lignin, 0.95 part of gummy stirring at normal temperature it is uniform, by temperature be increased to 45 DEG C after Continuous stirring 32min;
Sequentially add 2.5 parts of polysilicate aluminum chlorides, 2.3 parts of boric acid persistently to stir at 41 DEG C in S4, the material obtained to S3 4.5h, is warming up to 73 DEG C, adds 1.3 parts of potassium permanganate, 1.7 parts of isooctane to stir 4.5h, is cooled to room temperature and obtains coked waste water Inorganic agent.
The above, the only present invention preferably specific embodiment, but protection scope of the present invention is not limited thereto, Any those familiar with the art the invention discloses technical scope in, technology according to the present invention scheme and its Inventive concept equivalent or change in addition, should all be included within the scope of the present invention.

Claims (3)

1. a kind of preparation method of coking sewage treating agent, it is characterised in that comprise the steps:
S1, weigh 30 parts of water by weight, in whipping process, add 4 parts of concentrated sulfuric acids, 1 part of sodium metasilicate to be well mixed, continue plus Enter 40 parts of calcium oxide, 10 parts of Na2Fe04s, 8 parts of aluminium polychlorides, 10 parts of bodied ferric sulfates to be stirred, mixing time is 60min, is warming up to 60 DEG C and continues stirring 3h, and cooling obtains prefabricated material;
Be put in reactor in S2, the prefabricated material for obtaining S1, temperature of reaction kettle is raised to 40 DEG C of stirring 40min, plus Enter 1.5 parts of PAMAs, 0.2 part of aluminium salt, 0.1 part of molysite stirring reaction 15min, continue to rise high-temperature extremely 55 DEG C complete to fully reaction;
Sequentially add in S3, the material obtained to S2 2 parts of xanthans, 1 part of algin, 0.7 part of gelatin, 1 portion of modified starch, 1.5 Part modified fibre, 0.6 part of lignin, 1 part of gummy stirring at normal temperature are uniform, temperature is increased to 40 DEG C and continues stirring 40min;
1 part of polysilicate aluminum chloride, 3 parts of boric acid is sequentially added in S4, the material obtained to S3 and persistently stirs 5h at 30 DEG C, be warming up to 60 DEG C, add 1.5 parts of potassium permanganate, 1 part of isooctane to stir 5h, be cooled to room temperature and obtain coking sewage treating agent.
2. a kind of preparation method of coking sewage treating agent, it is characterised in that comprise the steps:
S1,50 parts of water are weighed by weight, add 2 parts of concentrated sulfuric acids, 4 parts of sodium metasilicate to be well mixed, continuously add in whipping process 20 parts of calcium oxide, 15 parts of Na2Fe04s, 2 parts of aluminium polychlorides, 13 parts of bodied ferric sulfates are stirred, and mixing time is 50min, It is warming up to 65 DEG C and continues stirring 1h, cooling obtains prefabricated material;
Be put in reactor in S2, the prefabricated material for obtaining S1, temperature of reaction kettle is raised to 50 DEG C of stirring 20min, plus Enter 1.9 parts of PAMAs, 0.1 part of aluminium salt, 0.2 part of molysite stirring reaction 10min, continue to rise high-temperature to 60 It is DEG C complete to fully reaction;
Sequentially add in S3, the material obtained to S2 1 part of xanthans, 2 parts of algins, 0.3 part of gelatin, 1.5 portions of modified starches, 1 Part modified fibre, 1 part of lignin, 0.6 part of gummy stirring at normal temperature are uniform, temperature is increased to 50 DEG C and continues stirring 20min;
4 parts of polysilicate aluminum chlorides, 1 part of boric acid are sequentially added in S4, the material obtained to S3 and persistently stirs 3h at 45 DEG C, be warming up to 85 DEG C, add 1 part of potassium permanganate, 2 parts of isooctane to stir 3h, be cooled to room temperature and obtain coking sewage treating agent.
3. a kind of preparation method of coking sewage treating agent, comprises the steps:
S1,42 parts of water are weighed by weight, add 2.8 parts of concentrated sulfuric acids, 2.5 parts of sodium metasilicate to be well mixed, continue in whipping process Add 32 parts of calcium oxide, 13 parts of Na2Fe04s, 4 parts of aluminium polychlorides, 11.5 parts of bodied ferric sulfates to be stirred, stir Time is 56min, is warming up to 63 DEG C and continues stirring 2h, and cooling obtains prefabricated material;
Be put in reactor in S2, the prefabricated material for obtaining S1, temperature of reaction kettle is raised to 46 DEG C of stirring 35min, plus Enter 1.7 parts of PAMAs, 0.16 part of aluminium salt, 0.18 part of molysite stirring reaction 13min, continue to rise high-temperature extremely 57 DEG C complete to fully reaction;
1.3 parts of xanthans, 1.6 parts of algins, 0.5 part of gelatin, 1.35 parts of modified shallow lakes are sequentially added in S3, the material obtained to S2 Powder, 1.25 parts of modified fibres, 0.75 part of lignin, 0.95 part of gummy stirring at normal temperature are uniform, temperature is increased to 45 DEG C and continues to stir Mix 32min;
2.5 parts of polysilicate aluminum chlorides, 2.3 parts of boric acid are sequentially added in S4, the material obtained to S3 and persistently stirs 4.5h at 41 DEG C, rise Temperature is added 1.3 parts of potassium permanganate, 1.7 parts of isooctane to stir 4.5h, is cooled to room temperature and obtains at coked waste water to 73 DEG C Reason agent.
CN201510247652.XA 2015-05-15 2015-05-15 Preparation method for coking wastewater treating agent Expired - Fee Related CN104803428B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201510247652.XA CN104803428B (en) 2015-05-15 2015-05-15 Preparation method for coking wastewater treating agent

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201510247652.XA CN104803428B (en) 2015-05-15 2015-05-15 Preparation method for coking wastewater treating agent

Publications (2)

Publication Number Publication Date
CN104803428A CN104803428A (en) 2015-07-29
CN104803428B true CN104803428B (en) 2017-03-22

Family

ID=53688700

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201510247652.XA Expired - Fee Related CN104803428B (en) 2015-05-15 2015-05-15 Preparation method for coking wastewater treating agent

Country Status (1)

Country Link
CN (1) CN104803428B (en)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105692723A (en) * 2016-01-22 2016-06-22 南通海陵环境检测有限公司 Dyeing waste water treating agent and preparing method thereof
CN106629888A (en) * 2016-11-23 2017-05-10 郑州源冉生物技术有限公司 Efficient sewage treatment agent based on xanthan gum and preparation method of efficient sewage treatment agent
CN110606537B (en) * 2019-09-09 2021-10-26 武汉纺织大学 Novel method for treating waste water glass sand wet regeneration sewage and application thereof

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104445562A (en) * 2014-11-05 2015-03-25 南华大学 Preparation method of coking wastewater treating agent

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6020074B2 (en) * 1979-04-11 1985-05-20 日本化学工業株式会社 How to treat grout wastewater
CN100386267C (en) * 2005-10-28 2008-05-07 上海工程技术大学 High efficiency composite flocculant, its preparation method and application
CN101503239B (en) * 2009-03-23 2012-05-30 中国科学院生态环境研究中心 Multicomponent composite flocculating setting agent and use in arsenic contamination water treatment
CN101519239B (en) * 2009-04-07 2011-02-02 甘肃宇辰化工器材装备有限公司 Coking wastewater treatment agent and use method thereof
CN102674519A (en) * 2012-06-13 2012-09-19 何斌 Preparation method of flocculant for sewage treatment

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104445562A (en) * 2014-11-05 2015-03-25 南华大学 Preparation method of coking wastewater treating agent

Also Published As

Publication number Publication date
CN104803428A (en) 2015-07-29

Similar Documents

Publication Publication Date Title
CN102060363B (en) Method for coagulating coal-bed gas produced water
CN104803428B (en) Preparation method for coking wastewater treating agent
CN106904807A (en) A kind of method that phosphorus is reclaimed from dewatered sludge
CN105948210A (en) Method for producing polymeric ferric sulfate from raw materials industrial waste acid and scrap iron
CN103145196A (en) Method for producing polymerization ferric chloride by utilizing waste hydrochloric acid and waste ferrous mud
CN102838197A (en) Method for preparing novel composite flocculant PSAFS (poly-silicate aluminum ferrous sulfate)
CN105174829A (en) Good thermal insulation effect silt curing agent for silt bricks
CN101851054B (en) Sludge dewatering conditioner, and preparation method and application thereof
CN103833116B (en) A kind of production method and application that utilizes waste hydrochloric acid, aluminium-containing sludge to prepare defluorinating agent
CN109250762A (en) Method for preparing poly-ferric chloride by using steel hydrochloric acid pickling wastewater
CN104761002B (en) A preparing process of energy-saving environmental-friendly type modified polymeric ferric sulfate
CN104817118A (en) Simple and quick method for preparing polyferric chloride
CN104986805A (en) Production method for polyferric chloride sulfate
CN101955251A (en) Coking sewage treating agent and preparation method thereof
CN105271435B (en) Seamless steel pipe pickle liquor prepares the production technology of polyaluminium ferric flocculant
CN104495809A (en) Purification method of microcrystalline graphite
CN106698890A (en) Method for preparing sludge treating agent through waste acid containing ferrous ions
CN106277068A (en) Galvanizing by dipping waste hydrochloric acid resource reuse method
CN108928954A (en) Boiler water treatment technology based on the water-saving preparation of boiler energy-saving
CN1552639A (en) Method for comprehensive treating waste emulsion liquid and chromium containing waste water by metallurgy chemical industry technology
CN104591249A (en) Preparation method for polyaluminum chloride
CN108455907A (en) It is a kind of using industrial residue as autoclaved lime-sand brick of raw material and preparation method thereof
CN108675418A (en) A kind of polysilicate aluminium ferric flocculant and preparation method thereof
CN103435107B (en) Method for producing sludge conditioner by recycling wastes
CN104250036B (en) Utilize dephosphorization composite flocculation agent and preparation method and using method that red mud makes

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
EXSB Decision made by sipo to initiate substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant
CF01 Termination of patent right due to non-payment of annual fee
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20170322

Termination date: 20180515