CN204232271U - Nicotine sulphate anti-emulsification device - Google Patents
Nicotine sulphate anti-emulsification device Download PDFInfo
- Publication number
- CN204232271U CN204232271U CN201420500001.8U CN201420500001U CN204232271U CN 204232271 U CN204232271 U CN 204232271U CN 201420500001 U CN201420500001 U CN 201420500001U CN 204232271 U CN204232271 U CN 204232271U
- Authority
- CN
- China
- Prior art keywords
- emulsification device
- shower
- inlet pipe
- orifice plate
- pipe
- 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
Links
- IECQULMJVNSKDB-RCWTXCDDSA-N 3-[(2s)-1-methylpyrrolidin-2-yl]pyridine;sulfuric acid Chemical compound OS(O)(=O)=O.CN1CCC[C@H]1C1=CC=CN=C1.CN1CCC[C@H]1C1=CC=CN=C1 IECQULMJVNSKDB-RCWTXCDDSA-N 0.000 title claims abstract description 23
- 238000004945 emulsification Methods 0.000 title claims abstract description 22
- 239000000919 ceramic Substances 0.000 claims abstract description 23
- 238000012856 packing Methods 0.000 claims abstract description 17
- 239000007921 spray Substances 0.000 claims abstract description 13
- 238000011084 recovery Methods 0.000 claims abstract description 9
- 239000002904 solvent Substances 0.000 claims abstract description 9
- 238000004140 cleaning Methods 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 238000005406 washing Methods 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 5
- 239000000523 sample Substances 0.000 claims description 4
- 241000208125 Nicotiana Species 0.000 abstract description 16
- 235000002637 Nicotiana tabacum Nutrition 0.000 abstract description 15
- 238000000605 extraction Methods 0.000 abstract description 10
- 239000000839 emulsion Substances 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 238000012545 processing Methods 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 18
- 239000010410 layer Substances 0.000 description 16
- 239000000243 solution Substances 0.000 description 15
- 239000007788 liquid Substances 0.000 description 8
- SNICXCGAKADSCV-UHFFFAOYSA-N nicotine Natural products CN1CCCC1C1=CC=CN=C1 SNICXCGAKADSCV-UHFFFAOYSA-N 0.000 description 8
- SNICXCGAKADSCV-JTQLQIEISA-N (-)-Nicotine Chemical compound CN1CCC[C@H]1C1=CC=CN=C1 SNICXCGAKADSCV-JTQLQIEISA-N 0.000 description 7
- 229960002715 nicotine Drugs 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- 238000000034 method Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 235000019504 cigarettes Nutrition 0.000 description 3
- 230000000149 penetrating effect Effects 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 2
- 229930013930 alkaloid Natural products 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 239000003995 emulsifying agent Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 235000013311 vegetables Nutrition 0.000 description 2
- 208000019901 Anxiety disease Diseases 0.000 description 1
- 241001124076 Aphididae Species 0.000 description 1
- 208000006820 Arthralgia Diseases 0.000 description 1
- BSYNRYMUTXBXSQ-UHFFFAOYSA-N Aspirin Chemical compound CC(=O)OC1=CC=CC=C1C(O)=O BSYNRYMUTXBXSQ-UHFFFAOYSA-N 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- 208000007101 Muscle Cramp Diseases 0.000 description 1
- 229960001138 acetylsalicylic acid Drugs 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 150000003797 alkaloid derivatives Chemical class 0.000 description 1
- 230000036506 anxiety Effects 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 210000004556 brain Anatomy 0.000 description 1
- 210000003169 central nervous system Anatomy 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 230000001713 cholinergic effect Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000012377 drug delivery Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000003317 industrial substance Substances 0.000 description 1
- 239000002917 insecticide Substances 0.000 description 1
- 238000000622 liquid--liquid extraction Methods 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 1
- -1 nicotine salt compound Chemical class 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 239000012044 organic layer Substances 0.000 description 1
- 230000003204 osmotic effect Effects 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 230000000144 pharmacologic effect Effects 0.000 description 1
- 239000002574 poison Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000010902 straw Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Landscapes
- Extraction Or Liquid Replacement (AREA)
Abstract
The utility model belongs to tobacco processing equipment field, is specifically related to a kind of nicotine sulphate anti-emulsification device.This device comprises cylindrical shell, and this cylindrical shell top is provided with solvent recovery pipe, and bottom is provided with solution inlet pipe and cleaning delivery pipe; Described inner barrel central authorities are also provided with the orifice plate of densely covered aperture; Random packing layer is provided with below this orifice plate; This random packing layer is filled by several ceramic Pall rings and is formed; Described solution inlet pipe is connected with shower, and this shower top seal, tube wall has and organizes spray apertures more.The nicotine sulphate anti-emulsification device that the utility model provides, eliminates the generation of emulsion, and extraction efficiency improves more than 26% simultaneously, greatly reduces the environmental protection treatment cost in emulsion later stage, improves product quality and production efficiency.
Description
Technical field
The utility model belongs to tobacco processing equipment field, is specifically related to a kind of nicotine sulphate anti-emulsification device.
Background technology
As tobacco leaf production big country, the annual yield of tobacco 450-500 of China ten thousand tons, wherein about has the leftover bits and pieces such as the tobacco leaf of nearly 25%, offal to go out of use, can not be used for production of cigarettes.If Yunnan is as the large province of tobacco, about have 30%-35% to belong in annual yield of flue-cured tobacco cannot to carry out Cigarette processing low grade or etc. outer level tobacco leaf, fail to obtain Appropriate application, each cigarette enterprise also contains a large amount of offals, also have the tobacco wastes such as a large amount of upper tobacco leaf, fireworks and tabacco straw, estimate the quantity more than about 600,000 tons of Yunnan tobacco discarded object.If carry out " resource " to these tobacco wastes to utilize, not only can obtain natural industrial chemicals, overcome difficulties for enterprise shakes off poverty, tap the potential and upgrade technologically and the opportunity of sustainable development is provided, also can alleviate the possibility that soil texture that tobacco waste brings changes, avoid wherein harmful components to the pollution of underground water.
Containing multiple alkaloid in tobacco, what obtained qualification just has kind more than 40, and wherein maximum with nicotine content, account for 95% of nicotiana alkaloids, nicotine accounts for the 0.5-6% of tobacco dry weight.Nicotine all has a wide range of applications in field of medicaments and chemical field.Pharmacological research shows: nicotine can be combined with the nicotine cholinergic of periphery and central nervous system, multiple effect is had to brain, can multiple neurochemistry passage be activated, can cause improving awakening, notice and reactivity to the effect of nervous centralis, reduce anxiety and nervous reaction.Some pharmaceutically acceptable nicotine salt compound is effective in cure to some disease, as by nicotine tartrate local drug delivery, can treat the muscle cramp and arthralgia that can not alleviate with massage or aspirin.In addition nicotine sulphate is a kind of high-efficiency low-toxicity, and without the resistance to the action of a drug, noresidue, does not poison, the very potential vegetable insecticide of contaminated land, is " environment friendly agricultural ", for control cotton and vegetable aphid effect excellent.
What generally adopt at present is in sulfuric acid and reextraction nicotine, in container, add sulfuric acid and extract carry out stirring and complete extraction, but facing maximum problem is exactly that emulsion in sulfuric acid solution reextraction process is serious, causes percent defective high, and cannot consecutive production.Main cause is when organic solvent exposure is to sulfuric acid, is that agitating mode or counter-current extraction mode all can produce the reasons such as the bubble that impurity in turbulent phenomenon, particularly Liquid-liquid Extraction Processes and convection current produce and cause emulsification even more serious.The domestic technical scheme also effectively not solving this difficult problem at present.
Utility model content
The utility model, for the deficiencies in the prior art, provides a kind of nicotine sulphate anti-emulsification device, its compact conformation, reasonable in design, eliminates the generation of emulsion, improves production efficiency.
The technical solution of the utility model is achieved in that a kind of nicotine sulphate anti-emulsification device cylindrical shell, and this cylindrical shell top is provided with solvent recovery pipe, and bottom is provided with solution inlet pipe and cleaning delivery pipe; Described inner barrel central authorities are also provided with the orifice plate of densely covered aperture, are provided with random packing layer below this orifice plate, and this random packing layer is filled by several ceramic Pall rings and formed; Described solution inlet pipe is connected with shower, and this shower top seal, tube wall has and organizes spray apertures more.
Further, described ceramic Pall ring is that perforate is circular, and this ceramic Pall ring sidewall surrounding is provided with the fenestra staggered on the contrary upper and lower two-layer position, and every layer of described fenestra is provided with 5 by the ligule of interior dactylogryposis to the ring heart.
Preferably, be provided with filter washing water inlet pipe between described solution inlet pipe and orifice plate, this filter washing water inlet pipe mouth of pipe peak is higher than random packing layer.
Preferably, described ceramic Pall ring diameter is 2 ~ 3cm, and this ceramic Pall ring height and equal diameters, thickness is 3mm.
Preferably, the length 100 ~ 180cm of described shower, diameter 50mm.
Preferably, the spray apertures diameter 8mm on described shower, this spray apertures is distributed on the tube wall surrounding of described shower.
Preferably, described cylindrical shell top is also provided with blast pipe, is also provided with probe tube above orifice plate.
Preferably, described solvent recovery pipe, solution inlet pipe, shower 8, orifice plate and cleaning delivery pipe are made up of PVC material.
The utility model solves the defect existed in background technology, and the utility model has beneficial effect and is:
The nicotine sulphate anti-emulsification device that the utility model provides, adopts radial jet and loose heap to carry out secondary buffer and is formed without pressure reduction uniformly penetrating, eliminate the generation of emulsion.Extraction efficiency improves more than 26% simultaneously, greatly reduces the environmental protection treatment cost in emulsion later stage, improves product quality and production efficiency.
Accompanying drawing explanation
Fig. 1 is the structural representation of nicotine sulphate anti-emulsification device;
Fig. 2 is the top view of Fig. 1 nicotine sulphate anti-emulsification device;
Fig. 3 is the perspective view of ceramic Pall ring;
In figure: 1-casing, 2-orifice plate, 3-steam vent, 4-solvent recovery pipe, 5-probe tube, 6-random packing layer, 7-filter washing water inlet is managed, 8-shower, 9-solution inlet pipe, and 10-cleans delivery pipe, 11-pottery Pall ring, 12-fenestra, 13-ligule.
Detailed description of the invention
Below in conjunction with the accompanying drawing in the utility model embodiment, be clearly and completely described the technical scheme in the utility model embodiment, obviously, described embodiment is only the utility model part embodiment, instead of whole embodiments.Based on the embodiment in the utility model, those of ordinary skill in the art are not making the every other embodiment obtained under creative work prerequisite, all belong to the scope of the utility model protection.
A kind of nicotine sulphate anti-emulsification device as depicted in figs. 1 and 2, comprises cylindrical tube 1, and this cylindrical shell 1 top is provided with solvent recovery pipe 4, and bottom is provided with solution inlet pipe 9 and cleaning delivery pipe 10; Inner barrel central authorities are also provided with the orifice plate 2 of densely covered aperture; Random packing layer 6 is provided with below orifice plate 2; This random packing layer 6 is filled by several ceramic Pall rings and is formed; Solution inlet pipe 9 is connected with shower 8, this shower 9 top seal, tube wall surrounding has organizes spray apertures more.As shown in Figure 3, ceramic Pall ring 11 is that perforate is circular, and this ceramic Pall ring 11 sidewall surrounding is provided with the fenestra 12 staggered on the contrary upper and lower two-layer position, and every layer of fenestra is provided with 5 by the ligule 13 of interior dactylogryposis to the ring heart.Pottery Pall ring 11 diameter is 2 ~ 3cm, and this ceramic Pall ring 11 height and equal diameters, thickness is 3mm.Pottery Pall ring 11 perforated area accounts for greatly about 30% of the ceramic Pall ring ring wall gross area, and ceramic Pall ring 11 makes the gas in this emulsifier unit and liquid from the comfortable process of fenestra, can improve gas-liquid and scatter, apply plentifully the interior appearance of ring.Pottery Pall ring 11 also has excellent acidproof resistance to, and various inorganic acids, organic acid and the organic solvent of ability except hydrofluoric acid except corrodes.The preferred 2.5cm of pottery Pall ring 11 diameter, if diameter is less than 2cm, then cylinder can through dividing plate 2, impact extraction; Diameter is greater than 3cm, then because volume is excessive, the gap between ceramic Pall ring 11 is just large, and random packing layer is comparatively loose, affects the osmotic effect of extract.In the present embodiment, the accumulation number 79000/M of ceramic Pall ring 11 in nicotine sulphate emulsifier unit
3, voidage 0.73, weight accumulation 520kg/M
3.Be provided with filter washing water inlet pipe 7 between solution inlet pipe 9 and orifice plate 2, this filter washing water inlet pipe 7 mouth of pipe peak is higher than random packing layer 6.The diameter 50mm of shower 8, the preferred 150cm of length, shower 8 be shorter in length than 100cm, then spraying effect is poor, reduce extraction efficiency; Length more than 180cm, then reduces the intensity of pipe, causes spray to rock, affects effect of extracting.Spray apertures diameter 8mm on shower 8.Cylindrical shell 1 top is also provided with blast pipe 3, is also provided with probe tube 5 above orifice plate 2.Solvent recovery pipe 4, shower 8, solution inlet pipe 9, orifice plate 2 and cleaning delivery pipe 10 are made up of PVC material.PVC has low flammability, high strength, resistance to climate variability and excellent geometrical stability.PVC has very strong resistance to oxidant, reducing agent and strong acid, is highly suitable for the manufactured materials of the pipeline of this device.
Utility model works principle is: according to sulfuric acid and extract proportion characteristic, heavy sulfuric acid extractant is as static phase, and the little organic extract liquid of proportion is as mobile phase, extract slowly upwards penetrates sulfuric acid solution from cylindrical shell bottom adverse current and completes extraction overall process.Take the spray apertures that shower 8 tube wall has, extract radially surrounding jet flow and going out, the axial compressive force decreasing traditional extract liquid is upwards impacted; Random packing layer 6 is set and carries out secondary buffer formation without pressure reduction uniformly penetrating, eliminate the generation of emulsion completely.
The course of work of the present utility model is: first open solution inlet pipe 9, piles the dilution heat of sulfuric acid of cylindrical shell 1, then puts into the nicotine extract being mixed with normal hexane from solution inlet pipe 9.Extract is by shower 8, and due to shower 8 top seal, extract is radial direction evenly ejection from the spray apertures tube wall to surrounding, and direct axially the ejection upward of traditional extract liquid is compared, and hydraulic shock power reduces a lot; Secondly the random packing layer 6 arranged below orifice plate 2, this random packing layer 6 is filled by some ceramic Pall rings 11 and is formed, this ceramic Pall ring diameter 2.5cm.When extract sprays, the dispersed liquid mobilization force of ceramic Pall ring 11 meeting of dense distribution, improves liquid dissemination, is formed without pressure reduction uniformly penetrating; Again also be provided with orifice plate 2 in the middle of cylindrical shell, orifice plate 2 is made up of PVC material, be densely covered with the aperture of diameter 2cm above, this orifice plate 2 is except separating random packing layer 6, also has cushioning effect, the extract of flowing is subject to the obstruct of orifice plate, again slows down the mobilization force of extract, is that extraction process is more evenly mild.Extract enters from lower end toward upper end continuously and evenly penetrates sulfuric acid liquid, when reaching cylindrical shell 1 top, automatically overflows and reclaims, namely obtain nicotine sulphate from solvent recovery pipe 4.Terminate when pH value reaches 6-6.5 extraction process.Adopt this nicotine sulphate anti-emulsification device, layering, than faster obvious, be easy to aqueous phase to be separated with organic layer, avoid the generation of emulsification.In addition be provided with filter washing water inlet pipe 7 between solution inlet pipe 9 and orifice plate 2, after production stops, from this filter washing water inlet pipe 7 by the residue after the extraction in buck and clean water cylindrical shell 1, finally can discharge from the cleaning delivery pipe 10 of cylinder body bottom.
The foregoing is only preferred embodiment of the present utility model; not in order to limit the utility model; all within spirit of the present utility model and principle, any amendment done, equivalent replacement, improvement etc., all should be included within protection domain of the present utility model.
Claims (8)
1. a nicotine sulphate anti-emulsification device, it is characterized in that: comprise cylindrical shell (1), this cylindrical shell (1) top is provided with solvent recovery pipe (4), and bottom is provided with solution inlet pipe (9) and cleaning delivery pipe (10); Described inner barrel central authorities are also provided with the orifice plate (2) of densely covered aperture, this orifice plate (2) below is provided with random packing layer (6), and this random packing layer (6) is filled by several ceramic Pall rings (11) and formed; Described solution inlet pipe (9) is connected with shower (8), and this shower (9) top seal, tube wall has and organizes spray apertures more.
2. nicotine sulphate anti-emulsification device according to claim 1, it is characterized in that: described ceramic Pall ring (11) for perforate circular, this ceramic Pall ring (11) sidewall surrounding is provided with the fenestra (12) staggered on the contrary upper and lower two-layer position, and described every layer of fenestra (12) is provided with 5 by the ligule (13) of interior dactylogryposis to the ring heart.
3. nicotine sulphate anti-emulsification device according to claim 1 and 2, is characterized in that: described ceramic Pall ring (11) diameter is 2 ~ 3cm, and this ceramic Pall ring (11) height and equal diameters, thickness is 3mm.
4. nicotine sulphate anti-emulsification device according to claim 1, it is characterized in that: be provided with filter washing water inlet pipe (7) between described solution inlet pipe (9) and orifice plate (2), this filter washing water inlet pipe (7) mouth of pipe peak is higher than random packing layer (6).
5. nicotine sulphate anti-emulsification device according to claim 1, is characterized in that: the length 100 ~ 180cm of described shower (8), diameter 50mm.
6. nicotine sulphate anti-emulsification device according to claim 1, is characterized in that: the spray apertures diameter 8mm on described shower (8), this spray apertures is distributed on the tube wall surrounding of described shower (8).
7. nicotine sulphate anti-emulsification device according to claim 1, is characterized in that: described cylindrical shell (1) top is also provided with blast pipe (3), and orifice plate (2) top is also provided with probe tube (5).
8. nicotine sulphate anti-emulsification device according to claim 1, is characterized in that: described solvent recovery pipe (4), solution inlet pipe (9), shower (8), orifice plate (2) and cleaning delivery pipe (10) are made up of PVC material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201420500001.8U CN204232271U (en) | 2014-09-01 | 2014-09-01 | Nicotine sulphate anti-emulsification device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201420500001.8U CN204232271U (en) | 2014-09-01 | 2014-09-01 | Nicotine sulphate anti-emulsification device |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN204232271U true CN204232271U (en) | 2015-04-01 |
Family
ID=52761849
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201420500001.8U Expired - Fee Related CN204232271U (en) | 2014-09-01 | 2014-09-01 | Nicotine sulphate anti-emulsification device |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN204232271U (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105312098A (en) * | 2015-11-30 | 2016-02-10 | 河南师范大学 | Separating funnel used in extraction process |
| CN114957210A (en) * | 2022-05-24 | 2022-08-30 | 云南叶贵生物科技有限公司 | Method for extracting 40 crude nicotine from tobacco waste |
-
2014
- 2014-09-01 CN CN201420500001.8U patent/CN204232271U/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105312098A (en) * | 2015-11-30 | 2016-02-10 | 河南师范大学 | Separating funnel used in extraction process |
| CN105312098B (en) * | 2015-11-30 | 2017-04-05 | 河南师范大学 | A kind of separatory funnel in extraction process |
| CN114957210A (en) * | 2022-05-24 | 2022-08-30 | 云南叶贵生物科技有限公司 | Method for extracting 40 crude nicotine from tobacco waste |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20150401 |