CN206692325U - A kind of system of continuous production pulverulent water-soluble APP - Google Patents
A kind of system of continuous production pulverulent water-soluble APP Download PDFInfo
- Publication number
- CN206692325U CN206692325U CN201720555484.5U CN201720555484U CN206692325U CN 206692325 U CN206692325 U CN 206692325U CN 201720555484 U CN201720555484 U CN 201720555484U CN 206692325 U CN206692325 U CN 206692325U
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- Prior art keywords
- phosphoric acid
- tubular reactor
- tail gas
- continuous production
- groove
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- 238000010924 continuous production Methods 0.000 title claims abstract description 14
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 160
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 80
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000007921 spray Substances 0.000 claims abstract description 28
- 238000007599 discharging Methods 0.000 claims abstract description 19
- 238000001816 cooling Methods 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000002002 slurry Substances 0.000 claims abstract description 8
- 230000008676 import Effects 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims description 24
- 238000010438 heat treatment Methods 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 7
- 238000005554 pickling Methods 0.000 claims description 7
- 238000004140 cleaning Methods 0.000 claims description 3
- 239000002826 coolant Substances 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- 229910021529 ammonia Inorganic materials 0.000 abstract description 16
- 239000003337 fertilizer Substances 0.000 abstract description 13
- 238000004519 manufacturing process Methods 0.000 abstract description 12
- 239000003795 chemical substances by application Substances 0.000 abstract description 4
- 239000000203 mixture Substances 0.000 abstract description 3
- 238000000034 method Methods 0.000 description 21
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 8
- 239000004202 carbamide Substances 0.000 description 8
- 238000006116 polymerization reaction Methods 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- 239000004254 Ammonium phosphate Substances 0.000 description 5
- 229910000148 ammonium phosphate Inorganic materials 0.000 description 5
- 235000019289 ammonium phosphates Nutrition 0.000 description 5
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 description 5
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 3
- 239000000428 dust Substances 0.000 description 3
- 229910052698 phosphorus Inorganic materials 0.000 description 3
- 239000011574 phosphorus Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000010410 dusting Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000003973 irrigation Methods 0.000 description 2
- 230000002262 irrigation Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- -1 And turn on agitator Chemical compound 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 description 1
- CLQQPGDRJJCZMQ-UHFFFAOYSA-N azane;phosphoric acid Chemical compound N.N.N.N.OP(O)(O)=O CLQQPGDRJJCZMQ-UHFFFAOYSA-N 0.000 description 1
- PPBAJDRXASKAGH-UHFFFAOYSA-N azane;urea Chemical compound N.NC(N)=O PPBAJDRXASKAGH-UHFFFAOYSA-N 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 description 1
- 239000003317 industrial substance Substances 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 235000021049 nutrient content Nutrition 0.000 description 1
- 238000010422 painting Methods 0.000 description 1
- LLDYDUXXNBDDFT-UHFFFAOYSA-N phosphoric acid urea Chemical compound NC(=O)N.P(=O)(O)(O)O.P(=O)(O)(O)O.P(=O)(O)(O)O LLDYDUXXNBDDFT-UHFFFAOYSA-N 0.000 description 1
- SWXKOPASTUVMMT-UHFFFAOYSA-N phosphoric acid;urea Chemical compound NC(N)=O.NC(N)=O.OP(O)(O)=O SWXKOPASTUVMMT-UHFFFAOYSA-N 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229920000137 polyphosphoric acid Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
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- Fertilizers (AREA)
Abstract
A kind of system of continuous production pulverulent water-soluble APP includes phosphoric acid preheating device, tubular reactor, spray tower;Phosphoric acid preheating device includes phosphoric acid groove, phosphoric acid discharging pump, agitating device, heater, the lower part outlet of described phosphoric acid groove is connected with phosphoric acid discharging pump entrance point, the port of export of phosphoric acid discharging pump is connected with tubular reactor, heater heats to phosphoric acid groove, to being stirred in phosphoric acid groove, the first temperature sensor is inserted into phosphoric acid groove agitating device；Tubular reactor is connected by the first phosphoric acid check-valves, first pressure table with the port of export of phosphoric acid discharging pump, and liquefied ammonia discharge nozzle is connected by second pressure gauge and second check-valve with the import of tubular reactor side, and cooling device is carried outside tubular reactor；Tubular reactor end is connected with spray tower and stretches to spray tower upper end；Tubular reactor terminal discharge mouth is connected with slurry temperature sensor and the 3rd pressure gauge.The utility model has the advantages that, there is provided a kind of continuous production aggregate rate height, good water solubility, the powdery APP production system easily with the agent of low hygroscopicity of other fertilizer mixtures.
Description
Technical field
It the utility model is related to a kind of water soluble phosphorous fertilizer production system, and in particular to a kind of continuous production pulverulent water-soluble gathers
The system and method for ammonium phosphate.
Background technology
APP (APP), general molecular formula are (NH4) n+2P nO(3n+1), it is a kind of important industrial chemicals, in industry
With all had a wide range of applications in agricultural.APP by its degree of polymerization can be divided into it is oligomeric, in gather and height gather, and its solubility with
The increase of the degree of polymerization and reduce.The middle and high long chain APP of the degree of polymerization, it is water-soluble not high, it is mainly used in industrial fireproof painting
The field such as material and flame retardant plastics, and the APP that the degree of polymerization is relatively low（The degree of polymerization≤5）For producing high-concentration slow-release composite fertilizer
Or Liquid Fertilizer.
APP（It is oligomeric）With nutrient content and utilization rate are high, fertilizer efficiency is long, good water solubility and easily with other fertilizer
The characteristics of compounding, it is particularly suitable for drip irrigation system, develops faster country, such as Israel and the U.S. in some water-fertilizer integrals
It is widely applied.The RCF companies of last century, U.S. TVA and India develop is gathered with 50 ~ 60% Wet-process Phosphoric Acid Production particles
The technique of ammonium phosphate, but polymeric form aggregate rate is not high in product, generally 15 ~ 30%.In addition, TVA companies also developed to cross phosphorus
Acid and gas ammonia are the production technology that raw material produces APP basal liquid fertilizer, but cost of transportation is higher, are only applicable soil ratio
Compared with the country concentrated, irrigating facility is more complete.The agricultural APP solution in China is then just in starting stage, only a small amount of factory
Family production, as Chinese patent CN104528682A disclose it is a kind of produce the full water-soluble APP aqueous solution with phosphoric acid by wet process
Method, use concentration to be reacted for 30-80% phosphoric acid by wet process with ammonia at a temperature of 150 DEG C to 300 DEG C, produce low polymerization degree
The aqueous solution of water-soluble poly ammonium phosphate.But due to being restricted by the factor such as production and transport cost and irrigation equipment backwardness, China's mesh
It is preceding still mainly based on solid fertilizer.
The industrial process of APP mainly has：（1）Phosphoric acid-urea method（Including urea phosphate-urea method）；（2）Phosphorus
Sour one ammonium-urea method；（3）Polyphosphoric acid-ammonia process；（4）MAP-P2O5- ammonia method.Method（4）It is poly- to be generally used for production industry
Ammonium phosphate, and method（1）~（3）Mainly for the production of the relatively low fertilizer APP of the degree of polymerization, such as the A of patent CN 105967164
Disclose a kind of method with MAP and urea production APP, control MAP and urea measure than for 0.8 ~
1.8:1, reaction temperature is 110-180 DEG C, is prepared for the APP of high aggregate rate；And for example the A of patent CN 105621381 are announced
A kind of method that water-soluble poly ammonium phosphate is prepared with phosphoric acid by wet process and urea reaction, raw material phosphoric acid by wet process pass sequentially through pre- place
Reason, slurrying, foaming, the step such as it polymerize, cool, crushing, is prepared for water miscible APP.
It is in place of above-mentioned the deficiencies in the prior art：（1）Polyphosphoric acid is prepared with urea reaction using MAP or phosphoric acid
Ammonium, problem are that both the above method is both needed to using urea as raw material, and urea then starts to decompose to produce largely at 60 DEG C
Carbon dioxide and ammonia so that the gas release of device is big, and filling rate is not high, easily produces ease material, and device continuity is not high, ammonia damage
Lose larger；（2）U.S. TVA and patent CN104528682A uses phosphoric acid to react production APP liquid fertilizer, fortune with ammonia
Defeated and storage is inconvenient and cost is higher；（3）U.S. TVA and India RCF reacts the poly- of preparation with 50% ~ 60% phosphoric acid by wet process and ammonia
Ammonium phosphate, aggregate rate is relatively low, and particle APP during other fertilizer mixtures with need to first be crushed.
The content of the invention
The purpose of the utility model patent is to be directed to above-mentioned the shortcomings of the prior art, there is provided a kind of continuous production is gathered
Conjunction rate height, good water solubility, the powdery APP production system easily with the agent of low hygroscopicity of other fertilizer mixtures.
Realize that technical solutions of the utility model are as follows：A kind of system of continuous production pulverulent water-soluble APP includes phosphorus
Sour preheating device, tubular reactor, spray tower, washing tail gas device;
Described phosphoric acid preheating device includes phosphoric acid groove, phosphoric acid discharging pump, agitating device, heater, described phosphoric acid
The lower part outlet of groove is connected with phosphoric acid discharging pump entrance point, and the port of export of phosphoric acid discharging pump is connected with tubular reactor, heating dress
Put and phosphoric acid groove is heated, to being stirred in phosphoric acid groove, the first temperature sensor is inserted into phosphoric acid groove agitating device；
Described tubular reactor is connected by the port of export of the first phosphoric acid check-valves, first pressure table and phosphoric acid discharging pump
Connect, liquefied ammonia discharge nozzle is connected by second pressure gauge and second check-valve with the import of tubular reactor side, outside tubular reactor
With cooling device；Tubular reactor end is connected with spray tower and stretches to spray tower upper end；Tubular reactor terminal discharge
Mouth is connected with slurry temperature sensor and the 3rd pressure gauge；
The tower bottom that dusts is connected with air-cooler, and APP powder is cooled；
Described washing tail gas device include tail gas washing tower, pickling circulating pump, tail gas washing tower upper end with provided with shower nozzle,
Lower end is provided with collecting-tank, and pickling pump inlet end is connected with collecting-tank, the connection of the port of export and shower nozzle, and spray tower discharge tail gas leads to
The import of tail gas washing tower side is crossed to enter.
Further, the heater is steam feeder apparatus, more heating tubes is provided with phosphoric acid groove, steam is by adding
Heat pipe passes through phosphoric acid groove.
Further, cooling tube is set in described tubular reactor, coolant is passed through in cooling tube.
Further, washing tail gas device also includes the fog spray head being located in tail gas washing tower, fog spray head and cleaning water pump
Connection.
Further, cooling tube is provided with electronic valve, and electronic valve is by controller and is located at phosphoric acid discharging pumping hole
Second temperature sensor connects.
The utility model has the advantages that reduce breaker compared to existing equipment, meanwhile, using the conjunction of the system
Reach more than 80 percent into reactivity.
Brief description of the drawings
Fig. 1 is the utility model structure diagram.
Fig. 2 is to prepare pulverulent water-soluble APP technique prostitute's route map using the utility model.
In such as figure, phosphoric acid preheating device 1, tubular reactor 2, spray tower 3, gas wash tower 5, pickling circulating pump 6, shower nozzle 7,
Collecting-tank 8, cooling tube 9, fog spray head 10, phosphoric acid groove 11, phosphoric acid discharging pump 12, excessively agitating device 13, heating tube 14, the first temperature
Sensor 15, the first phosphoric acid check-valves 21, first pressure table 22, liquefied ammonia discharge nozzle 23, second pressure gauge 24, second check-valve
25th, slurry temperature sensor 27, the 3rd pressure gauge 28, electronic valve 29, controller 30.
Specific embodiment
In Fig. 1, it is anti-that a kind of system of continuous production pulverulent water-soluble APP includes phosphoric acid preheating device 1, tubular type
Answer device 2, spray tower 3, washing tail gas device;
Phosphoric acid preheating device 1 includes phosphoric acid groove 11, phosphoric acid discharging pump 12, agitating device 13, heater, it is preferred that adds
Hot charging is set to steam feeder apparatus, is provided with more heating tubes 14 in the phosphoric acid groove 11, steam by heating tube 14 by phosphoric acid groove 11,
The lower part outlet of phosphoric acid groove 11 is connected with the entrance point of phosphoric acid discharging pump 12, the port of export and the tubular reactor 2 of phosphoric acid discharging pump 12
It is connected, heater heats to phosphoric acid groove 11（Cross in heating tube 14 by entering steam, i.e., the material in phosphoric acid groove 11 is entered
Row heating）, to being stirred in phosphoric acid groove 11, the first temperature sensor 15 is inserted into phosphoric acid groove 11 agitating device 13；
Tubular reactor 2 is connected by the port of export of the first phosphoric acid check-valves 21, first pressure table 22 and phosphoric acid discharging pump 12
Connect, liquefied ammonia discharge nozzle 23 is connected by second pressure gauge 24 and second check-valve 25 with the side import of tubular reactor 2, and tubular type is anti-
Answer and carry cooling device outside device 2；The end of tubular reactor 2 is connected with spray tower 3 and stretches to the upper end of spray tower 3；Pipe reaction
The terminal discharge mouth of device 2 is connected with the pressure gauge 28 of slurry temperature sensor 27 and the 3rd；
The bottom of spray tower 3 is connected with air-cooler, and APP powder is cooled；
Washing tail gas device include tail gas washing tower 5, pickling circulating pump 6, the upper end of tail gas washing tower 5 with provided with shower nozzle 7, under
End is provided with collecting-tank 8, and the entrance point of pickling circulating pump 6 is connected with collecting-tank 8, the port of export and shower nozzle 7 connect, and spray tower 3 discharges tail
Gas is entered by the side import of tail gas washing tower 5.
Preferably, cooling tube 9 is set in tubular reactor 2, coolant is passed through in cooling tube 9, washing tail gas device also includes
The fog spray head 10 being located in tail gas washing tower 5, fog spray head 10 connect with cleaning water pump.
Preferably, cooling tube 9 is provided with electronic valve 29, and electronic valve 29 passes through controller 30 and slurry temperature sensor
27 connections.
In Fig. 2, one kind utilizes said system continuous production pulverulent water-soluble APP step：
（a）Phosphoric acid preheats：
Phosphoric acid and condensing agent add to phosphoric acid groove 11, steam by a certain percentage to be entered from the pre- heat channel external heat exchanger of phosphoric acid,
And turn on agitator, phosphoric acid is uniformly heated, after certain temperature to be achieved, is delivered to tubular reactor 2, preferable scheme
It is as follows, P is added into phosphoric acid groove2O5Concentration is 65% phosphoric acid by wet process and condensing agent urea, wherein, the quality of urea is phosphoric acid
Mass ratio be 0.2：1, it is passed through steam and heats and stir and be allowed to thermally equivalent, phosphoric acid is preheated to 125 DEG C；
（b）Neutralize, polymerisation：
Phosphoric acid and liquefied ammonia after preheating respectively enter tubular reactor 2, and neutralization reaction is carried out in tubular reactor 2, in
With reaction caused by heat reaction mass is further polymerize, preferable scheme is as follows, and phosphoric acid is delivered to by syringe pump
Tubular reactor is neutralized with liquefied ammonia, polymerisation, and the pressure for controlling phosphoric acid and liquefied ammonia into tubular reactor is respectively
The ratio between amount of 1.6-1.8Mpa and 1.7-1.9Mpa, phosphoric acid and liquefied ammonia material is 0.45：1, pass through cooling outside tubular reactor
Water carries out countercurrent flow to neutralize slip, and it is 200 DEG C to control APP material liquid outlet temperature, pressure 1.8-1.9MPa；
（c）Dust：
APP slurry from tubular reactor 2 out enters spray tower 3, enters volute chamber through tangent line passage, with mist
Drop form sprays, meanwhile, air-cooler blasts cold wind from the tower bottom that dusts and APP material is cooled, the powdery after cooling
APP discharges from bottom oblique line（Preferably, in APP and feed liquid is under high pressure from spray tower, enter through tangent line passage
Volute chamber, sprayed with the formula of droplet shape, atomized liquid blasts temperature with bottom of dusting during decline and carried out for 30 DEG C of cold wind
Heat exchange, APP droplet solidify rapidly, from tower bottom oblique line discharging of dusting, obtain powdery APP product）；
（d）Tail gas and dust washing：
Contain unreacted ammonia and APP dust from spray tower out enter from tail gas washing tower side, by water
With phosphoric acid two-stage washing absorption, emptied after up to standard from washing tail gas top of tower；
The powdery APP product of gained after testing, P2O5Content 58%, N content 18%, average degree of polymerization 2.75,
Aggregate rate is 75%, pH=6.87, water-insoluble 0.09%.
Claims (5)
- A kind of 1. system of continuous production pulverulent water-soluble APP, it is characterised in that：The system includes the pre- hot charging of phosphoric acid Put, tubular reactor, spray tower, washing tail gas device;Described phosphoric acid preheating device includes phosphoric acid groove, phosphoric acid discharging pump, agitating device, heater, described phosphoric acid groove Lower part outlet is connected with phosphoric acid discharging pump entrance point, and the port of export of phosphoric acid discharging pump is connected with tubular reactor, heater pair Phosphoric acid groove is heated, and to being stirred in phosphoric acid groove, the first temperature sensor is inserted into phosphoric acid groove agitating device；Described tubular reactor is connected by the first phosphoric acid check-valves, first pressure table with the port of export of phosphoric acid discharging pump, liquid Ammonia discharge nozzle is connected by second pressure gauge and second check-valve with the import of tubular reactor side, with cold outside tubular reactor But device；Tubular reactor end is connected with spray tower and stretches to spray tower upper end；Tubular reactor terminal discharge mouth and material Slurry temperature sensor and the 3rd pressure gauge are connected；The tower bottom that dusts is connected with air-cooler, and APP powder is cooled；Described washing tail gas device includes tail gas washing tower, pickling circulating pump, and tail gas washing tower upper end is with being provided with shower nozzle, lower end Provided with collecting-tank, pickling pump inlet end is connected with collecting-tank, the connection of the port of export and shower nozzle, and spray tower discharge tail gas passes through tail The import of gas wash tower side enters.
- A kind of 2. system of continuous production pulverulent water-soluble APP according to claim 1, it is characterised in that：It is described Heater is steam feeder apparatus, and more heating tubes are provided with phosphoric acid groove, and steam passes through phosphoric acid groove by heating tube.
- A kind of 3. system of continuous production pulverulent water-soluble APP according to claim 1, it is characterised in that：It is described Tubular reactor in set cooling tube, be passed through coolant in cooling tube.
- A kind of 4. system of continuous production pulverulent water-soluble APP according to claim 1, it is characterised in that：It is described Washing tail gas device also include being located at fog spray head in tail gas washing tower, fog spray head connects with cleaning water pump.
- A kind of 5. system of continuous production pulverulent water-soluble APP according to claim 3, it is characterised in that：It is described Cooling tube is provided with electronic valve, and electronic valve is connected by controller with slurry temperature sensor.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201720555484.5U CN206692325U (en) | 2017-05-18 | 2017-05-18 | A kind of system of continuous production pulverulent water-soluble APP |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201720555484.5U CN206692325U (en) | 2017-05-18 | 2017-05-18 | A kind of system of continuous production pulverulent water-soluble APP |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN206692325U true CN206692325U (en) | 2017-12-01 |
Family
ID=60449484
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201720555484.5U Expired - Fee Related CN206692325U (en) | 2017-05-18 | 2017-05-18 | A kind of system of continuous production pulverulent water-soluble APP |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN206692325U (en) |
-
2017
- 2017-05-18 CN CN201720555484.5U patent/CN206692325U/en not_active Expired - Fee Related
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| Date | Code | Title | Description |
|---|---|---|---|
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20171201 |