CN218421060U - Solid-liquid separator for preparing agricultural ammonium chloride and industrial sodium carbonate from strong brine - Google Patents
Solid-liquid separator for preparing agricultural ammonium chloride and industrial sodium carbonate from strong brine Download PDFInfo
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- CN218421060U CN218421060U CN202222258195.2U CN202222258195U CN218421060U CN 218421060 U CN218421060 U CN 218421060U CN 202222258195 U CN202222258195 U CN 202222258195U CN 218421060 U CN218421060 U CN 218421060U
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- Prior art keywords
- crystallization
- chamber
- solid
- ammonium chloride
- liquid separator
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- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 239000007788 liquid Substances 0.000 title claims abstract description 33
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 title claims abstract description 26
- 235000019270 ammonium chloride Nutrition 0.000 title claims abstract description 21
- 239000012267 brine Substances 0.000 title claims abstract description 17
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 title claims abstract description 17
- 229910000029 sodium carbonate Inorganic materials 0.000 title claims abstract description 9
- 238000002425 crystallisation Methods 0.000 claims abstract description 62
- 230000008025 crystallization Effects 0.000 claims abstract description 61
- 238000003756 stirring Methods 0.000 claims abstract description 27
- 230000007246 mechanism Effects 0.000 claims abstract description 16
- 239000000463 material Substances 0.000 abstract description 14
- 238000001704 evaporation Methods 0.000 abstract description 11
- 238000010438 heat treatment Methods 0.000 abstract description 4
- 239000011550 stock solution Substances 0.000 description 14
- 239000013078 crystal Substances 0.000 description 10
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 8
- 230000008020 evaporation Effects 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 6
- 235000017550 sodium carbonate Nutrition 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 238000000034 method Methods 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 235000017557 sodium bicarbonate Nutrition 0.000 description 4
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 4
- 239000011780 sodium chloride Substances 0.000 description 3
- RSIJVJUOQBWMIM-UHFFFAOYSA-L sodium sulfate decahydrate Chemical compound O.O.O.O.O.O.O.O.O.O.[Na+].[Na+].[O-]S([O-])(=O)=O RSIJVJUOQBWMIM-UHFFFAOYSA-L 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 229910002651 NO3 Inorganic materials 0.000 description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 2
- 239000003245 coal Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000008014 freezing Effects 0.000 description 2
- 238000007710 freezing Methods 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 238000001728 nano-filtration Methods 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000007670 refining Methods 0.000 description 2
- 238000001223 reverse osmosis Methods 0.000 description 2
- 238000007790 scraping Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- BGOFCVIGEYGEOF-UJPOAAIJSA-N helicin Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1OC1=CC=CC=C1C=O BGOFCVIGEYGEOF-UJPOAAIJSA-N 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
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- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The utility model discloses a solid-liquid separator for preparing agricultural ammonium chloride and industrial soda by strong brine. The solid-liquid separator for preparing agricultural ammonium chloride and industrial sodium carbonate from concentrated brine comprises: the heating tank comprises a tank body, wherein a preheating cavity, a crystallization cavity and an equipment cavity are arranged in the tank body, a heat exchanger is installed at the top of the tank body, a heating plate is arranged in the equipment cavity, and a stirring mechanism is arranged in the tank body. The utility model provides a strong brine system agricultural ammonium chloride and industry are solid-liquid separator for soda include through the setting preheat the chamber, the jar body in crystallization chamber and equipment chamber, a heat exchanger, hot plate and rabbling mechanism, vapor when can utilizing the crystallization carries out a lot of preheating to the stoste that gets into the jar body, can reach evaporating temperature rapidly after making the stoste get into the crystallization intracavity, and then improve crystallization rate, the utilization ratio of heat energy has been improved, including driving motor through the setting, the rabbling mechanism of axis of rotation and spiral stirring leaf, can conveniently stir the stoste, conveniently clear up the crystallization chamber when conveniently arranging the material.
Description
Technical Field
The utility model relates to a chemical industry technical field especially relates to a strong brine system agricultural ammonium chloride and industrial sodium carbonate use solid-liquid separation ware.
Background
The strong brine of the water treatment center of the coal chemical industry enterprise is concentrated and separated again through a high-pressure reverse osmosis RO2 by a membrane concentration nanofiltration separator, and the sodium sulfate is prepared from the two-stage nanofiltration concentrated water by adopting a freezing crystallization and hot melting evaporation crystallization method. Dissolving the sodium sulfate decahydrate obtained by freezing crystallization, conveying the dissolved sodium sulfate decahydrate to a nitrate refining device, and treating the sodium sulfate decahydrate by the nitrate refining device to obtain anhydrous sodium sulfate with better quality. The high-pressure reverse osmosis RO2 concentrated water produced water is mainly sodium chloride, the produced water enters a triple-effect forced evaporative crystallization system to be evaporated and crystallized to obtain pure sodium chloride solid, and in order to ensure the purity of the sodium chloride solid, a certain amount of mother liquor is discharged from the evaporative crystallization system to remove impurity salt and drying system. At present, the coal chemical industry enterprises generally use a mechanical vapor compression (MVR) process, a multiple effect evaporation (MED) process, a multiple effect flash evaporation (MSF) process, and a Membrane Distillation (MD) process for "zero emission".
The solid-liquid separator for agricultural ammonium chloride and industrial soda ash adopted in the existing multi-effect evaporation (MED) process lacks a preheating device, so that the temperature of the input end of the separator is low, the temperature of the stock solution cannot be quickly raised to the temperature required by crystallization evaporation, and the improvement of the crystallization precipitation speed is not facilitated.
Therefore, it is necessary to provide a solid-liquid separator for preparing agricultural ammonium chloride from strong brine and industrial soda ash to solve the above technical problems.
SUMMERY OF THE UTILITY MODEL
To the above situation, for overcoming prior art defect, the utility model provides a solid-liquid separator is used to agricultural ammonium chloride of strong brine system and industrial soda can improve the crystallization rate when, improves the utilization ratio of heat energy.
In order to achieve the above object, the utility model adopts the following technical scheme:
the solid-liquid separator for preparing agricultural ammonium chloride and industrial sodium carbonate from concentrated brine comprises: the jar body, jar internal portion is equipped with preheats chamber, crystallization chamber and equipment chamber, the heat exchanger is installed at the top of the jar body, and one side and the crystallization chamber and the condenser of heat exchanger are connected, and the opposite side and the preheating chamber and the raw materials input pipeline of heat exchanger are connected, the equipment intracavity is equipped with the hot plate, and the top at the equipment chamber is installed to the hot plate, the internal rabbling mechanism that is equipped with of jar, rabbling mechanism are used for stirring the liquid in the crystallization chamber.
Preferably, the stirring mechanism is including installing driving motor in the equipment intracavity, driving motor with install rotation axis connection in the crystallization intracavity, install spiral stirring leaf in the axis of rotation, the edge of spiral stirring leaf and the bottom and the lateral wall contact in crystallization chamber.
Preferably, a plurality of scrapers are mounted on the rotating shaft, the scrapers are distributed in an annular array, and the edges of the scrapers are in contact with the side wall of the crystallization cavity.
Preferably, a guide plate is arranged in the preheating cavity and is spiral.
Preferably, feed liquor pipe, drain pipe and row's material pipe are installed to one side of jar body, and the both ends of feed liquor pipe are connected with heat exchanger and preheating chamber respectively, and the drain pipe is connected with the crystallization chamber, arranges the slope of material pipe and sets up and install the control valve, arranges the one end of material pipe and extends to the crystallization chamber in, arranges the one end and the conveyer of material pipe and is connected.
Preferably, the top of the tank body is provided with an exhaust pipe, the exhaust pipe is provided with an exhaust fan, one end of the exhaust fan extends into the crystallization cavity, the bottom of the preheating cavity is provided with a communicating pipe, and the communicating pipe is provided with an electric control valve.
Compared with the prior art, the utility model discloses following beneficial effect has:
(1) The utility model discloses a set up including preheating the jar body in chamber, crystallization chamber and equipment chamber, heat exchanger, hot plate and rabbling mechanism, can utilize the vapor when crystallizing to carry out a lot of preheating to the stoste that gets into the jar body, can reach evaporating temperature rapidly after making the stoste get into the crystallization intracavity, and then improve crystallization rate, improved the utilization ratio of heat energy;
(2) The utility model has the advantages that the stirring mechanism comprising the driving motor, the rotating shaft and the spiral stirring blade is arranged, so that the raw liquid can be conveniently stirred, the material can be conveniently discharged, and the crystallization cavity can be conveniently cleaned;
(3) The utility model can conveniently clean the inner wall of the crystallization cavity while stirring the stock solution by installing a plurality of scraping plates on the rotating shaft;
(4) The spiral guide plate is arranged in the preheating cavity, so that the time of the stock solution passing through the preheating cavity is prolonged, the stock solution can be fully preheated, and the temperature of each part of the stock solution is more uniform;
(5) The utility model discloses a set up feed liquor pipe, drain pipe, row's material pipe, blast pipe, air exhauster, can feed through preheating chamber, crystallization chamber and heat exchanger, can carry out reutilization, the utilization ratio of the energy is improved to the vapor that produces when the crystallization.
Drawings
Fig. 1 is a schematic sectional structure diagram of a solid-liquid separator for preparing agricultural ammonium chloride and industrial soda by using strong brine.
Wherein, the names corresponding to the reference numbers are: 1-tank body, 2-preheating cavity, 3-crystallizing cavity, 4-equipment cavity, 5-heat exchanger, 6-heating plate, 7-driving motor, 8-rotating shaft, 9-scraping plate, 10-spiral stirring blade, 11-guide plate, 12-liquid inlet pipe, 13-liquid outlet pipe, 14-discharge pipe, 15-exhaust pipe, 16-exhaust fan and 17-communicating pipe.
Detailed Description
The present invention will be further described with reference to the following description and examples, which are not intended to limit the scope of the invention.
Example 1:
as shown in fig. 1, for the utility model provides a solid-liquid separator for strong brine agricultural ammonium chloride and industrial soda ash, include: the utility model discloses a crystallization device, including a tank body 1, jar body 1 is inside to be equipped with preheating chamber 2, crystallization chamber 3 and equipment chamber 4, heat exchanger 5 is installed at the top of jar body 1, and one side and crystallization chamber 3 and the condenser of heat exchanger 5 are connected, and the opposite side and the preheating chamber 2 and the raw materials input pipeline of heat exchanger 5 are connected, be equipped with hot plate 6 in the equipment chamber 4, hot plate 6 installs the top at equipment chamber 4, jar body 1 is equipped with rabbling mechanism, and rabbling mechanism is used for stirring the liquid in crystallization chamber 3, and during the use, preheating chamber 2 and crystallization chamber 3 all are equipped with the intake pipe, are used for balancing internal pressure, and the stoste enters preheating chamber 2 after the primary temperature rise through heat exchanger 5, then enters crystallization chamber 3 after preheating the second grade in preheating chamber 2, and hot plate 4 heats the bottom of crystallization chamber 3, makes the stoste temperature after preheating rise to evaporating temperature rapidly, makes the moisture evaporation, and crystallization, and meanwhile, rabbling mechanism stirs stoste, further accelerates the precipitation speed, and the vapor in the preheating chamber 3 heats the stoste in preheating chamber 2, and then enters in the heat exchanger 5, and the condenser is preheated stoste.
Through setting up including preheating the jar body 1 of chamber 2, crystallization chamber 3 and equipment chamber 4, heat exchanger 5, hot plate 6 and rabbling mechanism, vapor when can utilizing the crystallization carries out a lot of preheating to the stoste that gets into jar body 1, makes the stoste get into and can reach evaporating temperature rapidly behind the crystallization chamber 3, and then improves the crystallization rate, has improved the utilization ratio of heat energy.
Example 2:
as shown in fig. 1, rabbling mechanism is including installing driving motor 7 in the equipment chamber 4, driving motor 7 with install rotation axis 8 in the crystallization chamber 3 is connected, install spiral stirring leaf 10 on the rotation axis 8, the edge of spiral stirring leaf 10 and the bottom and the lateral wall contact of crystallization chamber 3, during the use, on the one hand, driving motor 7 starts and drives rotation axis 8 and rotate, rotation axis 8 rotates and drives spiral stirring leaf 10 and rotate, and then stir the stoste, and on the other hand, adnexed crystal on the bottom of crystallization chamber 3 and the lateral wall is scraped off and is concentrated to the middle part to pivoted spiral stirring leaf 10, when conveniently arranging the material, the crystal that reduces the inner wall of crystallization chamber 3 adheres to, and then conveniently clears up.
Through setting up the rabbling mechanism including driving motor 7, axis of rotation 8 and spiral stirring leaf 10, conveniently clear up crystallization chamber 3 when can conveniently stir the stoste, conveniently arrange the material.
Example 3:
as shown in figure 1, a plurality of scrapers 9 are installed on the rotating shaft 3, the scrapers 9 are distributed in an annular array, the edge of the scraper 9 is in contact with the side wall of the crystallization cavity 3, when the crystallizer is used, the rotating shaft 8 rotates to drive the scrapers 9 to rotate, and the scrapers 9 rotate to hang down the attachments on the inner wall of the crystallization cavity 3 and stir the stock solution.
Through installing a plurality of scraper blades 9 on the axis of rotation 3, can conveniently carry out the convenience when stirring to the stoste and clear up the inner wall of crystallization chamber 3.
Example 4:
as shown in fig. 1, a guide plate 11 is arranged in the preheating chamber 2, and the guide plate 13 is spiral, so that when in use, the stock solution flows from the outer side of the guide plate 13 to the middle along the trend of the guide plate 13, all parts of the stock solution can be in contact with the bottom of the preheating chamber 2, and the temperature of all parts of the stock solution is more uniform.
Through set up spiral helicine deflector 11 in preheating chamber 2, prolonged the time that the stoste passes through preheating chamber 2, make the stoste can fully preheat the temperature that makes each part of stoste more even simultaneously.
Example 5:
as shown in fig. 1, a liquid inlet pipe 12, a liquid outlet pipe 13 and a material outlet pipe 14 are installed at one side of a tank body 1, two ends of the liquid inlet pipe 12 are respectively connected with a heat exchanger 5 and a preheating chamber 2, the liquid outlet pipe 13 is connected with a crystallization chamber 3, the material outlet pipe 14 is obliquely arranged and provided with a control valve, one end of the material outlet pipe 14 extends into the crystallization chamber 3, one end of the material outlet pipe 14 is connected with a conveyor, an exhaust pipe 15 is arranged at the top of the tank body 1, an exhaust fan 16 is arranged on the exhaust pipe 15, one end of the exhaust fan 16 extends into the crystallization chamber 3, a communicating pipe 17 is arranged at the bottom of the preheating chamber 2, and an electric control valve is installed on the communicating pipe 17.
Through setting up feed liquor pipe 12, drain pipe 13, row's material pipe 14, blast pipe 15, air exhauster 16, can communicate preheating chamber 2, crystallization chamber 3 and heat exchanger 5, can carry out the reutilization to the vapor that produces during the crystallization, improve the utilization ratio of the energy.
When in use, the preheating cavity 2 and the crystallization cavity 3 are both provided with air inlet pipes for balancing the internal pressure;
the stock solution enters the heat exchanger 5 and is primarily heated, passes through the liquid inlet pipe 12 and enters the preheating cavity 2 from the side surface of the preheating cavity 2, flows to the middle part from the outer side of the guide plate 13 along the trend of the guide plate 13, is secondarily heated by the bottom of the preheating cavity 2, and then enters the crystallization cavity 3 through the communicating pipe 17 in the middle part;
the driving motor 7 is started and drives the rotating shaft 8 to rotate, the rotating shaft 8 rotates and drives the spiral stirring blade 10 to rotate, so that the stock solution is stirred, the rotary spiral stirring blade 10 scrapes attached crystals on the bottom and the side wall of the crystallization cavity 3 and concentrates the crystals towards the middle part, the discharge is facilitated, and meanwhile, the attachment of crystals on the inner wall of the crystallization cavity 3 is reduced, so that the cleaning is facilitated;
discharging residual liquid into the evaporator through a liquid outlet pipe 13 for the next operation;
after the residual liquid is discharged, the rotating spiral stirring blade 10 sends the crystal substances to a conveyer through a discharge pipe 5 and conveys the crystal substances to a crystallizer for purification;
the heating plate 4 heats the bottom of the crystallization cavity 3, so that the temperature of the preheated stock solution is rapidly raised to an evaporation temperature, water is evaporated and crystallized and separated out, after the bottom of the preheating cavity 2 is heated by vapor, the exhaust fan 16 is started, the exhaust fan 16 extracts the vapor and conveys the vapor to the heat exchanger 5, and further the stock solution in the second heat exchanger 5 is heated;
the stock solution mainly refers to a concentrated slurry containing sodium bicarbonate and ammonium chloride, the crystal substance refers to sodium bicarbonate crystal and a small part of ammonium chloride crystal, the water vapor refers to an aqueous solution containing a small amount of sodium bicarbonate and ammonium chloride, and the residual solution refers to an ammonium chloride solution and a small part of sodium bicarbonate solution.
The above embodiment is only one of the preferred embodiments of the present invention, and should not be used to limit the protection scope of the present invention, but all the insubstantial changes or color modifications made in the main body design concept and spirit of the present invention, the technical problems solved by the embodiments are still consistent with the present invention, and all should be included in the protection scope of the present invention.
Claims (6)
1. A solid-liquid separator for preparing agricultural ammonium chloride and industrial sodium carbonate from strong brine is characterized by comprising:
the jar body, jar internal portion is equipped with preheats chamber, crystallization chamber and equipment chamber, the heat exchanger is installed at the top of the jar body, the equipment intracavity is equipped with the hot plate, the internal rabbling mechanism that is equipped with of jar.
2. The solid-liquid separator for preparing agricultural ammonium chloride and industrial soda from concentrated brine according to claim 1, wherein the stirring mechanism comprises a driving motor installed in the equipment cavity, the driving motor is connected with a rotating shaft installed in the crystallization cavity, and a spiral stirring blade is installed on the rotating shaft.
3. The solid-liquid separator for preparing agricultural ammonium chloride and industrial soda from concentrated brine according to claim 2, wherein the rotating shaft is provided with a plurality of scrapers.
4. The solid-liquid separator according to claim 1, wherein a guide plate is disposed in the preheating chamber.
5. The solid-liquid separator for preparing agricultural ammonium chloride and industrial soda from concentrated brine according to claim 1, wherein a liquid inlet pipe, a liquid outlet pipe and a discharge pipe are installed on one side of the tank body.
6. The solid-liquid separator for preparing agricultural ammonium chloride and industrial soda from concentrated brine according to claim 1, wherein an exhaust pipe is arranged at the top of the tank body, an exhaust fan is arranged on the exhaust pipe, and a communicating pipe is arranged at the bottom of the preheating cavity.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202222258195.2U CN218421060U (en) | 2022-08-26 | 2022-08-26 | Solid-liquid separator for preparing agricultural ammonium chloride and industrial sodium carbonate from strong brine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202222258195.2U CN218421060U (en) | 2022-08-26 | 2022-08-26 | Solid-liquid separator for preparing agricultural ammonium chloride and industrial sodium carbonate from strong brine |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN218421060U true CN218421060U (en) | 2023-02-03 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202222258195.2U Expired - Fee Related CN218421060U (en) | 2022-08-26 | 2022-08-26 | Solid-liquid separator for preparing agricultural ammonium chloride and industrial sodium carbonate from strong brine |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN218421060U (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116891263A (en) * | 2023-09-11 | 2023-10-17 | 山东承锦海洋生物科技有限公司 | Sewage aftertreatment device for sea cucumber and hyaluronic acid stock solution preparation |
-
2022
- 2022-08-26 CN CN202222258195.2U patent/CN218421060U/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116891263A (en) * | 2023-09-11 | 2023-10-17 | 山东承锦海洋生物科技有限公司 | Sewage aftertreatment device for sea cucumber and hyaluronic acid stock solution preparation |
| CN116891263B (en) * | 2023-09-11 | 2023-12-19 | 山东承锦海洋生物科技有限公司 | Sewage aftertreatment device for sea cucumber and hyaluronic acid stock solution preparation |
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| CF01 | Termination of patent right due to non-payment of annual fee |
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