CN217042545U - System for preparing large-particle ammonium polyvanadate - Google Patents
System for preparing large-particle ammonium polyvanadate Download PDFInfo
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- CN217042545U CN217042545U CN202123106278.1U CN202123106278U CN217042545U CN 217042545 U CN217042545 U CN 217042545U CN 202123106278 U CN202123106278 U CN 202123106278U CN 217042545 U CN217042545 U CN 217042545U
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Abstract
The utility model provides a system for preparing large-particle ammonium polyvanadate, which comprises a raw material unit, an acid regulating reactor and a crystallization unit, wherein the raw material unit comprises a sulfuric acid preparation tank, a sodium vanadate solution storage tank and an ammonium sulfate solution storage tank; the acid regulating reactor is divided into a pre-acid regulating area, a primary acid regulating area, a secondary acid regulating area and a pre-reaction area; the crystallization unit is communicated with the discharge hole so as to crystallize large particles of the solution in the pre-reaction zone. The utility model provides a system for preparing large granule ammonium polyvanadate has solved current production system and has easily leaded to the problem of local peracid.
Description
Technical Field
The utility model belongs to the technical field of chemical production, concretely relates to system for preparing large granule polyvanadate.
Background
Ammonium polyvanadate is a main intermediate product in the production process of vanadium products at present, and is mainly used as a chemical reagent, a catalyst, a drier and the like. Ammonium polyvanadate is a main raw material for producing vanadium pentoxide and is commonly used for preparing high-end vanadium-aluminum alloys, titanium alloys, metal vanadium products and the like.
In the prior art, a common method for preparing ammonium polyvanadate is to add ammonium sulfate into a neutralized vanadium solution at a temperature higher than 50 ℃, add sulfuric acid to adjust the pH of the solution to 5.0, heat the solution to about 90 ℃ under continuous stirring, adjust the pH of the solution to 1.5-2.5, and precipitate and crystallize ammonium polyvanadate. The production system is easy to generate local peracid in the acid adjusting process, so that the product quality is difficult to control.
SUMMERY OF THE UTILITY MODEL
The embodiment of the utility model provides a system for preparing large granule polyvanadate ammonium solves current production system and is transferring sour in-process sulfuric acid solution and vanadium solution reaction insufficient, leads to the problem of local peracid.
In order to achieve the purpose, the utility model adopts the technical proposal that: the system for preparing the large-particle ammonium polyvanadate sequentially comprises a raw material unit, an acid regulating reactor and a crystallization unit according to a reaction process; wherein the content of the first and second substances,
the raw material unit comprises a sulfuric acid preparation tank, a sodium vanadate solution storage tank and an ammonium sulfate solution storage tank;
the acid regulating reactor is provided with a reaction cavity, and the reaction cavity is internally provided with a plurality of partition plates which can divide the reaction cavity along the horizontal direction to form a pre-acid regulating zone, a primary acid regulating zone, a secondary acid regulating zone and a pre-reaction zone which are sequentially communicated; the acid regulating reactor is also provided with a first feeding hole, a second feeding hole, a third feeding hole and a discharging hole; the first feed port is respectively communicated with the pre-acid adjusting area and the sodium vanadate solution storage tank; the second feed port is respectively communicated with the pre-acid adjusting area and the ammonium sulfate solution storage tank; the third feed ports are respectively communicated with the pre-acid adjusting zone, the primary acid adjusting zone, the secondary acid adjusting zone and the pre-reaction zone in a one-to-one correspondence manner, and the discharge port is communicated with the pre-reaction zone; the mixed solution of sodium vanadate and ammonium sulfate entering the pre-acid regulating area is subjected to pre-acid regulation, then sequentially passes through the primary acid regulating area, the secondary acid regulating area and the pre-reaction area, and is subjected to acid regulation in the process;
and the crystallization unit is communicated with the discharge hole so as to crystallize large particles of the solution everywhere in the pre-reaction zone.
In one possible implementation, the acid regulation reactor comprises:
the tank body is horizontally arranged; the reaction cavity is positioned in the tank body, and the first feed port, the second feed port, the third feed port and the discharge port are all arranged on the tank body;
and four stirring components are arranged, and each stirring component is arranged in one-to-one correspondence with the pre-acid adjusting zone, the primary acid adjusting zone, the secondary acid adjusting zone and the pre-reaction zone respectively so as to stir the solution entering the pre-acid adjusting zone, the primary acid adjusting zone, the secondary acid adjusting zone and the pre-reaction zone respectively.
In a possible implementation manner, three partition plates are provided, each partition plate is arranged along the vertical direction, and the height of each partition plate is smaller than that of the reaction chamber; the height of each partition plate is reduced in sequence along the direction from the pre-acid adjusting zone to the pre-reaction zone.
In a possible implementation manner, the first feed port, the second feed port, the third feed port and the discharge port are all provided with a first opening/closing valve.
In one possible implementation, the crystallization unit includes:
the forced circulator is provided with a forced circulator feeding hole, a circulating feeding hole and a forced circulator discharging hole; the feed inlet of the forced circulator is communicated with the discharge outlet;
the crystallizer is provided with a crystallizer feeding hole and a crystallizer discharging hole; the feed inlet of the crystallizer is communicated with the discharge outlet of the forced circulator;
the filtering washer is provided with a filtering washer feed port, a washing water inlet, a washing water outlet and a liquid discharge port; the feed inlet of the filtering washer is communicated with the discharge outlet of the crystallizer;
the washing liquid device is provided with a steam inlet, a temperature measuring port, a washing liquid return port and a washing liquid outlet, the washing liquid outlet is communicated with the washing water inlet, and the washing water outlet is communicated with the washing liquid return port;
and the discharge hole of the forced circulator is also communicated with the circulating feed hole and is used for crystal growing reaction.
In a possible realization mode, a second opening and closing valve is arranged between the crystallizer and the filtering washer.
In one possible implementation, a first slurry pump is provided between the washing liquid outlet and the washing water inlet to pump the liquid in the washing liquid device into the filter scrubber.
In a possible implementation manner, a second slurry pump is arranged between the acid adjusting reactor and the crystallization unit so as to pump the solution in the acid adjusting reactor into the crystallization unit.
The utility model provides a system for preparation large granule ammonium polyvanadate compares with prior art, transfers sour reactor through the setting, makes the vanadium solution after mixing react many times with sulphuric acid solution in transferring sour reactor, and the reaction is more abundant, reaches the pH valve of technological requirement, has solved current production system and has easily appeared local peracid and lead to product quality uncontrollable problem in transferring sour in-process.
Drawings
Fig. 1 is a schematic diagram of a system for preparing large-particle ammonium polyvanadate according to an embodiment of the present invention.
In the figure: 100. a feedstock unit; 110. an ammonium sulfate solution storage tank; 120. a sodium vanadate solution storage tank; 130. a sulfuric acid blending tank; 140. a flow control valve; 200. an acid adjusting reactor; 210. a tank body; 220. a stirring assembly; 230. a first on-off valve; 240. a partition plate; 300. a crystallization unit; 310. a forced circulator; 320. a circulation pump; 321. a three-way control valve; 330. a crystallizer; 331. a second on-off valve; 340. a filtration scrubber; 341. a filtration scrubber feed inlet; 342. a wash water inlet; 343. a wash water outlet; 344. a liquid discharge port; 350. a washing liquid device; 351. returning the washing liquid; 352. a washing liquid outlet; 400. a first slurry pump; 410. a second slurry pump.
Detailed Description
In order to make the technical problem, technical solution and advantageous effects to be solved by the present invention more clearly understood, the following description is given in conjunction with the accompanying drawings and embodiments to illustrate the present invention in further detail. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the invention.
It should be noted that the terms "length," "width," "height," "thickness," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," "head," "tail," and the like, are used in the orientation or positional relationship indicated in the drawings for convenience in describing the invention and for simplicity in description, and do not indicate or imply that the device or element so referred to must have a particular orientation, be constructed and operated in a particular orientation, and therefore should not be construed as limiting the invention.
It is also noted that, unless expressly stated or limited otherwise, the terms "mounted," "connected," "secured," "disposed," and the like are intended to be inclusive and mean, for example, that they may be fixedly connected, detachably connected, or integrally formed; can be mechanically or electrically connected; either directly or indirectly through intervening media, either internally or in any other relationship. The specific meaning of the above terms in the present invention can be understood according to specific situations by those of ordinary skill in the art.
Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. Further, "plurality" or "a plurality" means two or more unless specifically limited otherwise.
Referring to fig. 1, an embodiment of a system for preparing large-particle ammonium polyvanadate according to the present invention will now be described. The system for preparing the large-particle ammonium polyvanadate is suitable for producing the large-particle ammonium polyvanadate from a high-concentration vanadium solution. Wherein the arrow indicates the solution flowing direction, the system for preparing large-particle ammonium polyvanadate provided by the embodiment of the invention comprises a raw material unit 100, an acid regulating reactor 200 and a crystallization unit 300.
The feedstock unit 100 includes a sulfuric acid preparation tank 130, a sodium vanadate solution storage tank 120, and an ammonium sulfate solution storage tank 110.
The acid regulating reactor 200 has a reaction chamber, and a plurality of partition plates 240 which can partition the reactor along the horizontal direction to form a pre-acid regulating zone, a primary acid regulating zone, a secondary acid regulating zone and a pre-reaction zone which are sequentially communicated are arranged in the reaction chamber. The acid adjusting reactor 200 further comprises a first feed port, a second feed port, a third feed port and a discharge port, wherein the first feed port is respectively communicated with the pre-acid adjusting area and the sodium vanadate solution storage tank 120, the second feed port is respectively communicated with the pre-acid adjusting area and the ammonium sulfate solution storage tank 110, the third feed ports are multiple, each third feed port is respectively communicated with the pre-acid adjusting area, the primary acid adjusting area, the secondary acid adjusting area and the pre-reaction area in a one-to-one correspondence manner, and the discharge port is communicated with the pre-reaction area. The mixed solution of sodium vanadate and ammonium sulfate entering the pre-acid regulation area is subjected to acid regulation in advance, and then sequentially passes through the primary acid regulation area, the secondary acid regulation area and the pre-reaction area, and the acid is sequentially regulated in the process.
The crystallization unit 300 is communicated with a discharge port to crystallize large particles of the solution in the pre-reaction zone.
The sulfuric acid blending tank 130 is arranged at the upper end of the acid blending reactor 200, and the sulfuric acid solution can respectively enter the pre-acid blending zone, the primary acid blending zone, the secondary acid blending zone and the pre-reaction zone through a third feed inlet. The sodium vanadate solution and the ammonium sulfate solution are mixed in a pre-acid adjusting area in the acid adjusting reactor 200 through a first feed port and a second feed port respectively, sulfuric acid is added, the sodium vanadate solution and the ammonium sulfate solution sequentially pass through a primary acid adjusting area, a secondary acid adjusting area and a pre-reaction area, the pH value of the sulfuric acid adjusting solution is added, and the sodium vanadate solution and the ammonium sulfate solution enter the crystallization unit 300 through a discharge port after the process requirements are met to perform crystallization reaction and subsequent processes.
The utility model provides a system for preparation large granule polyvanadate ammonium compares with prior art, transfers sour reactor through setting up, makes the vanadium solution after mixing react with sulphuric acid solution many times in transferring sour reactor, and the reaction is more abundant, reaches the pH valve of technological requirement, has solved current production system and has easily appeared local peracid and lead to product quality unmanageable problem in transferring sour in-process.
In some embodiments, referring to fig. 1, the acid adjusting reactor 200 includes a tank 210 horizontally disposed, a reaction chamber is located in the tank 210, and a first feeding port, a second feeding port, a third feeding port and a discharging port are all disposed on the tank 210.
The number of the stirring assemblies 220 is four, and optionally, the stirring assemblies 220 are two layers of four-blade stirring paddles. Each stirring assembly 220 is arranged in one-to-one correspondence with the pre-acid adjusting zone, the primary acid adjusting zone, the secondary acid adjusting zone and the pre-reaction zone, so as to stir the solution entering the pre-acid adjusting zone, the primary acid adjusting zone, the secondary acid adjusting zone and the pre-reaction zone.
In some embodiments, referring to fig. 1, three partition plates 240 are provided, each partition plate 240 is disposed along a vertical direction, and the height of each partition plate 240 is smaller than the height of the reaction chamber, so that the solution can flow in the reaction chamber, and the heights of the partition plates 240 are sequentially reduced along the direction from the pre-acid adjusting zone to the pre-reaction zone, so as to prevent the solution from flowing back.
In some embodiments, referring to fig. 1, the first inlet, the second inlet, the third inlet and the outlet are provided with a first open/close valve 230, and when the sulfuric acid solution is added to the pre-acid adjusting zone, the first acid adjusting zone, the second acid adjusting zone and the pre-reaction zone, the first open/close valve 230 on the pre-acid adjusting zone, the first acid adjusting zone, the second acid adjusting zone and the pre-reaction zone is controlled respectively.
In some embodiments, referring to FIG. 1, the crystallization unit comprises a forced circulator 310 having a forced circulator feed port, a circulation feed port, and a forced circulator discharge port. The feed inlet of the forced circulator is communicated with the discharge outlet.
The crystallizer 330 has a crystallizer feed inlet and a crystallizer discharge outlet, and the crystallizer feed inlet is communicated with the discharge outlet of the forced circulator.
The filtering scrubber 340 is provided with a filtering scrubber feeding hole 341, a washing water inlet 342, a washing water outlet 343 and a liquid outlet 344, and the filtering scrubber feeding hole 341 is communicated with the crystallizer discharging hole;
the washing liquid device 350 is provided with a steam inlet, a temperature measuring port, a washing liquid return port 351 and a washing liquid outlet 352, wherein the washing liquid outlet 352 is communicated with the washing water inlet 342, and the washing water outlet 343 is communicated with the washing liquid return port 351;
wherein, the discharge hole of the forced circulator is also communicated with the circulating feed hole to be used for crystal growing reaction in the forced circulator 310.
In some embodiments, referring to fig. 1, the discharge port of the forced circulator is provided with a circulation pump 320, a three-way control valve 321 is installed between the circulation pump 320 and the crystallizer 330, and the three-way control valve 321 is respectively connected with the circulation pump 320, the crystallizer 330 and the circulation feed port. When the solution in the forced circulator 310 does not reach the standard of entering the crystallizer 330, the channel between the discharge port of the forced circulator and the crystallizer 330 is closed, the channel between the discharge port of the forced circulator and the circulation feed port is opened to realize the multiple circulation crystal growing reaction in the forced circulator 310, after the requirement is met, the channel between the discharge port of the forced circulator and the crystallizer 330 is opened, and the channel between the discharge port of the forced circulator and the circulation feed port is closed to enable the solution with the crystal seeds to enter the crystallizer 330 for crystallization.
In some embodiments, referring to fig. 1, after the crystals with the solution enter the filtering scrubber 340, the washing and filtering operation is performed, the liquid discharge port 344 is opened to recover the solution on the crystals, but the combination of the liquid and the solid does not completely discharge the solution, and multiple washing operations are required, the liquid discharge port 344 is closed, so that the solution in the washing device 350 passes through the washing liquid outlet 352, the washing water inlet 342, the washing water outlet 343, and the washing liquid return port 351, and multiple cycles are performed in the washing device 350 and the filtering scrubber 340, after the solution reaches a certain concentration, the solution is discharged through the liquid discharge port 344, and the crystals in the filtering scrubber 340 are taken out.
In some embodiments, referring to fig. 1, a second open/close valve 331 is disposed between the crystallizer 330 and the filter scrubber 340, when the crystallization reaction in the crystallizer 330 is not completed, the second open/close valve 331 is in a closed state, and after the crystallization reaction is completed, the second open/close valve 331 is opened to allow the crystals to enter the filter scrubber 340.
In some embodiments, referring to fig. 1, a first slurry pump 400 is disposed between the washing liquid outlet 352 and the washing water inlet 342 to pump the solution in the washing liquid device 350 into the filtering washer 340 for repeated washing.
In some embodiments, referring to fig. 1, a second slurry pump 410 is disposed between the acid adjusting reactor 200 and the crystallization unit 300 to pump the solution in the acid adjusting reactor 200 into the crystallization unit 300 to provide power for the solution.
In some embodiments, referring to fig. 1, the washing liquid device 350 is provided with a steam inlet and a temperature measuring port, wherein the washing liquid device 350 is heated by steam, and the distance from the steam outlet to the bottom kettle wall is 100 mm and 400 mm.
In some embodiments, when the system for preparing large-particle ammonium polyvanadate provided by the embodiments of the present invention is used, the method comprises the following steps:
s100, a sodium vanadate solution, an ammonium sulfate solution, and a sulfuric acid solution are mixed in the acid adjusting reactor 200 through the flow control valve 140 and the first open/close valve 230.
Wherein the vanadium concentration of the sodium vanadate solution is 40-70g/L, the pH value is 9.5-10.5, the temperature of the vanadium liquid is controlled at 65-75 ℃, and the pH value is adjusted by adopting a sulfuric acid solution with the volume fraction of 50%. When preparing sulfuric acid in the sulfuric acid preparation tank 130, water is added to the tank, and then sulfuric acid is introduced and continuously stirred to dilute the sulfuric acid to 50% sulfuric acid solution.
The temperature of the pre-acid adjusting zone is controlled to be 85-90 ℃, the pH value is controlled to be 8.0-8.5, the stirring speed is controlled to be 300-350r/min, the temperature of the primary acid adjusting zone is controlled to be 70-80 ℃, the pH value is controlled to be 7.0-8.0, the stirring speed is controlled to be 220-min, the temperature of the secondary acid adjusting zone is controlled to be 60-70 ℃, the pH value is controlled to be 5-6, the stirring speed is controlled to be 100-220r/min, the temperature of the pre-reaction zone is controlled to be 90-95 ℃, the pH value is controlled to be 2.1-2.3, and the stirring speed is controlled to be 50-100 r/min.
S200, the solution passing through the pre-reaction zone enters the forced circulator 310 through the second slurry pump 410 to carry out the circulating crystal growth reaction through the circulating pump 320.
The solution after S300 circulation enters a crystallizer 330 through a three-way control valve 321 for heat preservation crystallization.
And carrying out a circulating crystal growing reaction in the forced circulator 310, regulating and controlling a valve to close and circulate after a large amount of crystals are generated, and allowing the material to enter a crystallizer 330 at the temperature of 90-95 ℃ for carrying out a crystallization reaction for 30-60 min.
S400, filtering and washing the slurry after crystallization by a filtering and washing device 340, wherein more than 80% of the high-purity ammonium polyvanadate product obtained after the reaction is finished has the particle size of 300-500 mu m.
The solution in the washing liquid device 350 is controlled to be sulfuric acid solution with the mass fraction of 0.5-1%, the temperature is above 90 ℃, and washing liquid enters through the washing water inlet 342 and returns to the washing liquid device through the washing liquid return opening 351 for circular washing.
The above description is only exemplary of the present invention and should not be taken as limiting the scope of the present invention, as any modifications, equivalents, improvements and the like made within the spirit and principles of the present invention are intended to be included within the scope of the present invention.
Claims (8)
1. The system for preparing the large-particle ammonium polyvanadate is characterized by sequentially comprising a raw material unit, an acid regulating reactor and a crystallization unit according to a reaction process; wherein the content of the first and second substances,
the raw material unit comprises a sulfuric acid preparation tank, a sodium vanadate solution storage tank and an ammonium sulfate solution storage tank;
the acid regulating reactor is provided with a reaction cavity, and the reaction cavity is internally provided with a plurality of partition plates which can divide the reaction cavity along the horizontal direction to form a pre-acid regulating zone, a primary acid regulating zone, a secondary acid regulating zone and a pre-reaction zone which are sequentially communicated; the acid regulating reactor is also provided with a first feeding hole, a second feeding hole, a third feeding hole and a discharging hole; the first feed port is respectively communicated with the pre-acid adjusting area and the sodium vanadate solution storage tank; the second feed port is respectively communicated with the pre-acid adjusting area and the ammonium sulfate solution storage tank; the third feed ports are respectively communicated with the pre-acid adjusting zone, the primary acid adjusting zone, the secondary acid adjusting zone and the pre-reaction zone in a one-to-one correspondence manner, and the discharge port is communicated with the pre-reaction zone; the mixed solution of sodium vanadate and ammonium sulfate entering the pre-acid adjusting area is pre-acid-adjusted, then sequentially passes through the primary acid adjusting area, the secondary acid adjusting area and the pre-reaction area, and sequentially acid-adjusted in the process;
and the crystallization unit is communicated with the discharge hole so as to crystallize large particles of the solution in the pre-reaction zone.
2. The system for preparing large particle ammonium polyvanadate according to claim 1, wherein the acid regulation reactor comprises:
the tank body is horizontally arranged; the reaction cavity is positioned in the tank body, and the first feed port, the second feed port, the third feed port and the discharge port are all arranged on the tank body;
and four stirring assemblies are arranged, and each stirring assembly is respectively arranged in one-to-one correspondence with the pre-acid adjusting area, the primary acid adjusting area, the secondary acid adjusting area and the pre-reaction area so as to respectively stir the solution entering the pre-acid adjusting area, the primary acid adjusting area, the secondary acid adjusting area and the pre-reaction area.
3. The system for preparing large-particle ammonium polyvanadate according to claim 2, wherein the number of the partition plates is three, each partition plate is arranged along the vertical direction, and the height of each partition plate is smaller than that of the reaction chamber; the height of each partition plate is reduced in sequence along the direction from the pre-acid adjusting zone to the pre-reaction zone.
4. The system for preparing large-particle ammonium polyvanadate according to claim 2, wherein first opening and closing valves are arranged at the first feeding port, the second feeding port, the third feeding port and the discharging port.
5. The system for preparing large-particle ammonium polyvanadate according to claim 1, wherein the crystallization unit comprises:
the forced circulator is provided with a forced circulator feeding hole, a circulating feeding hole and a forced circulator discharging hole; the feed inlet of the forced circulator is communicated with the discharge outlet;
the crystallizer is provided with a crystallizer feeding hole and a crystallizer discharging hole; the feed inlet of the crystallizer is communicated with the discharge outlet of the forced circulator;
the filtering washer is provided with a filtering washer feed inlet, a washing water outlet and a liquid outlet; the feed inlet of the filtering washer is communicated with the discharge outlet of the crystallizer;
the washing liquid device is provided with a steam inlet, a temperature measuring port, a washing liquid return port and a washing liquid outlet, the washing liquid outlet is communicated with the washing water inlet, and the washing water outlet is communicated with the washing liquid return port;
and the discharge hole of the forced circulator is also communicated with the circulating feed hole and is used for crystal growing reaction.
6. The system for preparing large-particle ammonium polyvanadate according to claim 5, wherein a second opening and closing valve is arranged between the crystallizer and the filtration scrubber.
7. The system for preparing large-particle ammonium polyvanadate according to claim 5, wherein a first slurry pump is arranged between the washing liquid outlet and the washing water inlet so as to pump the solution in the washing liquid device into the filtration scrubber.
8. The system for preparing large-particle ammonium polyvanadate according to claim 1, wherein a second slurry pump is arranged between the acid adjusting reactor and the crystallization unit so as to pump the solution in the acid adjusting reactor into the crystallization unit.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115072778A (en) * | 2022-07-27 | 2022-09-20 | 西安航天华威化工生物工程有限公司 | Ammonium polyvanadate continuous reaction crystallization process |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115072778A (en) * | 2022-07-27 | 2022-09-20 | 西安航天华威化工生物工程有限公司 | Ammonium polyvanadate continuous reaction crystallization process |
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Address after: 067000 Chenggang No.1 office building, Luanhe Town, Shuangluan District, Chengde City, Hebei Province Patentee after: HBIS Chengde Vanadium & Titanium New Material Co.,Ltd. Patentee after: CHENGDE BRANCH OF HBIS Group Patentee after: Hebei Yanshan vanadium titanium industry technology research Co.,Ltd. Address before: 067000 Chenggang No.1 office building, Luanhe Town, Shuangluan District, Chengde City, Hebei Province Patentee before: Hegang Chengde vanadium titanium New Material Co.,Ltd. Patentee before: CHENGDE BRANCH OF HBIS Group Patentee before: Hebei Yanshan vanadium titanium industry technology research Co.,Ltd. |
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