CN113526553A - Preparation method and production equipment of superfine niobium hydroxide - Google Patents
Preparation method and production equipment of superfine niobium hydroxide Download PDFInfo
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- CN113526553A CN113526553A CN202111002132.4A CN202111002132A CN113526553A CN 113526553 A CN113526553 A CN 113526553A CN 202111002132 A CN202111002132 A CN 202111002132A CN 113526553 A CN113526553 A CN 113526553A
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- WPCMRGJTLPITMF-UHFFFAOYSA-I niobium(5+);pentahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[Nb+5] WPCMRGJTLPITMF-UHFFFAOYSA-I 0.000 title claims abstract description 64
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 238000004519 manufacturing process Methods 0.000 title claims description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 63
- 238000001914 filtration Methods 0.000 claims abstract description 51
- 238000006243 chemical reaction Methods 0.000 claims abstract description 48
- 239000003513 alkali Substances 0.000 claims abstract description 41
- 239000000243 solution Substances 0.000 claims abstract description 38
- 239000012528 membrane Substances 0.000 claims abstract description 37
- 238000005406 washing Methods 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 150000003839 salts Chemical class 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 9
- 239000000047 product Substances 0.000 claims abstract description 8
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 6
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 5
- 238000010790 dilution Methods 0.000 claims abstract description 5
- 239000012895 dilution Substances 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims description 33
- 238000005374 membrane filtration Methods 0.000 claims description 15
- 238000002347 injection Methods 0.000 claims description 14
- 239000007924 injection Substances 0.000 claims description 14
- 239000007788 liquid Substances 0.000 claims description 13
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 11
- 239000000706 filtrate Substances 0.000 claims description 10
- 238000003860 storage Methods 0.000 claims description 9
- 239000000084 colloidal system Substances 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 239000012465 retentate Substances 0.000 claims 2
- 238000011010 flushing procedure Methods 0.000 claims 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 abstract description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 abstract description 6
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 abstract 1
- 238000011033 desalting Methods 0.000 abstract 1
- 230000007613 environmental effect Effects 0.000 abstract 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 10
- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 description 10
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 description 10
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 8
- 229910052700 potassium Inorganic materials 0.000 description 8
- 239000011591 potassium Substances 0.000 description 8
- 229910052757 nitrogen Inorganic materials 0.000 description 6
- 239000010955 niobium Substances 0.000 description 5
- 239000011698 potassium fluoride Substances 0.000 description 5
- 235000003270 potassium fluoride Nutrition 0.000 description 5
- 239000011775 sodium fluoride Substances 0.000 description 5
- 235000013024 sodium fluoride Nutrition 0.000 description 5
- 238000011001 backwashing Methods 0.000 description 4
- 238000001035 drying Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 150000004673 fluoride salts Chemical class 0.000 description 2
- -1 fluorine ions Chemical class 0.000 description 2
- 229910052758 niobium Inorganic materials 0.000 description 2
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 239000012670 alkaline solution Substances 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G33/00—Compounds of niobium
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention provides a preparation method of superfine niobium hydroxide, which comprises the following steps: s1: uniformly adding a dilute alkali solution into the fluoroniobate solution; s2: the fluoroniobate and the dilute alkali solution are fully mixed and react in the reaction kettle in a long tube pass; s3: filtering the mixed reaction product by using a membrane filtering device, and filtering out water-soluble salt and excessive alkali; s4: adding pure water into the reaction kettle for dilution and washing to obtain a niobium hydroxide diluted solution, and circularly washing and filtering the niobium hydroxide diluted solution by using a membrane filtering device; s5: and repeating S4 until the salt and alkali content is lower than the product purity requirement. According to the invention, diluted sodium hydroxide solution is used for replacing ammonia water to react with fluoroniobate, a high-purity niobium hydroxide product can be obtained after filtering and washing for multiple times through the silicon carbide film, compared with the water consumption of 1:400 per ton of products in the traditional plate-and-frame desalting process, the process is only about 1:60, water saving and consumption reduction are realized, and the problem of ammonia nitrogen environmental protection in the traditional process is solved.
Description
Technical Field
The invention relates to the field of preparation of niobium hydroxide, in particular to a preparation method and production equipment of ultrafine niobium hydroxide.
Background
The niobium hydroxide is generally prepared by neutralizing the niobium solution with aqueous ammonia in a precipitation tank to obtain Nb (OH)5Precipitating, pumping into a filter press for solid-liquid separation, washing with dilute ammonia water, filtering to remove Nb (OH)5Washing with pure water, and drying with air of 0.6-0.7 Mpa to obtain wet Nb (OH)5And putting the niobium hydroxide into a hot air circulation drying box to be dried to obtain the niobium hydroxide. Drying niobium hydroxide which is not treated by hydrochloric acid to obtain niobium hydroxideNb in Nb2O5When the content is 72-78%, the nitrogen content is not less than 3.5%, and the low nitrogen requirement cannot be met.
The invention has patent number "201911087457. X" and discloses a method for preparing low-nitrogen niobium hydroxide, wherein nitrogen in niobium hydroxide is mainly carried in by dilute ammonia water after removing fluorine ions by washing, and then the nitrogen content in niobium hydroxide is not reduced to below 0.2% by washing with pure water. The method is complex, has more processing steps and can not completely remove nitrogen ions.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a method for preparing ultrafine niobium hydroxide, which adopts fluoroniobate as a raw material and comprises the following steps:
a preparation method of superfine niobium hydroxide adopts fluoroniobate as a raw material, and is characterized by comprising the following steps:
s1: uniformly adding a dilute alkali solution into the fluoroniobate solution;
s2: the fluoroniobate and the dilute alkali solution are fully mixed and reacted in a long pipe pass and a reaction kettle to obtain superfine niobium hydroxide, water-soluble salt and excessive alkali;
s3: filtering the mixed reaction product by using a membrane filtering device, intercepting niobium hydroxide colloid by using the membrane filtering device, and filtering out water-soluble salt and excessive alkali;
s4: adding pure water into the reaction kettle for dilution and washing to obtain a niobium hydroxide diluted solution, and circularly washing and filtering the niobium hydroxide diluted solution by using a membrane filtering device;
s5: and repeating S4 until the salt and alkali content is lower than the product purity requirement.
Further, the dilute alkaline solution comprises one of: sodium hydroxide solution, potassium hydroxide solution.
The invention also provides production equipment of the superfine niobium hydroxide, which comprises the following components: reation kettle, circulating pump, dilute alkali injection device, mixing reactor, membrane filter equipment, reation kettle's bottom through the mixing pipe with the entry of circulating pump links to each other, the exit of circulating pump is equipped with two branch pipelines, and two branch pipelines link to each other with mixing reactor, membrane filter equipment's entry end respectively, all be equipped with return line on mixing reactor, the membrane filter equipment, return line links to each other with reation kettle's top, be equipped with the switch switching valve on the return line, dilute alkali injection device passes through the connecting pipe and links to each other with the middle part of mixing pipe.
Furthermore, the membrane filtration device specifically adopts a silicon carbide membrane for filtration, a mixed liquid inlet is arranged at the bottom of the membrane filtration device, a trapped liquid outlet is arranged at the top of the membrane filtration device, a filtrate outlet is arranged at the side of the membrane filtration device, the mixed liquid inlet is communicated with the circulating pump, the return pipeline is communicated with the trapped liquid outlet, and the filtrate outlet is connected with the post-treatment device.
Further, the dilute alkali injection device comprises: the bottom of the dilute alkali storage tank is connected with the metering pump, and the metering pump is connected with the middle part of the mixing pipe through a connecting pipe.
Furthermore, stirring devices are arranged in the reaction kettle and the dilute alkali storage tank.
Further, the mixing reactor comprises: the reaction barrel is vertically arranged, a plurality of horizontally arranged baffle plates are mounted on the inner side wall of the reaction barrel, and the reaction barrel is internally divided into serpentine channels through the baffle plates.
Further, the mixing reactor comprises: the reaction barrel is vertically arranged, and a reaction coil pipe arranged in a turbulent flow mode is installed in the reaction barrel.
Furthermore, the pipelines of the material inlet and the material outlet of the reaction kettle, the dilute alkali injection device, the mixing reactor and the membrane filtering device are all provided with switch switching valves.
Furthermore, a back washing device is arranged at the filtrate discharge port.
Compared with the prior art, the invention provides a preparation method of superfine niobium hydroxide, which has the following beneficial effects:
according to the invention, diluted sodium hydroxide or potassium hydroxide solution is used for replacing ammonia water to react with fluoroniobate, so that niobium hydroxide colloid is prepared, the byproduct is water-soluble fluoride salt, a high-purity niobium hydroxide product can be obtained after the niobium hydroxide colloid is filtered through a silicon carbide film and washed for multiple times, and the problem that the byproduct generated by ammonia water reaction is not environment-friendly is solved.
The invention also provides production equipment of the superfine niobium hydroxide, which has the following beneficial effects:
1. the diluted sodium hydroxide solution is quantitatively injected into the flow of the mixing pipe through the metering pump, and the sodium hydroxide solution is quantitatively injected in the flow process of the fluoroniobate solution, so that the local over-high concentration of the sodium hydroxide can be avoided, and the problem of non-uniform particles after hydrolysis is solved.
2. According to the invention, niobium hydroxide is filtered and intercepted through the silicon carbide film, so that impurity ions such as fluoride salt dissolved in water and excessive alkali are effectively removed, and high-purity superfine niobium hydroxide powder is obtained.
Drawings
FIG. 1 is a schematic structural diagram of an embodiment 3 of an apparatus for producing ultrafine niobium hydroxide.
FIG. 2 is a schematic structural diagram of an embodiment 4 of an apparatus for producing ultra-fine niobium hydroxide.
FIG. 3 is a schematic structural view of an embodiment 6 of an apparatus for producing ultra-fine niobium hydroxide.
Wherein: 1-a reaction kettle; 2-a mixing pipe; 3-a circulating pump; 401-a reaction barrel; 402-a baffle plate; 403-reaction coil pipe; 5-a membrane filtration unit; 6-dilute alkali storage tank; 7-a metering pump; 8-a stirring device; 9-switching the switching valve; 10-filtration forced circulation pump.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, specific embodiments accompanied with figures are described in detail below, and it is apparent that the described embodiments are a part of the embodiments of the present invention, not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without making creative efforts based on the embodiments of the present invention, shall fall within the protection scope of the present invention.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways than those specifically described and will be readily apparent to those of ordinary skill in the art without departing from the spirit of the present invention, and therefore the present invention is not limited to the specific embodiments disclosed below.
Furthermore, reference herein to "one embodiment" or "an embodiment" means that a particular feature, structure, or characteristic described in connection with the embodiment is included in at least one implementation of the invention. The appearances of the phrase "in one embodiment" in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments.
The present invention will be described in detail with reference to the drawings, wherein the cross-sectional views illustrating the structure of the device are not enlarged partially in general scale for convenience of illustration, and the drawings are only exemplary and should not be construed as limiting the scope of the present invention. In addition, the three-dimensional dimensions of length, width and depth should be included in the actual fabrication.
Meanwhile, in the description of the present invention, it should be noted that the terms "upper, lower, inner and outer" and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only for convenience of describing the present invention and simplifying the description, but do not indicate or imply that the referred device or element must have a specific orientation, be constructed in a specific orientation and operate, and thus, cannot be construed as limiting the present invention. Furthermore, the terms first, second, or third are used for descriptive purposes only and are not to be construed as indicating or implying relative importance. The terms "mounted, connected and connected" in the present invention are to be understood broadly, unless otherwise explicitly specified or limited, for example: can be fixedly connected, detachably connected or integrally connected; they may be mechanically, electrically, or directly connected, or indirectly connected through intervening media, or may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
Example 1
The invention provides a preparation method of superfine niobium hydroxide, which adopts fluoroniobate as a raw material and comprises the following steps:
s1: uniformly adding a sodium hydroxide solution into the fluoroniobate solution;
s2: the fluoroniobate and the sodium hydroxide solution are fully mixed and reacted in the long tube pass and the reaction kettle to obtain superfine niobium hydroxide, sodium fluoride and excessive sodium hydroxide;
s3: filtering the mixed reaction product by using a membrane filtering device, intercepting niobium hydroxide colloid by using the membrane filtering device, and filtering out sodium fluoride and excessive sodium hydroxide;
s4: adding pure water into the reaction kettle for dilution and washing to obtain a niobium hydroxide diluted solution, and circularly washing and filtering the niobium hydroxide diluted solution by using a membrane filtering device;
s5: and repeating S4 until the salt and alkali content is lower than the product purity requirement.
Example 2
S1: uniformly adding a potassium hydroxide solution into the fluoroniobate solution;
s2: the fluoroniobate and the potassium hydroxide solution are fully mixed and reacted in a long pipe pass and a reaction kettle to obtain superfine niobium hydroxide, potassium fluoride and excessive potassium hydroxide;
s3: filtering the mixed reaction product by using a membrane filtering device, intercepting niobium hydroxide colloid by using the membrane filtering device, and filtering out potassium fluoride and excessive potassium hydroxide;
s4: adding pure water into the reaction kettle for dilution and washing to obtain a niobium hydroxide diluted solution, and circularly washing and filtering the niobium hydroxide diluted solution by using a membrane filtering device;
s5: and repeating S4 until the salt and alkali content is lower than the product purity requirement.
Example 3
As shown in fig. 1, the present invention also provides an apparatus for producing ultra-fine niobium hydroxide, comprising: reation kettle 1, circulating pump 3, dilute alkali injection device, mixing reactor, membrane filter equipment 5, reation kettle 1's bottom through mixing pipe 2 with circulating pump 3's entry links to each other, circulating pump 3's exit is equipped with two branch pipelines, and two branch pipelines link to each other with mixing reactor, membrane filter equipment 5's entry end respectively, all be equipped with return line on mixing reactor, the membrane filter equipment 5, return line links to each other with reation kettle 1's top, the last switch switching valve 9 that is equipped with of return line, dilute alkali injection device passes through the connecting pipe and links to each other with mixing pipe 2's middle part, and dilute alkali injection device includes: the device comprises a dilute alkali storage tank 6 and a metering pump 7, wherein the bottom of the dilute alkali storage tank 6 is connected with the metering pump 7, the metering pump 7 is connected with the middle part of a mixing pipe 2 through a connecting pipe, and the pipelines at the bottoms of a reaction kettle 1, a dilute alkali injection device, a mixing reactor and a membrane filtering device 5 are all provided with switch switching valves 9.
Adding a potassium fluoroniobate solution into a reaction kettle 1, opening a switch switching valve 9 at the bottom of the reaction kettle 1, a dilute alkali injection device and a mixing reactor, closing the switch switching valve 9 at the bottom of a membrane filtering device 5, starting a circulating pump 3 to inject the potassium fluoroniobate into a mixing pipe 2, simultaneously opening a metering pump 7 to inject a sodium hydroxide solution into the mixing pipe 2 to be mixed with the potassium fluoroniobate solution and to be conveyed into the mixing reactor together, closing the switch switching valve 9 at the bottom of the dilute alkali injection device after the sodium hydroxide is injected, and easily enabling the sodium hydroxide solution and the potassium fluoroniobate to circularly flow and react in the reaction kettle 1 and the mixing reactor; after the reaction is finished, closing a switch switching valve 9 at the bottom of the mixing reactor, simultaneously opening the switch switching valve 9 at the bottom of the membrane filtering device 5, pumping the niobium hydroxide, the potassium fluoride, the sodium fluoride and the residual sodium hydroxide into the membrane filtering device 5 by using the circulating pump 3, injecting pure water into the reaction kettle 1 to wash the niobium hydroxide after the niobium hydroxide is concentrated to 15-20% by using the membrane filtering device 5, and performing circulating filtration; and repeating the washing and filtering operations for a plurality of times until the purity of the retained niobium hydroxide reaches the requirement.
In order to further limit the production equipment of the ultrafine niobium hydroxide, the membrane filtration device 5 of the invention specifically adopts a silicon carbide membrane for filtration, the bottom of the membrane filtration device 5 is provided with a mixed liquid inlet, the top of the membrane filtration device 5 is provided with a trapped liquid outlet, the side of the membrane filtration device 5 is provided with a filtrate outlet, the mixed liquid inlet is communicated with the circulating pump 3, the return pipeline is communicated with the trapped liquid outlet, and the filtrate outlet is connected with a post-treatment device. Niobium hydroxide, potassium fluoride, sodium fluoride and the rest sodium hydroxide enter the membrane filtration device 5 from the mixed liquid inlet together, the niobium hydroxide is intercepted and returns to the reaction kettle 1 from the intercepted liquid outlet, and the potassium fluoride, the sodium fluoride and the rest sodium hydroxide are filtered out and discharged from the filtrate outlet for post-treatment.
In order to make the potassium fluoroniobate fully contact with the sodium hydroxide and accelerate the reaction rate, stirring devices 8 are arranged in the reaction kettle 1 and the dilute alkali storage tank 6.
In order to improve the tube pass that potassium fluoroniobate and sodium hydroxide are easy to mix, the mixing reactor of the invention comprises: the reaction barrel 401 is vertically arranged, a plurality of horizontally arranged baffle plates 402 are arranged on the inner side wall of the reaction barrel 401, and the interior of the reaction barrel 401 is divided into serpentine channels through the baffle plates 402. The potassium fluoroniobate in the reaction kettle 1 is accurately matched with the sodium hydroxide and then is subjected to a primary reaction through a long tube pass, and the potassium fluoroniobate and the sodium hydroxide are matched and then return to the reaction kettle 1 again for a dynamic mixing reaction.
Example 4
As shown in FIG. 2, the present invention provides an ultrafine niobium hydroxide production apparatus, and compared to example 1, the mixing reactor of the present invention comprises: the reaction barrel 401 is internally provided with a reaction coil 403 with turbulent flow.
The rest of the structure was the same as in example 3.
Example 5
Compared with the embodiment 3, the invention provides the superfine niobium hydroxide production equipment, a back washing device is arranged at the position of the filtrate discharge port of the membrane filtering device 5, and the back washing device carries out back washing on the membrane filtering device 5 by using pure water, so that the membrane filtering device is prevented from being blocked.
The rest of the structure was the same as in example 3.
Example 6
As shown in fig. 3, compared with example 3, the present invention further provides a filtering forced circulation pump 10, wherein two ends of the filtering forced circulation pump 10 are respectively connected to the inlet of the membrane filtering device and the outlet of the trapped fluid, and the filtering forced circulation pump 10 is arranged to increase the flow velocity of the membrane surface to accelerate the filtering process.
The rest of the structure was the same as in example 3.
It should be noted that the above-mentioned embodiments are only for illustrating the technical solutions of the present invention and not for limiting, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, which should be covered by the claims of the present invention.
Claims (10)
1. A preparation method of superfine niobium hydroxide adopts fluoroniobate as a raw material, and is characterized by comprising the following steps:
s1: uniformly adding a dilute alkali solution into the fluoroniobate solution;
s2: the fluoroniobate and the dilute alkali solution are fully mixed and reacted in a long pipe pass and a reaction kettle to obtain superfine niobium hydroxide, water-soluble salt and excessive alkali;
s3: filtering the mixed reaction product by using a membrane filtering device, intercepting niobium hydroxide colloid by using the membrane filtering device, and filtering out water-soluble salt and excessive alkali;
s4: adding pure water into the reaction kettle for dilution and washing to obtain a niobium hydroxide diluted solution, and circularly washing and filtering the niobium hydroxide diluted solution by using a membrane filtering device;
s5: and repeating S4 until the salt and alkali content is lower than the product purity requirement.
2. The method as claimed in claim 1, wherein the dilute alkali solution comprises one of the following: sodium hydroxide solution, potassium hydroxide solution.
3. The production equipment of the superfine niobium hydroxide is characterized by comprising the following steps: reation kettle (1), circulating pump (3), dilute alkali injection device, hybrid reactor, membrane filter equipment (5), the bottom of reation kettle (1) through mixing material pipe (2) with the entry of circulating pump (3) links to each other, the exit of circulating pump (3) is equipped with two branch pipelines, and two branch pipelines link to each other with the entry end of hybrid reactor, membrane filter equipment (5) respectively, all be equipped with return line on hybrid reactor, the membrane filter equipment (5), return line links to each other with the top of reation kettle (1), the last switch switching valve (9) that is equipped with of return line, dilute alkali injection device passes through the connecting pipe and links to each other with the middle part of mixing material pipe (2).
4. The ultrafine niobium hydroxide production equipment according to claim 3, wherein the membrane filtration device (5) is specifically a silicon carbide membrane for filtration, the bottom of the membrane filtration device (5) is provided with a mixed liquid inlet, the top of the membrane filtration device (5) is provided with a retentate outlet, the side of the membrane filtration device (5) is provided with a filtrate outlet, the mixed liquid inlet is communicated with the circulating pump (3), the return pipeline is communicated with the retentate outlet, and the filtrate outlet is connected with a post-treatment device.
5. The apparatus for producing ultra-fine niobium hydroxide as claimed in claim 4, wherein the dilute alkali injection device comprises: the device comprises a dilute alkali storage tank (6) and a metering pump (7), wherein the bottom of the dilute alkali storage tank (6) is connected with the metering pump (7), and the metering pump (7) is connected with the middle part of the mixing pipe (2) through a connecting pipe.
6. The equipment for producing ultra-fine niobium hydroxide as claimed in claim 5, wherein the reaction kettle (1) and the dilute alkali storage tank (6) are equipped with stirring devices (8).
7. The apparatus for producing ultra-fine niobium hydroxide as claimed in claim 6, wherein the mixing reactor comprises: the reaction barrel (401) is characterized in that a plurality of horizontally arranged baffle plates (402) are arranged on the inner side wall of the reaction barrel (401), and the reaction barrel (401) is internally divided into serpentine channels through the baffle plates (402).
8. The apparatus for producing ultra-fine niobium hydroxide as claimed in claim 6, wherein the mixing reactor comprises: the reaction barrel (401), install reaction coil pipe (403) that the vortex set up in reaction barrel (401).
9. The production equipment of ultra-fine niobium hydroxide as claimed in claim 6, wherein the pipelines of the material inlet and outlet of the reaction kettle (1), the dilute alkali injection device, the mixing reactor and the membrane filtration device (5) are all provided with switch valves (9).
10. The apparatus for producing ultrafine niobium hydroxide as claimed in claim 6, wherein a back-flushing device is installed at the filtrate discharge port.
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