CN106276827A - Utilize the method that waste and old tantalum capacitor prepares tantalum nitride oxide catalysis material - Google Patents
Utilize the method that waste and old tantalum capacitor prepares tantalum nitride oxide catalysis material Download PDFInfo
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- CN106276827A CN106276827A CN201610552294.8A CN201610552294A CN106276827A CN 106276827 A CN106276827 A CN 106276827A CN 201610552294 A CN201610552294 A CN 201610552294A CN 106276827 A CN106276827 A CN 106276827A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/082—Compounds containing nitrogen and non-metals and optionally metals
- C01B21/0821—Oxynitrides of metals, boron or silicon
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
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Abstract
A kind of method utilizing waste and old tantalum capacitor to prepare tantalum nitride oxide catalysis material, comprises the following steps: various waste and old tantalum capacitors are carried out Mechanical Crushing shelling；It is then peeled off metal with nonmetal；Metalliferous material is carried out magnetic separation separation ferronickel magnetic material；Screening obtains containing tantalum powder；Tantalic chloride is obtained to carrying out chloridized containing tantalum powder；Tantalic chloride is dissolved in alcoholic solution subsequently, logical ammonia separates out ammonium chloride, is filtrated to get the alcoholic solution of tantalum；Again the alcoholic solution hydrolysis of tantalum is obtained tantalum oxide colloidal sol, is dried to obtain tantalum oxide gel；High-temperature calcination under tantalum oxide gel ammonia atmosphere is obtained tantalum nitride oxide catalysis material.The present invention utilizes the waste and old tantalum capacitor on market, minimizing preparation photocatalysis tantalum material need tantalum ore stone and reclaim the advantages such as ferronickel electrode therein.
Description
Technical field
The present invention relates to waste and old tantalum electric capacity resource treatment technique field, especially relate to one and utilize waste and old tantalum capacitor
The method preparing visible light-responded tantalum nitride oxide catalysis material.
Background technology
At present, the aspects such as semiconductor light-catalyst is used for organic matter degradation, and water processes, air cleaning have obtained widely should
With, but the quasiconductor often forbidden band of a lot of chemical stabilization, function admirable is wider, is only capable of uptake zone ultraviolet light, and ultraviolet light is only
Account for the 4% of sunlight.So exploitation has visible light-responded high efficiency photocatalyst, there is important theory significance and practical valency
Value.The band gap of TaON is narrower (2.5eV), stable during light-catalyzed reaction, molten containing suitable electron donor and receptor
Discharge while liquid is capable of hydrogen and oxygen.And, the conduction band current potential of TaON is more negative than standard hydrogen electrode current potential, for-
0.3V, and its valence band current potential is than oxygen electrode current potential the most just, for+2.2V, therefore disclosure satisfy that the redox reaction requirement of water decomposition.
Therefore, TaON is considered as a kind of visible light-responded catalysis material having a extensive future.
Although the TaON the most promising semi-conducting material that is one, but its raw material tantalum (Ta) is a kind of your gold dilute
Belonging to, in the earth's crust, content is only 7/10000000ths.Ta is in periodic table of chemical element Zhong Shu VB race, and atomic number is 73, its chemical
Matter is closely similar with niobium of the same clan.Therefore tantalum and niobium usually closely symbiosis in nature.The semi-conducting material purity to itself
There is the highest requirement, the most usually need Ta to be purified process to obtain high-purity Ta2O5, the most again to Ta2O5Carry out ammonification
Process and obtain TaON.Ta can consume the substantial amounts of energy and chemical reagent during purifying, thus serious ring served by band
Border problem.Simultaneously as the fast development of semi-conducting material, the demand of TaON and then cause the consumption of tantalum to be continuously increased.
On the other hand, tantalum capacitor contains the Ta of 45%, and these tantalums have been typically free of niobium, and therefore tantalum capacitor is a kind of high
The Ta resource of quality.Correlational study shows, the annual whole world there are about the electronic waste of 4.5 hundred million tons and produces, and creates substantial amounts of simultaneously
Waste and old tantalum capacitor.Visible light-responded TaON catalysis material is prepared if, with waste and old tantalum capacitor, not only can be real
The resource reutilization of existing waste and old tantalum capacitor, solution environmental problem, also can bring huge economic benefit.But, the most also do not have
It is related to the report utilizing waste and old tantalum capacitor to prepare visible light-responded TaON catalysis material.
At present, preparation TaON catalysis material is typically high purity tantalum oxide high-temperature calcination in ammonia atmosphere.But, high
Pure tantalum oxide is expensive so that TaON catalysis material is restricted in commercial Application.Waste and old tantalum capacitor is a kind of honest and clean
The high-quality tantalum resources of valency, if developing the set of environmental side preparing TaON from waste and old tantalum capacitor friendly, economically viable
Method will bring huge economy and environmental benefit.Therefore, the most eco-friendly tantalum that reclaims from waste and old tantalum capacitor, and
Prepare TaON catalysis material with the tantalum success reclaimed and become urgent problem.
Summary of the invention
The present invention is directed to the problems referred to above, it is provided that a kind of utilize waste and old tantalum capacitor to prepare visible light-responded TaON photocatalysis
The method of material.Various waste and old tantalum capacitors are carried out Mechanical Crushing shelling by the method；It is then peeled off metal with nonmetal；To gold
Belong to material and carry out magnetic separation separation ferronickel magnetic material；Screening obtains containing Ta powder；Obtain carrying out chloridized containing Ta powder
TaCl5；Subsequently by TaCl5Be dissolved in alcoholic solution, logical ammonia separates out ammonium chloride (removing removing chloride), is filtrated to get the alcoholic solution of Ta；Again
The alcoholic solution of Ta is hydrolyzed and obtains Ta2O5Colloidal sol, it is dried to obtain Ta2O5Gel；Finally, by Ta2O5High temperature under gel ammonia atmosphere
Calcining obtains TaON catalysis material.
For achieving the above object, the present invention comprises the following steps:
Step 1: waste and old tantalum capacitor is carried out Mechanical Crushing, the mean diameter of broken rear material is 0.5～0.01mm, broken
It is broken the resin enclosure of tantalum capacitor, makes metal will be completely dissociated with nonmetal simultaneously；
Step 2: will broken after metal in material and nonmetal separate, it is thus achieved that metalliferous material；
Step 3: metalliferous material carries out magnetic separation, separates nickel, ferrum；Screening subsequently obtains tantalum enrichment powder；
Step 4: tantalum is enriched with powder and is placed in tube furnace, carries out chloridized and obtains TaCl5；
Step 5: by TaCl5Be dissolved in alcoholic solution, be passed through ammonia generate ammonium chloride crystals to remove removing chloride, be filtrated to get Ta
Alcoholic solution；
Step 6: the alcoholic solution of Ta is hydrolyzed and obtains Ta2O5Colloidal sol, it is dried to obtain Ta2O5Gel；
Step 7: finally by Ta2O5Gel high-temperature calcination under ammonia atmosphere obtains TaON catalysis material.
Described step 1 Mechanical Crushing method includes ball mill or hammer breaking machine.
The method that metalliferous material separates with non-metallic material is included that electrostatic separation or hydraulic cyclone divide by described step 2
Choosing.
Chlorination reaction in described step 4, specifically: control argon flow amount 50～100ml/min, tantalum enrichment powder and chlorine
Salt mass ratio is 1:1～4, and reaction temperature is 400～650 DEG C, and the response time is 0.5～4h.
In step 4, the chemical equation of chlorination reaction is:
2Ta+5MCl2=2TaCl5+ 5M (M is metal)
In step 4 tantalum enrichment powder other materials not with villaumite generation chlorination reaction；The tantalic chloride boiling point generated is
231.4 DEG C, so under chlorination temperature, tantalic chloride can volatilize away with argon in a gaseous form, result is condensate in tantalic chloride and receives
In storage.
The alcoholic solution of described step 5 can be ethanol, n-butyl alcohol or isopropanol.
The hydrolysis temperature 25 of described step 6～40 DEG C, hydrolysis time 3～8h；Baking temperature 80～120 DEG C, drying time 6
～12h.
Described step 7 ammonia flow 50～100ml/min；Calcining heat 500～800 DEG C, calcination time 2～4h.
Compared with prior art, the invention has the beneficial effects as follows:
1) make full use of the waste and old tantalum capacitor on market, tantalum ore stone is needed and returns by minimizing preparation photocatalysis tantalum material
Receive the advantages such as ferronickel electrode therein.
2) tantalum nitride oxide prepared has the highest photocatalytic activity under visible light, in photolysis water hydrogen, air cleaning
And the aspect such as sewage disposal has broad application prospects and economic benefit.
Accompanying drawing explanation
Fig. 1 is the schematic flow sheet of the preparation method of the visible light-responded tantalum nitride oxide catalysis material of the present invention；
Fig. 2 is the tantalum nitride oxide photocatalytic hydrogen production by water decomposition rate diagram under visible light illumination of preparation.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in detail.Following example will assist in the technology of this area
Personnel are further appreciated by the present invention, but limit the present invention the most in any form.It should be pointed out that, the ordinary skill to this area
For personnel, without departing from the inventive concept of the premise, it is also possible to make certain adjustments and improvements.These broadly fall into the present invention
Protection domain.
Embodiment 1
The method preparing visible light-responded TaON catalysis material with waste and old tantalum capacitor described in the present patent application, bag
Include the steps:
1. Mechanical Crushing: taking the waste and old tantalum capacitor of the resin-encapsulate that 10g tantalum content is 35.9%, analysis result is as follows:
Ta:35.9%, Ag:0.3%, Ni:2.08%, Fe:3.85%.Waste and old tantalum capacitor employing ball mill is carried out broken being put down
All particle diameters are the material of 0.5～0.01mm；
2. the material after crushing carries out electrostatic separation, makes metal and nonmetal separation；
3. metalliferous material is carried out magnetic separation, separates nickel, ferrum；Screening subsequently obtains Ta and is enriched with powder；
4. Ta is enriched with powder be placed in tube furnace, carries out chloridized and obtain TaCl5.Control argon flow amount is 50ml/
Min, Ta enrichment powder is 1:1 with villaumite mass ratio, and reaction temperature is 500 DEG C, and the response time is 4h；
5. by TaCl5Be dissolved in ethanol solution, be passed through ammonia generate ammonium chloride crystals to remove removing chloride, the alcohol obtaining Ta is molten
Liquid；
6. the alcoholic solution of Ta is hydrolyzed, is dried to obtain Ta2O5Gel.Control hydrolysis temperature 25 DEG C, hydrolysis time 7h；It is dried
Temperature 80 DEG C, drying time 12h；
7. by Ta2O5Gel high-temperature calcination obtains TaON catalysis material.Control ammonia flow 50ml/min, calcining heat
500 DEG C, calcination time 4h.Obtain the TaON that quality is about 4.3g.
Being detected according to GB/T15076-2008 regulation by the TaON obtained, testing result is that the purity of TaON is more than
99.9%.TaON is carried out photocatalytic hydrogen production by water decomposition speed detection according to GB/T26915-2011 regulation.Test result such as Fig. 2
Shown in, the maximum rate producing hydrogen is about 5.5 μm ol/h.
Comparative example
" preparation method of a kind of tantalum nitride oxide catalysis material " (Zhang Qinghong, application number CN201510020555.7)
1. being distributed in 40ml deionized water by 1g ta powder under room temperature, the Fluohydric acid. adding 1ml after being uniformly dispersed is molten
Liquid (concentration 40%) and 4ml hydrogenperoxide steam generator (concentration 30%), form reactant liquor；
2. above-mentioned reactant liquor is put in water heating kettle, be warming up to 160 DEG C of reaction 12h；
3. products therefrom is cooled to room temperature, centrifugal product of collecting, washed product, dry, grind；
4. above-mentioned gained powder body is put in tube furnace and is warming up to 850 DEG C, ammonia atmosphere nitrogenizes 10h, the stream of ammonia
Amount is 100ml/min, and gained powder body is put in Muffle furnace and is warming up to 500 DEG C, is incubated 30min.Obtain catalysis material γ-
TaON。
By comparative example, the present invention uses step 4～7 to prepare tantalum nitride oxide and has the advantage that employing price is low
Honest and clean tantalum capacitor is as the raw material of tantalum, cost-effective, and effectively achieves the recycling of waste and old tantalum capacitor；System
For during containing tantalum solution, eco-friendly villaumite and alcoholic solution is selected to avoid the environment dirt that strong oxidizers such as using strong acid causes
Dye；Temperature in hydrolysis and heat treatment process is low, the time is short, has saved the energy；The tantalum nitride oxide purity of preparation is high, at visible ray
Under there is preferable photocatalysis performance.
Embodiment 2
The method preparing visible light-responded TaON catalysis material with waste and old tantalum capacitor described in the present patent application, bag
Include following steps:
1. Mechanical Crushing: taking the waste and old tantalum capacitor of the resin-encapsulate that 10g tantalum content is 35.9%, analysis result is as follows:
Ta:35.9%, Ag:0.3%, Ni:2.08%, Fe:3.85%.Carry out crushing by waste and old tantalum capacitor employing hammer breaking machine
To the material that mean diameter is 0.5～0.01mm；
2. the material after crushing carries out hydraulic cyclone sorting, makes metal and nonmetal separation；
3. metalliferous material is carried out magnetic separation, separates nickel, ferrum；Screening subsequently obtains Ta and is enriched with powder；
4. Ta is enriched with powder be placed in tube furnace, carries out chloridized and obtain TaCl5.Control argon flow amount is 80ml/
Min, Ta enrichment powder is 1:2 with villaumite mass ratio, and reaction temperature is 600 DEG C, and the response time is 2h；
5. by TaCl5Be dissolved in ethanol solution, be passed through ammonia generate ammonium chloride crystals to remove removing chloride, the alcohol obtaining Ta is molten
Liquid；
6. the alcoholic solution of Ta is hydrolyzed, is dried to obtain Ta2O5Gel.Control hydrolysis temperature 30 DEG C, hydrolysis time 6h；It is dried
Temperature 100 DEG C, drying time 10h；
7. by Ta2O5Gel high-temperature calcination obtains TaON catalysis material.Control ammonia flow 80ml/min, calcining heat
700 DEG C, calcination time 3h.Obtain the TaON that quality is about 4.0g.
Being detected according to GB/T15076-2008 regulation by the TaON obtained, testing result is that the purity of TaON is more than
99.9%.TaON is carried out photocatalytic hydrogen production by water decomposition speed detection according to GB/T26915-2011 regulation.Test result such as Fig. 2
Shown in, the maximum rate producing hydrogen is about 4.3 μm ol/h.
Embodiment 3
The method preparing visible light-responded TaON catalysis material with waste and old tantalum capacitor described in the present patent application, bag
Include following steps:
1. Mechanical Crushing: taking the waste and old tantalum capacitor of the resin-encapsulate that 10g tantalum content is 35.9%, analysis result is as follows:
Ta:35.9%, Ag:0.3%, Ni:2.08%, Fe:3.85%.Carry out crushing by waste and old tantalum capacitor employing hammer breaking machine
To the material that mean diameter is 0.5～0.01mm；
2. the material after crushing carries out electrostatic separation, makes metal and nonmetal separation；
3. metalliferous material is carried out magnetic separation, separates nickel, ferrum；Screening subsequently obtains Ta and is enriched with powder；
4. Ta is enriched with powder be placed in tube furnace, carries out chloridized and obtain TaCl5.Control argon flow amount is 100ml/
Min, Ta enrichment powder is 1:3 with villaumite mass ratio, and reaction temperature is 650 DEG C, and the response time is 1h；
5. by TaCl5Be dissolved in ethanol solution, be passed through ammonia generate ammonium chloride crystals to remove removing chloride, the alcohol obtaining Ta is molten
Liquid；
6. the alcoholic solution of Ta is hydrolyzed, is dried to obtain Ta2O5Gel.Control hydrolysis temperature 40 DEG C, hydrolysis time 4h；It is dried
Temperature 120 DEG C, drying time 8h；
7. by Ta2O5Gel high-temperature calcination obtains TaON catalysis material.Control ammonia flow 100ml/min, calcining heat
800 DEG C, calcination time 2h.Obtain the TaON that quality is about 3.9g.
Being detected according to GB/T15076-2008 regulation by the TaON obtained, testing result is that the purity of TaON is more than
99.9%.TaON is carried out photocatalytic hydrogen production by water decomposition speed detection according to GB/T26915-2011 regulation.Test result such as Fig. 2
Shown in, the maximum rate producing hydrogen is about 3.7 μm ol/h.
Claims (7)
1. one kind utilizes the method that waste and old tantalum capacitor prepares tantalum nitride oxide catalysis material, it is characterised in that the method includes
The following step:
Step 1: waste and old tantalum capacitor is carried out Mechanical Crushing, the mean diameter of broken rear material is 0.5～0.01mm, destroys tantalum
The resin enclosure of capacitor, makes metal will be completely dissociated with nonmetal；
Step 2: will broken after metal in material and nonmetal separate, it is thus achieved that metalliferous material；
Step 3: metalliferous material carries out magnetic separation, separates nickel, ferrum；Screening subsequently obtains tantalum enrichment powder；
Step 4: tantalum is enriched with powder and is placed in tube furnace, carries out chloridized and obtains tantalic chloride；
Step 5: tantalic chloride is dissolved in alcoholic solution, be passed through ammonia generate ammonium chloride crystals to remove removing chloride, then, be filtrated to get
The alcoholic solution of tantalum；
Step 6: the alcoholic solution of tantalum is hydrolyzed after obtaining tantalum oxide colloidal sol, be dried to obtain tantalum oxide gel；
Step 7: the high-temperature calcination under ammonia atmosphere of tantalum oxide gel is obtained tantalum nitride oxide catalysis material.
The preparation method of the most visible light-responded tantalum nitride oxide catalysis material, it is characterised in that institute
The Mechanical Crushing method in step 1 of stating uses ball mill or hammer breaking machine.
The preparation method of the most visible light-responded tantalum nitride oxide catalysis material, it is characterised in that institute
State and the method that metalliferous material separates with non-metallic material is included electrostatic separation or hydraulic cyclone sorting by step 2.
The preparation method of the most visible light-responded tantalum nitride oxide catalysis material, it is characterised in that institute
State the chlorination reaction of step 4, specifically: argon flow amount 50～100ml/min, tantalum enrichment powder and villaumite mass ratio be 1:1～
4, reaction temperature is 400～650 DEG C, and the response time is 0.5～4h.
The preparation method of the most visible light-responded tantalum nitride oxide catalysis material, it is characterised in that institute
The alcoholic solution stating step 5 is ethanol, n-butyl alcohol or isopropanol.
The preparation method of the most visible light-responded tantalum nitride oxide catalysis material, it is characterised in that institute
State the hydrolysis temperature 25 of step 6～40 DEG C, hydrolysis time 3～8h；Baking temperature 80～120 DEG C, drying time 6～12h.
The preparation method of the most visible light-responded tantalum nitride oxide catalysis material, it is characterised in that institute
State step 7 ammonia flow 50～100ml/min；Calcining heat 500～800 DEG C, calcination time 2～4h.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108751148A (en) * | 2018-06-29 | 2018-11-06 | 上海交通大学 | A kind of tantalum nitride oxide (TaOxNy) and/or tantalum nitride (Ta3N5) nano-photocatalyst preparation method |
| CN108855073A (en) * | 2018-06-29 | 2018-11-23 | 上海交通大学 | A kind of niobium lead codope, the preparation method of the titanium dioxide/titanium acid barium nano heterojunction photocatalysis agent of palladium load |
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| KR100327587B1 (en) * | 1999-07-01 | 2002-03-14 | 박종섭 | Method of forming capacitor provided with TaON dielectric layer |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108751148A (en) * | 2018-06-29 | 2018-11-06 | 上海交通大学 | A kind of tantalum nitride oxide (TaOxNy) and/or tantalum nitride (Ta3N5) nano-photocatalyst preparation method |
| CN108855073A (en) * | 2018-06-29 | 2018-11-23 | 上海交通大学 | A kind of niobium lead codope, the preparation method of the titanium dioxide/titanium acid barium nano heterojunction photocatalysis agent of palladium load |
| CN108855073B (en) * | 2018-06-29 | 2021-01-01 | 上海交通大学 | Preparation method of niobium-lead co-doped palladium-loaded titanium dioxide/barium titanate nano heterojunction photocatalyst |
| CN108751148B (en) * | 2018-06-29 | 2022-05-17 | 上海交通大学 | Tantalum oxynitride (TaO)xNy) And/or tantalum nitride (Ta)3N5) Preparation method of nano photocatalyst |
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| CN106276827B (en) | 2018-12-07 |
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