CN106276827B - The method for preparing tantalum nitride oxide catalysis material using waste and old tantalum capacitor - Google Patents
The method for preparing tantalum nitride oxide catalysis material using waste and old tantalum capacitor Download PDFInfo
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- CN106276827B CN106276827B CN201610552294.8A CN201610552294A CN106276827B CN 106276827 B CN106276827 B CN 106276827B CN 201610552294 A CN201610552294 A CN 201610552294A CN 106276827 B CN106276827 B CN 106276827B
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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
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
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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
- 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
- C01B3/04—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
- C01B3/042—Decomposition of water
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
A method of tantalum nitride oxide catalysis material is prepared using waste and old tantalum capacitor, comprising the following steps: various waste and old tantalum capacitors are subjected to Mechanical Crushing shelling;Then separation metal with it is nonmetallic;Magnetic separation is carried out to metalliferous material and separates ferronickel magnetic material;Screening is obtained containing tantalum powder;It handles to obtain tantalic chloride to chlorination is carried out containing tantalum powder;Tantalic chloride is then dissolved in alcoholic solution, logical ammonia precipitation ammonium chloride, the alcoholic solution of tantalum is obtained by filtration;It hydrolyzes the alcoholic solution of tantalum to obtain tantalum oxide colloidal sol again, be dried to obtain tantalum oxide gel;High-temperature calcination under tantalum oxide gel ammonia atmosphere is obtained into tantalum nitride oxide catalysis material.The advantages that present invention needs to tantalum ore stone using waste and old tantalum capacitor, reduction preparation photocatalysis tantalum material in the market and recycles ferronickel electrode therein.
Description
Technical field
The present invention relates to waste and old tantalum capacitor resource treatment technique fields, utilize waste and old tantalum capacitor more particularly, to a kind of
The method for preparing visible light-responded tantalum nitride oxide catalysis material.
Background technique
Currently, semiconductor light-catalyst is used for organic matter degradation, water process, air cleaning etc. has obtained widely answering
With, but often forbidden band is wider for the semiconductor of many chemical stabilizations, function admirable, is only capable of uptake zone ultraviolet light, 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 valence
Value.The band gap of TaON is relatively narrow (2.5eV), stablizes during light-catalyzed reaction, molten containing suitable electron donor and receptor
Release while can be realized hydrogen and oxygen in liquid.Moreover, the conduction band current potential of TaON is slightly more negative than standard hydrogen electrode current potential, for-
0.3V, and its valence band current potential is slightly just than oxygen electrode current potential, is+2.2V, therefore can satisfy 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 TaON is a kind of very promising semiconductor material, its raw material tantalum (Ta) is your a kind of dilute gold
Belong to, content is only 7/10000000ths in the earth's crust.Ta is in periodic table of chemical element Zhong Shu VB race, atomic number 73, chemically
Matter and niobium of the same clan are closely similar.Therefore tantalum and niobium usually close symbiosis in nature.Purity of the semiconductor material to itself
There is very high requirement, therefore needs to carry out Ta purification process usually to obtain high-purity Ta2O5, then again to Ta2O5Carry out ammonification
It handles and obtains TaON.Ta can consume a large amount of energy and chemical reagent during purifying, thus bring some serious rings
Border problem.Simultaneously as the fast development of semiconductor material, the demand of TaON causes the consumption of tantalum to be continuously increased in turn.
On the other hand, tantalum capacitor contains 45% Ta, these tantalums have been typically free of niobium, therefore tantalum capacitor is a kind of high
The Ta resource of quality.Correlative study shows that there are about the generations of 4.5 hundred million tons of electronic waste in the annual whole world, while producing a large amount of
Waste and old tantalum capacitor.It, not only can be real if preparing visible light-responded TaON catalysis material using waste and old tantalum capacitor
The resource reutilization of existing waste and old tantalum capacitor solves environmental problem, can also bring huge economic benefit.However, not having also at present
About the report for preparing visible light-responded TaON catalysis material using waste and old tantalum capacitor.
Currently, preparation TaON catalysis material is usually to calcine high purity tantalum oxide in ammonia atmosphere high temperature.However, high
Pure tantalum oxide is expensive, so that TaON catalysis material is restricted in industrial application.Waste and old tantalum capacitor is a kind of honest and clean
The high-quality tantalum resources of valence, if developing set of environmental close friend, the economically viable side for preparing TaON from waste and old tantalum capacitor
Method will bring huge economy and environmental benefit.Therefore, how it is environmental-friendly recycle tantalum from waste and old tantalum capacitor, and
TaON catalysis material is prepared as urgent problem with the tantalum success of recycling.
Summary of the invention
The present invention a kind of prepares visible light-responded TaON photocatalysis using waste and old tantalum capacitor in view of the above-mentioned problems, providing
The method of material.Various waste and old tantalum capacitors are carried out Mechanical Crushing shelling by this method;Then separation metal with it is nonmetallic;To gold
Belong to material and carries out magnetic separation separation ferronickel magnetic material;Screening obtains powder containing Ta;Chlorination is carried out to powder containing Ta to handle to obtain
TaCl5;Then by TaCl5It is dissolved in alcoholic solution, logical ammonia precipitation ammonium chloride (removing removing chloride), the alcoholic solution of Ta is obtained by filtration;Again
It hydrolyzes the alcoholic solution of Ta to obtain Ta2O5Colloidal sol is dried to obtain Ta2O5Gel;Finally, by Ta2O5High temperature under gel ammonia atmosphere
Calcining obtains TaON catalysis material.
To achieve the above object, the present invention includes the following steps:
Step 1: waste and old tantalum capacitor being subjected to Mechanical Crushing, the average grain diameter of material is 0.5~0.01mm after being crushed, and is broken
It is broken the resin enclosure of tantalum capacitor, while will be completely dissociated metal with nonmetallic;
Step 2: will it is broken after metal in material and it is nonmetallic separate, obtain metalliferous material;
Step 3: metalliferous material being subjected to magnetic separation, separates nickel, iron;Then screening obtains tantalum and is enriched with powder;
Step 4: tantalum enrichment powder being placed in tube furnace, chlorination is carried out and handles to obtain TaCl5;
Step 5: by TaCl5It is dissolved in alcoholic solution, ammonia is passed through and generates ammonium chloride crystals to remove removing chloride, Ta is obtained by filtration
Alcoholic solution;
Step 6: hydrolyzing the alcoholic solution of Ta to obtain Ta2O5Colloidal sol is dried to obtain Ta2O5Gel;
Step 7: finally by Ta2O5Gel high-temperature calcination under ammonia atmosphere obtains TaON catalysis material.
The step 1 Mechanical Crushing method includes ball mill or hammer breaking machine.
It by the method that metalliferous material is separated with non-metallic material include electrostatic separation or hydraulic cyclone point in the step 2
Choosing.
Chlorination reaction in the step 4, specifically: control 50~100ml/min of argon flow, tantalum are enriched with powder and chlorine
Salt quality ratio is 1:1~4, and reaction temperature is 400~650 DEG C, and the reaction time is 0.5~4h.
The chemical equation of chlorination reaction in step 4 are as follows:
2Ta+5MCl2=2TaCl5+ 5M (M is metal)
With villaumite chlorination reaction does not occur for other substances of tantalum enrichment powder in step 4;The tantalic chloride boiling point of generation is
231.4 DEG C, so tantalic chloride can volatilize away with argon gas in a gaseous form under chlorination temperature, as a result it is condensate in tantalic chloride receipts
In storage.
The alcoholic solution of the step 5 can be ethyl alcohol, n-butanol or isopropanol.
25~40 DEG C of the hydrolysis temperature of the step 6,3~8h of hydrolysis time;80~120 DEG C of drying temperature, drying time 6
~12h.
50~100ml/min of step 7 ammonia flow;500~800 DEG C of calcination temperature, 2~4h of calcination time.
Compared with prior art, the beneficial effects of the present invention are:
1) waste and old tantalum capacitor, reduction preparation photocatalysis tantalum material in the market is made full use of to need and return tantalum ore stone
The advantages that receiving ferronickel electrode therein.
2) tantalum nitride oxide prepared has very high photocatalytic activity under visible light, in photolysis water hydrogen, air cleaning
And sewage treatment etc. has broad application prospects and economic benefit.
Detailed description of the invention
Fig. 1 is the flow diagram 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.
Specific embodiment
The present invention is described in detail combined with specific embodiments below.Following embodiment will be helpful to the technology of this field
Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that the ordinary skill of this field
For personnel, without departing from the inventive concept of the premise, it can also make certain adjustments and improvements.These belong to the present invention
Protection scope.
Embodiment 1
The method for preparing visible light-responded TaON catalysis material described in the present patent application with waste and old tantalum capacitor, packet
Include following step:
1. Mechanical Crushing: taking 10g tantalum content is the waste and old tantalum capacitor of 35.9% resin-encapsulate, and analysis result is as follows:
Ta:35.9%, Ag:0.3%, Ni:2.08%, Fe:3.85%.Waste and old tantalum capacitor is crushed using ball mill and is put down
The material that equal partial size is 0.5~0.01mm;
2. broken material is carried out electrostatic separation, make metal and nonmetallic separation;
3. metalliferous material is carried out magnetic separation, nickel, iron are separated;Then screening obtains Ta and is enriched with powder;
4. Ta enrichment powder is placed in tube furnace, carries out chlorination and handle to obtain TaCl5.Control argon flow is 50ml/
Min, Ta are enriched with powder and villaumite mass ratio is 1:1, and reaction temperature is 500 DEG C, reaction time 4h;
5. by TaCl5It is dissolved in ethanol solution, ammonia is passed through and generates ammonium chloride crystals to remove removing chloride, the alcohol for obtaining Ta is molten
Liquid;
6. by the alcoholic solution hydrolysis of Ta, being dried to obtain Ta2O5Gel.25 DEG C of hydrolysis temperature of control, hydrolysis time 7h;It is dry
80 DEG C of temperature, drying time 12h;
7. by Ta2O5Gel high-temperature calcination obtains TaON catalysis material.Control ammonia flow 50ml/min, calcination temperature
500 DEG C, calcination time 4h.Obtain the TaON that quality is about 4.3g.
Obtained TaON is detected according to GB/T15076-2008 regulation, testing result is that the purity of TaON is greater than
99.9%.TaON is provided to carry out the detection of photocatalytic hydrogen production by water decomposition rate according to GB/T26915-2011.Test result such as Fig. 2
Shown, the maximum rate for producing hydrogen is about 5.5 μm of ol/h.
Comparative example
" a kind of preparation method of tantalum nitride oxide catalysis material " (Zhang Qinghong, application number CN201510020555.7)
1. 1g ta powder is distributed in 40ml deionized water at room temperature, the hydrofluoric acid that 1ml is added after being uniformly dispersed is molten
Liquid (concentration 40%) and 4ml hydrogenperoxide steam generator (concentration 30%) form reaction solution;
2. above-mentioned reaction solution is put into water heating kettle, it is warming up to 160 DEG C of reaction 12h;
3. products therefrom is cooled to room temperature, product is collected by centrifugation, washed product is dried, grinding;
4. above-mentioned gained powder is put in tube furnace and is warming up to 850 DEG C, 10h, the stream of ammonia are nitrogenized in ammonia atmosphere
Amount is 100ml/min, and gained powder, which is put in Muffle furnace, is warming up to 500 DEG C, keeps the temperature 30min.Obtain catalysis material γ-
TaON。
By comparative example, the present invention using step 4~7 prepare tantalum nitride oxide have the advantage that it is low using price
Raw material of the honest and clean tantalum capacitor as tantalum, save the cost, and effectively realize the resource utilization of waste and old tantalum capacitor;System
Standby when containing tantalum solution, selects environmental-friendly villaumite and alcoholic solution to avoid using the dirt of environment caused by the strong oxidizers such as strong acid
Dye;In hydrolysis and heat treatment process temperature is low, the time is short, saved the energy;The tantalum nitride oxide purity is high of preparation, in visible light
There is down preferable photocatalysis performance.
Embodiment 2
The method for preparing visible light-responded TaON catalysis material described in the present patent application with waste and old tantalum capacitor, packet
Include following steps:
1. Mechanical Crushing: taking 10g tantalum content is the waste and old tantalum capacitor of 35.9% resin-encapsulate, and analysis result is as follows:
Ta:35.9%, Ag:0.3%, Ni:2.08%, Fe:3.85%.Waste and old tantalum capacitor is carried out using hammer breaking machine broken
The material for being 0.5~0.01mm to average grain diameter;
2. broken material is carried out hydraulic cyclone sorting, make metal and nonmetallic separation;
3. metalliferous material is carried out magnetic separation, nickel, iron are separated;Then screening obtains Ta and is enriched with powder;
4. Ta enrichment powder is placed in tube furnace, carries out chlorination and handle to obtain TaCl5.Control argon flow is 80ml/
Min, Ta are enriched with powder and villaumite mass ratio is 1:2, and reaction temperature is 600 DEG C, reaction time 2h;
5. by TaCl5It is dissolved in ethanol solution, ammonia is passed through and generates ammonium chloride crystals to remove removing chloride, the alcohol for obtaining Ta is molten
Liquid;
6. by the alcoholic solution hydrolysis of Ta, being dried to obtain Ta2O5Gel.30 DEG C of hydrolysis temperature of control, hydrolysis time 6h;It is dry
100 DEG C of temperature, drying time 10h;
7. by Ta2O5Gel high-temperature calcination obtains TaON catalysis material.Control ammonia flow 80ml/min, calcination temperature
700 DEG C, calcination time 3h.Obtain the TaON that quality is about 4.0g.
Obtained TaON is detected according to GB/T15076-2008 regulation, testing result is that the purity of TaON is greater than
99.9%.TaON is provided to carry out the detection of photocatalytic hydrogen production by water decomposition rate according to GB/T26915-2011.Test result such as Fig. 2
Shown, the maximum rate for producing hydrogen is about 4.3 μm of ol/h.
Embodiment 3
The method for preparing visible light-responded TaON catalysis material described in the present patent application with waste and old tantalum capacitor, packet
Include following steps:
1. Mechanical Crushing: taking 10g tantalum content is the waste and old tantalum capacitor of 35.9% resin-encapsulate, and analysis result is as follows:
Ta:35.9%, Ag:0.3%, Ni:2.08%, Fe:3.85%.Waste and old tantalum capacitor is carried out using hammer breaking machine broken
The material for being 0.5~0.01mm to average grain diameter;
2. broken material is carried out electrostatic separation, make metal and nonmetallic separation;
3. metalliferous material is carried out magnetic separation, nickel, iron are separated;Then screening obtains Ta and is enriched with powder;
4. Ta enrichment powder is placed in tube furnace, carries out chlorination and handle to obtain TaCl5.Control argon flow is 100ml/
Min, Ta are enriched with powder and villaumite mass ratio is 1:3, and reaction temperature is 650 DEG C, reaction time 1h;
5. by TaCl5It is dissolved in ethanol solution, ammonia is passed through and generates ammonium chloride crystals to remove removing chloride, the alcohol for obtaining Ta is molten
Liquid;
6. by the alcoholic solution hydrolysis of Ta, being dried to obtain Ta2O5Gel.40 DEG C of hydrolysis temperature of control, hydrolysis time 4h;It is dry
120 DEG C of temperature, drying time 8h;
7. by Ta2O5Gel high-temperature calcination obtains TaON catalysis material.Control ammonia flow 100ml/min, calcination temperature
800 DEG C, calcination time 2h.Obtain the TaON that quality is about 3.9g.
Obtained TaON is detected according to GB/T15076-2008 regulation, testing result is that the purity of TaON is greater than
99.9%.TaON is provided to carry out the detection of photocatalytic hydrogen production by water decomposition rate according to GB/T26915-2011.Test result such as Fig. 2
Shown, the maximum rate for producing hydrogen is about 3.7 μm of ol/h.
Claims (7)
1. a kind of method for preparing tantalum nitride oxide catalysis material using waste and old tantalum capacitor, which is characterized in that this method includes
The following steps:
Step 1: waste and old tantalum capacitor being subjected to Mechanical Crushing, the average grain diameter of material is 0.5~0.01mm after being crushed, and destroys tantalum
The resin enclosure of capacitor will be completely dissociated metal with nonmetallic;
Step 2: will it is broken after metal in material and it is nonmetallic separate, obtain metalliferous material;
Step 3: metalliferous material being subjected to magnetic separation, separates nickel, iron;Then screening obtains tantalum and is enriched with powder;
Step 4: tantalum enrichment powder being placed in tube furnace, chlorination is carried out and handles to obtain tantalic chloride;
Step 5: tantalic chloride being dissolved in alcoholic solution, ammonia is passed through and generates ammonium chloride crystals to go removing chloride, then, be obtained by filtration
The alcoholic solution of tantalum;
Step 6: the alcoholic solution of tantalum being hydrolyzed after obtaining tantalum oxide colloidal sol, tantalum oxide gel is dried to obtain;
Step 7: by tantalum oxide gel, high-temperature calcination obtains tantalum nitride oxide catalysis material under ammonia atmosphere.
2. the method for preparing tantalum nitride oxide catalysis material using waste and old tantalum capacitor as described in claim 1, feature exist
In the Mechanical Crushing method in the step 1 uses ball mill or hammer breaking machine.
3. the method for preparing tantalum nitride oxide catalysis material using waste and old tantalum capacitor as described in claim 1, feature exist
In by the method that metalliferous material is separated with non-metallic material including that electrostatic separation or hydraulic cyclone sort in the step 2.
4. the method for preparing tantalum nitride oxide catalysis material using waste and old tantalum capacitor as described in claim 1, feature exist
In the chlorination reaction of the step 4, specifically: 50~100mL/min of argon flow, tantalum are enriched with powder with villaumite mass ratio and are
1:1~4, reaction temperature are 400~650 DEG C, and the reaction time is 0.5~4h.
5. the method for preparing tantalum nitride oxide catalysis material using waste and old tantalum capacitor as described in claim 1, feature exist
In the alcoholic solution of the step 5 is ethyl alcohol, n-butanol or isopropanol.
6. the method for preparing tantalum nitride oxide catalysis material using waste and old tantalum capacitor as described in claim 1, feature exist
In, 25~40 DEG C of the hydrolysis temperature of the step 6,3~8h of hydrolysis time;80~120 DEG C of drying temperature, drying time 6~
12h。
7. the method for preparing tantalum nitride oxide catalysis material using waste and old tantalum capacitor as described in claim 1, feature exist
In 50~100mL of step 7 ammonia flow/min;500~800 DEG C of calcination temperature, 2~4h of calcination time.
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2016
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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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