CN107774226A - A kind of copper tungstate sorbing material and preparation method thereof - Google Patents
A kind of copper tungstate sorbing material and preparation method thereof Download PDFInfo
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- CN107774226A CN107774226A CN201711230023.1A CN201711230023A CN107774226A CN 107774226 A CN107774226 A CN 107774226A CN 201711230023 A CN201711230023 A CN 201711230023A CN 107774226 A CN107774226 A CN 107774226A
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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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0233—Compounds of Cu, Ag, Au
- B01J20/0237—Compounds of Cu
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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Abstract
The present invention relates to a kind of copper tungstate sorbing material, CuO content is 52~61wt%, WO2Content be 25~30wt%, the average grain diameter of copper tungstate particle is 0.4~0.6 μm.Preparation method, comprise the following steps：Copper sulphate is mixed with deionized water, then ultrasound a period of time, obtains primary solution；Sodium tungstate and deionized water are mixed, then ultrasound a period of time, obtain secondary solution；The primary solution is mixed with the secondary solution, then ultrasound a period of time, obtains mixed solution；The mixed solution is aged；Solution after ageing is filtered, washed, a period of time is then dried, obtains primary stage solids product；The primary stage solids product is put into roasting kiln roasting, then obtains copper tungstate sorbing material.Copper tungstate impurity content of the present invention is small, and purity is high, and uniform particle sizes' degree is good, has good adsorption capacity to xanthate.
Description
Technical field
The present invention relates to the field of Environment Protection of beneficiation wastewater processing, specially a kind of copper tungstate sorbing material and its preparation side
Method.
Background technology
China has reached its maturity, past since reform and opening-up with the introduction and domestic market environment of foreign technology
In 30 years, industry is able to swift and violent development.Advancing triumphantly for industry promotes the rapid development of economy, but can not be ignored, for a long time
Since, Industry Structure heavy industrialization causes the high consumption of resource, the energy, and high pollution is caused to environment.Atmosphere pollution, industry
The harm of waste water drastically influence the health of people.Pollution, have become the livelihood issues of maximum, adjust industry knot
Structure, strict energy-saving and emission-reduction are very urgent.
Pillar of the mining industry as Chinese national economy, consumes substantial amounts of water resource every year.It is reported that the whole world is every year by floating
The ore of choosing processing has 2,000,000,000 tons, accordingly also generates substantial amounts of flotation waste water, wherein sulfide flotation, which can produce, largely contains
The waste water of xanthate, xanthate are that maximally efficient and extensive collecting agent is used in sulfide flotation.Most of xanthate can be with flotation
End enters froth pulp, if the remaining xanthate in waste water directly discharges without processing, very big harm can be caused to environment.
At present, in terms of the improvement both at home and abroad for xanthate waste water is concentrated mainly on contamination control, chemical breakdown, absorption, biological decomposition etc.
Method is applied to remove remaining xanthate.These method intention are novel, respectively have quality, such as chemical method can typically be present
The problem of secondary pollution, and biological wayss need to spend longer time degraded xanthate, it is less efficient.Absorption method adsorption efficiency
It is of a relatively high and pollution-free, therefore be increasingly promoted in the treatment of waste water.But the common adsorbent for xanthate waste water is total
Body and practical application also have certain distance.
Therefore the necessary material for exploring remaining xanthate in a kind of new practicable removal flotation waste water.
The content of the invention
The shortcomings that for above-mentioned prior art, the present invention provide a kind of ore dressing xanthate wastewater treatment green, cost is low
Material and preparation method thereof.
The present invention solves above-mentioned technical problem and uses following technical scheme：A kind of copper tungstate sorbing material, CuO content are
52~61wt%, WO2Content be 25~30wt%, the average grain diameter of copper tungstate particle is 0.4~0.6 μm.
Preferably, the average grain diameter of copper tungstate particle is 0.45~0.55 μm.
As further preferred, the average grain diameter of copper tungstate particle is 0.46~0.50 μm.
The present invention also provides a kind of method for preparing the copper tungstate sorbing material, comprises the following steps：
(1) copper sulphate is mixed with deionized water, then ultrasound a period of time, obtains primary solution；
(2) sodium tungstate and deionized water are mixed, then ultrasound a period of time, obtains secondary solution；
(3) primary solution is mixed with the secondary solution, then ultrasound a period of time, obtains mixed solution；
(4) mixed solution is aged；
(5) solution after ageing is filtered, washed, a period of time is then dried, obtains primary stage solids product；
(6) the primary stage solids product is put into roasting kiln roasting, then obtains copper tungstate sorbing material.
Preferably, copper sulphate and deionized water are according to (1~2) in step (1)：The ratio mixing of (5~6), ultrasound 5~
8min。
Preferably, sodium tungstate and deionized water are according to (1.2~1.5) in step (2)：The ratio mixing of (5~6), surpasses
5~8min of sound.
Preferably, primary solution described in step (3) and the secondary solution are according to 1:1 ratio mixing, ultrasound 1~
2h。
Preferably, 12~14h is aged at normal temperatures in step (4).
Preferably, drying temperature described in step (5) is 70~80 DEG C, drying time is 2~3h, ion water washing 3
~5 times.
Preferably, sintering temperature is 500~800 DEG C in step (6), roasting time is 2~3h.
The present invention has the following advantages that compared with prior art：Copper tungstate impurity content of the present invention is small, and purity is high, and particle diameter is equal
Evenness is good, and pattern is good；To the saturated extent of adsorption of xanthate, far above activated carbon, resin etc., other give up copper tungstate of the present invention for xanthate
The adsorbent of water, copper tungstate have good adsorption capacity as a kind of efficient novel nano sorbing material for xanthate；This
Invention also provides the preparation method of copper tungstate, and technique is simple, equipment is uncomplicated, and reaction condition easily reaches, and reaction is also easy to control；
Method is green, and energy consumption is small, it is easy to accomplish industrial-scale production.
Embodiment
In order that the technical means, the inventive features, the objects and the advantages of the present invention are easy to understand, tie below
Specific embodiment is closed, the present invention is expanded on further.It should be appreciated that specific embodiment described herein is only explaining this hair
It is bright, it is not intended to limit the present invention.
Embodiment 1：
By copper sulphate and deionized water according to 1：5 ratio mixing, then ultrasonic 5min, obtains primary solution.By wolframic acid
Sodium and deionized water are according to 1.2：5 ratio mixing, then ultrasonic 5min, obtains secondary solution.By the primary solution and institute
Secondary solution is stated according to 1:1 ratio mixing, then ultrasonic 1h, obtains mixed solution.The mixed solution is aged
12h, the solution after ageing is filtered, be washed with deionized 3 times, be then dried, drying temperature is 70 DEG C, is dried
Time is 2h, obtains primary stage solids product；The primary stage solids product is put into roasting kiln roasting, sintering temperature is 500 DEG C,
Roasting time is 2h, then obtains copper tungstate sorbing material.The copper tungstate sorbing material, CuO content is 52~61wt%,
WO2Content be 25~30wt%, the average grain diameter of copper tungstate particle is 0.4 μm.After testing, saturation of the copper tungstate to xanthate
Far above activated carbon, resin etc., other are directed to the adsorbent of xanthate waste water to adsorbance, illustrate copper tungstate as it is a kind of it is efficient newly
Type nano adsorption material, there is good adsorption capacity for xanthate.
Embodiment 2：
By copper sulphate and deionized water according to 1.5：5.5 ratio mixing, then ultrasonic 6min, obtains primary solution.Will
Sodium tungstate and deionized water are according to 1.4：5.5 ratio mixing, then ultrasonic 7min, obtains secondary solution.The primary is molten
Liquid is with the secondary solution according to 1:1 ratio mixing, then ultrasonic 1.5h, obtains mixed solution.The mixed solution is entered
Row ageing 13h, the solution after ageing is filtered, is washed with deionized 4 times, is then dried, drying temperature 75
DEG C, drying time 2.5h, obtain primary stage solids product；The primary stage solids product is put into roasting kiln roasting, roasting temperature
Spend for 600 DEG C, roasting time 2.5h, then obtain copper tungstate sorbing material.The copper tungstate sorbing material, CuO content are
52~61wt%, WO2Content be 25~30wt%, the average grain diameter of copper tungstate particle is 0.45 μm.After testing, the copper tungstate
To the saturated extent of adsorption of xanthate, far above activated carbon, resin etc., other are directed to the adsorbent of xanthate waste water, illustrate copper tungstate conduct
A kind of efficient novel nano sorbing material, has good adsorption capacity for xanthate.
Embodiment 3：
By copper sulphate and deionized water according to 2：6 ratio mixing, then ultrasonic 8min, obtains primary solution.By wolframic acid
Sodium and deionized water are according to 1.5：6 ratio mixing, then ultrasonic 8min, obtains secondary solution.By the primary solution and institute
Secondary solution is stated according to 1:1 ratio mixing, then ultrasonic 2h, obtains mixed solution.The mixed solution is aged
14h, the solution after ageing is filtered, be washed with deionized 5 times, be then dried, drying temperature is 80 DEG C, is dried
Time is 3h, obtains primary stage solids product；The primary stage solids product is put into roasting kiln roasting, sintering temperature is 800 DEG C,
Roasting time is 3h, then obtains copper tungstate sorbing material.The copper tungstate sorbing material, CuO content is 52~61wt%,
WO2Content be 25~30wt%, the average grain diameter of copper tungstate particle is 0.6 μm.After testing, saturation of the copper tungstate to xanthate
Far above activated carbon, resin etc., other are directed to the adsorbent of xanthate waste water to adsorbance, illustrate copper tungstate as it is a kind of it is efficient newly
Type nano adsorption material, there is good adsorption capacity for xanthate.
Embodiment 4：
By copper sulphate and deionized water according to 2：5 ratio mixing, then ultrasonic 7min, obtains primary solution.By wolframic acid
Sodium and deionized water are according to 1.5：5 ratio mixing, then ultrasonic 6min, obtains secondary solution.By the primary solution and institute
Secondary solution is stated according to 1:1 ratio mixing, then ultrasonic 1h, obtains mixed solution.The mixed solution is aged
12h, the solution after ageing is filtered, be washed with deionized 5 times, be then dried, drying temperature is 78 DEG C, is dried
Time is 2h, obtains primary stage solids product；The primary stage solids product is put into roasting kiln roasting, sintering temperature is 700 DEG C,
Roasting time is 3h, then obtains copper tungstate sorbing material.The copper tungstate sorbing material, CuO content is 52~61wt%,
WO2Content be 25~30wt%, the average grain diameter of copper tungstate particle is 0.55 μm.After testing, the copper tungstate is satisfied to xanthate
Far above activated carbon, resin etc., other are directed to the adsorbent of xanthate waste water with adsorbance, illustrate copper tungstate as it is a kind of efficiently
Novel nano sorbing material, there is good adsorption capacity for xanthate.
Embodiment 5：
By copper sulphate and deionized water according to 1：6 ratio mixing, then ultrasonic 8min, obtains primary solution.By wolframic acid
Sodium and deionized water are according to 1.2：6 ratio mixing, then ultrasonic 5min, obtains secondary solution.By the primary solution and institute
Secondary solution is stated according to 1:1 ratio mixing, then ultrasonic 2h, obtains mixed solution.The mixed solution is aged
12h, the solution after ageing is filtered, be washed with deionized 4 times, be then dried, drying temperature is 75 DEG C, is dried
Time is 3h, obtains primary stage solids product；The primary stage solids product is put into roasting kiln roasting, sintering temperature is 600 DEG C,
Roasting time is 3h, then obtains copper tungstate sorbing material.The copper tungstate sorbing material, CuO content is 52~61wt%,
WO2Content be 25~30wt%, the average grain diameter of copper tungstate particle is 0.46~0.50 μm.After testing, the copper tungstate is to Huang
Far above activated carbon, resin etc., other are directed to the adsorbent of xanthate waste water to the saturated extent of adsorption of medicine, illustrates copper tungstate as one kind
Efficient novel nano sorbing material, has good adsorption capacity for xanthate.
The general principle and principal character and advantages of the present invention of the present invention, the technology of the industry has been shown and described above
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the simply explanation described in above-described embodiment and specification is originally
The principle of invention, without departing from the spirit and scope of the present invention, various changes and modifications of the present invention are possible, these changes
Change and improvement all fall within the protetion scope of the claimed invention, the claimed scope of the invention by appended claims and its
Equivalent thereof.
Claims (10)
- A kind of 1. copper tungstate sorbing material, it is characterised in that：CuO content is 52~61wt%, WO2Content for 25~ 30wt%, the average grain diameter of copper tungstate particle is 0.4~0.6 μm.
- 2. material according to claim 1, it is characterised in that：The average grain diameter of copper tungstate particle is 0.45~0.55 μm.
- 3. material according to claim 2, it is characterised in that：The average grain diameter of copper tungstate particle is 0.46~0.50 μm.
- 4. a kind of method for preparing copper tungstate sorbing material any one of claims 1 to 3, comprises the following steps：(1) copper sulphate is mixed with deionized water, then ultrasound a period of time, obtains primary solution；(2) sodium tungstate and deionized water are mixed, then ultrasound a period of time, obtains secondary solution；(3) primary solution is mixed with the secondary solution, then ultrasound a period of time, obtains mixed solution；(4) mixed solution is aged；(5) solution after ageing is filtered, washed, a period of time is then dried, obtains primary stage solids product；(6) the primary stage solids product is put into roasting kiln roasting, then obtains copper tungstate sorbing material.
- 5. according to the method for claim 4, in step (1) copper sulphate with deionized water according to (1~2)：The ratio of (5~6) Example mixing, 5~8min of ultrasound.
- 6. according to the method for claim 4, in step (2) sodium tungstate and deionized water according to (1.2~1.5)：(5~6) Ratio mixing, 5~8min of ultrasound.
- 7. according to the method for claim 4, primary solution described in step (3) and the secondary solution are according to 1:1 ratio Example mixing, 1~2h of ultrasound.
- 8. according to the method for claim 4, step is aged 12~14h at normal temperatures in (4).
- 9. according to the method for claim 4, drying temperature described in step (5) be 70~80 DEG C, drying time be 2~ 3h, ion water washing 3~5 times.
- 10. according to the method for claim 4, sintering temperature is 500~800 DEG C in step (6), roasting time is 2~3h.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109279654A (en) * | 2018-12-06 | 2019-01-29 | 盐城工学院 | A kind of preparation method of copper wolframic acid |
| CN113231084A (en) * | 2021-05-21 | 2021-08-10 | 北京理工大学 | Copper tungstate/copper sulfide photocatalyst, preparation method and application |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103223494A (en) * | 2013-03-27 | 2013-07-31 | 河南科技大学 | Preparation method of tungsten copper oxide composite powder through hydro-thermal synthesis |
| CN106745490A (en) * | 2016-12-21 | 2017-05-31 | 沈阳化工大学 | A kind of method of degradable organic pollutant methylene blue |
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2017
- 2017-11-29 CN CN201711230023.1A patent/CN107774226A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103223494A (en) * | 2013-03-27 | 2013-07-31 | 河南科技大学 | Preparation method of tungsten copper oxide composite powder through hydro-thermal synthesis |
| CN106745490A (en) * | 2016-12-21 | 2017-05-31 | 沈阳化工大学 | A kind of method of degradable organic pollutant methylene blue |
Non-Patent Citations (1)
| Title |
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| 百度快照：X技术-最新专利-物理化学装置的制造及其应用技术: "一种磷酸铜吸附材料及其制备方法与流程", 《百度快照：X技术-最新专利-物理化学装置的制造及其应用技术》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109279654A (en) * | 2018-12-06 | 2019-01-29 | 盐城工学院 | A kind of preparation method of copper wolframic acid |
| CN113231084A (en) * | 2021-05-21 | 2021-08-10 | 北京理工大学 | Copper tungstate/copper sulfide photocatalyst, preparation method and application |
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Application publication date: 20180309 |