CN107754753A - A kind of cupric phosphate sorbing material and preparation method thereof - Google Patents
A kind of cupric phosphate sorbing material and preparation method thereof Download PDFInfo
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- CN107754753A CN107754753A CN201711228350.3A CN201711228350A CN107754753A CN 107754753 A CN107754753 A CN 107754753A CN 201711228350 A CN201711228350 A CN 201711228350A CN 107754753 A CN107754753 A CN 107754753A
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Abstract
The present invention relates to a kind of cupric phosphate sorbing material, CuO content is 56~60wt%, PO2Content be 32~35wt%, the average grain diameter of cupric phosphate particle is 220~260nm.Preparation method, copper nitrate is mixed with deionized water, and stir a period of time, obtain primary solution；Ammonium hydrogen phosphate and deionized water are mixed, and also stirring a period of time；Sodium hydroxide is added into solution, continues stirring a period of time, obtains secondary solution；The secondary solution is quickly adding into the primary solution, is then aged, the mixed liquor after ageing is placed in water bath heating device, continues stirring a period of time, is then filtrated to get primary stage solids product；The primary stage solids product is washed with deionized, a period of time is then dried, obtains secondary solid product；The secondary solid product is put into roasting kiln roasting, then obtains cupric phosphate sorbing material.Cupric phosphate impurity content of the present invention is small, and purity is high, and uniform particle sizes' degree is good, has good adsorption capacity for xanthate.
Description
Technical field
The present invention relates to the field of Environment Protection of beneficiation wastewater processing, specially a kind of cupric phosphate 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 cupric phosphate sorbing material, CuO content are
56~60wt%, PO2Content be 32~35wt%, the average grain diameter of cupric phosphate particle is 220~260nm.
Preferably, the average grain diameter of cupric phosphate particle is 230~250nm.
As further preferred, the average grain diameter of cupric phosphate particle is 240~245nm.
The present invention also provides a kind of method for preparing the cupric phosphate sorbing material, comprises the following steps：
(1) copper nitrate is mixed with deionized water, and stirs a period of time, obtain primary solution；
(2) ammonium hydrogen phosphate and deionized water are mixed, and also stirring a period of time；
(3) sodium hydroxide is added in solution into step (2), continues stirring a period of time, obtain secondary solution；
(4) the secondary solution is quickly adding into the primary solution, is then aged 4~6h, obtains mixed liquor；
(5) mixed liquor after ageing is placed in water bath heating device, continues stirring a period of time, be then filtrated to get just
Level solid product；
(6) the primary stage solids product is washed with deionized, a period of time is then dried, obtains secondary solid
Product；
(7) the secondary solid product is put into roasting kiln roasting, then obtains cupric phosphate sorbing material.
Preferably, copper nitrate and deionized water are according to (2.2~3) in step (1)：The ratio mixing of (8.5~9), is adopted
With 10~15min of magnetic agitation.
Preferably, ammonium hydrogen phosphate and deionized water are according to (2.5~3.2) in step (2)：The ratio of (9.3~10.2)
Mixing, using 5~8min of magnetic agitation.
Preferably, step (3) in add sodium hydroxide to pH be 8~8.8, using 5~6min of magnetic agitation.
Preferably, the temperature of heating water bath is 50~60 DEG C in step (5), continue 12~14h of stirring.
Preferably, deionized water is washed 3~5 times in step (6), the drying temperature is 90~100 DEG C, drying time
For 2~3h.
Preferably, sintering temperature is 600~850 DEG C in step (7), roasting time is 5~6h.
The present invention has the following advantages that compared with prior art：Cupric phosphate 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 cupric phosphate of the present invention for xanthate
The adsorbent of water, cupric phosphate have good adsorption capacity as a kind of efficient novel nano sorbing material for xanthate；This
Invention also provides the preparation method of cupric phosphate, 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 nitrate and deionized water according to 2.2：8.5 ratio mixing, and magnetic agitation 10min is used, obtain primary
Solution.By ammonium hydrogen phosphate and deionized water according to 2.5：9.3 ratio mixing, and also uses magnetic agitation 5min, then to solution
Middle addition sodium hydroxide regulation pH value is 8, continues to use magnetic agitation 5min, obtains secondary solution.The secondary solution is fast
Speed is added in the primary solution, is then aged 4h, obtains mixed liquor.Mixed liquor after ageing is placed in water bath heating device
In, the temperature of heating water bath is 50 DEG C, continues to stir 12h, is then filtrated to get primary stage solids product.The primary stage solids are produced
Thing is washed with deionized 3 times, and a period of time is then dried, and drying temperature is 90 DEG C, drying time 2h, obtains secondary
Solid product.The secondary solid product is put into roasting kiln roasting, sintering temperature is 600 DEG C, roasting time 5h, then
Obtain cupric phosphate sorbing material.The cupric phosphate sorbing material, CuO content is 56~60wt%, PO2Content for 32~
35wt%, the average grain diameter of cupric phosphate particle is 220nm.After testing, the cupric phosphate is far above to the saturated extent of adsorption of xanthate and lived
Property charcoal, resin etc. other be directed to the adsorbent of xanthate waste water, illustrate cupric phosphate as a kind of efficiently novel nano sorbing material,
There is good adsorption capacity for xanthate.
Embodiment 2：
By copper nitrate and deionized water according to 2.6：8.8 ratio mixing, and magnetic agitation 12min is used, obtain primary
Solution.By ammonium hydrogen phosphate and deionized water according to 3：10 ratio mixing, and magnetic agitation 6min is also used, then add into solution
It is 8.5 to enter sodium hydroxide regulation pH value, continues to use magnetic agitation 6min, obtains secondary solution.The secondary solution is rapid
It is added in the primary solution, is then aged 5h, obtains mixed liquor.Mixed liquor after ageing is placed in water bath heating device
In, the temperature of heating water bath is 55 DEG C, continues to stir 13h, is then filtrated to get primary stage solids product.The primary stage solids are produced
Thing is washed with deionized 4 times, and a period of time is then dried, and drying temperature is 95 DEG C, drying time 2.5h, obtains secondary
Level solid product.The secondary solid product is put into roasting kiln roasting, sintering temperature is 700 DEG C, roasting time 6h, so
After obtain cupric phosphate sorbing material.The cupric phosphate sorbing material, CuO content is 56~60wt%, PO2Content for 32~
35wt%, the average grain diameter of cupric phosphate particle is 230nm.After testing, the cupric phosphate is far above to the saturated extent of adsorption of xanthate and lived
Property charcoal, resin etc. other be directed to the adsorbent of xanthate waste water, illustrate cupric phosphate as a kind of efficiently novel nano sorbing material,
There is good adsorption capacity for xanthate.
Embodiment 3：
By copper nitrate and deionized water according to 3：9 ratio mixing, and magnetic agitation 15min is used, obtain primary solution.
By ammonium hydrogen phosphate and deionized water according to 3.2：10.2 ratio mixing, and magnetic agitation 8min is also used, then add into solution
It is 8.8 to enter sodium hydroxide regulation pH value, continues to use magnetic agitation 6min, obtains secondary solution.The secondary solution is rapid
It is added in the primary solution, is then aged 6h, obtains mixed liquor.Mixed liquor after ageing is placed in water bath heating device
In, the temperature of heating water bath is 60 DEG C, continues to stir 14h, is then filtrated to get primary stage solids product.The primary stage solids are produced
Thing is washed with deionized 5 times, and a period of time is then dried, and drying temperature is 100 DEG C, drying time 3h, obtains secondary
Level solid product.The secondary solid product is put into roasting kiln roasting, sintering temperature is 850 DEG C, roasting time 6h, so
After obtain cupric phosphate sorbing material.The cupric phosphate sorbing material, CuO content is 56~60wt%, PO2Content for 32~
35wt%, the average grain diameter of cupric phosphate particle is 260nm.After testing, the cupric phosphate is far above to the saturated extent of adsorption of xanthate and lived
Property charcoal, resin etc. other be directed to the adsorbent of xanthate waste water, illustrate cupric phosphate as a kind of efficiently novel nano sorbing material,
There is good adsorption capacity for xanthate.
Embodiment 4：
By copper nitrate and deionized water according to 3：8.5 ratio mixing, and magnetic agitation 14min is used, obtain primary molten
Liquid.By ammonium hydrogen phosphate and deionized water according to 3.2：9.3 ratio mixing, and magnetic agitation 7min is also used, then into solution
It is 8.6 to add sodium hydroxide regulation pH value, continues to use magnetic agitation 5min, obtains secondary solution.The secondary solution is fast
Speed is added in the primary solution, is then aged 5h, obtains mixed liquor.Mixed liquor after ageing is placed in water bath heating device
In, the temperature of heating water bath is 50 DEG C, continues to stir 13h, is then filtrated to get primary stage solids product.The primary stage solids are produced
Thing is washed with deionized 5 times, and a period of time is then dried, and drying temperature is 100 DEG C, drying time 2h, obtains secondary
Level solid product.The secondary solid product is put into roasting kiln roasting, sintering temperature is 800 DEG C, roasting time 5h, so
After obtain cupric phosphate sorbing material.The cupric phosphate sorbing material, CuO content is 56~60wt%, PO2Content for 32~
35wt%, the average grain diameter of cupric phosphate particle is 250nm.After testing, the cupric phosphate is far above to the saturated extent of adsorption of xanthate and lived
Property charcoal, resin etc. other be directed to the adsorbent of xanthate waste water, illustrate cupric phosphate as a kind of efficiently novel nano sorbing material,
There is good adsorption capacity for xanthate.
Embodiment 5：
By copper nitrate and deionized water according to 2.2：9 ratio mixing, and magnetic agitation 11min is used, obtain primary molten
Liquid.By ammonium hydrogen phosphate and deionized water according to 2.5：10.2 ratio mixing, and magnetic agitation 8min is also used, then into solution
It is 8.4 to add sodium hydroxide regulation pH value, continues to use magnetic agitation 6min, obtains secondary solution.The secondary solution is fast
Speed is added in the primary solution, is then aged 6h, obtains mixed liquor.Mixed liquor after ageing is placed in water bath heating device
In, the temperature of heating water bath is 60 DEG C, continues to stir 12h, is then filtrated to get primary stage solids product.The primary stage solids are produced
Thing is washed with deionized 4 times, and a period of time is then dried, and drying temperature is 95 DEG C, drying time 3h, obtains secondary
Solid product.The secondary solid product is put into roasting kiln roasting, sintering temperature is 650 DEG C, roasting time 6h, then
Obtain cupric phosphate sorbing material.The cupric phosphate sorbing material, CuO content is 56~60wt%, PO2Content for 32~
35wt%, the average grain diameter of cupric phosphate particle is 240~245nm.After testing, the cupric phosphate is far high to the saturated extent of adsorption of xanthate
The adsorbent that other are directed to xanthate waste water in activated carbon, resin etc., illustrate that cupric phosphate adsorbs as a kind of efficient novel nano
Material, there is 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. cupric phosphate sorbing material, it is characterised in that：CuO content is 56~60wt%, PO2Content for 32~ 35wt%, the average grain diameter of cupric phosphate particle is 220~260nm.
- 2. material according to claim 1, it is characterised in that：The average grain diameter of cupric phosphate particle is 230~250nm.
- 3. material according to claim 2, it is characterised in that：The average grain diameter of cupric phosphate particle is 240~245nm.
- 4. a kind of method for preparing cupric phosphate sorbing material any one of claims 1 to 3, comprises the following steps：(1) copper nitrate is mixed with deionized water, and stirs a period of time, obtain primary solution；(2) ammonium hydrogen phosphate and deionized water are mixed, and also stirring a period of time；(3) sodium hydroxide is added in solution into step (2), continues stirring a period of time, obtain secondary solution；(4) the secondary solution is quickly adding into the primary solution, is then aged 4~6h, obtains mixed liquor；(5) mixed liquor after ageing is placed in water bath heating device, continues stirring a period of time, be then filtrated to get primary solid Body product；(6) the primary stage solids product is washed with deionized, a period of time is then dried, obtain secondary solid production Thing；(7) the secondary solid product is put into roasting kiln roasting, then obtains cupric phosphate sorbing material.
- 5. according to the method for claim 4, in step (1) copper nitrate with deionized water according to (2.2~3)：(8.5~9) Ratio mixing, using 10~15min of magnetic agitation.
- 6. according to the method for claim 4, in step (2) ammonium hydrogen phosphate and deionized water according to (2.5~3.2)：(9.3 ~10.2) ratio mixing, using 5~8min of magnetic agitation.
- 7. the method according to claim 11, the middle addition sodium hydroxide of step (3) to pH is 8~8.8, using magnetic agitation 5 ~6min.
- 8. according to the method for claim 4, the temperature of heating water bath is 50~60 DEG C in step (5), continue stirring 12~ 14h。
- 9. according to the method for claim 4, deionized water is washed 3~5 times in step (6), the drying temperature is 90~ 100 DEG C, drying time is 2~3h.
- 10. according to the method for claim 4, sintering temperature is 600~850 DEG C in step (7), roasting time is 5~6h.
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|---|---|---|---|---|
| CN110171811A (en) * | 2019-06-10 | 2019-08-27 | 河南大学 | A kind of preparation method of heat-staple cupric phosphate crystalline nanometric materials |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105148845A (en) * | 2015-10-09 | 2015-12-16 | 承德新华炭业集团有限公司 | Preparation method of YMSC composite water purification material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105148845A (en) * | 2015-10-09 | 2015-12-16 | 承德新华炭业集团有限公司 | Preparation method of YMSC composite water purification material |
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| 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"", 《X技术-最新专利-物理化学装置的制造及其应用技术》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110171811A (en) * | 2019-06-10 | 2019-08-27 | 河南大学 | A kind of preparation method of heat-staple cupric phosphate crystalline nanometric materials |
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Application publication date: 20180306 |