CN107930574A - A kind of alkali formula copper tungstate sorbing material and preparation method thereof - Google Patents
A kind of alkali formula copper tungstate sorbing material and preparation method thereof Download PDFInfo
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- CN107930574A CN107930574A CN201711231267.1A CN201711231267A CN107930574A CN 107930574 A CN107930574 A CN 107930574A CN 201711231267 A CN201711231267 A CN 201711231267A CN 107930574 A CN107930574 A CN 107930574A
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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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- 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
- B01J20/0218—Compounds of Cr, Mo, W
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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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28016—Particle form
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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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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/40—Organic compounds containing sulfur
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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
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/10—Nature of the water, waste water, sewage or sludge to be treated from quarries or from mining activities
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The present invention relates to a kind of alkali formula copper tungstate sorbing material, the content of CuO is 25~30wt%, WO2Content be 10~19wt%, the average grain diameter of alkali formula copper tungstate particle is 6~10nm.Preparation method, primary solvent is hybridly prepared into by 1 propyl alcohol and deionized water;Copper chloride and potassium hydroxide are mixed, add primary solvent, then stirring a period of time, low speed concussion a period of time is then carried out in earthquake device again, obtains primary solution;Sodium tungstate is mixed with primary solvent, is then added in primary solution, then stirring a period of time, then earthquake device high speed shakes the first segment time again, obtains secondary solution;Secondary solution is put into autoclave, autoclave is positioned in baking oven and is reacted, then natural cooling, primary stage solids product is obtained by filtration;Primary stage solids product is washed with deionized, is dried to obtain alkali formula copper tungstate sorbing material.Alkali formula copper tungstate impurity content of the present invention is small, and purity is high, and uniform particle sizes' degree is good, to xanthate excellent adsorption.
Description
Technical field
The present invention relates to the field of environment protection of beneficiation wastewater processing, is specially a kind of alkali formula copper tungstate sorbing material and its preparation
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, has become the livelihood issues of maximum, adjusts industry knot
Structure, stringent 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 is directly discharged 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 generally exist
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 the 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 alkali formula copper tungstate sorbing material, CuO's contains
Measure as 25~30wt%, the content of WO2 is 10~19wt%, and the average grain diameter of alkali formula copper tungstate particle is 6~10nm.
Preferably, the average grain diameter of alkali formula copper tungstate particle is 7~9nm.
As further preferred, the average grain diameter of alkali formula copper tungstate particle is 7~8nm.
The present invention also provides a kind of method for preparing the alkali formula copper tungstate sorbing material, comprise the following steps:
(1) 1- propyl alcohol and deionized water are hybridly prepared into primary solvent;
(2) copper chloride and potassium hydroxide are mixed, adds the primary solvent, then stirring a period of time, Ran Houzai
Low speed concussion a period of time is carried out in earthquake device, obtains primary solution;
(3) sodium tungstate is mixed with the primary solvent, is then added in the primary solution, then stir one section
Time, then earthquake device high speed shakes the first segment time again, obtains secondary solution;
(4) the secondary solution is put into autoclave, autoclave is positioned in baking oven and reacts a period of time, then certainly
So cooling, is obtained by filtration primary stage solids product;
(5) the primary stage solids product is washed with deionized, a period of time is then dried, obtains alkali formula wolframic acid
Polluted by copper material.
Preferably, 1- propyl alcohol and deionized water are according to (4~5) in step (1):The ratio mixing of (1~2).
Preferably, copper chloride and potassium hydroxide are according to (2~3) in step (2):The ratio mixing of (1.5~2);It is described
Mixing time is 20~30min;The low speed concussion time is 30~40min.
Preferably, sodium tungstate and the primary solvent are according to 2 in step (3):1 ratio mixing;The mixing time
For 35~45min, the high speed concussion time is 40~50min.
Preferably, it is 100~120 DEG C that autoclave is positioned in baking oven temperature in step (4), the reaction time for 24~
26h。
Preferably, drying temperature described in step (5) is 60~70 DEG C, drying time is 6~7h.
Preferably, step (5) intermediate ion water washing 3~5 times.
The present invention has the following advantages that compared with prior art:Alkali formula copper tungstate impurity content of the present invention is small, and purity is high, grain
Footpath good evenness, pattern are good;Alkali formula copper tungstate of the present invention is to the saturated extent of adsorption of xanthate far above other pins such as activated carbon, resins
To the adsorbent of xanthate waste water, alkali formula copper tungstate has fine as a kind of efficient novel nano sorbing material for xanthate
Adsorption capacity;The present invention also provides the preparation method of alkali formula copper tungstate, technique is simple, equipment is uncomplicated, and reaction condition is easy
Reach, reaction is also easy to control;Method is environmentally protective, and energy consumption is small, it is easy to accomplish industrial-scale production.
Embodiment
In order to make the technical means, the creative features, the aims and the efficiencies achieved by the present invention easy to understand, tie below
Specific embodiment is closed, the present invention is further explained.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 1- propyl alcohol and deionized water according to 4:1 ratio is hybridly prepared into primary solvent;By copper chloride and potassium hydroxide
According to 2:1.5 ratio mixing, adds the primary solvent, then stirs 20min, then carry out low speed in earthquake device again
30min is shaken, obtains primary solution.By sodium tungstate and the primary solvent according to 2:1 ratio mixing, is then added to described first
In level solution, 35min is then stirred, then earthquake device high speed shakes 40min again, obtains secondary solution.By the secondary
Solution is put into autoclave, and autoclave is positioned in baking oven and reacts a period of time, and temperature is 100 DEG C in baking oven, the reaction time
For 24h, then natural cooling, is obtained by filtration primary stage solids product.The primary stage solids product is washed with deionized 3 times,
Then a period of time is dried, drying temperature is 60 DEG C, drying time 6h, obtains alkali formula copper tungstate sorbing material.The alkali
The content of CuO is 25~30wt%, WO in formula copper tungstate sorbing material2Content be 10~19wt%, alkali formula copper tungstate particle
Average grain diameter be 6nm.After testing, the alkali formula copper tungstate to the saturated extent of adsorption of xanthate far above activated carbon, resin etc. other
For the adsorbent of xanthate waste water, illustrate that alkali formula copper tungstate as a kind of efficient novel nano sorbing material, has for xanthate
There is good adsorption capacity.
Embodiment 2:
By 1- propyl alcohol and deionized water according to 4.5:1.5 ratio is hybridly prepared into primary solvent;By copper chloride and hydrogen-oxygen
Change potassium according to 2.5:1.8 ratio mixing, add the primary solvent, then stir 25min, then again in earthquake device into
Row low speed shakes 35min, obtains primary solution.By sodium tungstate and the primary solvent according to 2:1 ratio mixing, is then added to
In the primary solution, 40min is then stirred, then earthquake device high speed shakes 45min again, obtains secondary solution.By institute
State secondary solution to be put into autoclave, autoclave is positioned in baking oven and reacts a period of time, temperature is 110 DEG C in baking oven, instead
It is 25h between seasonable, then natural cooling, is obtained by filtration primary stage solids product.The primary stage solids product is washed with deionized water
Wash 4 times, a period of time is then dried, drying temperature is 65 DEG C, drying time 6.5h, obtains alkali formula copper tungstate adsorption material
Material.The content of CuO is 25~30wt%, WO in the alkali formula copper tungstate sorbing material2Content be 10~19wt%, alkali formula wolframic acid
The average grain diameter of copper particle is 7nm.After testing, which is far above activated carbon, resin to the saturated extent of adsorption of xanthate
The adsorbent of xanthate waste water is directed to Deng other, illustrate alkali formula copper tungstate as a kind of efficiently novel nano sorbing material, for
Xanthate has good adsorption capacity.
Embodiment 3:
By 1- propyl alcohol and deionized water according to 5:2 ratio is hybridly prepared into primary solvent;By copper chloride and potassium hydroxide
According to 3:2 ratio mixing, adds the primary solvent, then stirs 30min, then carry out low speed shake in earthquake device again
40min is swung, obtains primary solution.By sodium tungstate and the primary solvent according to 2:1 ratio mixing, is then added to the primary
In solution, 45min is then stirred, then earthquake device high speed shakes 50min again, obtains secondary solution.The secondary is molten
Liquid is put into autoclave, and autoclave is positioned in baking oven and reacts a period of time, and temperature is 120 DEG C in baking oven, and the reaction time is
26h, then natural cooling, is obtained by filtration primary stage solids product.The primary stage solids product is washed with deionized 5 times, so
After be dried a period of time, drying temperature be 70 DEG C, drying time 7h, obtain alkali formula copper tungstate sorbing material.The alkali formula
The content of CuO is 25~30wt%, WO in copper tungstate sorbing material2Content be 10~19wt%, alkali formula copper tungstate particle
Average grain diameter is 8nm.After testing, which is far above other pins such as activated carbon, resin to the saturated extent of adsorption of xanthate
To the adsorbent of xanthate waste water, illustrate that alkali formula copper tungstate as a kind of efficient novel nano sorbing material, has for xanthate
Good adsorption capacity.
Embodiment 4:
By 1- propyl alcohol and deionized water according to 4:2 ratio is hybridly prepared into primary solvent;By copper chloride and potassium hydroxide
According to 2:1.6 ratio mixing, adds the primary solvent, then stirs 26min, then carry out low speed in earthquake device again
38min is shaken, obtains primary solution.By sodium tungstate and the primary solvent according to 2:1 ratio mixing, is then added to described first
In level solution, 42min is then stirred, then earthquake device high speed shakes 48min again, obtains secondary solution.By the secondary
Solution is put into autoclave, and autoclave is positioned in baking oven and reacts a period of time, and temperature is 110 DEG C in baking oven, the reaction time
For 25h, then natural cooling, is obtained by filtration primary stage solids product.The primary stage solids product is washed with deionized 5 times,
Then a period of time is dried, drying temperature is 60 DEG C, drying time 6h, obtains alkali formula copper tungstate sorbing material.The alkali
The content of CuO is 25~30wt%, WO in formula copper tungstate sorbing material2Content be 10~19wt%, alkali formula copper tungstate particle
Average grain diameter be 9nm.After testing, the alkali formula copper tungstate to the saturated extent of adsorption of xanthate far above activated carbon, resin etc. other
For the adsorbent of xanthate waste water, illustrate that alkali formula copper tungstate as a kind of efficient novel nano sorbing material, has for xanthate
There is good adsorption capacity.
Embodiment 5:
By 1- propyl alcohol and deionized water according to 5:1 ratio is hybridly prepared into primary solvent;By copper chloride and potassium hydroxide
According to 3:1.7 ratio mixing, adds the primary solvent, then stirs 24min, then carry out low speed in earthquake device again
34min is shaken, obtains primary solution.By sodium tungstate and the primary solvent according to 2:1 ratio mixing, is then added to described first
In level solution, 45min is then stirred, then earthquake device high speed shakes 45min again, obtains secondary solution.By the secondary
Solution is put into autoclave, and autoclave is positioned in baking oven and reacts a period of time, and temperature is 120 DEG C in baking oven, the reaction time
For 24h, then natural cooling, is obtained by filtration primary stage solids product.The primary stage solids product is washed with deionized 3 times,
Then a period of time is dried, drying temperature is 68 DEG C, drying time 7h, obtains alkali formula copper tungstate sorbing material.The alkali
The content of CuO is 25~30wt%, WO in formula copper tungstate sorbing material2Content be 10~19wt%, alkali formula copper tungstate particle
Average grain diameter be 10nm.After testing, the alkali formula copper tungstate to the saturated extent of adsorption of xanthate far above activated carbon, resin etc. other
For the adsorbent of xanthate waste water, illustrate that alkali formula copper tungstate as a kind of efficient novel nano sorbing material, has for xanthate
There is good adsorption capacity.
The basic principle and main feature 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 above embodiments and description only describe this
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. alkali formula copper tungstate sorbing material, it is characterised in that:The content of CuO is 25~30wt%, WO2Content for 10~ 19wt%, the average grain diameter of alkali formula copper tungstate particle is 6~10nm.
- 2. material according to claim 1, it is characterised in that:The average grain diameter of alkali formula copper tungstate particle is 7~9nm.
- 3. material according to claim 2, it is characterised in that:The average grain diameter of alkali formula copper tungstate particle is 7~8nm.
- 4. a kind of method for preparing alkali formula copper tungstate sorbing material any one of claims 1 to 3, comprises the following steps:(1) 1- propyl alcohol and deionized water are hybridly prepared into primary solvent;(2) copper chloride and potassium hydroxide are mixed, adds the primary solvent, then stirring a period of time, then shaken again Swing and low speed concussion a period of time is carried out in device, obtain primary solution;(3) sodium tungstate is mixed with the primary solvent, is then added in the primary solution, when then stirring one section Between, then earthquake device high speed shakes the first segment time again, obtains secondary solution;(4) the secondary solution is put into autoclave, autoclave is positioned in baking oven and reacts a period of time, it is then naturally cold But, primary stage solids product is obtained by filtration;(5) the primary stage solids product is washed with deionized, a period of time is then dried, obtain the suction of alkali formula copper tungstate Enclosure material.
- 5. according to the method described in claim 4,1- propyl alcohol and deionized water are according to (4~5) in step (1):The ratio of (1~2) Example mixing.
- 6. according to the method described in claim 4, copper chloride and potassium hydroxide are according to (2~3) in step (2):(1.5~2) Ratio mixes;The mixing time is 20~30min;The low speed concussion time is 30~40min.
- 7. according to the method described in claim 4, sodium tungstate and the primary solvent are according to 2 in step (3):1 ratio mixing; The mixing time is 35~45min, and the high speed concussion time is 40~50min.
- 8. according to the method described in claim 4, it is 100~120 DEG C that autoclave is positioned in baking oven temperature in step (4), Reaction time is 24~26h.
- 9. according to the method described in claim 4, drying temperature described in step (5) is 60~70 DEG C, drying time for 6~ 7h。
- 10. according to the method described in claim 4, step (5) intermediate ion water washing 3~5 times.
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CN109279654A (en) * | 2018-12-06 | 2019-01-29 | 盐城工学院 | A kind of preparation method of copper wolframic acid |
Citations (1)
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CN106064832A (en) * | 2016-07-05 | 2016-11-02 | 陕西科技大学 | A kind of nanoscale cuboid alkali formula copper molybdate and preparation method thereof |
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CN106064832A (en) * | 2016-07-05 | 2016-11-02 | 陕西科技大学 | A kind of nanoscale cuboid alkali formula copper molybdate and preparation method thereof |
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: "一种碱式钨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 (1)
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CN109279654A (en) * | 2018-12-06 | 2019-01-29 | 盐城工学院 | A kind of preparation method of copper wolframic acid |
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