CN106086392A - A kind of for suppressing the passivator of oxidation of pyrite and processing pyritous method based on passivator - Google Patents
A kind of for suppressing the passivator of oxidation of pyrite and processing pyritous method based on passivator Download PDFInfo
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- CN106086392A CN106086392A CN201610546463.7A CN201610546463A CN106086392A CN 106086392 A CN106086392 A CN 106086392A CN 201610546463 A CN201610546463 A CN 201610546463A CN 106086392 A CN106086392 A CN 106086392A
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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Abstract
The invention discloses a kind of for suppressing the passivator of oxidation of pyrite and processing pyritous method based on passivator, passivator includes silane and nano silicon, using passivator to process pyritous method is that pyrite surface is carried out coating film layer, can effectively slow down pyritous oxidation, suppress or slow down the generation of acidic mine waste water from source, the use of this passivator reduces the consumption of organosilan, improve the stability of passivating film, greatly reduce the processing cost of acidic mine waste water, and environmental friendliness.
Description
Technical field
The present invention relates to a kind of passivator for suppressing oxidation of pyrite, particularly to a kind of organosilan/nanometer two
Silicon oxide composite passivant and be used for processing pyrite, from the method for watershed management acidic mine waste water.Belong to Acid mine
Waste water treatment field.
Background technology
Metal sulfide mine can produce substantial amounts of mine tailing, the bacterial attachment in these mine tailings in recovery process
(the most typical such as pyrite), under weathering effect, is susceptible to oxidation reaction and forms acidic mine waste water (AMD).
AMD is generally of stronger acidity, and rich in SO in water body4 2-、Fe3+, and the poisonous and harmful of substantial amounts of bioavailable form
Heavy metal ion, such as lead, arsenic, chromium, copper, cadmium etc..AMD not only can strengthen chemism and the biology of poisonous and harmful heavy metallic element
Utilizability, the most also can cause the acidifying of water body and soil so that the environment remediation after pollution is got up and become more difficult.For
Realizing the control to AMD from source, Chinese scholars proposes " surface passivation method " and processes the mine tailings such as pyrite, and surface is blunt
Change method is to utilize the bacterial attachments such as organic or inorganic passivator and pyrite to react to make its surface form one layer of antioxidation
Film, protects bacterial attachment from microcosmic (individual particle) angle so that it is not oxidized.At numerous pyrite passivator
In, organosilan is because having feature safe and reliable, nontoxic, pollution-free, that resistance to oxidation, water proofing property are strong and the concern of extremely people.
At present, there are employing siloxanes passivating metallic surfaces, the method preventing burning.But siloxanes passivator makes
There is the defect of some essence during with, 1) the minimizing problem of organosilan consumption.Organosilan can realize metal watch
Face is passivated, and mainly forms one layer of reticular membrane by the cross-linked polymeric of Si-O-Si key between silane molecule, then passes through Si-O-
Me key (Me is metallic element) firmly adsorbs in metal surface.Therefore, for making organosilane passivating film in processing procedure enough
Densification, the organosilan concentration added is the highest causes processing cost higher.2) stability problem of passivating film.In passivation
In processing procedure, due to inhomogeneities and the restriction of organosilan reaction condition of mineral surfaces, inevitably in passivation
Film surface forms some microcracks, and the passivator concentration used is the lowest, and quantity and the width of microcrack are the biggest.And outward
Oxide in boundary's environment is (such as O2、Fe3+With microorganism etc.) easily with these microcracks as break-through point, gradually corrode sulfide mine
Stone, the entirety ultimately resulting in surface passivated membrane comes off.
Summary of the invention
The defect existed for existing type siloxane passivator, it is an object of the invention to be to provide the one can be at yellow ferrum
Surface, ore deposit forms stable passivating film, and it is low to reduce siloxanes consumption, can effectively suppress oxidation of pyrite, be substantially reduced Acid mine
The organosilan of cost for wastewater treatment/nano silicon composite passivant.
Another object of the present invention is to be to provide described passivator to process pyritous method, and this passivator can be at Huang
Iron mine surface forms stable compact film, obtains preferable passivation effect under conditions of organosilan consumption is low, improves passivating film
Stability, greatly reduce acidic mine waste water processing cost, and beneficially environmental conservation, meet existing green production and want
Ask.
In order to realize above-mentioned technical purpose, the invention provides a kind of passivator for suppressing oxidation of pyrite, this is blunt
Agent includes organosilan and nano silicon (NS).
Preferably scheme, passivator is made up of following content of component: organosilan 1～3 parts；Nano silicon 1～4
Part.
More preferably scheme, organosilan is γ-mercaptopropyl trimethoxysilane (PropS-SH).
Present invention also offers a kind of based on the described passivator pyritous method of process, the method is that employing is described blunt
Agent carries out surface-coating process to pyrite.
Preferably scheme, the process using described passivator that pyrite is carried out surface-coating process comprises the following steps:
1) organosilan is dissolved in ethanol/water mixed solvent formation organosilane solution, at described organosilane solution
Middle addition nano silicon, supersound process, obtain organosilan/nano silicon composite solution；
2) pH regulating described organosilan/nano silicon composite solution is the most acid, and be hydrolyzed reaction, is answered
Close silanol solution；
3) being joined by pyrite dust in described comprehensive silicon alcoholic solution, regulation pH, to alkalescence, cross-links successively and solidifies
Reaction, is i.e. coated with silica film layer in pyrite surface.
More preferably scheme, in ethanol/water mixed solvent, the volume ratio of water and ethanol is 1:5～1:8.
More preferably scheme, organosilane solution mass percent concentration is 1%～3%.
More preferably scheme, after organosilan/nano silicon composite solution is by acid for adjusting pH to 4.0～4.5,
Under the conditions of 40 DEG C～45 DEG C, stir 1h～1.5h, obtain comprehensive silicon alcoholic solution.
More preferably scheme, pyrite dust joins in described comprehensive silicon alcoholic solution, regulates pH to 8.0～9.0, at 50 DEG C
～55 DEG C of stirring reaction 2h～2.5h, after product is scrubbed, solidify 10h～12h under the conditions of being placed in 100 DEG C～110 DEG C, i.e.
In pyrite surface coated Si oxygen layer.
More preferably scheme, pyrite dust granularity is 75～150 μm.
Technical scheme, it is important to introducing nano silicon in organosilan, both produce Synergistic
Effect, organosilan primarily forms passivating film skeleton and is coated on pyrite surface, and nano silicon is by corresponding chemical key
Power is distributed in the grid of passivating film securely.Nano-silica filled in the grid of passivating film, on the one hand significantly carry
High passivating film consistency, thickness and mechanical strength；On the other hand, nano silicon can also be greatly increased corrosive medium infiltration blunt
Change the tortuous path of film, hinder corrosive medium infiltration, slow down its diffusion in passivating film, for increasing passivating film, corrosion is situated between
The obstructing capacity of matter and Stability of Passive Film play key effect.Sum it up, nano silicon can be in organosilan
Serve as " filler ", it is achieved to the improvement of organosilane passivating dose of physicochemical properties and passivating film microcrack is filled up, because of
This can realize pyritous well passivated and the stability of raising passivating film under conditions of relatively low organosilan concentration.
The beneficial effect that technical scheme is brought:
1) passivator of the present invention, by adding a small amount of nano silicon in organosilan, substantially increases blunt
The filming performance of agent, hinge structure, the usage amount of organosilan can be substantially reduced, effectively reduce the use of passivator
Cost.
2) passivator of the present invention utilizes organosilan and nano silicon to form densification, stability in pyrite surface
Good composite membrane, and under conditions of reducing the usage amount of organosilan, the stability of passivating film can be improved, can effectively slow down
Pyritous oxidation, suppresses or slows down the generation of acidic mine waste water, and greatly reduce the place of acidic mine waste water from source
Reason cost, and environmental friendliness.
3) passivator of the present invention processes pyritous method simply, and environmental friendliness has certain application prospect.
Accompanying drawing explanation
[Fig. 1] be the embodiment of the present invention 1～5 and comparative example 1 and 2 in total iron content change over figure；
[Fig. 2] be the embodiment of the present invention 1～5 and comparative example 1 and 2 in sulfate radical content change over figure.
Detailed description of the invention
Following example are intended to further illustrate present invention rather than limit the protection model of the claims in the present invention
Enclose.
Embodiment 1
(1) configuration water: ethanol is the mixed solvent of 1:8, adds γ-mercaptopropyl trimethoxysilane (PropS-SH), joins
It is set to the organosilane solution of 3wt%；Adding the nano silicon (NS) of mixed solvent quality 1%, supersound process is to homogeneous
Transparent with machine silane/nano silicon composite solution.
(2) with 0.5MHCl regulating step (1) gained composite solution pH to 4.0, under the conditions of 40 DEG C, stir 1h, be allowed to water
Solution becomes effective comprehensive silicon alcoholic solution.
(3) pyrite powder (granularity is about 100 μm) is thrown to step (2) gained silanol solution, then use 0.5M ammonia
Solution is adjusted to 9.0, under the conditions of 50 DEG C, stirs 2h, take out and wash away unnecessary composite passivant with ethanol, under the conditions of 100 DEG C
Solidification 12h, vacuum preserves.
(4) step (3) gained pyrite passive sample is put into 120mL0.5%H2O2Middle reaction 12h, measures Fe3+、
SO4 2-Concentration, respectively 119.8mg/L and 383.8mg/L, deactivation rate is 68.5% and 68.7%.
Embodiment 2
(1) configuration water: ethanol is the mixed solvent of 1:8, adds γ-mercaptopropyl trimethoxysilane (PropS-SH), joins
It is set to the organosilane solution of 3wt%.Adding the nano silicon (NS) of mixed solvent quality 2%, supersound process is to homogeneous
Transparent with machine silane/nano silicon composite solution.
(2) with 0.5MHCl regulating step (1) gained composite solution pH to 4.4, under the conditions of 40 DEG C, stir 1h, be allowed to water
Solution becomes effective comprehensive silicon alcoholic solution.
(3) pyrite powder (granularity is about 100 μm) is thrown to step (2) gained silanol solution, then use 0.5M ammonia
Solution is adjusted to 9.0, under the conditions of 55 DEG C, stirs 2h, take out and wash away unnecessary composite passivant with ethanol, under the conditions of 100 DEG C
Solidification 12h, vacuum preserves.
(4) step (3) gained pyrite passive sample is put into 120mL0.5%H2O2Middle reaction 12h, measures Fe3+、
SO4 2-Concentration, respectively 71.9mg/L and 241.2mg/L, deactivation rate is 81.1% and 80.4%.
Embodiment 3
(1) configuration water: ethanol is the mixed solvent of 1:6, adds γ-mercaptopropyl trimethoxysilane (PropS-SH), joins
It is set to the organosilane solution of 3wt%.Adding the nano silicon (NS) of mixed solvent quality 3%, supersound process is to homogeneous
Transparent with machine silane/nano silicon composite solution.
(2) with 0.5MHCl regulating step (1) gained composite solution pH to 4.0, under the conditions of 45 DEG C, stir 1h, be allowed to water
Solution becomes effective comprehensive silicon alcoholic solution.
(3) pyrite powder (granularity is about 100 μm) is thrown to step (2) gained silanol solution, then use 0.5M ammonia
Solution is adjusted to 8.5, under the conditions of 50 DEG C, stirs 2h, take out and wash away unnecessary composite passivant with ethanol, under the conditions of 110 DEG C
Solidification 12h, vacuum preserves.
(4) step (3) gained pyrite passive sample is put into 120mL0.5%H2O2Middle reaction 12h, measures Fe3+、
SO4 2-Concentration, respectively 92.5mg/L and 269.7mg/L, deactivation rate is 75.7% and 78.0%.
Embodiment 4
(1) configuration water: ethanol is the mixed solvent of 1:8, adds γ-mercaptopropyl trimethoxysilane (PropS-SH), joins
It is set to the organosilane solution of 3wt%.Adding the nano silicon (NS) of mixed solvent quality 4%, supersound process is to homogeneous
Transparent with machine silane/nano silicon composite solution.
(2) with 0.5MHCl regulating step (1) gained composite solution pH to 4.3, under the conditions of 40 DEG C, stir 1h, be allowed to water
Solution becomes effective comprehensive silicon alcoholic solution.
(3) pyrite powder (granularity is about 100 μm) is thrown to step (2) gained silanol solution, then use 0.5M ammonia
Solution is adjusted to 8.2, under the conditions of 50 DEG C, stirs 2h, take out and wash away unnecessary composite passivant with ethanol, under the conditions of 100 DEG C
Solidification 12h, vacuum preserves.
(4) step (3) gained pyrite passive sample is put into 120mL0.5%H2O2Middle reaction 12h, measures Fe3+、
SO4 2-Concentration, respectively 105.2mg/L and 322.4mg/L, deactivation rate is 73.7% and 72.3%.
Comparative example 1
(1) undressed pyrite powder sample is put into 120mL0.5%H2O2Middle reaction 12h, measures Fe3+、SO4 2-
Concentration, respectively 380.2mg/L and 1228.0mg/L.
Comparative example 2
(1) configuration water: ethanol is the mixed solvent of 1:8, adds γ-mercaptopropyl trimethoxysilane (PropS-SH), joins
It is set to the organosilane solution of 3wt%.
(2) with 0.5MHCl regulating step (1) gained composite solution pH to 4.0, under the conditions of 40 DEG C, stir 1h, be allowed to water
Solution becomes effective comprehensive silicon alcoholic solution.
(3) pyrite powder (granularity is about 100 μm) is thrown to step (2) gained silanol solution, then use 0.5M ammonia
Solution is adjusted to 9.0, under the conditions of 50 DEG C, stirs 2h, take out and wash away unnecessary composite passivant with ethanol, under the conditions of 100 DEG C
Solidification 12h, vacuum preserves.
(4) step (3) gained pyrite passive sample is put into 120mL0.5%H2O2Middle reaction 12h, measures Fe3+、
SO4 2-Concentration, respectively 177.7mg/L and 600.9mg/L, deactivation rate is 53.3% and 51.1%.
Claims (10)
1. the passivator being used for suppressing oxidation of pyrite, it is characterised in that: include organosilan and nano silicon.
It is the most according to claim 1 for suppressing the passivator of oxidation of pyrite, it is characterised in that: by following mass parts group
It is grouped into:
Organosilan 1～3 parts；
Nano silicon 1～4 parts.
It is the most according to claim 1 for suppressing the passivator of oxidation of pyrite, it is characterised in that: described organosilan
For γ-mercaptopropyl trimethoxysilane.
4. process pyritous method based on the passivator described in any one of claims 1 to 3, it is characterised in that: use described
Passivator carries out surface-coating process to pyrite.
It is the most according to claim 4 based on the passivator pyritous method of process, it is characterised in that: use described passivator
The process that pyrite carries out surface-coating process comprises the following steps:
1) organosilan is dissolved in ethanol/water mixed solvent formation organosilane solution, adds in described organosilane solution
Enter nano silicon, supersound process, obtain organosilan/nano silicon composite solution；
2) pH regulating described organosilan/nano silicon composite solution is the most acid, and be hydrolyzed reaction, obtains comprehensive silicon
Alcoholic solution；
3) being joined by pyrite dust in described comprehensive silicon alcoholic solution, regulation pH, to alkalescence, carries out curing reaction successively,
I.e. it is coated with silica film layer in pyrite surface.
It is the most according to claim 5 based on the passivator pyritous method of process, it is characterised in that: described ethanol/water
In mixed solvent, the volume ratio of water and ethanol is 1:5～1:8.
It is the most according to claim 5 based on the passivator pyritous method of process, it is characterised in that: described organosilan
Solution quality percent concentration is 1%～3%.
It is the most according to claim 5 based on the passivator pyritous method of process, it is characterised in that: described organosilicon
Alkane/nano silicon composite solution by acid for adjusting pH to behind 4.0～4.5, under the conditions of 40 DEG C～45 DEG C, stirring 1h～
1.5h, obtains comprehensive silicon alcoholic solution.
It is the most according to claim 5 based on the passivator pyritous method of process, it is characterised in that: described pyrite dust adds
Enter in described comprehensive silicon alcoholic solution, regulate pH to 8.0～9.0, in 50 DEG C～55 DEG C stirring reaction 2h～2.5h, product
After scrubbed, solidify 10h～12h under the conditions of being placed in 100 DEG C～110 DEG C, i.e. in pyrite surface coated Si oxygen layer.
It is the most according to claim 5 based on the passivator pyritous method of process, it is characterised in that: described pyrite
Powder Particle Size is 75～150 μm.
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| CN109207723A (en) * | 2017-07-05 | 2019-01-15 | 中国科学院过程工程研究所 | A method of inhibit oxidation of pyrite to put acid |
| CN112961975A (en) * | 2021-01-21 | 2021-06-15 | 桂林理工大学 | Preparation method for inhibiting photo-corrosion by modifying pyrite through DTC-TETA |
| CN113019154A (en) * | 2021-02-22 | 2021-06-25 | 北京科技大学 | Preparation method of water-soluble composite organosilane passivation film on surface of pyrite |
| CN114032029A (en) * | 2021-10-28 | 2022-02-11 | 成都理工大学 | Novel composite passivator for inhibiting oxidation of pyrite, and preparation method and application thereof |
| CN114504759A (en) * | 2022-01-17 | 2022-05-17 | 华南理工大学 | Long-acting tailing passivator capable of being cured at normal temperature and preparation method and application thereof |
| CN115367808A (en) * | 2022-08-23 | 2022-11-22 | 湘潭大学 | Method for surface passivation treatment of pyrite |
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| CN112961975A (en) * | 2021-01-21 | 2021-06-15 | 桂林理工大学 | Preparation method for inhibiting photo-corrosion by modifying pyrite through DTC-TETA |
| CN113019154A (en) * | 2021-02-22 | 2021-06-25 | 北京科技大学 | Preparation method of water-soluble composite organosilane passivation film on surface of pyrite |
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| CN114504759A (en) * | 2022-01-17 | 2022-05-17 | 华南理工大学 | Long-acting tailing passivator capable of being cured at normal temperature and preparation method and application thereof |
| CN114504759B (en) * | 2022-01-17 | 2022-11-18 | 华南理工大学 | Long-acting tailing passivator capable of being cured at normal temperature and preparation method and application thereof |
| CN115367808A (en) * | 2022-08-23 | 2022-11-22 | 湘潭大学 | Method for surface passivation treatment of pyrite |
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