CN106745624A - A kind of inorganic-organic hybrid flocculation material and preparation method thereof - Google Patents
A kind of inorganic-organic hybrid flocculation material and preparation method thereof Download PDFInfo
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- CN106745624A CN106745624A CN201710030880.0A CN201710030880A CN106745624A CN 106745624 A CN106745624 A CN 106745624A CN 201710030880 A CN201710030880 A CN 201710030880A CN 106745624 A CN106745624 A CN 106745624A
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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
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
- C02F1/56—Macromolecular compounds
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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
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F220/56—Acrylamide; Methacrylamide
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Abstract
The invention provides a kind of inorganic-organic hybrid flocculant and preparation method thereof, the raw material components of the inorganic-organic hybrid flocculant include that initiator and mass ratio are 1:9‑1:6 inorganic flocculating agent and organic monomer, the organic monomer includes that mass ratio is 1:9‑1:5 dimethyl diallyl ammonium chloride and acrylamide, the quality of the initiator is the 0.02 5% of organic monomer quality.The inorganic-organic hybrid flocculant is obtained by acrylamide and dimethyl diallyl ammonium chloride is introduced in inorganic flocculating agent, triggering in-situ copolymerization of two kinds of monomers in inorganic system to close.The inorganic-organic hybrid flocculant passes through reasonable selection raw material and proportioning, the sedimentation of powered fine tailings can be better adapted to, the rate of settling of mine tailing suspension is remarkably improved in the case of low dosage, reduce the turbidity of supernatant, the quality of backwater is improved while cost for wastewater treatment is reduced, the purpose of energy-saving and emission-reduction is reached.
Description
Technical field
The invention belongs to industrial waste water treatment, it is related to a kind of inorganic-organic hybridization flocculation material and its preparation
Method.
Background technology
In Mineral Processing Industry, after ore is by sorting, the mine tailing suspension of 10%-20% can be typically produced.At present should
Mine tailing there are problems that a series of：(1) in order to effectively extract the valuable element in ore, ore particles are ground superfine, i.e. d50
Below 30 μm, and particle surface is through carrying negative electrical charge after absorption, hydrolysis, therefore suspended particulate is gravity is small, electrostatic reprimand
Under the influence of the factor such as power is big, it is difficult to settled rapidly in suspension；(2) it is micro- in the mine tailing supernatant for being obtained by natural subsidence
Fine grained residual quantity is higher, and direct reuse can seriously wait cause influence ore dressing effect because of argillization phenomenon, and outer row then can be because of ore dressing medicine
The residual of agent and cause the pollution to environment；(3) tailings recycling water rate is low, and low-density conveying can consume substantial amounts of electric power.Therefore it is real
Existing tailings particles rapid subsidence, the mine tailing effectively dehydration of the target such as backwater solid content is low, beneficiation wastewater is recycled are at present urgently
Problem to be solved.
Flocculation technique is a kind of current economic, easy and effective tailings dewatering processing method for realizing separation of solid and liquid, because
This efficient flocculant is in tailings dewatering link in occupation of irreplaceable status.Now widely used flocculant includes nothing
Machine flocculant, organic flocculant, microbial flocculant and composite flocculation agent.
Inorganic flocculating agent includes aluminium, iron class low molecule flocculant or high polymer coagulant, it is generally the case that such flocculant
With a certain amount of positive charge, can play charge neutrality effect neutralization Particle surface charge makes particle de- steady, or by inorganic high score
The adsorption bridging of son acts on forming big and closely knit flco and rapid subsidence.Inorganic flocculating agent is widely used in water treatment field,
But when using it for solid content mine tailing flocculation treatment higher, dosage is larger, relatively costly.
Organic flocculant flocculates including the synthetic organic polymer such as polyacrylamide and PDDA
The natural organic high-molecular flocculant such as agent and starch, natural plant gum class, such flocculant possesses higher because of its macromolecular long-chain
Adsorption bridging ability, therefore preferable flocculating effect can be reached in the case where dosage is small.Current organic flocculant by
It is widely used in the tailings dewatering link of Mineral Processing Enterprises, but in cationic monomer high cost, flocculant in non-ion type for colloid
The aspect such as de- steady effect difference and space steric effect has some shortcomings.
Microbial flocculant originates from the bacterium for producing flocculant that nineteen thirty-five Butterfield is filtered out from activated sludge,
Such flocculant is to be acted on producing by microbial metabolism, including protein, cellulose etc..Microbial flocculant possesses consumption
Less, environmental protection, it is degradable the advantages of, but limit the extensive of it the shortcomings of the cost of raw material is higher, flocculant yields poorly
Using.
Composite flocculant be in recent years both inorganic flocculating agent, organic flocculant and microbial flocculant after
The novel flocculant of generation, including two kinds or two or more above-mentioned flocculants hydridization, compound, in order to have concurrently various
The flocculation feature of flocculant, so as to realize efficiently separating for solid-liquid in suspension.It was verified that the wadding of composite flocculant
Solidifying effect is better than single flocculant, and the effect of especially inorganic/organic flocculant preferably, is expected to turn into neozoic flocculation
Agent.
CN103011359A discloses a kind of PAFC dimethyl diallyl ammonium chloride homopolymer inorganic-organic
Composite flocculation agent, the flocculant is inorganic and organic principle simple composite at normal temperatures, is produced without chemical bond, and inorganic constituents
Content is high, and when being applied to tailings dewatering, consumption is big, high cost；CN103351047A discloses a kind of inorganic-organic hybridization flocculation
Agent, inorganic part is aluminium polychloride, and organic moiety is PDDA, and the two is connected with ionic bond.It is poly-
Close iron chloride accounting example in the hybrid flocculant higher, show slightly not enough in terms of organic polymer chain adsorption bridging is played, use
When solid content mine tailing suspension higher is processed, the dosage of flocculant is higher, equally exists that consumption is big, cost is high etc. and asks
Topic.CN 1554592A disclose a kind of organic-inorganic ionic hetero high efficiency flocculant, and the flocculant is by weight percentage
Including hydroxide colloid 0.5-15%, acrylamide 50-95%, cationic monomer 0-45%.The hydroxide colloid
Refer to aluminium hydroxide, iron hydroxide, magnesium hydroxide or zinc hydroxide, its colloidal particle size is 10-200nm, the cationic list
Body includes N, N- dimethyl diallyl ammonium chlorides or (methyl) acryloyl-oxy and trimethyl ammonium chloride.The system of the flocculant
Preparation Method is：Acrylamide, cationic monomer are mixed with hydroxide colloid solution, deionized water is added, is stirred and is led to
Enter nitrogen, be warming up to 50-60 DEG C, add initiator aqueous solvent, stir, the flocculant is obtained after isothermal reaction.
Therefore, need to study a kind of inorganic constituents content novel inorganic higher-organic hybrid flocculant, Reasonable Regulation And Control without
The load capacity of machine-organic hybrid flocculant, when being applied to the dewater treatment of different-grain diameter mine tailing suspension, efficiently collaboration is sent out
Charge neutrality and adsorption bridging flocculation are waved, the purpose of more excellent flocculating effect can be reached in the case where dosage is small.
The content of the invention
In view of the shortcomings of the prior art, it is an object of the invention to provide a kind of inorganic-organic hybridization flocculant and
Its preparation method, the inorganic-organic hybridization flocculant can be better adapted to powered thin by reasonable selection raw material and proportioning
The sedimentation of grain mine tailing, preferably flocculating effect is reached in the case where dosage is small.
It is that, up to this purpose, the present invention uses following technical scheme：
An object of the present invention is to provide a kind of inorganic-organic hybridization flocculant, the inorganic-organic hybridization flocculation
The raw material components of agent include that initiator and mass ratio are 1:9-1:6 inorganic flocculating agent and organic monomer, the organic monomer
It is 1 including mass ratio:9-1:5 dimethyl diallyl ammonium chloride and acrylamide, the quality of the initiator is organic list
The 0.02-5% of weight.
The inorganic flocculating agent can be 1 with the mass ratio of organic monomer:6.5、1:7、1:7.5、1:8 or 1:8.5 etc.；It is described
Dimethyl diallyl ammonium chloride can be 1 with the mass ratio of acrylamide:5.5、1:6、1:6.5、1:7、1:7.5、1:8 or 1:
8.5 etc.；The quality of the initiator can be organic monomer quality 0.05%, 0.08%, 0.1%, 0.3%, 0.5%,
0.8%th, 1%, 2%, 3%, 4% or 4.5% etc..
If the mass ratio of inorganic flocculating agent and organic monomer is not in this range, the carrying capacity mistake of hybrid material can be caused
It is low influence charge neutrality effect performance, or hybrid material organic molecule chain it is too short influence adsorption bridging effect performance.
If the quality of dimethyl diallyl ammonium chloride and acrylamide is not in this range, same influence hybrid material
The length of load capacity or macromolecular chain, so as to influence flocculation.
If initiator accounts for the mass fraction of organic monomer not in this range, can cause that efficiency of initiation is relatively low, cause miscellaneous
The molecular weight for changing material is smaller, ultimately results in the reduction of material flocculation.
The structure of the inorganic-organic hybridization flocculant and the organic and inorganic ionic hydridization disclosed in CN1554592A
The structure of efficient flocculant is identical.Difference is inorganic flocculating agent and organic list in the inorganic-organic hybridization flocculant
When dimethyl diallyl ammonium chloride is different with the mass ratio of acrylamide for the quality of body.
The inorganic-organic hybridization flocculant that the present invention is provided by the quality that adjusts inorganic flocculating agent and organic monomer when
The mass ratio of dimethyl diallyl ammonium chloride and acrylamide, the product for obtaining has suitable surface charge, inorganic-organic
Hybrid flocculant is applied to the sedimentation of powered fine tailings, in the case of dosage is less, can play the work of efficient flocculating
With.
The inorganic-organic hybridization flocculant that the present invention is provided is by acrylamide monomer and dimethyl diallyl amide monomer
Be combined, the effect of the adsorption bridging of the organic polymer long-chain for effectively being obtained by copolymerization, and by adjust inorganic flocculating agent and
The component ratio of dimethyl diallyl monomer controls the carrying capacity of inorganic-organic hybridization flocculant, and collaboration plays charge neutrality and makees
With and inorganic flocculating agent polyhydroxy suction-operated, efficiently separating for subparticle and water is realized under low dosage.
The inorganic-organic hybridization flocculant that the present invention is provided is by inorganic flocculating agent and organic acrylamide-dimethyl two
Pi-allyl copolymerization long-chain connects to form ionic bond hybrid structure.In inorganic component and cationic monomer and pending particle surface
Electric charge, reduces the repulsion of suspension system, and inorganic component polyhydroxy is long with organic polyacrylamide-dimethyl diallyl ammonium chloride
Chain is then acted on by strong adsorption bridging and for granular absorption to form big flco, the two mutual cooperative achievement efficient flocculating.
The organic monomer includes that mass ratio is 1:8-1:7 dimethyl diallyl ammonium chloride and acrylamide, such as matter
Amount is than being 1:7.1、1:7.2、1:7.3、1:7.5、1:7.6 or 1:7.8 etc..The organic monomer is the dimethyl of the mass ratio
When diallyl ammonium chloride and acrylamide, the effect of the inorganic-organic hybridization flocculant is optimal.
The initiator is oxidation-reduction initiator, the matter of oxidant and reducing agent in the oxidation-reduction initiator
Amount is than being 1.05:1-2:1.
The oxidant is selected from ammonium persulfate and/or potassium peroxydisulfate, and the reducing agent is selected from sodium hydrogensulfite.
The inorganic flocculating agent is selected from aluminium hydroxide, iron hydroxide, aluminium polychloride, bodied ferric sulfate, polymer aluminium silicate
In polyferric silicate sulfate any one or at least two combination, typical but non-limiting combination such as aluminium hydroxide and hydrogen-oxygen
Change iron, iron hydroxide and aluminium polychloride, iron hydroxide and bodied ferric sulfate, polymer aluminium silicate and polyferric silicate sulfate, be polymerized chlorine
Change aluminium, bodied ferric sulfate, polymer aluminium silicate and polyferric silicate sulfate, preferably aluminium polychloride, bodied ferric sulfate, polymer aluminium silicate
In polyferric silicate sulfate any one or at least two combination.
It is (2-5) that the inorganic flocculating agent is selected from mass ratio:The mixture of 1 aluminium hydroxide and polymer aluminium silicate, such as quality
Than 2.5:1、3:1、3.5:1、4:1 or 4.5:1 etc..When selecting the mixture as inorganic flocculating agent, the inorganic-organic for obtaining
The effect of hybrid flocculant is best.
The second object of the present invention is to provide a kind of preparation method of inorganic-organic hybridization flocculant as described above,
The preparation method comprises the following steps：
(1) under an inert atmosphere, by inorganic flocculating agent solution or inorganic flocculating agent colloid, dimethyl diallyl ammonium chloride
Mix with acrylamide, obtain mixed liquor；Afterwards, to initiator is added in mixed liquor, polymerisation is carried out, obtains product
Gel；
(2) extracted after product gel is dissolved, be precipitated thing；
(3) by drying precipitate, the inorganic-organic hybridization flocculant is obtained.
Step (1) described inert atmosphere is selected from any one in nitrogen atmosphere, helium atmosphere or argon gas atmosphere or at least
Two kinds of combination.Typical but non-limiting combination such as nitrogen atmosphere and helium atmosphere, nitrogen atmosphere and argon gas atmosphere, nitrogen gas
Atmosphere, argon gas atmosphere and helium atmosphere.
Preferably, step (1) described initiator is added drop-wise in mixed liquor, to cause the polymerisation gentleer.
Preferably, step (1) described polymerisation is carried out under the conditions of water bath with thermostatic control, and the temperature of the water bath with thermostatic control is
40-90 DEG C, such as 42 DEG C, 45 DEG C, 48 DEG C, 50 DEG C, 52 DEG C, 55 DEG C, 58 DEG C, 60 DEG C, 62 DEG C, 65 DEG C, 70 DEG C, 75 DEG C, 80 DEG C or
85 DEG C etc..
Preferably, the time of step (1) described polymerisation is 4-12h, such as 5h, 6h, 7h, 8h, 9h, 10h or 11h.
Step (2) the product gel dissolves in deionized water.
Preferably, step (2) solvent for using that extracts is acetone.
Used as preferred technical scheme, the preparation method of the inorganic-organic hybridization flocculant comprises the following steps：
(1) under an inert atmosphere, by inorganic flocculating agent solution or inorganic flocculating agent colloid, dimethyl diallyl ammonium chloride
Mix with acrylamide, obtain mixed liquor；Afterwards, to initiator is added dropwise in mixed liquor, in the water bath with thermostatic control that temperature is 40-90 DEG C
Under the conditions of carry out polymerisation, the reaction time is 4-12h, obtains product gel；
(2) product gel is dissolved in deionized water, the glue that obtains will be dissolved afterwards also is added dropwise in acetone and take out
Carry, be precipitated thing；
(3) by drying precipitate to constant weight, the inorganic-organic hybridization flocculant is obtained.
Compared with prior art, beneficial effects of the present invention are：
(1) the inorganic-organic hybridization flocculant that the present invention is provided is by the conjunction to inorganic-organic hybridization flocculant carrying capacity
Reason regulation and control are capable of achieving the efficient flocculating to average particle size distribution subparticle between 0-100 μm, in low dosage 10g/t-
The rate of settling of mine tailing suspension can be improved more than 5 times in the case of in the range of 40g/t, supernatant fluid turbidity clearance is reachable
More than 80%, the quality of backwater is improved while cost for wastewater treatment is reduced, reach the purpose of energy-saving and emission-reduction；
(2) the inorganic-organic hybridization flocculant that the present invention is provided introduces inexpensive inorganic flocculating agent, is remarkably improved electric charge
Neutralization, realizes elimination of colloid stability, and polyhydroxy absorption plays synergy simultaneously；
(3) the inorganic-organic hybridization flocculant that the present invention is provided is using acrylamide monomer and dimethyl-allyl chlorination
The macromolecular organic long-chain that ammonium copolymerization is obtained, realizes strong adsorption bridging effect, it is possible to decrease organic component cationic monomer group
Point so that cost reduction by more than 30%.
Specific embodiment
Technical scheme is further illustrated below by specific embodiment.
Embodiment 1
A kind of preparation method of inorganic-organic hybridization flocculant, comprises the following steps：
(1) toward aluminium hydroxide (Al (OH)3) acrylamide (AM) and dimethyl diallyl ammonium chloride are added in colloid
(DMDAAC) monomer is complete to dissolving, and is placed in the constant temperature water bath apparatus that temperature is 40 DEG C, after leading to high pure nitrogen 30min, delays
It is slow that ammonium persulfate ((NH is added dropwise4)2S2O8) and sodium hydrogensulfite (NaHSO3) mixed initiator solution, confined reaction system, instead
Terminate after answering 12h；Wherein Al (OH)3It is 1 with the quality of organic monomer:9, DMDAAC is 1 with the mass ratio of AM:9, initiator matter
It is the 0.1% of organic monomer quality to measure, (NH4)2S2O8With NaHSO3Mass ratio is 1.5:1；
(2) gel for terminating to obtain will be reacted soluble in water, the glue for obtaining will be dissolved and extracted in acetone, be precipitated
Thing；
(3) sediment that obtains will be extracted be placed in drying box and dry to constant weight, after grinding inorganic-organic hybridization flocculation
Agent powder.
Above-mentioned inorganic-organic hybridization flocculant is dissolved in ultra-pure water and is configured to the solution that concentration is 1g/L, for average grain
Footpath is the flocculation treatment of 30 μm of cyaniding tailing suspension.When dosage is 40g/t (flocculant usage/tailing dry ore deposit amount),
Initial settlement rate reaches 10.9m/h, and supernatant fluid turbidity is reduced to 15.7NTU.(mine tailing natural subsidence speed is 0.6m/h, on
Clear liquid turbidity is 291.59NTU).
Embodiment 2
A kind of preparation method of inorganic-organic hybridization flocculant, comprises the following steps：
(1) toward iron hydroxide (Fe (OH)3) acrylamide (AM) and dimethyl diallyl ammonium chloride are added in colloid
(DMDAAC) monomer is complete to dissolving, and is placed in the constant temperature water bath apparatus that temperature is 50 DEG C, after leading to high pure nitrogen 30min, delays
It is slow that potassium peroxydisulfate (K is added dropwise2S2O8)) and sodium hydrogensulfite (NaHSO3) mixed initiator solution, confined reaction system, reaction
Terminate after 6h；Wherein Fe (OH)3It is 1 with the quality of organic monomer:6, DMDAAC is 1 with the mass ratio of AM:8, initiator quality
It is 0.02%, K of organic monomer quality2S2O8With NaHSO3Mass ratio is 2:1；
(2) gel for terminating to obtain will be reacted soluble in water, the glue for obtaining will be dissolved and extracted in acetone, be precipitated
Thing.
(3) sediment that obtains will be extracted be placed in drying box and dry to constant weight, after grinding inorganic-organic hybridization flocculation
Agent powder；
Above-mentioned inorganic-organic hybridization flocculant is dissolved in ultra-pure water and is configured to the solution that concentration is 1g/L, for average grain
Footpath is the flocculation treatment of 20 μm of cyaniding tailing suspension.When dosage is 40g/t (flocculant usage/tailing dry ore deposit amount),
Initial settlement rate reaches 9.5m/h, and supernatant fluid turbidity is reduced to 38.6NTU.(mine tailing natural subsidence speed is 0.52m/h, on
Clear liquid turbidity is 294.69NTU)
Embodiment 3
A kind of preparation method of inorganic-organic hybridization flocculant, comprises the following steps：
(1) toward addition acrylamide (AM) and dimethyl diallyl ammonium chloride in aluminium polychloride (PAC) solution
(DMDAAC) monomer is complete to dissolving, and is placed in the constant temperature water bath apparatus that temperature is 50 DEG C, after leading to high pure nitrogen 30min, delays
It is slow that ammonium persulfate ((NH is added dropwise4)2S2O8) and sodium hydrogensulfite (NaHSO3) mixed initiator solution, confined reaction system, instead
Terminate after answering 6h；Wherein PAC is 1 with the quality of organic monomer:6, DMDAAC is 1 with the mass ratio of AM:9, initiator quality is
The 5% of organic monomer quality, (NH4)2S2O8With NaHSO3Mass ratio is 1.05:1
(2) gel for terminating to obtain will be reacted soluble in water, the glue for obtaining will be dissolved and extracted in acetone, be precipitated
Thing；
(3) sediment that obtains will be extracted be placed in drying box and dry to constant weight, after grinding inorganic-organic hybridization flocculation
Agent powder.
Above-mentioned inorganic-organic hybridization flocculant is dissolved in ultra-pure water and is configured to the solution that concentration is 1g/L, for average grain
Footpath is the flocculation treatment of 14 μm of cyaniding tailing suspension.When dosage is 40g/t (flocculant usage/tailing dry ore deposit amount),
Initial settlement rate reaches 11.2m/h, and supernatant fluid turbidity is reduced to 9.3NTU, and (mine tailing natural subsidence speed is 0.46m/h, supernatant
Liquid turbidity is 295.69NTU).
Embodiment 4
A kind of preparation method of inorganic-organic hybridization flocculant, comprises the following steps：
(1) toward addition acrylamide (AM) and dimethyl diallyl ammonium chloride in bodied ferric sulfate (PFS) solution
(DMDAAC) monomer is complete to dissolving, and is placed in the constant temperature water bath apparatus that temperature is 90 DEG C, after leading to high pure nitrogen 30min, delays
It is slow that ammonium persulfate (K is added dropwise2S2O8) and sodium hydrogensulfite (NaHSO3) mixed initiator solution, confined reaction system, react 4h
After terminate；Wherein PFS is 1 with the quality of organic monomer:6, DMDAAC is 1 with the mass ratio of AM:5, initiator quality is organic
0.5%, K of monomer mass2S2O8With NaHSO3Mass ratio is 2:1；
(2) gel for terminating to obtain will be reacted soluble in water, the glue for obtaining will be dissolved and extracted in acetone, be precipitated
Thing；
(3) sediment that obtains will be extracted be placed in drying box and dry to constant weight, after grinding inorganic-organic hybridization white
Flocculant powder.
Above-mentioned inorganic-organic hybridization flocculant is dissolved in ultra-pure water and is configured to the solution that concentration is 1g/L, for average grain
Footpath is the flocculation treatment of 10 μm of cyaniding tailing suspension.When dosage is 40g/t (flocculant usage/tailing dry ore deposit amount),
Initial settlement rate reaches 10.4m/h, supernatant fluid turbidity be reduced to 15.8NTU (mine tailing natural subsidence speed is 0.28m/h, on
Clear liquid turbidity is 298.59NTU).
Embodiment 5
A kind of preparation method of inorganic-organic hybridization flocculant, comprises the following steps：
(1) toward addition acrylamide (AM) and dimethyl diallyl ammonium chloride in polymer aluminium silicate (PASiFC) solution
(DMDAAC) monomer is complete to dissolving, and is placed in the constant temperature water bath apparatus that temperature is 90 DEG C, after leading to high pure nitrogen 30min, delays
It is slow that ammonium persulfate ((NH is added dropwise4)2S2O8) and sodium hydrogensulfite (NaHSO3) mixed initiator solution, confined reaction system, instead
Terminate after answering 4h；Wherein PASiFC is 1 with the quality of organic monomer:8, DMDAAC is 1 with the mass ratio of AM:6, initiator quality
It is the 1% of organic monomer quality, (NH4)2S2O8With NaHSO3Mass ratio is 2:1；
(2) gel for terminating to obtain will be reacted soluble in water, the glue for obtaining will be dissolved and extracted in acetone, be precipitated
Thing；
(3) sediment that obtains will be extracted be placed in drying box and dry to constant weight, after grinding inorganic-organic hybridization flocculation
Agent powder.
Above-mentioned inorganic-organic hybridization flocculant is dissolved in ultra-pure water and is configured to the solution that concentration is 1g/L, for average grain
Footpath is the flocculation treatment of 6 μm of cyaniding tailing suspension.When dosage is 40g/t (flocculant usage/tailing dry ore deposit amount), just
The beginning rate of settling reaches 11.7m/h, and supernatant fluid turbidity is reduced to 26.7NTU, and (mine tailing natural subsidence speed is 0.20m/h, supernatant
Liquid turbidity is 298.0NTU).
Embodiment 6
A kind of preparation method of inorganic-organic hybridization flocculant, comprises the following steps：
(1) toward addition acrylamide (AM) and dimethyl diallyl ammonium chloride in polyferric silicate sulfate (PSiFC) solution
(DMDAAC) monomer is complete to dissolving, and is placed in the constant temperature water bath apparatus that temperature is 80 DEG C, after leading to high pure nitrogen 30min, delays
It is slow that ammonium persulfate ((NH is added dropwise4)2S2O8) and sodium hydrogensulfite (NaHSO3) mixed initiator solution, confined reaction system, instead
Terminate after answering 6h；Wherein PASiFC is 1 with the quality of organic monomer:6, DMDAAC is 1 with the mass ratio of AM:6, initiator quality
It is the 1% of organic monomer quality, (NH4)2S2O8With NaHSO3Mass ratio is 2:1；
(2) gel for terminating to obtain will be reacted soluble in water, the glue for obtaining will be dissolved and extracted in acetone, be precipitated
Thing；
(3) sediment that obtains will be extracted be placed in drying box and dry to constant weight, after grinding inorganic-organic hybridization flocculation
Agent powder.
Above-mentioned inorganic-organic hybridization flocculant is dissolved in ultra-pure water and is configured to the solution that concentration is 1g/L, for average grain
The flocculation treatment of the cyaniding tailing suspension in 3 μm of footpath.When dosage is 40g/t (flocculant usage/tailing dry ore deposit amount), initially
The rate of settling reaches 8.6m/h, and supernatant fluid turbidity is reduced to 36.7NTU, and (mine tailing natural subsidence speed is 0.11m/h, and supernatant is turbid
It is 299.78NTU to spend).
Embodiment 7
A kind of preparation method of inorganic-organic hybridization flocculant, comprises the following steps：
(1) it is 2 toward mass ratio:Added in the mixture solution of 1 aluminium hydroxide and polymer aluminium silicate acrylamide (AM) and
Dimethyl diallyl ammonium chloride (DMDAAC) monomer is complete to dissolving, and is placed in the constant temperature water bath apparatus that temperature is 80 DEG C,
After logical high pure nitrogen 30min, ammonium persulfate ((NH is slowly added dropwise4)2S2O8) and sodium hydrogensulfite (NaHSO3) mixed initiator
Solution, confined reaction system terminates after reaction 6h；The wherein matter of the mixture of aluminium hydroxide and polymer aluminium silicate and organic monomer
Measure is 1:6, DMDAAC is 1 with the mass ratio of AM:7.5, initiator quality is the 5% of organic monomer quality, (NH4)2S2O8With
NaHSO3Mass ratio is 2:1；
(2) gel for terminating to obtain will be reacted soluble in water, the glue for obtaining will be dissolved and extracted in acetone, be precipitated
Thing；
(3) sediment that obtains will be extracted be placed in drying box and dry to constant weight, after grinding inorganic-organic hybridization flocculation
Agent powder.
Above-mentioned inorganic-organic hybridization flocculant is dissolved in ultra-pure water and is configured to the solution that concentration is 1g/L, for average grain
The flocculation treatment of the cyaniding tailing suspension in 3 μm of footpath.When dosage is 40g/t (flocculant usage/tailing dry ore deposit amount), initially
The rate of settling reaches 9.6m/h, and supernatant fluid turbidity is reduced to 19.7NTU, and (mine tailing natural subsidence speed is 0.11m/h, and supernatant is turbid
It is 299.78NTU to spend).
Embodiment 8
A kind of preparation method of inorganic-organic hybridization flocculant, comprises the following steps：
(1) it is 5 toward mass ratio:Acrylamide (AM) is added in 1 aluminium hydroxide and the mixture solution of polymer aluminium silicate
It is complete to dissolving with dimethyl diallyl ammonium chloride (DMDAAC) monomer, it is placed in the constant temperature water bath apparatus that temperature is 80 DEG C
In, after leading to high pure nitrogen 30min, it is slowly added dropwise ammonium persulfate ((NH4)2S2O8) and sodium hydrogensulfite (NaHSO3) mixing trigger
Agent solution, confined reaction system terminates after reaction 6h；The wherein mixture of aluminium hydroxide and polymer aluminium silicate and organic monomer
Quality is 1:7, DMDAAC is 1 with the mass ratio of AM:8, initiator quality is the 1% of organic monomer quality, (NH4)2S2O8With
NaHSO3Mass ratio is 2:1；
(2) gel for terminating to obtain will be reacted soluble in water, the glue for obtaining will be dissolved and extracted in acetone, be precipitated
Thing；
(3) sediment that obtains will be extracted be placed in drying box and dry to constant weight, after grinding inorganic-organic hybridization flocculation
Agent powder.
Above-mentioned inorganic-organic hybridization flocculant is dissolved in ultra-pure water and is configured to the solution that concentration is 1g/L, for average grain
The flocculation treatment of the cyaniding tailing suspension in 3 μm of footpath.When dosage is 40g/t (flocculant usage/tailing dry ore deposit amount), initially
The rate of settling reaches 10.5m/h, and supernatant fluid turbidity is reduced to 12.6NTU, and (mine tailing natural subsidence speed is 0.11m/h, supernatant
Turbidity is 299.78NTU).
Embodiment 9
A kind of preparation method of inorganic-organic hybridization flocculant, comprises the following steps：
(1) it is 4 toward mass ratio:Added in the mixture solution of 1 aluminium hydroxide and polymer aluminium silicate acrylamide (AM) and
Dimethyl diallyl ammonium chloride (DMDAAC) monomer is complete to dissolving, and is placed in the constant temperature water bath apparatus that temperature is 80 DEG C,
After logical high pure nitrogen 30min, ammonium persulfate ((NH is slowly added dropwise4)2S2O8) and sodium hydrogensulfite (NaHSO3) mixed initiator
Solution, confined reaction system terminates after reaction 6h；The wherein matter of the mixture of aluminium hydroxide and polymer aluminium silicate and organic monomer
Measure is 1:8, DMDAAC is 1 with the mass ratio of AM:7, initiator quality is the 1% of organic monomer quality, (NH4)2S2O8With
NaHSO3Mass ratio is 2:1；
(2) gel for terminating to obtain will be reacted soluble in water, the glue for obtaining will be dissolved and extracted in acetone, be precipitated
Thing；
(3) sediment that obtains will be extracted be placed in drying box and dry to constant weight, after grinding inorganic-organic hybridization flocculation
Agent powder.
Above-mentioned inorganic-organic hybridization flocculant is dissolved in ultra-pure water and is configured to the solution that concentration is 1g/L, for average grain
The flocculation treatment of the cyaniding tailing suspension in 3 μm of footpath.When dosage is 40g/t (flocculant usage/tailing dry ore deposit amount), initially
The rate of settling reaches 10.6m/h, and supernatant fluid turbidity is reduced to 15.9NTU, and (mine tailing natural subsidence speed is 0.11m/h, supernatant
Turbidity is 299.78NTU).
Comparative example 1-3
The comparative example 1-3 is the embodiment 1-3 in CN1554592A specifications.
The inorganic-organic hybridization flocculant that comparative example 1-3 is obtained is dissolved in ultra-pure water and is configured to the solution that concentration is 1g/L,
For the flocculation treatment of 3 μm of cyaniding tailing suspension of average grain diameter.When dosage is 40g/t (flocculant usages/tailing dry ore deposit
Amount) when, initial settlement rate reaches 4.2m/h, and supernatant fluid turbidity is reduced to 160.4NTU, and (mine tailing natural subsidence speed is
0.11m/h, supernatant fluid turbidity is 299.78NTU).
Comparative example 4
Except the mass ratio of aluminium polychloride and organic monomer is 1:Outside 5.5, remaining is same as Example 3.
Above-mentioned inorganic-organic hybridization flocculant is dissolved in ultra-pure water and is configured to the solution that concentration is 1g/L, for average grain
Footpath is the flocculation treatment of 14 μm of cyaniding tailing suspension.When dosage is 40g/t (flocculant usage/tailing dry ore deposit amount),
Initial settlement rate reaches 7.4m/h, and supernatant fluid turbidity is reduced to 40.2NTU, and (mine tailing natural subsidence speed is 0.46m/h, supernatant
Liquid turbidity is 295.69NTU).
Comparative example 5
Except the mass ratio of aluminium polychloride and organic monomer is 1:Outside 9.5, remaining is same as Example 3.
Above-mentioned inorganic-organic hybridization flocculant is dissolved in ultra-pure water and is configured to the solution that concentration is 1g/L, for average grain
Footpath is the flocculation treatment of 14 μm of cyaniding tailing suspension.When dosage is 40g/t (flocculant usage/tailing dry ore deposit amount),
Initial settlement rate reaches 8.8m/h, and supernatant fluid turbidity is reduced to 60.6NTU, and (mine tailing natural subsidence speed is 0.46m/h, supernatant
Liquid turbidity is 295.69NTU).
Comparative example 6
Except the mass ratio of dimethyl diallyl ammonium chloride and acrylamide is 1:Outside 4.5, remaining is same as Example 3.
Above-mentioned inorganic-organic hybridization flocculant is dissolved in ultra-pure water and is configured to the solution that concentration is 1g/L, for average grain
Footpath is the flocculation treatment of 14 μm of cyaniding tailing suspension.When dosage is 40g/t (flocculant usage/tailing dry ore deposit amount),
Initial settlement rate reaches 6.7m/h, and supernatant fluid turbidity is reduced to 28.6NTU, and (mine tailing natural subsidence speed is 0.46m/h, supernatant
Liquid turbidity is 295.69NTU).
Comparative example 7
Except the mass ratio of dimethyl diallyl ammonium chloride and acrylamide is 1:Outside 9.5, remaining is same as Example 3.
Above-mentioned inorganic-organic hybridization flocculant is dissolved in ultra-pure water and is configured to the solution that concentration is 1g/L, for average grain
Footpath is the flocculation treatment of 14 μm of cyaniding tailing suspension.When dosage is 40g/t (flocculant usage/tailing dry ore deposit amount),
Initial settlement rate reaches 7.9m/h, and supernatant fluid turbidity is reduced to 55.4NTU, and (mine tailing natural subsidence speed is 0.46m/h, supernatant
Liquid turbidity is 295.69NTU).
Applicant states that the present invention illustrates method detailed of the invention by above-described embodiment, but the present invention not office
It is limited to above-mentioned method detailed, that is, does not mean that the present invention has to rely on above-mentioned method detailed and could implement.Art
Technical staff it will be clearly understood that any improvement in the present invention, equivalence replacement and auxiliary element to each raw material of product of the present invention
Addition, selection of concrete mode etc., within the scope of all falling within protection scope of the present invention and disclosing.
Claims (10)
1. a kind of inorganic-organic hybridization flocculant, it is characterised in that the raw material components bag of the inorganic-organic hybridization flocculant
It is 1 to include initiator and mass ratio:9-1:6 inorganic flocculating agent and organic monomer, the organic monomer includes that mass ratio is 1:
9-1:5 dimethyl diallyl ammonium chloride and acrylamide, the quality of the initiator is the 0.02- of organic monomer quality
5%.
2. inorganic-organic hybridization flocculant according to claim 1, it is characterised in that the organic monomer includes quality
Than being 1:8-1:7 dimethyl diallyl ammonium chloride and acrylamide.
3. inorganic-organic hybridization flocculant according to claim 1 and 2, it is characterised in that the initiator for oxidation-
Reduction initiator, oxidant and the mass ratio of reducing agent in the oxidation-reduction initiator are 1.05:1-2:1.
4. inorganic-organic hybridization flocculant according to claim 3, it is characterised in that the oxidant is selected from persulfuric acid
Ammonium and/or potassium peroxydisulfate, the reducing agent are selected from sodium hydrogensulfite.
5. according to the inorganic-organic hybridization flocculant that one of claim 1-4 is described, it is characterised in that the inorganic flocculating agent
It is any one in selected from aluminium hydroxide, iron hydroxide, aluminium polychloride, bodied ferric sulfate, polymer aluminium silicate or polyferric silicate sulfate
Kind or at least two combination, it is preferably any in aluminium polychloride, bodied ferric sulfate, polymer aluminium silicate or polyferric silicate sulfate
It is a kind of or at least two combination.
6. according to the inorganic-organic hybridization flocculant that one of claim 1-5 is described, it is characterised in that the inorganic flocculating agent
It is (2-5) selected from mass ratio:The mixture of 1 aluminium hydroxide and polymer aluminium silicate.
7. according to the preparation method of one of claim 1-6 described inorganic-organic hybridization flocculant, it is characterised in that described
Preparation method comprises the following steps：
(1) under an inert atmosphere, by inorganic flocculating agent solution or inorganic flocculating agent colloid, dimethyl diallyl ammonium chloride and third
Acrylamide mixes, and obtains mixed liquor；Afterwards, to initiator is added in mixed liquor, polymerisation is carried out, obtains product and coagulate
Glue；
(2) extracted after product gel is dissolved, be precipitated thing；
(3) by drying precipitate, the inorganic-organic hybridization flocculant is obtained.
8. method according to claim 7, it is characterised in that step (1) described inert atmosphere is selected from nitrogen atmosphere, helium
In atmosphere or argon gas atmosphere any one or at least two combination；
Preferably, step (1) described initiator is added drop-wise in mixed liquor；
Preferably, step (1) described polymerisation is carried out under the conditions of water bath with thermostatic control, and the temperature of the water bath with thermostatic control is 40-90
℃；
Preferably, the time of step (1) described polymerisation is 4-12h.
9. the preparation method according to claim 7 or 8, it is characterised in that step (2) the product gel go from
Dissolved in sub- water；
Preferably, step (2) solvent for using that extracts is acetone.
10. according to the preparation method that one of claim 7-9 is described, it is characterised in that the preparation method comprises the following steps：
(1) under an inert atmosphere, by inorganic flocculating agent solution or inorganic flocculating agent colloid, dimethyl diallyl ammonium chloride and third
Acrylamide mixes, and obtains mixed liquor；Afterwards, to initiator is added dropwise in mixed liquor, in the water bath with thermostatic control condition that temperature is 40-90 DEG C
Under carry out polymerisation, the reaction time is 4-12h, obtains product gel；
(2) product gel is dissolved in deionized water, will dissolves afterwards during the glue for obtaining also is added dropwise to acetone and extract, obtained
To sediment；
(3) by drying precipitate to constant weight, the inorganic-organic hybridization flocculant is obtained.
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