CN106622681A - Ore slurry flocculating agent and preparation method and application thereof - Google Patents

Ore slurry flocculating agent and preparation method and application thereof Download PDF

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Publication number
CN106622681A
CN106622681A CN201611169426.5A CN201611169426A CN106622681A CN 106622681 A CN106622681 A CN 106622681A CN 201611169426 A CN201611169426 A CN 201611169426A CN 106622681 A CN106622681 A CN 106622681A
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flocculant
slime
preparation
flotation
phosphoric acid
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CN201611169426.5A
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CN106622681B (en
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刘养春
徐会会
杨勇
刘国举
刘云涛
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Bluestar Lehigh Engineering Institute
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Bluestar Lehigh Engineering Institute
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03DFLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D3/00Differential sedimentation
    • B03D3/06Flocculation

Abstract

The invention discloses an ore slurry flocculating agent. The ore slurry flocculating agent is an acid aluminum phosphate polymer which is formed through polymerization of aluminum oxide and phosphoric acid under an acidic condition. The invention further discloses a preparation method of the ore slurry flocculating agent. The preparation method of the ore slurry flocculating agent comprises the steps that solid aluminum oxide is dissolved in a phosphoric acid solution for a stirring reaction at the temperature of 30-50 DEG C, sulfuric acid is added for controlling the pH value of a reaction system to 3-4, a stirring reaction is conducted at the temperature of 50-80 DEG C, and thus the acid aluminum phosphate polymer of a branched structure is obtained. The ore slurry flocculating agent can be used for selective flocculation-flotation during reverse flotation of collophanite, flotation froth can be improved, and a reverse-flotation desilicication process can be conducted smoothly; and the ore slurry flocculating agent can restrain the collophanite to a certain extent, and flotation indexes can be optimized.

Description

A kind of slime flocculant and its production and use
Technical field
The present invention relates to a kind of slime flocculant, in being mainly used in silicon calcium collophanite Counterfloatating desiliconization;The present invention is also related to And the slime flocculant and its production and use.
Background technology
China's phosphate rock resource enriches, and prospective reserves occupies second place of the world, but China's phosphorus ore in ore quality and washability Etc. aspect have larger difference, China's phosphate rock resource is rich and not rich, middle and low grade bauxite is more, and 85% is in explored reserves Middle-low grade appositional pattern collophane.The flotation for solving the problems, such as mid-low grade collophanite ore is the key that phosphorus ore is developed.For this The ore of class could meet phosphate fertilizer processing using must simultaneously discharge carbonate and silicate gangue in floatation process Require.
In flotation process of phosphorite, the exclusion of silicate gangue is mainly direct-flotation desiliconisation and Counterfloatating desiliconization.Direct flotation Although desilication process is industrially used, have the shortcomings that more:Ore pulp Acidity of Aikalinity differs greatly during flotation, and backwater is difficult to Process and utilize, flotation temperature influence, the shortcomings of dosing is big.It is former that Counterfloatating desiliconization technique meets many flotation of floating few suppression Then, flotation can be carried out under normal temperature and thicker granularity, dosing is few, the efficiency of separation is high, is the optimal desiliconization work of collophane Skill.But the Counterfloatating desiliconization technique of collophane is not industrially applied always, its reason is Counterfloatating desiliconization cation collecting Agent is especially sensitive to sludge, and the foam produced in flotation is excessive and tacky, causes floatation process to be difficult to be normally carried out.To understand Certainly this problem, Chinese patent(Publication number:CN102009001A)Selective flocculation reverse flotation containing primary slime collophane takes off Silicon technology, for the rational technological process of a comparison that a current difficult problem is proposed, by adding flocculant, makes particulate sludge wad a quilt with cotton It is solidifying, impact of the particulate sludge to flotation is eliminated, improve frothing.At present, conventional inorganic flocculating agent has aluminum sulfate, six inclined phosphorus Sour sodium, sodium pyrophosphate etc., organic flocculant has polyacrylamide, carboxymethylcellulose calcium etc..But these flocculations are in Counterfloatating desiliconization In all there are various shortcomings, flocculating effect improves little than relatively limited to foam when inorganic flocculation is used, and organic flocculant makes Used time medicament is costly, and organic flocculant can reduce collecting agent sorting when using, and affects the efficiency of separation.
The content of the invention
The technical problem to be solved is for the deficiencies in the prior art, there is provided a kind of new inorganic polymer ore deposit Mud flocculant.The flocculant is used in collophane Counterfloatating desiliconization, not only can improve flotation froth, eliminates sludge to flotation Affect, and the flocculant can play certain inhibition to collophane, can improve sorting, optimize floatation indicators.
Another technical problem to be solved by this invention there is provided the preparation method of flocculant as above.
Another technical problem to be solved by this invention there is provided the purposes of flocculant as above.
The technical problem solved needed for of the invention is to be achieved through the following technical solutions.The present invention is a kind of sludge flocculation Agent, is characterized in, the flocculant is polymerized in acid condition acid phosphate aluminium polymer by aluminum oxide and phosphoric acid.
A kind of slime flocculant of the present invention, its further preferred technical scheme is:Described aluminium acid phosphate Polymer has multiple-branching construction.
The invention also discloses a kind of preparation method of the slime flocculant as described in above technical scheme, is characterized in: Being dissolved in alumina solid under the conditions of 30 ~ 50 DEG C in phosphoric acid solution carries out a stirring reaction, adds sulfuric acid control reactant The pH of system carries out secondary agitation reaction in the range of 3 ~ 4, under the conditions of 50 ~ 80 DEG C, obtains required flocculant.
In a kind of preparation method of slime flocculant of the present invention:The matter of described solid alumina and phosphoric acid solution Amount ratio preferably 1:1.5 ~ 2.5, more preferably 1:2.1 ~ 2.3, further preferably 51:115.
In a kind of preparation method of slime flocculant of the present invention:The mass concentration of described phosphoric acid solution can be by Needs carry out being deployed into any concentration, preferably analyze pure concentration 85%.
A kind of preparation method of slime flocculant of the present invention, further preferred technical scheme or technical characteristic It is:The time of stirring reaction is 1 ~ 2 hour, and the time of secondary agitation reaction is 3 ~ 5 hours.
A kind of preparation method of slime flocculant of the present invention, further preferred technical scheme or technical characteristic It is:The pH of reaction system is 3.5.
The invention also discloses the purposes of the slime flocculant any one of above technical scheme, its purposes is to use Make flocculant in collophane Counterfloatating desiliconization operation, for improving flotation froth, improve sorting mineral.Float collophane is counter The usage amount for selecting flocculant in desiliconization is preferably 200 ~ 1000 g/t raw ores, more preferably 400 ~ 600 g/t raw ores.
The collophane reverse flotation slime flocculant preparation process is simple of the present invention, cost of material is low.The flocculant of preparation exists Flocculating effect is good when used in collophane Counterfloatating desiliconization, can effectively eliminate impact of the sludge to flotation, improves flotation froth, makes Counterfloatating desiliconization technological process is smoothed out.The flocculant of preparation plays certain inhibitory action to collophane, hence it is evident that improve ore deposit The sorting of thing.
Specific embodiment
The present invention is further illustrated by the following example, but is not restricted by the embodiments.
Embodiment 1, a kind of slime flocculant, the flocculant is polymerized in acid condition acid by aluminum oxide and phosphoric acid Formula phosphoric acid aluminium polymer.Described acid phosphate aluminium polymer has multiple-branching construction.
Embodiment 2, a kind of preparation method of slime flocculant as described in Example 1:By aluminum oxide under the conditions of 30 DEG C Solid is dissolved in phosphoric acid solution carries out a stirring reaction, adds sulfuric acid to control the pH=3 of reaction system, enters under the conditions of 50 DEG C Row secondary agitation reacts, and obtains required flocculant.The mass concentration of described phosphoric acid solution is 30%.
Described solid alumina is 1 with the mass ratio of phosphoric acid solution:1.5.The time of stirring reaction is 1 hour, The time of secondary agitation reaction is 3 hours.Resulting slime flocculant is used to be flocculated in collophane Counterfloatating desiliconization operation Agent, for improving flotation froth, improves sorting mineral.And the consumption of described flocculant is 200 g/t raw ores.
Embodiment 3, a kind of preparation method of slime flocculant as described in Example 1:By aluminum oxide under the conditions of 50 DEG C Solid is dissolved in phosphoric acid solution carries out a stirring reaction, adds sulfuric acid to control the pH=4 of reaction system, enters under the conditions of 80 DEG C Row secondary agitation reacts, and obtains required flocculant.The mass concentration of described phosphoric acid solution is 50%.
Described solid alumina is 1 with the mass ratio of phosphoric acid solution:2.5.The time of stirring reaction is 2 hours, The time of secondary agitation reaction is 5 hours.Resulting slime flocculant is used to be flocculated in collophane Counterfloatating desiliconization operation Agent, for improving flotation froth, improves sorting mineral.And the consumption of described flocculant is 1000 g/t raw ores.
Embodiment 4, a kind of preparation method of slime flocculant as described in Example 1:By aluminum oxide under the conditions of 40 DEG C Solid is dissolved in phosphoric acid solution carries out a stirring reaction, adds the pH of sulfuric acid control reaction system in the range of 3.5,65 Secondary agitation reaction is carried out under the conditions of DEG C, required flocculant is obtained.The mass concentration of described phosphoric acid solution is 85%.
Described solid alumina is 51 with the mass ratio of phosphoric acid solution:115.The time of stirring reaction is 1.5 little When, the time of secondary agitation reaction is 4 hours.Resulting slime flocculant is used to be wadded a quilt with cotton in collophane Counterfloatating desiliconization operation Solidifying agent, for improving flotation froth, improves sorting mineral.And the consumption of described flocculant is 500 g/t raw ores.
Embodiment 5, a kind of preparation method of slime flocculant as described in Example 1:By aluminum oxide under the conditions of 35 DEG C Solid is dissolved in phosphoric acid solution carries out a stirring reaction, adds the pH of sulfuric acid control reaction system in the range of 3.8,60 Secondary agitation reaction is carried out under the conditions of DEG C, required flocculant is obtained.The mass concentration of described phosphoric acid solution is 85%.
Described solid alumina is 1 with the mass ratio of phosphoric acid solution:2.2.The time of stirring reaction is 2 hours, The time of secondary agitation reaction is 4 hours.Resulting slime flocculant is used to be flocculated in collophane Counterfloatating desiliconization operation Agent, for improving flotation froth, improves sorting mineral.And the consumption of described flocculant is 600 g/t raw ores.
Embodiment 6:A kind of preparation method experiment of slime flocculant as described in Example 1:
In a kettle. add 115 part 85% phosphoric acid solution and 51 parts of solid aluminas, stirring reaction 1 is little under the conditions of 35 DEG C When, add the pH of sulfuric acid control reaction system 3.5, stirring reaction 4 hours under the conditions of 70 DEG C of heating up obtain being tied with branch The aluminium acid phosphate polymer flocculants of structure.Unless otherwise specified all parts and percentages refer both to quality in embodiment.
Embodiment 7:Hubei silicon calcium collophanite Counterfloatating desiliconization test:
Be selected in ore deposit be flotation magnesium rough concentrate, the P after flotation magnesium2O5Grade be 23.46%, SiO2Grade be 24%.No Using flocculant, it is directly added into pH regulators and carries out flotation after desiliconization collecting agent is sized mixing, it is many to produce foam, and foam is from floating Machine surrounding is selected to overflow, foam is piled up cannot be processed so that Counterfloatating desiliconization technique can not be normally carried out.
Using organic flocculant, the polyacrylamide of 150 g/t is added, add pH regulators and desiliconization collecting agent is sized mixing After carry out flotation.Flotation froth amount is significantly reduced, and foam is no longer tacky, and Counterfloatating desiliconization technique can be smoothed out.Jing is once Roughly selecting desiliconization can obtain grade 28.97%, and the rate of recovery is 85.96% phosphorus concentrate.
Using the inorganic polymer flocculant of synthesis, phosphoric acid aluminium polymer obtained in the embodiment 6 of 450 g/t is added, then PH regulators and desiliconization collecting agent is added to carry out flotation after sizing mixing.Flotation froth amount is also significantly reduced, and foam is no longer tacky, anti-floating Desilication process is selected to be smoothed out.The desiliconization of Jing one roughings can obtain grade 30.35%, and the rate of recovery is 85.06% phosphorus concentrate.
Embodiment 8, Sichuan silico-calcium matter Counterfloatating desiliconization test:
Be selected in ore deposit be flotation magnesium rough concentrate, the P after flotation magnesium2O5Grade be 26.26%, SiO2Grade be 18.12%.Flocculant is not used, pH regulators is directly added into and is carried out flotation after desiliconization collecting agent is sized mixing, it is many to produce foam, And foam overflows from flotation device surrounding, foam is piled up cannot be processed, and Counterfloatating desiliconization technique can not be normally carried out.
Using organic flocculant, the carboxymethylcellulose calcium of 200 g/t is added, add pH regulators and desiliconization collecting agent is adjusted Flotation is carried out after slurry.Flotation froth amount is significantly reduced, and foam is no longer tacky, and Counterfloatating desiliconization technique can be smoothed out.Jing mono- Secondary to roughly select desiliconization and obtain grade 30.83%, the rate of recovery is 86.13% phosphorus concentrate.
Using the inorganic polymer flocculant of synthesis, phosphoric acid aluminium polymer obtained in the embodiment 6 of 550 g/t is added, then PH regulators and desiliconization collecting agent is added to carry out flotation after sizing mixing.Flotation froth amount is also significantly reduced, and foam is no longer tacky, anti-floating Desilication process is selected to be smoothed out.The desiliconization of Jing one roughings can obtain grade 32.79%, and the rate of recovery is 83.46% phosphorus concentrate.

Claims (10)

1. a kind of slime flocculant, it is characterised in that the flocculant is polymerized in acid condition by aluminum oxide and phosphoric acid Acid phosphate aluminium polymer.
2. a kind of slime flocculant according to claim 1, it is characterised in that described acid phosphate aluminium polymer has Multiple-branching construction.
3. a kind of preparation method of slime flocculant as claimed in claim 1 or 2, it is characterised in that:Under the conditions of 30 ~ 50 DEG C Alumina solid is dissolved in phosphoric acid solution carries out a stirring reaction, adds models of the pH of sulfuric acid control reaction system 3 ~ 4 In enclosing, secondary agitation reaction is carried out under the conditions of 50 ~ 80 DEG C, obtain required flocculant.
4. the preparation method of a kind of slime flocculant according to claim 3, it is characterised in that:Described phosphoric acid solution Mass concentration is 85%.
5. the preparation method of a kind of slime flocculant according to claim 3, it is characterised in that:Described solid alumina It is 1 with the mass ratio of phosphoric acid solution:1.5 ~ 2.5, preferably 51:115.
6. the preparation method of a kind of slime flocculant according to claim 3, it is characterised in that:Stirring reaction when Between be 1 ~ 2 hour, secondary agitation reaction time be 3 ~ 5 hours.
7. the preparation method of a kind of slime flocculant according to claim 3, it is characterised in that the pH of reaction system is 3.5。
8. a kind of purposes of slime flocculant, it is characterised in that the slime flocculant is the sludge wadding described in claim 1 or 2 Solidifying agent, or slime flocculant obtained in the preparation method described in claim 3-7 any one, its purposes is for glue phosphorus Make flocculant in ore inverse flotation desiliconization operation, for improving flotation froth, improve sorting mineral.
9. the application of a kind of slime flocculant according to claim 8, it is characterised in that:In collophane Counterfloatating desiliconization The usage amount of flocculant is 200 ~ 1000 g/t raw ores.
10. the application of a kind of slime flocculant according to claim 9, it is characterised in that:In collophane Counterfloatating desiliconization The usage amount of middle flocculant is 400 ~ 600 g/t raw ores.
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