CN106583057B - A kind of preparation and application vulcanizing copper-molybdenum separating flotation inhibitor - Google Patents
A kind of preparation and application vulcanizing copper-molybdenum separating flotation inhibitor Download PDFInfo
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- CN106583057B CN106583057B CN201611159089.1A CN201611159089A CN106583057B CN 106583057 B CN106583057 B CN 106583057B CN 201611159089 A CN201611159089 A CN 201611159089A CN 106583057 B CN106583057 B CN 106583057B
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- copper
- molybdenum
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- inhibitor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION 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
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D1/00—Flotation
- B03D1/001—Flotation agents
- B03D1/004—Organic compounds
- B03D1/016—Macromolecular compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0024—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid beta-D-Glucans; (beta-1,3)-D-Glucans, e.g. paramylon, coriolan, sclerotan, pachyman, callose, scleroglucan, schizophyllan, laminaran, lentinan or curdlan; (beta-1,6)-D-Glucans, e.g. pustulan; (beta-1,4)-D-Glucans; (beta-1,3)(beta-1,4)-D-Glucans, e.g. lichenan; Derivatives thereof
- C08B37/0027—2-Acetamido-2-deoxy-beta-glucans; Derivatives thereof
- C08B37/003—Chitin, i.e. 2-acetamido-2-deoxy-(beta-1,4)-D-glucan or N-acetyl-beta-1,4-D-glucosamine; Chitosan, i.e. deacetylated product of chitin or (beta-1,4)-D-glucosamine; Derivatives thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION 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
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D2201/00—Specified effects produced by the flotation agents
- B03D2201/06—Depressants
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION 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
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D2203/00—Specified materials treated by the flotation agents; specified applications
- B03D2203/02—Ores
Abstract
The present invention relates to a kind of ore dressing sorting, especially a kind of vulcanization copper-molybdenum mixes the preparation and application of smart separating flotation inhibitor.It is characterized in that thioacetic acid and chitosan generation esterification with better inhibition effect are prepared thio chitosan mixture by the depressing agent.The inhibitor is made of the thio chitosan that the thioacetic acid with better inhibition effect and the chitosan macromolecular containing active hydroxyl and amino and esterification generate, and the flotation as vulcanization copper-molybdenum bulk concentrate separation has preferable suppression copper to float the effect of molybdenum.Preparation method of the present invention is simple, and mild condition, cost of material is low, meets demand of industrial production, while overcoming that common amount of sodium sulfide is big, severe operational environment, disadvantage seriously polluted, beneficiation cost is high.
Description
Technical field
The invention belongs to technical field of mineral processing, and in particular to a kind of preparation for vulcanizing copper-molybdenum separating flotation inhibitor
And application.
Background technique
The inhibitor generallyd use in the FLOTATION SEPARATION of copper-molybdenum bulk concentrate is Cymag, but main existing for Cymag
Problem is that toxicity is big, cyanide wastewater is not degradable, big to human body and environmental hazard and dosage is big, causes copper-cobalt ore cost inclined
It is high.Therefore efficient, non-toxic or low-toxic inhibitor is selected to have important practical significance instead of Cymag.
Thioacetic acid has been shown in copper-cobalt ore using upper since selectivity is high, pollution is small, dosage is few, inhibitory effect is good for it
Its superiority is shown.Thioacetic acid can carry out flotation under relatively broad pH value, and action time is short, inhibit selectivity high,
Hypotoxicity and water solubility all promote its application industrially, are just showing that good development becomes in copper-cobalt ore industry
Gesture.Since vulcanized sodium stability is poor, dosage is big, and thioacetic acid higher cost, therefore develops new and effective cheap copper-molybdenum point
From the main direction of studying that inhibitor is still current copper-cobalt ore.It has been reported that and chitosan is used as copper-cobalt ore inhibitor, but press down
Effect processed needs the problem of being further increased.Chinese patent (CN105537002A) is that sulfhydrylization reagent is modified shell by research group
Glycan prepares thio chitosan, and is applied to the inhibitor of vulcanization copper-molybdenum separation of pulp concentrate.But in subsequent application
Although invention, the inhibitor have the floating molybdenum effect of suppression copper well, there is also products to be insoluble in water even weak acid, simultaneously synthesizing cost
Height, because of the inherently good depressing agent of thioacetic acid and chitosan, during the preparation process, by be filtered, washed by
Unreacted thioacetic acid and chitosan increase production cost further through drying.The present invention overcomes the deficiency of the invention,
Using the mixture of thioacetic acid and the esterification of chitosan as inhibitor product, form is colloidal cpd, is soluble in weak
The production technology of acid, product simplifies significantly, reduces the step for being filtered, washed, drying, simultaneous reactions temperature at room temperature into
Row, reaction time also greatly shorten.The inhibitor effect of product utilization thioacetic acid, chitosan and thio chitosan three,
It is more convenient in practical applications, equally there is preferable suppression copper to float molybdenum effect.
Summary of the invention
The purpose of the present invention is for deficiency existing for prior art, provide one kind have production cost it is low, using secure side
Just, the preparation and application of the inhibitor of vulcanization copper-molybdenum concentrate copper-cobalt ore flotation low in the pollution of the environment.
The purpose of the present invention is achieved by the following technical programs:
A kind of preparation method vulcanizing copper-molybdenum separating flotation inhibitor, it is characterised in that the suppression of the copper-molybdenum minerals separation
The preparation step of preparation is as follows: by percentage to the quality, weighing a certain amount of chitosan and is added in a certain amount of thioacetic acid, stir
Dissolution is mixed, adds in a certain amount of concentrated sulfuric acid, is stirred to react certain time at room temperature, be inhibited agent product.
The deacetylation of the chitosan is greater than or equal to 70%.
The chitosan and the mass ratio of thioacetic acid are 1:10~20.
The concentrated sulfuric acid is the 0.5~1.0% of gross mass.
The mixing time is 5~12h.
A kind of vulcanization copper-molybdenum separating flotation inhibitor is applied to the separation process of copper-molybdenum bulk concentrate, by the flotation
Inhibitor realizes the isolated copper concentrate of copper-molybdenum mineral and molybdenum concentrate as the inhibitor of copper mineral.
The copper-molybdenum bulk concentrate is that copper-molybdenum green ore is carried out flotation, obtained copper-molybdenum bulk concentrate.
The inhibitor of the copper is thio chitosan mixture, dosage 100~150g/t copper-molybdenum bulk concentrate.
Depressing agent of the present invention prepares thioacetic acid and chitosan generation esterification with better inhibition effect
At thio chitosan mixture.The inhibitor is by the thioacetic acid with better inhibition effect and contains active hydroxyl and amino
Chitosan macromolecular and esterification generate thio chitosan composition, as vulcanization copper-molybdenum bulk concentrate separation flotation,
There is preferable suppression copper to float the effect of molybdenum.
Compared with the existing technology, the present invention has following remarkable advantage:
1, the thio chitosan mixture that the copper sulfide molybdenum concentrate floatation inhibitor that the present invention synthesizes is used passes through sulfydryl second
With chitosan esterification, chitosan and Cu occur for acid2+Chelate is formed, and-SH group has stronger reproducibility, Cu+With-
SH combination is more stable, and suppression copper effect is more obvious.
2, thio chitosan mixture thioacetic acid, chitosan and the thio chitosan synthesized, it is any former in synthesis
Material does not lose, and gives full play to the inhibitor effect of each substance.
3, synthesis technology is mild, easy to operate, and manufacturing cost is low, and effect is good.
Detailed description of the invention
Fig. 1 shows thio chitosan synthetic route.
Specific embodiment
The present invention is further described below with reference to embodiment, but the scope of protection of the present invention is not limited thereto.
The preparation and application of present invention vulcanization copper-molybdenum separating flotation inhibitor, it is characterised in that the separation copper-molybdenum concentrate
The preparation step of depressing agent is as follows: it weighs a certain amount of chitosan and is added in a certain amount of thioacetic acid, stirring and dissolving, then
It is added in a certain amount of concentrated sulfuric acid, is stirred to react certain time at room temperature, be inhibited agent product.
The deacetylation of the chitosan is greater than or equal to 70%.
The mass ratio of chitosan described in the method for the present invention and sulfhydrylization reagent is 1:10~20.
The concentrated sulfuric acid described in the method for the present invention is the 0.5~1.0% of gross mass.
Mixing time described in the method for the present invention is 5~12h.
Depressing agent described in the method for the present invention is used to vulcanize the copper-cobalt ore process of copper-molybdenum bulk concentrate, will be described
Depressing agent the isolated copper concentrate of copper-molybdenum mineral and molybdenum concentrate are realized as the inhibitor of copper mineral.
Copper-molybdenum bulk concentrate described in the method for the present invention is will to vulcanize copper-molybdenum raw ore to carry out flotation, and obtained copper-molybdenum is mixed
Close concentrate.
The inhibitor of copper described in the method for the present invention is thio chitosan, dosage 100~150g/t copper-molybdenum bulk concentrate.
Preparation method of the present invention is simple, and mild condition, cost of material is low, meets demand of industrial production, while overcoming often
Amount of sodium sulfide is big, severe operational environment, disadvantage seriously polluted, beneficiation cost is high.
Embodiment 1:
(1) preparation of thio chitosan: weighing deacetylation is 70% chitosan 10g, is added to the thioacetic acid of 100g
In the 1g concentrated sulfuric acid, 12h is stirred at room temperature, obtains thio chitosan mixture.
(2) copper-cobalt ore depressing agent prepared by the present invention is subjected to Within Monominerals flotation experiments to verify it and press down the floating molybdenum of copper
Effect.200g molybdenite and 200g chalcopyrite are added in 3000mL distilled water respectively, are 9.5 with lime white tune pH, successively
The thio chitosan mixture of various concentration step (1) preparation is added, stirs 5min, kerosene 70mg is added, stirs 5min, is added
Terpenic oil 20mg stirs 5min;Scrape bubble 5min, foam and product from failing be collected, dry, weigh after calculate the rate of recovery.It is identical
Under the conditions of vulcanized sodium make inhibitor comparing result, be shown in Table 1, table 2.
Influence of the 1 thio chitosan dosage of table to mineral floatability
Influence of 2 amount of sodium sulfide of table to mineral floatability
(3) by the copper-cobalt ore depressing agent of preparation be used as artificial mixed ore (molybdenite and chalcopyrite mix by 1:1 and
At) separation, experimental result is shown in Table 3, and terpenic oil dosage is 10mg/L, as can be seen from Table 3: with thio chitosan mixture
The increase of dosage, chalcopyrite rate of recovery straight line declines and recovery rate of molybdenite is barely affected, meanwhile, chalcopyrite and molybdenite
The gap of the rate of recovery is increasing, and therefore, separating effect is become better and better.
3 thio chitosan mixture of table is used as inhibitor and separates artificial mixed ore
(4) the copper-cobalt ore depressing agent of preparation is used as to the separation of practical copper-molybdenum bulk concentrate, is first passed through cupric
The raw ore of molybdenum carries out flotation, obtains copper-molybdenum bulk concentrate, and resulting copper-molybdenum bulk concentrate is directly then carried out separation roughing behaviour
Make, be 9.5 with lime white tune pH specifically, during carrying out separation roughing, joined the inhibitor of copper, (sulfydryl shell is poly-
Sugared mixture) 100g/t and molybdenum collecting agent (kerosene) 100g/t and foaming agent (terpenic oil) 10g/t, and then it is thick to have obtained molybdenum
Ore pulp after concentrate and separation roughing, product is collected, dries, weigh after calculate the rate of recovery.It the results are shown in Table 4
4 thio chitosan mixture of table is used as inhibitor separation copper-molybdenum bulk concentrate (%)
By experiment process, inhibitor changes vulcanized sodium into, dosage 25kg/t, and when flotation adds in two times, identical floating
Select in the time, obtain concentrate grade be 0.68%, the rate of recovery 78.84%, when this with thio chitosan dosage is 100g/t
The rate of recovery is substantially close, but molybdenum concentrate grade is 1.67 percentage points low.Sorting effect when thio chitosan dosage is 100g/t
Fruit has been approached selected as a result, its reagent consumption is only the 0.4% of vulcanized sodium in original commerical test process.
Embodiment 2:
(1) preparation of thio chitosan: weigh deacetylation be 80% chitosan 5g, be added to 100g thioacetic acid and
In the 0.5g concentrated sulfuric acid, 5h is stirred at room temperature, obtains thio chitosan mixture.
(2) copper-cobalt ore depressing agent prepared by the present invention is subjected to Within Monominerals flotation experiments to verify it and press down the floating molybdenum of copper
Effect.200g molybdenite and 200g chalcopyrite are added in 3000mL distilled water respectively, are 10.5 with lime white tune pH, successively
The thio chitosan of various concentration step (1) preparation is added, stirs 5min, kerosene 70mg is added, stirs 5min, terpenic oil is added
20mg stirs 5min;Scrape bubble 5min, foam and product from failing be collected, dry, weigh after calculate the rate of recovery.Under the same terms
Vulcanized sodium makees inhibitor comparing result, is shown in Table 5, table 6.
Influence of the 5 thio chitosan amount of mixture of table to mineral floatability
Influence of 6 amount of sodium sulfide of table to mineral floatability
(3) by the copper-cobalt ore depressing agent of preparation be used as artificial mixed ore (molybdenite and chalcopyrite mix by 1:1 and
At) separation, experimental result is shown in Table 7, and terpenic oil dosage is 6mg/L, as can be seen from Table 7: with thio chitosan dosage
Increasing, chalcopyrite rate of recovery straight line declines and recovery rate of molybdenite is barely affected, meanwhile, chalcopyrite and recovery rate of molybdenite
Gap it is increasing, therefore, separating effect is become better and better.
7 thio chitosan of table is used as inhibitor and separates artificial mixed ore
(4) the copper-cobalt ore depressing agent of preparation is used as to the separation of practical copper-molybdenum bulk concentrate, is first passed through cupric
The raw ore of molybdenum carries out flotation, obtains copper-molybdenum bulk concentrate, and resulting copper-molybdenum bulk concentrate is directly then carried out separation roughing behaviour
Make, specifically, during carrying out separation roughing, joined copper inhibitor (thio chitosan mixture) 80g/t and
Collecting agent (kerosene) 100g/t and foaming agent (terpenic oil) 10g/t of molybdenum, and then obtained mine after molybdenum rough concentrate and separation roughing
Slurry, product is collected, dries, weigh after calculate the rate of recovery.It the results are shown in Table 8
8 thio chitosan of table is used as inhibitor separation copper-molybdenum bulk concentrate (%)
Product | Yield | Molybdenum grade | Molybdenum recovery |
Concentrate | 10.43 | 6.12 | 75.24 |
Tailing | 91.70 | 0.07 | 24.76 |
To mine | 100 | 0.290 | 100 |
By experiment process, inhibitor changes vulcanized sodium into, dosage 25kg/t, and when flotation adds in two times, identical floating
Select in the time, obtain concentrate grade be 0.68%, the rate of recovery 80.04%, when this with thio chitosan dosage is 150g/t
The rate of recovery is substantially close, but molybdenum concentrate grade is 5.44 percentage points low.Separating effect when thio chitosan dosage is 150g/t,
It has been approached selected as a result, its reagent consumption is only the 0.6% of vulcanized sodium in original commerical test process.
Claims (6)
1. a kind of preparation method for vulcanizing copper-molybdenum separating flotation inhibitor, it is characterised in that the inhibition of the copper-molybdenum minerals separation
The preparation step of agent is as follows: by percentage to the quality, weighing a certain amount of chitosan and is added in a certain amount of thioacetic acid, stirs
Dissolution, adds in a certain amount of concentrated sulfuric acid, is stirred to react certain time at room temperature, obtains the inhibition of thio chitosan mixture
Agent,
The deacetylation of the chitosan is greater than or equal to 70%;
The chitosan and the mass ratio of thioacetic acid are 1:10~20.
2. a kind of preparation method for vulcanizing copper-molybdenum separating flotation inhibitor according to claim 1, it is characterised in that: institute
State 0.5~1.0% that the concentrated sulfuric acid is gross mass.
3. a kind of preparation method for vulcanizing copper-molybdenum separating flotation inhibitor according to claim 1, it is characterised in that: institute
Stating mixing time is 5~12h.
4. the application of the vulcanization copper-molybdenum separating flotation inhibitor of -3 any the method preparations according to claim 1, feature
It is: in the separation process of copper-molybdenum bulk concentrate, the depressing agent is realized into copper-molybdenum as the inhibitor of copper mineral
The isolated copper concentrate of object and molybdenum concentrate.
5. vulcanizing the application of copper-molybdenum separating flotation inhibitor according to claim 4, it is characterised in that: the copper-molybdenum is mixed
Closing concentrate is that copper-molybdenum green ore is carried out flotation, obtained copper-molybdenum bulk concentrate.
6. vulcanizing the application of copper-molybdenum separating flotation inhibitor according to claim 4, it is characterised in that: the sulfydryl shell is poly-
The dosage of sugared mixture is 100~150g/t copper-molybdenum bulk concentrate.
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CN108079964B (en) * | 2017-12-18 | 2021-02-12 | 浙江丰润生物科技股份有限公司 | Preparation process and production equipment of sulfydryl modified chitosan adsorbent |
CN111468302B (en) * | 2020-04-16 | 2021-12-31 | 湖南有色金属研究院 | Beneficiation inhibitor and purification method of molybdenum rough concentrate |
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Effective date of registration: 20201211 Address after: No. 690, Xuefu Road, Wuhua District, Kunming City, Yunnan Province Patentee after: YUNNAN LUNYANG TECHNOLOGY Co.,Ltd. Address before: 650093 University Science Park, Kunming University of science and technology b9118, Xuefu Road, Kunming City, Yunnan Province Patentee before: YUNNAN JIANNIU BIOLOGICAL TECHNOLOGY Co.,Ltd. |