CN108144753A - A kind of preparation method of zinc oxide ore collecting agent - Google Patents
A kind of preparation method of zinc oxide ore collecting agent Download PDFInfo
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- CN108144753A CN108144753A CN201711464332.5A CN201711464332A CN108144753A CN 108144753 A CN108144753 A CN 108144753A CN 201711464332 A CN201711464332 A CN 201711464332A CN 108144753 A CN108144753 A CN 108144753A
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- zinc oxide
- oxide ore
- collecting agent
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- ore collecting
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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
- B03D1/01—Organic compounds containing nitrogen
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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
- B03D2201/00—Specified effects produced by the flotation agents
- B03D2201/02—Collectors
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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
- B03D2203/00—Specified materials treated by the flotation agents; specified applications
- B03D2203/02—Ores
- B03D2203/04—Non-sulfide ores
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- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention discloses a kind of preparation methods of zinc oxide ore collecting agent, belong to mineral manufacture field.The specific steps are：The mixed solution of octadecylamine and lauryl amine is configured, is placed in heating in water-bath；NaOH adjustment pH are added in acquired solution, methanol, propyl alcohol, methyl orthophosphoric acid is sequentially added, is placed in heating in water-bath；Water bath with thermostatic control is stirred, while using ultrasonication, finally obtains zinc oxide ore collecting agent.The method of the present invention is poor for existing amine collector medicament dissolution present in zinc oxide flotation, the problems such as use condition is limited, function and effect are bad, it is mixed using organic interaction and ultrasonic wave hydrotropy, the means such as heating stirring, under the premise of original collecting property is not influenced, enhance the dissolubility of medicament, improve property easy to use, be finally reached the purpose for improving flotation effect.
Description
Technical field
The invention belongs to mineral manufacture field, specifically, being related to a kind of preparation method of zinc oxide ore collecting agent.
Background technology
Zinc exists in the form of sulfide mineral and oxide mineral in nature.Zinc is mainly with zincblende shape in sulfide ore
State exists, and zinc mainly exists in the form of smithsonite and smithsonite in oxidized ore.But zinc resource presentation in China's is characterized in
" rich ore is few, and type is miscellaneous ", " large ore is few, and middle-size and small-size ore deposit is more ", although the raw material used in modern zinc metallurgy industry is mostly
Zinc sulfide ore, but brought into schedule with exhaustion, the processing and utilization of zinc oxide ore increasingly of zinc sulfide ore resource.China's zinc oxide
Ore reserves is very abundant, and according to statistics, the zinc oxide ore reserves contained is up to 80,000,000 t, be mainly distributed on Yunnan, Guizhou and
Just there are about 7,100,000 t in the provinces such as Gansu, only Yunnan Province.Zinc oxide is a kind of secondary mineral of zinc, mainly with smithsonite (ZnCO3), it is different
Pole ore deposit [Zn4Si2O7(OH)2·H2O], willemite (Zn2SiO4), marionite [Zn5(CO3)2(OH)6], the forms such as zincite (ZnO)
In the presence of gangue mineral therein is mainly calcite, dolomite, quartz, clay, iron oxide and iron hydroxide.
At present, the beneficiating method of zinc oxide ore is mainly based on flotation, mainly including vulcanization-amine salt floatation, vulcanization-xanthate
Floatation, fatty acid collecting agent floatation, flocculation-floatation and joint floatation etc..However these methods have respective lack
Point, as vulcanization-amine salt floatation is easily influenced by sludge and saline minerals, and should not be handled containing a large amount of micas, thin,tough silk cloud
Mother, chlorite, culmiferous ore；Vulcanization-xanthate floatation is to the silicates mineral of zinc and the high ore deposit of iron oxide content
Stone floatation indicators are undesirable, meanwhile, heating and activation are needed in floatation process, vulcanization dosing need to be controlled strictly；Aliphatic acid
Class direct flotation method should not handle the zinc oxide ore of iron-holder height and carbonate containing class gangue；The key of flocculation-floatation is selection
The zinc oxide ore has the medicament of specific flocculating effect.
In the latest 20 years, the processing and utilization of zinc oxide ore has been brought into schedule, uses most extensive zinc oxide ore medicament in practice
For two kinds of amine and xanthate, there are many research be the experiment acted on after vulcanizing treatment with amine or xanthate for mineral
Condition is carried out with mechanism.Wherein in amine collector, lauryl amine, octadecylamine and mixed amine are frequent in zinc oxide ore flotation
Three kinds used, but amine collector dissolubility is poor, lead to that inconvenient for use, function and effect are bad so that the medicament
Do not have adaptability in many aspects.With the development of science and technology, the cavitation of high amplitude ultrasonic wave can make micro- in solute
Violent interaction occurs for intergranular, good stirring action is played, so as to make two kinds of immiscible liquid（Ru Shui and oil）
It emulsifies, and accelerates the dissolving and fusion of solute.Therefore, the present invention provides a kind of preparation side of new zinc oxide ore collecting agent
Method：By the way that original amine medicament is carried out organic dissolution, and use ultrasonic wave hydrotropy, heating stirring is not influencing original collecting
Under the premise of property, the dissolubility of medicament is enhanced, improves convenience and flotation effect that medicament uses.
Invention content
In order to overcome existing amine collector in zinc oxide flotation, there is certain collecting effect to Zinc oxide minerals, but
Dissolubility is poor, leads to that inconvenient for use, function and effect are bad, and the present invention proposes a kind of system of zinc oxide ore collecting agent
Preparation Method, this method by original amine medicament by carrying out organic dissolution, and use ultrasonic wave hydrotropy, heating stirring, in not shadow
Under the premise of ringing original collecting property, the dissolubility of medicament is enhanced, improves convenience and flotation effect that medicament uses.
To achieve the above object, the present invention uses following technical scheme：
A kind of preparation method of zinc oxide ore collecting agent, the specific steps are：
1）The mixed solution of octadecylamine and lauryl amine is configured, is placed in heating in water-bath；
2）In step 1）NaOH adjustment pH are added in acquired solution, methanol, propyl alcohol, methyl orthophosphoric acid is sequentially added, is placed in water
It is heated in bath；
3）Water bath with thermostatic control is stirred, while using ultrasonication, finally obtains zinc oxide ore collecting agent.
Further, step 1）In, the mass ratio of the octadecylamine and lauryl amine is 3 ~ 1：1, the mixed solution
A concentration of 10% ~ 20%, heating and temperature control is 40 DEG C ~ 45 DEG C.
Further, step 2）In, it is 9 ~ 11 to adjust pH value of solution；Methanol, propyl alcohol, methyl orthophosphoric acid mass ratio be 4:4:1,
Methanol, propyl alcohol, methyl orthophosphoric acid gross mass for octadecylamine and lauryl amine gross mass 10% ~ 20%, control heating temperature for 55 DEG C ~
60℃。
Further, step 3）In, constant temperature whipping temp is 75 DEG C ~ 85 DEG C, and speed of agitator is 120 ~ 180 r/min, is surpassed
Frequency of sound wave is 25000 ~ 50000 Hz, and ultrasonic power density is 0.5 ~ 1.5W/cm2, action time is 2 ~ 3h.
Beneficial effects of the present invention：Original amine medicament is carried out organic dissolution by the method for the present invention, and using ultrasonic-wave assisted
Molten, heating stirring is simple for process, at low cost, under the premise of original collecting property is not influenced, enhances the dissolubility of medicament,
Improve convenience and the flotation effect that medicament uses；It can promote absorption of the amine collector on zinc oxide ore surface, improve choosing
Other index.
Specific embodiment
A kind of preparation method of zinc oxide ore collecting agent, the specific steps are：
1）The mixed solution of octadecylamine and lauryl amine is configured, is placed in heating in water-bath, wherein the matter of octadecylamine and lauryl amine
Amount is than being 3 ~ 1：1, a concentration of the 10% ~ 20% of mixed solution, heating and temperature control is 40 DEG C ~ 45 DEG C；
2）In step 1）It is 9 ~ 11 that NaOH adjustment pH is added in acquired solution, sequentially adds methanol, propyl alcohol, methyl orthophosphoric acid, and
Be placed in water-bath and heat, wherein methanol, propyl alcohol, methyl orthophosphoric acid mass ratio be 4:4:1, methanol, propyl alcohol, methyl orthophosphoric acid it is total
Quality is octadecylamine and the 10% ~ 20% of lauryl amine gross mass, and control heating temperature is 55 DEG C ~ 60 DEG C；
3）75 DEG C ~ 85 DEG C stirring in water bath of constant temperature, speed of agitator control are 120 ~ 180 r/min, while using ultrasonication, are surpassed
Frequency of sound wave is 25000 ~ 50000 Hz, and ultrasonic power density is 0.5 ~ 1.5W/cm2, action time is 2 ~ 3h, is finally obtained
Zinc oxide ore collecting agent.This method utilizes the cavitation effect of ultrasonic wave, and amine collector and alcohol, ester molecule is promoted to mix row
Row in a manner that the interaction of different organic molecules mixes, strengthen dissolving, promote absorption of the medicament in mineral surfaces.
Embodiment 1
By taking Lincang Prefecture of Yunnan Province low-grade zinc oxide ore as an example, which contains zinc 10.5%, oxygenation efficiency 60%, main zinc-bearing mineral
For smithsonite, zincblende, there are a small amount of smithsonite and franklinite, preparing collecting agent to handle the ore deposit includes the following steps：
Configuration quality ratio is 3 first：1, a concentration of 15% octadecylamine and the mixed solution of lauryl amine, be placed in water-bath plus
Heat, heating temperature are 41 DEG C；Then NaOH adjustment pH to 11 are added in the solution, sequentially add methanol, propyl alcohol, phosphoric acid first
Ester, methanol, propyl alcohol, methyl orthophosphoric acid mass ratio be 4:4:1, methanol, propyl alcohol, methyl orthophosphoric acid gross mass be octadecylamine and 12
The 10% of amine gross mass is placed in heating in water-bath, and heating temperature is 60 DEG C；It is permanent in the water-bath for being finally 82 DEG C in temperature
Temperature stirring, speed of agitator are 150 r/min, while using ultrasonication, and ultrasonic frequency is 25000 Hz, ultrasonic power
Density is 0.5W/cm2, action time 2h finally obtains the collecting agent for zinc oxide ore.Amine is substituted using the collecting agent
Collecting agent sorts Lincang Prefecture's low-grade zinc oxide ore, and Beneficiation flowsheet and remaining regime of agent are constant, finally obtain
Concentrate zinc grade 38.12%, zinc recovery 89.45%, the more former technique of grade improve 2 percentage points, and the more former technique of the rate of recovery improves 3
Percentage point.
Comparative example 1：Configuration quality ratio is 3 first：1, a concentration of 15% octadecylamine and the mixed solution of lauryl amine, juxtaposition
It is heated in water-bath, heating temperature is 35 DEG C；Then in the solution add in NaOH adjustment pH to 11, sequentially add methanol,
Propyl alcohol, methyl orthophosphoric acid, methanol, propyl alcohol, methyl orthophosphoric acid mass ratio be 4:4:1, methanol, propyl alcohol, methyl orthophosphoric acid gross mass be
Octadecylamine and the 10% of lauryl amine gross mass, is placed in heating in water-bath, and heating temperature is 50 DEG C；It it is finally 75 DEG C in temperature
Water-bath in constant temperature stir, speed of agitator is 150 r/min, while using ultrasonication, ultrasonic frequency 25000
Hz, ultrasonic power density 0.5W/cm2, action time 2.5h finally obtains the collecting agent for zinc oxide ore.Using
This collecting agent sorts low-grade zinc oxide ore, and obtain concentrate grade reduces by 0.1 ~ 1 percentage point compared with embodiment 1, recycling
Rate reduces by 0.2 ~ 1 percentage point compared with embodiment 1.
Embodiment 2
By taking certain regional zinc oxide ore of Yunnan Province Shangri-la as an example, which contains zinc 13.5%, oxygenation efficiency 76%, and main zinc-bearing mineral is
Smithsonite, smithsonite have a small amount of galena and franklinite, but the ore deposit location height above sea level is higher, and temperature is relatively low, amine
Collecting agent dissolubility is poor, and solution must be heated before, and in this area, use is extremely inconvenient.To handle the ore deposit
Collecting agent is prepared to include the following steps：
Configuration quality ratio is 1 first：1, a concentration of 20% octadecylamine and the mixed solution of lauryl amine, be placed in water-bath plus
Heat, heating temperature are 40 DEG C；Then NaOH adjustment pH to 10 are added in the solution, sequentially add methanol, propyl alcohol, phosphoric acid first
Ester, methanol, propyl alcohol, methyl orthophosphoric acid mass ratio be 4:4:1, methanol, propyl alcohol, methyl orthophosphoric acid gross mass be octadecylamine and 12
The 15% of amine gross mass is placed in heating in water-bath, and heating temperature is 55 DEG C；It is permanent in the water-bath for being finally 80 DEG C in temperature
Temperature stirring, speed of agitator are 140 r/min, while using ultrasonication, and ultrasonic frequency is 30000 Hz, ultrasonic power
Density is 1.2W/cm2, action time 2h；Finally obtain the collecting agent for zinc oxide ore.Using the collecting agent in fragrant lattice
Certain regional zinc oxide ore is drawn to be sorted, Beneficiation flowsheet and remaining regime of agent are constant, finally obtain concentrate zinc grade 36.51%,
Zinc recovery 80.45%, the more former technique of zinc grade improve 1.5 percentage points, and the more former technique of the rate of recovery improves 2.7 percentage points.
Comparative example 2：Configuration quality ratio is 1 first：1, a concentration of 20% octadecylamine and the mixed solution of lauryl amine, juxtaposition
It is heated in water-bath, heating temperature is 40 DEG C；Then in the solution add in NaOH adjustment pH to 10, sequentially add methanol,
Propyl alcohol, methyl orthophosphoric acid, methanol, propyl alcohol, methyl orthophosphoric acid mass ratio be 4:4:1, methanol, propyl alcohol, methyl orthophosphoric acid gross mass be
Octadecylamine and the 15% of lauryl amine gross mass, is placed in heating in water-bath, and heating temperature is 55 DEG C；It it is finally 80 DEG C in temperature
Water-bath in constant temperature stir, speed of agitator be 140 r/min, finally obtain the collecting agent for zinc oxide ore.It is caught using this
Receive agent low-grade zinc oxide ore is sorted, obtain concentrate grade compared with embodiment 2 reduce by 0.2 ~ 2 percentage point, the rate of recovery compared with
Embodiment 2 reduces by 0.3 ~ 1.5 percentage point.
Embodiment 3
By taking Yunnan Province's Simao Diqu zinc oxide ore as an example, which contains zinc 9.64%, and oxygenation efficiency is more than 99%, and main zinc-bearing mineral is
Smithsonite, smithsonite, a small amount of marionite, bloodstone and cerussite, gangue mineral sericite, kaolin content are higher, ore
Overall structure is loose, frangible, is also easy to produce secondary slime.Collecting agent is prepared to handle the ore deposit to include the following steps：
Configuration quality ratio is 2 first：1, a concentration of 20% octadecylamine and the mixed solution of lauryl amine, be placed in water-bath plus
Heat, heating temperature are 45 DEG C；Then NaOH adjustment pH to 9 are added in the solution, sequentially add methanol, propyl alcohol, methyl orthophosphoric acid,
Methanol, propyl alcohol, methyl orthophosphoric acid mass ratio be 4:4:1, methanol, propyl alcohol, methyl orthophosphoric acid gross mass be octadecylamine and lauryl amine
The 20% of gross mass is placed in heating in water-bath, and heating temperature is 55 DEG C；Constant temperature in the water-bath for being finally 75 DEG C in temperature
Stirring, speed of agitator are 160 r/min, while using ultrasonication, and ultrasonic frequency is 40000 Hz, and ultrasonic power is close
It spends for 1.2W/cm2, action time 3h；Finally obtain the collecting agent for zinc oxide ore.
Simao Diqu low-grade zinc oxide ore is sorted using the collecting agent, Beneficiation flowsheet and remaining regime of agent
It is constant, concentrate zinc grade 26.5%, zinc recovery 78.45% are finally obtained, the more former technique of zinc grade improves 2.1 percentage points, returns
The more former technique of yield improves 4 percentage points.If do not used ultrasonication or the collecting agent being prepared at a temperature of other, final
0.5 ~ 2 percentage point is reduced to the more former technique of concentrate grade, the more former technique of the rate of recovery reduces by 0.1 ~ 1.5 percentage point.
Finally illustrate, preferred embodiment above is merely illustrative of the technical solution of the present invention and unrestricted, although logical
It crosses above preferred embodiment to be described in detail the present invention, however, those skilled in the art should understand that, can be
Various changes are made to it in form and in details, without departing from claims of the present invention limited range.
Claims (7)
1. a kind of preparation method of zinc oxide ore collecting agent, it is characterised in that：The specific steps are：
1）The mixed solution of octadecylamine and lauryl amine is configured, is placed in heating in water-bath；
2）In step 1）NaOH adjustment pH are added in acquired solution, methanol, propyl alcohol, methyl orthophosphoric acid is sequentially added, is placed in water
It is heated in bath；
3）Water bath with thermostatic control is stirred, while using ultrasonication, finally obtains zinc oxide ore collecting agent.
2. a kind of preparation method of zinc oxide ore collecting agent according to claim 1, it is characterised in that：Step 1）In, institute
The octadecylamine and the mass ratio of lauryl amine stated are 3 ~ 1：1, a concentration of the 10% ~ 20% of the mixed solution.
3. a kind of preparation method of zinc oxide ore collecting agent according to claim 1, it is characterised in that：Step 1）In, add
Hot temperature control is 40 DEG C ~ 45 DEG C.
4. a kind of preparation method of zinc oxide ore collecting agent according to claim 1, it is characterised in that：Step 2）In, it adjusts
It is 9 ~ 11 to save pH value of solution.
5. a kind of preparation method of zinc oxide ore collecting agent according to claim 1, it is characterised in that：Step 2）In, institute
The methanol stated, propyl alcohol, methyl orthophosphoric acid mass ratio be 4:4:1, methanol, propyl alcohol, methyl orthophosphoric acid gross mass be octadecylamine and ten
The 10% ~ 20% of diamines gross mass.
6. a kind of preparation method of zinc oxide ore collecting agent according to claim 1, it is characterised in that：Step 2）In, control
Heating temperature processed is 55 DEG C ~ 60 DEG C.
7. a kind of preparation method of zinc oxide ore collecting agent according to claim 1, it is characterised in that：Step 3）In, it is permanent
Warm whipping temp is 75 DEG C ~ 85 DEG C, and speed of agitator is 120 ~ 180 r/min, and ultrasonic frequency is 25000 ~ 50000 Hz, ultrasonic
Wave power density is 0.5 ~ 1.5W/cm2, action time is 2 ~ 3h.
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Cited By (3)
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| CN109590115A (en) * | 2018-12-24 | 2019-04-09 | 中南大学 | A kind of mineral floating collecting agent and its preparation method and application |
| CN110142144A (en) * | 2019-06-03 | 2019-08-20 | 云南金鼎锌业有限公司 | The method that low-grade difficulty selects Flotation of Zinc Oxide in oxysulphied lead-zinc ore tailings |
| CN115921123A (en) * | 2022-10-11 | 2023-04-07 | 昆明理工大学 | Novel galena-chalcopyrite separation composite inhibitor and application thereof |
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