CN108906333A - A kind of mineral floating separation inhibitor and preparation method thereof - Google Patents
A kind of mineral floating separation inhibitor and preparation method thereof Download PDFInfo
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- CN108906333A CN108906333A CN201810729228.2A CN201810729228A CN108906333A CN 108906333 A CN108906333 A CN 108906333A CN 201810729228 A CN201810729228 A CN 201810729228A CN 108906333 A CN108906333 A CN 108906333A
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- preparation
- inhibitor
- sulfonyl chloride
- dodecyl benzene
- fluorite
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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
- C08B3/00—Preparation of cellulose esters of organic acids
- C08B3/08—Preparation of cellulose esters of organic acids of monobasic organic acids with three or more carbon atoms, e.g. propionate or butyrate
- C08B3/10—Preparation of cellulose esters of organic acids of monobasic organic acids with three or more carbon atoms, e.g. propionate or butyrate with five or more carbon-atoms, e.g. valerate
-
- 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
- B03D2203/04—Non-sulfide ores
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- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
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- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
A kind of mineral floating separation inhibitor and preparation method thereof, it is related to technical field of beneficiation, in particular to the preparation method and application of a kind of scheelite and gangue mineral FLOTATION SEPARATION inhibitor, the mineral floating separation inhibitor is the carboxymethyl cellulose under dodecyl benzene sulfonyl chloride changes, and infared spectrum is in 2926.35cm‑1、1038.56cm‑1、1400cm‑1、1600cm‑1There are absorption peak, degree of substitution 0.300-0.503 in place.The preparation method of the mineral floating separation inhibitor comprising:Carboxymethyl cellulose, dodecyl benzene sulfonyl chloride, polar organic solvent, acid binding agent are sequentially added into reaction vessel and is modified reaction, are heated to 50 DEG C of -80 DEG C of stirrings 2-6 hours.Dodecyl benzene sulfonyl chloride modified carboxy methyl cellulose prepared by the present invention can effectively inhibit the mineral such as fluorite, calcite, be used for scheelite and gangue mineral FLOTATION SEPARATION.
Description
Technical field
The present invention relates to technical field of beneficiation, in particular to the system of a kind of scheelite and gangue mineral FLOTATION SEPARATION inhibitor
Preparation Method and application.
Background technique
From sulphide ore, black tungsten, white tungsten, fluorite, calcite symbiosis complex multi-metal mine in flotation black and white tungsten ore, this kind of mine
Stone FLOTATION SEPARATION is relatively difficult, is all utilized in inhibition fluorite, calcite in strongly basic medium both at home and abroad at present, uses fatty acid
Ore, i.e., be ground to after the granularity of requirement and first floatingly select vulcanization by the method for collecting agent (Oxidized paraffin wax or oleic acid) Scheelite Flotation mine
Mine, flotation black and white tungsten (or Scheelite Flotation), general method are the addition sodium carbonate 1000 into ore pulp to sulfide flotation tailing again
G ton or more, addition waterglass inhibits fluorite, calcite and other gangue minerals, does collecting using Oxidized paraffin wax or oleic acid
Agent flotation black and white tungsten (or Scheelite Flotation).China Hunan persimmon bamboo plantation polymetallic ore is one large-scale tungsten, molybdenum, bismuth, fluorite symbiosis
Complex multi-metal mine.Major metal mineral have scheelite, wolframite, bismuthine, molybdenite, magnetic iron ore, pyrite etc., main arteries and veins
Stone ore object is garnet, quartz, fluorite, calcite, pyroxene, hornblend etc..Raw ore contains tungstic acid 0.56%, wherein 2/3 is
Scheelite, 1/3 is wolframite.Raw ore contains 0.09% bismuth-containing 0.18% of molybdenum, calcium fluoride containing 18-20%.Current ore-dressing technique stream
Cheng Shi:After raw ore is milled to the fineness that -200 mesh account for 85%, first Flotation of Sulfide Ores respectively obtains molybdenum concentrate, bismuth concentrate and iron concentrate.
Sulfide flotation tailing carries out tungsten flotation, and the floating agent used is:Sodium carbonate, waterglass, Oxidized paraffin wax, flotation pulp pH
Value is 10-11, after slurry pH is adjusted to 9 or so with sulfuric acid by tungsten flotation tailing, then with fatty acid collecting agent flotation fluorite.It is existing
Floatation major defect is:The flotation recovery effect of black and white tungsten ore is poor, generally also to add before or after tungsten flotation operation
Reselection operation (spiral concentrator and shaking table) recycles wolframite.Keep process flow complicated, while the flotation recovery after tungsten flotation
When fluorite, it is also necessary to which slurry pH is transferred to 9 or so by the sulfuric acid of 600-1000 g tons of reagent removal or addition, not only increases medicament expense
With, and the floatation indicators of fluorite are also poor.
A kind of beneficiation method of Flotation of Sulfide Ores recycling black and white tungsten first from complex multi-metal mine of CN95117062.7,
Invention is characterized in that the method from the tailing flotation of tungsten after Flotation of Sulfide Ores is:A. 250-500 g tons of sodium metasilicate, carboxylic are added
It 20-40 g tons of methylcellulose, stirs 2-5 minutes;B. 800-1200 g tons of plumbi nitras is added, nitrito- phenylhydroxylamine amine is added
It 500-800 g tons of ammonium salt, stirs 6-10 minutes;C. 2-12 g tons of oleic acid of addition emulsification, is stirred 2-5 minutes;D. thick through 1 time
Choosing, 2 times it is selected, scan for 2 times, obtain tungsten rough concentrate.
Summary of the invention
The present invention for existing scheelite needs that a large amount of waterglass are added in flotation, and beneficiation wastewater is caused to be difficult to settle place
The problem of reason, provides a kind of scheelite and gangue mineral FLOTATION SEPARATION inhibitor and preparation method thereof.
Technical solution of the present invention is as follows:
A kind of mineral floating separation inhibitor, the carboxymethyl cellulose under changing for dodecyl benzene sulfonyl chloride are infrared
Map is in 2926.35cm-1、1038.56cm-1、1400cm-1、1600cm-1There are absorption peak, degree of substitution 0.300-0.503 in place.
The preparation method of the mineral floating separation inhibitor comprising:Carboxymethyl fibre is sequentially added into reaction vessel
Dimension element, dodecyl benzene sulfonyl chloride, polar organic solvent, acid binding agent are modified reaction, are heated to 50 DEG C of -80 DEG C of stirring 2-6
Hour.
The mass ratio of the carboxymethyl cellulose and dodecyl benzene sulfonyl chloride is 1:0.6~1.2, preferably 1.2.
The viscosity of the carboxymethyl cellulose is 800-1200 (2% aqueous solution, mpa.s).
The polar organic solvent is N,N-dimethylformamide (DMF), DMAC N,N' dimethyl acetamide, dimethyl sulfoxide, second
Nitrile;The acid binding agent is triethylamine, isopropylamine, diethylamine, pyridine.
The modified-reaction temperature is 60 DEG C, and the modified-reaction time is 4 hours.
It is after the modified-reaction carries out 4 hours, reaction mixture sat is cooling, it is then slow while stirring with stirring rod
It is poured into the container equipped with dehydrated alcohol, generates sediment, filtering precipitate, drying change to get dodecyl benzene sulfonyl chloride
Under carboxymethyl cellulose.
The mineral floating separation inhibitor is fluorite, calcite mineral inhibitor, is applied to scheelite and fluorite, Fang Xie
The separation of stone floatation process.
The separation of the scheelite and fluorite, Calcite by Flotation process mainly comprises the following steps, and is fluorite by main gangue mineral
With the scheelite of calcite it is levigate after, be added flotation device in stir, be added sodium hydroxide adjust slurry pH, the preparation is added
Inhibitor, 20mg/L, finally add collecting agent enuatrol 30mg/L, carry out flotation.
Dodecyl benzene sulfonyl chloride modified carboxy methyl cellulose prepared by the present invention can effectively inhibit fluorite, calcite etc.
Mineral are used for scheelite, gangue mineral FLOTATION SEPARATION.
Detailed description of the invention
Fig. 1 shows influence of the SDS-CMC dosage to three kinds of mineral floatabilities;
Fig. 2 shows influence of the SDS-CMC to three kinds of mineral floatabilities under different pH value;
Fig. 3 shows dodecyl benzene sulfonyl chloride modified carboxy methyl cellulose infrared spectrogram.
Specific embodiment
The preparation of 1 dodecyl benzene sulfonyl chloride modified carboxy methyl cellulose of embodiment
The carboxymethyl cellulose (buying from Tianjin great Mao chemical reagent factory) for weighing 3.5g pours into 100ml three-necked flask
In, be subsequently added into the dodecyl benzene sulfonyl chloride of 2.8g, then use graduated cylinder measure 40ml n,N-Dimethylformamide (DMF) as
Solvent pours into flask, and the triethylamine solution of 0.3g is and then added as acid binding agent.After putting up device, recirculated water is opened,
Start agitating and heating.60 DEG C are warming up to, the reaction time is 4 hours.To after reaction, reaction product is put into stand on one side it is cold
But, it is then poured slowly into while stirring with stirring rod in the beaker equipped with 200ml dehydrated alcohol, there is pale yellow precipitate.Then
Suction filtration separation is carried out using bottle,suction, finally 70 DEG C is adjusted to baking oven and dries product, is weighed.Obtain dodecyl benzene sulfonyl chloride
Modified carboxymethyl cellulose.
The preparation of 2 dodecyl benzene sulfonyl chloride modified carboxy methyl cellulose of embodiment
The carboxymethyl cellulose for weighing 3.5g pours into 100ml three-necked flask, is subsequently added into the detergent alkylate sulphur of 4.2g
Acyl chlorides, then the n,N-Dimethylformamide (DMF) for using graduated cylinder to measure 40ml are poured into flask as solvent, and 0.3g is and then added
Pyridine solution as acid binding agent.After putting up device, recirculated water is opened,;Start agitating and heating.60 DEG C are warming up to, when reaction
Between be 4 hours.It cools down to after reaction, reaction product is put into stand on one side, is then slowly fallen while stirring with stirring rod
Enter in the beaker equipped with 200ml dehydrated alcohol, there is pale yellow precipitate.Then suction filtration separation is carried out using bottle,suction, finally used
Baking oven, which is adjusted to 70 DEG C, dries product, weighs, and obtains the modified carboxymethyl cellulose of dodecyl benzene sulfonyl chloride, and degree of substitution is
0.579。
The modified carboxymethyl cellulose performance characterization of 3 dodecyl benzene sulfonyl chloride of embodiment
Infrared spectrum measurement
Using Bruker Fourier transformation infrared spectrometer (model:VERTEX 70), sample is detected using KBr pressed disc method
It is in 400~4000cm-1Infrared spectrogram, at room temperature (25 DEG C), humidity 50% detect.
By modified carboxy methyl cellulose take it is micro be put into agate Yan Portland, potassium bromide is added and is ground, until be ground into
Powder.Later by pressed powder, be pressed into it is thin and transparent after be just put among instrument, carry out the detection of infrared spectroscopy.
Degree of substitution refers to the average number replaced dodecyl benzene sulfonyl chloride on each Aglycone of carboxymethyl cellulose,
According to the infared spectrum of the carboxymethyl cellulose after modification, being acquired using integral in characteristic peak is 2926.35cm-1The long-chain at place
Alkyl vibration peak and characteristic peak are 1038.56cm-1The area ratio at the C-O key chattering peak at place, i.e. A2926.35/A1038.56。
3 dodecyl benzene sulfonyl chloride modified carboxy methyl cellulose (being abbreviated as SDS-CMC) of embodiment can float three kinds of mineral
The research of property
The separation of scheelite and fluorite, Calcite by Flotation process mainly comprises the following steps, and is fluorite and side by main gangue mineral
It after the scheelite of Xie Shi is levigate, is added in flotation device and stirs, sodium hydroxide is added and adjusts slurry pH, the suppression of the preparation is added
Preparation, 20mg/L finally add collecting agent enuatrol 30mg/L, are carrying out flotation.
It is 120mg/L that Fig. 1, which show test collecting agent enuatrol dosage, and pH value is controlled 10 ± 0.2.Data can from figure
To obtain, for scheelite substantially not by the inhibiting effect of SDS-CMC, the rate of recovery is 90% or so, is held essentially constant;Calcite exists
SDS-CMC dosage starts when being 4-8mg/L by strong inhibition, and the rate of recovery reduces rapidly, and is down to 1.05% from 79.28%, it
Calcite, which is constantly in, afterwards is totally constrained;Fluorite with the dosage of SDS-CMC increase, the rate of recovery with reduction, from
71.35% is down to 29.71%.
Fig. 2 is SDS-CMC as inhibitor, and when enuatrol is as collecting agent, slurry pH is to three kinds of mineral floatabilities
Research.At inhibitor SDS-CMC dosage 10mg/L, the flotation conditions of collecting agent enuatrol dosage 120mg/L, SDS-CMC exists
There is stronger inhibiting effect to calcite and fluorite under soda acid (pH=6-12) ore pulp environment, especially to calcite inhibitory effect
Preferably, the rate of recovery is all very low;Preferable than alkaline environment in acidic environment to the inhibitory effect of fluorite, fluorite returns before pH=8
Yield increases with pH and amount of increase is little, and when pH is before 8-10, Fluorite recovery rate goes up suddenly, is risen to by 46.65%
68.79%;And SDS-CMC does not have inhibiting effect to scheelite, and the rate of recovery of scheelite, white tungsten can be improved to a certain extent
The mine rate of recovery rises as pH increases, and the rate of recovery is increased to 88.65% from 63.87%.
4 dodecyl benzene sulfonyl chloride modified carboxy methyl cellulose of embodiment (abbreviation SDS-CMC) composite ore float test
Effect of the SDS-CMC inhibitor prepared by the present invention in composite ore flotation system is probed into, test uses white tungsten-firefly
Stone composite ore system conducts a research with white tungsten-calcite composite ore system.
1, white tungsten-fluorite composite ore separation test
Using enuatrol as collecting agent, inhibitor is respectively the dodecyl benzene sulfonic acid-carboxymethyl cellulose synthesized for test, is mixed
Closing mine ratio is 1:1.Inquire into the separation situation of white tungsten and fluorite in the case where best collector dosage and inhibitor dosage.
Test result such as table 1.
The test result of table 1 white tungsten and fluorite composite ore
2, white tungsten-calcite composite ore separation test
Using enuatrol as collecting agent, inhibitor is respectively methylcellulose, hydroxyethyl cellulose, the carboxylic without viscosity for test
Dodecyl benzene sulfonic acid-carboxymethyl cellulose of methylcellulose and synthesis is inquired into and is used in best collector dosage and inhibitor
In the case where amount, the separation situation of white tungsten and calcite.Test result such as table 2.
The test result of table 2 white tungsten and calcite composite ore
Claims (9)
1. a kind of mineral floating separates inhibitor, it is characterised in that:It is the modified carboxymethyl cellulose of dodecyl benzene sulfonyl chloride
Element, infared spectrum is in 2926.35cm-1、1038.56cm-1、1400cm-1、1600cm-1There is absorption peak at place, and degree of substitution is
0.300-0.579。
2. the preparation method of the separation inhibitor of mineral floating described in claim 1 comprising:Carboxylic is sequentially added into reaction vessel
Methylcellulose, dodecyl benzene sulfonyl chloride, polar organic solvent, acid binding agent are modified reaction, are heated to 50 DEG C -80 DEG C and stir
It mixes 2-6 hours.
3. the mass ratio of preparation method as described in claim 1, the carboxymethyl cellulose and dodecyl benzene sulfonyl chloride is
1:0.6~1.2.
4. preparation method as described in claim 1, the viscosity of the carboxymethyl cellulose is 300-800mpas.
5. preparation method as described in claim 1, the polar organic solvent is n,N-Dimethylformamide, N, N- dimethyl
Acetamide, dimethyl sulfoxide, acetonitrile;The acid binding agent is triethylamine, isopropylamine, diethylamine, pyridine.
6. preparation method as described in claim 1, the modified-reaction temperature is 60 DEG C, and the modified-reaction time is 4 hours.
7. preparation method as described in claim 1, cooling by reaction mixture sat after the modified-reaction carries out 4 hours, so
It is poured slowly into while stirring with stirring rod in the container equipped with dehydrated alcohol afterwards, generation sediment, filtering precipitate, drying,
Carboxymethyl cellulose under changing up to dodecyl benzene sulfonyl chloride.
8. the inhibitor is fluorite, calcite mineral inhibitor on claims 1, it is applied to scheelite and fluorite, side
Solve the separation of stone floatation process.
9. the separation of scheelite described in claims 8 and fluorite, Calcite by Flotation process mainly comprises the following steps, by main gangue mine
Object is to feed in flotation device and stir after the scheelite of fluorite and calcite is levigate, and sodium hydroxide is added and adjusts slurry pH, is added
The inhibitor of the preparation, 20mg/L finally add collecting agent enuatrol 30mg/L, carry out flotation.
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Citations (4)
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AU2008348262A1 (en) * | 2008-01-14 | 2009-07-23 | The University Of Melbourne | Flotation aids and processes for using the same |
CN102146140A (en) * | 2010-12-20 | 2011-08-10 | 成都理工大学 | Method for preparing temperature-resistance modified water soluble cellulose ether |
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2018
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AU2008348262A1 (en) * | 2008-01-14 | 2009-07-23 | The University Of Melbourne | Flotation aids and processes for using the same |
CN102146140A (en) * | 2010-12-20 | 2011-08-10 | 成都理工大学 | Method for preparing temperature-resistance modified water soluble cellulose ether |
CN104919062A (en) * | 2012-11-28 | 2015-09-16 | 佐治亚-太平洋化工品有限公司 | Mixed collector compositions |
CN106280235A (en) * | 2016-08-26 | 2017-01-04 | 芜湖雪丛林建材有限公司 | A kind of thermally-stabilised good phenolic aldehyde thermal insulation material of exterior wall good toughness |
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Application publication date: 20181130 |