CN107175165B - A kind of hydrophobic sur- face modification method improving oxidized coal slime flotation effect - Google Patents
A kind of hydrophobic sur- face modification method improving oxidized coal slime flotation effect Download PDFInfo
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- CN107175165B CN107175165B CN201710442539.6A CN201710442539A CN107175165B CN 107175165 B CN107175165 B CN 107175165B CN 201710442539 A CN201710442539 A CN 201710442539A CN 107175165 B CN107175165 B CN 107175165B
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- 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
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Abstract
A kind of hydrophobic sur- face modification method improving oxidized coal slime flotation effect, the method are that calcium hydroxide is added to the water to stirring to form alkaline calcium hydroxide solution；Stirring in calcium hydroxide solution is added in oxidized coal slime and carries out neutralization reaction, drying is filtered, acid-base neutralization oxidized coal slime filter cake is made；Organic carboxyl acid is dissolved in water agitating and heating again, acid-base neutralization oxidized coal slime filter cake is added in organic carboxyl acid solution, stirring at normal temperature carries out graft reaction, filters drying afterwards, and hydrophobic modification oxidized coal slime filter cake is made.Hydrophobic segment is grafted in the acidic hydrophilic functional group on coal surface by this method using chemical complexometry, the not influence vulnerable to flotation solution chemistry environment, it is firmly combined, improves the problem of oxidized coal slime surface hydrophobic difference well, cleaned coal flotation recovery rate can be improved.
Description
Technical field
The present invention relates to a kind of oxidized coal slime surface modifying method, especially a kind of improvement oxidized coal slime surface hydrophobic
Method belongs to coal preparation technical field.
Background technique
Flotation is widely applied method and the effective way of slime separation in fine-grained mineral separation.Coal slime flotation mistake
Hydrophobic coal particle is adhered on bubble in journey, with bubble floating, enters froth bed, and hydrophilic spoil then stays in coal slurry
In, it is separated from each other to realize.
In general, coal is the preferable substance of native floatability, majority just can by addition oils collecting agent and foaming agent
Obtain fabulous separating effect.It, can be with the phases such as oxygen gas and water in air after exposure in air but since coal is oxidizable
Different degrees of weathering oxidation occurs for interaction.
Coal oxidation can make its Surface Creation polarity oxygen-containing functional group, especially highly polar hydrophilic carboxyl, phenolic hydroxyl group function
Group, to weaken the hydrophobicity of coal particle surface.Kerosene, diesel oil etc. are industrial common nonpolar oils collecting agent.Floating
It, cannot be in the coal slime particle of oxidation since the polar functional group compatibility of these collecting agents and coal particle surface is poor during choosing
Surface is effectively adsorbed and is sprawled, and it is very low to typically result in floatation clean coal yield；If increasing collector dosage merely, not only
This situation cannot be improved, the ash content of floatation clean coal can be made exceeded instead, and increase the expense of floating operation.Therefore, it is necessary to
By process for modifying surface, enhances the hydrophobicity on oxidized coal slime surface, improve the selectivity and the rate of recovery of the flotation of oxidized coal slime.
In order to improve the surface hydrophobic and flotation effect of oxidized coal, domestic and foreign scholars are conducted extensive research.Jia etc.
（Jia, R.; Harris, G. H.; Fuerstenau, D. W. An improved class of universal
collectors for the flotation of oxidized and/or low-rank coal. Int. J. Miner. Process. 2000, 58 (1-4), 99-118.）According to the characteristic of low order oxidized coal slime, develop containing tetrahydrofuran base
The serial flotation collector of group.This kind of medicament can form Hydrogen Binding Adsorption with the oxygen-containing group on coal slime surface, improve oxidized coal slime
Hydrophobicity, and then improve the floatability and flotation effect of oxidized coal.MS Jena etc.（Jena, M.; Biswal, S.;
Rudramuniyappa, M. Study on flotation characteristics of oxidised Indian high
ash sub-bituminous coal. Int. J. Miner. Process. 2008, 87 (1), 42-50.）It develops
A kind of pair of India's oxidized coal slime flotation has the heavy oil of facilitation.They have found that the flotation of oxidized coal slime can be improved in the promotor
Performance improves clean coal yield and cleans ash is greatly lowered.Mark's jade etc.（Mark is beautiful;Song Shuyu;The strong surface Fan Min is living
Experimental study coal preparation technology 2011,4,9-12. of the property agent SPAN80 to coal slime flotation facilitation）It is sent out by test
Existing, Span80 surfactant has good facilitation to Datong District's coal flotation, and rate of economizing gasoline is up to 72.6%.Chen Qiang（Chen Qiang
The Study of flotation clean coal technology 2012,18 (2) of high ash oxidized coal, 10-12.）Fatty alcohol has been investigated to oxidized coal
Synergistic effect, discovery butanol pretreatment after oxidized coal combustible recovery and cleans ash be better than not processed original
Coal.However, the studies above only shows preferable effect in laboratory research.Due to aqueous solution during industrial coal flotation
Chemical environment is complicated and changeable, and discovery is not effective yet at present aoxidizes coal flotation solution.
Summary of the invention
It is an object of the invention to two kinds of hydrophilic functional groups of carboxyl, phenolic hydroxyl group using combination medicament to oxidized coal surface
Graft reaction is carried out, the hydrophobicity on oxidized coal slime surface is improved, so as to improve nonpolar oils collecting agent on oxidized coal slime
Effect is adsorbed and sprawled, solves the problems, such as that oxidation coal flotation is difficult.
The present invention is achieved through the following technical solutions.
A kind of hydrophobic sur- face modification method improving oxidized coal slime flotation effect, the hydrophobic sur- face modification method are
Follow these steps progress：
（1）It is 0~0.15: 100 by the mass ratio of calcium hydroxide and water, calcium hydroxide is added to the water, stirring 0.1~
5h makes it dissolve, and forms alkaline calcium hydroxide solution；
（2）Step is added in oxidized coal slime by granularity less than 0.5mm（1）It is formed by calcium hydroxide solution, stirring 0.1
~5h carries out room temperature acid-base neutralization reaction, to neutralize carboxyl, the phenolic hydroxyl group functional group on oxidized coal slime surface；Followed by filter,
Obtain filter cake, and in 50~90 DEG C dry 3~for 24 hours, acid-base neutralization oxidized coal slime filter cake is made；The calcium hydroxide and oxidized coal
The mass ratio of mud is 0~0.6: 100；
（3）It is 0~2: 100 by the mass ratio of organic carboxyl acid and water, organic carboxyl acid is dissolved in water, forms organic carboxyl acid water
Solution, stirring, heating promote the dissolution of organic carboxyl acid；
（4）By step（2）The acid-base neutralization oxidized coal slime filter cake of acquisition is added to step（3）The organic carboxyl acid solution of formation
In, 0.1~5h of stirring at normal temperature carries out graft reaction, followed by filters, obtain filter cake in 50~90 DEG C dry 3~for 24 hours, be made
Hydrophobic modification oxidized coal slime filter cake；The mass ratio of the organic carboxyl acid and acid-base neutralization oxidized coal slime filter cake is 0~0.5:
100。
In the above-mentioned technical solutions, the organic carboxyl acid is one of n-caproic acid, positive enanthic acid and caprylic acid.
Above-mentioned technical proposal compared with prior art, has the following advantages that and good effect.
First is that absorption is stablized, do not influenced by solution chemistry.
The flotation promoter of existing oxidized coal is surfactant, they are adsorbed on the surface of coal by physical action,
Act on unstable influence vulnerable to pulp chemical environment；The surface-hydrophobicized method of modifying of coal proposed by the invention can incite somebody to action
Hydrophobic alkane chain forms precipitating by chemical reaction, and orientation is grafted on coal surface, does not interfere vulnerable to pulp chemical environment.
Second is that hydrophobic segment can be guaranteed towards water phase.
It is well known that it includes hydrophilic polar group that surfactant includes hydrophobic non-polar group again；Equally, it aoxidizes
Also existing hydrophobic region has hydrophilic region again on the surface of coal, since presently used coal surfactant is physical absorption, such as
Fruit surfactant molecule is adsorbed on coal surface hydrophobicity region, then its hydrophilic radical will be directed toward water phase, this cannot play improvement coal
The purpose of surface hydrophobic, but in existing technical solution, this phenomenon not can avoid again；Coal table proposed by the invention
The modified scheme in face is then completely different, and since coal is solid, the carboxyl on oxidized coal surface, phenolic hydroxyl group position are fixed, each carboxylics
Base or phenolic hydroxyl group are only capable of one molecule calcium hydroxide of consumption（Ca(OH)2）A basic hydroxide group, organic acid used is dissolved in water
In, it can move freely in aqueous solution, carboxyl, the phenolic hydroxyl group location proximate on oxidized coal surface can be moved to molecular forms
Acid-base neutralization reaction occurs, consumes another remaining basic hydroxide group, such organic carboxyl acid can pass through calcium ion chemical complexing
In the carboxyl on oxidized coal surface, phenolic hydroxyl group anionic sites, due to the carboxyl anion of organic acid and carboxyl, the phenol on coal surface
Hydroxyl anion is negatively charged, and mutual exclusion can occur for the two, guarantees the hydrophobic chain of organic carboxyl acid far from coal surface and towards floating
Select water phase, so as to improve the hydrophobicity on oxidized coal surface, it is met with without the prior art the problem of.
Detailed description of the invention
Fig. 1 is 1 water of the embodiment of the present invention oxidized coal contact angle optical photograph modified to non-surface, and measuring contact angle is
32.3°。
Fig. 2 is 1 water of the embodiment of the present invention to the modified oxidized coal contact angle optical photograph in surface, and measuring contact angle is
90.8°。
Fig. 3 is 2 water of the embodiment of the present invention oxidized coal contact angle optical photograph modified to non-surface, and measuring contact angle is
17.1°。
Fig. 4 is 2 water of the embodiment of the present invention to the modified oxidized coal contact angle optical photograph in surface, and measuring contact angle is
68.3°。
Fig. 5 is 3 water of the embodiment of the present invention oxidized coal contact angle optical photograph modified to non-surface, and measuring contact angle is
27.2°。
Fig. 6 is 3 water of the embodiment of the present invention to the modified oxidized coal contact angle optical photograph in surface, and measuring contact angle is
91.4°。
Specific embodiment
Further explanation is made to a specific embodiment of the invention below, but the present invention is not limited thereto.
Embodiment 1
Implement a kind of hydrophobic sur- face modification method for improving oxidized coal slime flotation effect, institute provided by aforementioned present invention
Hydrophobic sur- face modification method is stated to follow these steps to carry out：
The first step weighs calcium hydroxide 0.10g, measures deionized water 500ml, is placed in a beaker and is stirred, when stirring
Between 0.2h so that calcium hydroxide is dissolved in water to form alkaline calcium hydroxide solution.
Granularity is less than 0.5mm, ash content 20.1wt%, moisture 6.1wt%, volatile matter 8.4wt%, fixed carbon by second step
Calcium hydroxide solution prepared by the first step is added in the oxidized coal slime 100g of 65.4wt%, and stirring 0.5h carries out room temperature acid-base neutralization
Reaction, by the acidic functionality of oxidized coal slime particle surface（Carboxyl, phenolic hydroxyl group）It neutralizes.Thereafter, using the machine of suction filtration to institute's shape
At coal slurry filtered, the slime filter cake filtered is put into 60 DEG C of drying box dry 12h, obtains acid-base neutralization oxidized coal slime
Filter cake.
The beaker for filling 1000ml deionized water is added in 0.22g caprylic acid by third step, stirs 60min so that caprylic acid
Dissolution forms caprylic acid aqueous solution.
4th step, the caprylic acid aqueous solution that the preparation of 200ml third step is measured with beaker, the acid-base neutralization that second step is obtained
Oxidized coal slime filter cake is added in beaker, and stirring at normal temperature 0.5h carries out hydrophobization graft reaction.It is taken out after having reacted with suction filtration machine
Filter, the slime filter cake filtered are put into 60 DEG C of drying box dry 12h, obtain hydrophobic modification oxidized coal slime filter cake.
Fig. 1 is the contact angle optical photograph of the present embodiment water above-mentioned oxidized coal modified to non-surface, and measuring contact angle is
32.3°.Fig. 2 is the contact angle optical photograph of the present embodiment water above-mentioned oxidized coal modified to surface, and measuring contact angle is
90.8°.Thus, the hydrophobicity of oxidized coal slime can be improved in method of modifying provided by the present invention.
Use kerosene as collecting agent, hydrophobic modification oxidized coal slime conduct of the sec-octyl alcohol as foaming agent to above-mentioned preparation
Pan feeding carries out flotation.As a comparison, flotation equally has been carried out to the former oxidized coal slime handled without hydrophobic modification.Flotation is set
Standby to inflate single-trough flotating machine, speed of mainshaft 1200r/min, aeration quantity 3.0L/min using XFD-1.5L type, flotation cell volume is
1.5L, coal-water fluid concentration are about 66.7g/L.Floatation process is as follows：Kerosene is added according to 250g/t coal slime into pulp, sizes mixing
Stir 1min;Then sec-octyl alcohol is added according to 60g/t coal slime, sizes mixing and stirs 30s.Air intake valve is opened, bubble 5min is scraped in timing,
Products obtained therefrom filtering, drying, carry out weighing chemical examination.
Result of laboratory test shows that the combustible recovery after the former oxidized coal slime flotation handled without hydrophobic modification is
44.2wt%, cleans ash 8.2wt%；It is increased to 82.8wt% by the combustible recovery of the oxidized coal slime of hydrophobic modification,
And cleans ash is 9.7wt%, it is only slight to rise.Thus the present embodiment can prove that the oxidized coal slime that the present invention is announced is dredged
Aquation method of modifying can remarkably promote the flotation effect of oxidized coal slime.
Embodiment 2
Implement a kind of hydrophobic sur- face modification method for improving oxidized coal slime flotation effect, institute provided by aforementioned present invention
Hydrophobic sur- face modification method is stated to follow these steps to carry out：
The first step weighs calcium hydroxide 0.50g, measures deionized water 500ml, is placed in a beaker and is stirred, when stirring
Between 3h so that calcium hydroxide is dissolved in water to form alkaline calcium hydroxide solution.
Granularity is less than 0.5mm, ash content 26.2wt%, moisture 6.9wt%, volatile matter 23.1wt%, fixed carbon by second step
Calcium hydroxide solution prepared by the first step is added in the oxidized coal slime 100g of 43.8wt%, and it is anti-that stirring 2h carries out room temperature acid-base neutralization
It answers, by the acidic functionality of oxidized coal slime particle surface（Carboxyl, phenolic hydroxyl group）It neutralizes.Thereafter, using suction filtration machine to being formed
Coal slurry filtered, the slime filter cake filtered is put into 60 DEG C of drying box dry 12h, obtains the filter of acid-base neutralization oxidized coal slime
Cake.
The beaker for filling 1000ml deionized water is added in 0.70 positive enanthic acid by third step, in 60 DEG C of stirred in water bath 30min
So that positive enanthic acid dissolution, forms positive enanthic acid aqueous solution.
4th step, the positive enanthic acid aqueous solution that the preparation of 200ml third step is measured with beaker, the acid-base neutralization that second step is obtained
Oxidized coal slime filter cake is added in beaker, and stirring at normal temperature 1h carries out hydrophobization graft reaction.It is filtered after having reacted with suction filtration machine,
It filters obtained slime filter cake and is put into 60 DEG C of drying box dry 12h, obtain hydrophobic modification oxidized coal slime filter cake.
Fig. 3 is the contact angle optical photograph of the present embodiment water above-mentioned oxidized coal modified to non-surface, and measuring contact angle is
17.1°.Fig. 4 is the contact angle optical photograph of the present embodiment water above-mentioned oxidized coal modified to surface, and measuring contact angle is
68.3°.Thus, the hydrophobicity of oxidized coal slime can be improved in method of modifying provided by the present invention.
Use diesel oil as collecting agent, methyl isobutyl carbinol is aoxidized as hydrophobic modification of the foaming agent to above-mentioned preparation
Coal slime carries out flotation as pan feeding.As a comparison, equally the former oxidized coal slime handled without hydrophobic modification is floated
Choosing.Floatation equipment inflates single-trough flotating machine, speed of mainshaft 1200r/min, aeration quantity 3.0L/min, flotation using XFD-1.5L type
Slot volume is 1.5L, and coal-water fluid concentration is about 66.7g/L.Floatation process is as follows：It is added into pulp according to 240g/t coal slime
Diesel oil sizes mixing and stirs 1min；Then methyl isobutyl carbinol is added according to 70g/t coal slime, sizes mixing and stirs 1min.Open air inlet
Bubble 5min is scraped in valve, timing, and products obtained therefrom filtering, drying carry out weighing chemical examination.
Result of laboratory test shows that the combustible recovery after the former oxidized coal slime flotation handled without hydrophobic modification is
15.3wt%, cleans ash 7.9wt%；It is increased to 55.0wt% by the combustible recovery of the oxidized coal slime of hydrophobic modification,
And cleans ash is 10.3wt%, is slightly improved, but still conform to quality of cleaned coal requirement.Thus the present embodiment can prove the present invention
The oxidized coal slime hydrophobic modification method announced can remarkably promote the flotation effect of oxidized coal slime.
Embodiment 3
Implement a kind of hydrophobic sur- face modification method for improving oxidized coal slime flotation effect, institute provided by aforementioned present invention
Hydrophobic sur- face modification method is stated to follow these steps to carry out：
The first step：It weighs calcium hydroxide 0.33g, measures deionized water 500ml, be placed in a beaker and be stirred, when stirring
Between 1h so that calcium hydroxide is dissolved in water to form alkaline calcium hydroxide solution.
Second step：Granularity is less than 0.5mm, ash content 24.7wt%, moisture 8.2wt%, volatile matter 17.1wt%, fixed carbon
Calcium hydroxide solution prepared by the first step is added in the oxidized coal slime 100g of 50.0wt%, and it is anti-that stirring 2h carries out room temperature acid-base neutralization
It answers, by the acidic functionality of oxidized coal slime particle surface（Carboxyl, phenolic hydroxyl group）It neutralizes.Thereafter, using suction filtration machine to being formed
Coal slurry filtered, the slime filter cake filtered is put into 60 DEG C of drying box dry 8h, obtains the filter of acid-base neutralization oxidized coal slime
Cake.
Third step：2.00g n-caproic acid is added and fills the beaker of 1000ml deionized water, 60 DEG C of stirred in water bath 1h with
N-caproic acid is dissolved, n-caproic acid aqueous solution is formed.
4th step：The n-caproic acid aqueous solution that the preparation of 200ml third step is measured with beaker, the acid-base neutralization that second step is obtained
Oxidized coal slime filter cake is added in beaker, and stirring at normal temperature 3h carries out hydrophobization graft reaction.It is filtered after having reacted with suction filtration machine,
It filters obtained slime filter cake and is put into 60 DEG C of drying box dry 8h, obtain hydrophobic modification oxidized coal slime filter cake.
Fig. 5 is the contact angle optical photograph of the present embodiment water above-mentioned oxidized coal modified to non-surface, and measuring contact angle is
27.2°.Fig. 6 is the contact angle optical photograph of the present embodiment water above-mentioned oxidized coal modified to surface, and measuring contact angle is
91.4°.Thus, the hydrophobicity of oxidized coal slime can be improved in method of modifying provided by the present invention.
Use diesel oil as collecting agent, methyl isobutyl carbinol is aoxidized as hydrophobic modification of the foaming agent to above-mentioned preparation
Coal slime carries out flotation as pan feeding.As a comparison, equally the former oxidized coal slime handled without hydrophobic modification is floated
Choosing.Floatation equipment inflates single-trough flotating machine, speed of mainshaft 1200r/min, aeration quantity 3.0L/min, flotation using XFD-1.5L type
Slot volume is 1.5L, and coal-water fluid concentration is about 66.7g/L.Floatation process is as follows：It is added into pulp according to 240g/t coal slime
Diesel oil sizes mixing and stirs 1min;Then methyl isobutyl carbinol is added according to 70g/t coal slime, sizes mixing and stirs 1min.Open air inlet
Bubble 5min is scraped in valve, timing, and products obtained therefrom filtering, drying carry out weighing chemical examination.
Result of laboratory test shows that the combustible recovery after the former oxidized coal slime flotation handled without hydrophobic modification is
46.9wt%, cleans ash 7.3wt%；It is increased to 77.8wt% by the combustible recovery of the oxidized coal slime of hydrophobic modification,
And cleans ash is 9.7wt%, is slightly improved, but still conform to quality of cleaned coal requirement.Thus the present embodiment can prove institute of the present invention
The oxidized coal slime hydrophobic modification method of announcement can remarkably promote the flotation effect of oxidized coal slime.
Claims (2)
1. it is a kind of improve oxidized coal slime flotation effect hydrophobic sur- face modification method, the hydrophobic sur- face modification method be by
What the following steps carried out：
（1）It is 0.02~0.15: 100 by the mass ratio of calcium hydroxide and water, calcium hydroxide is added to the water, stirs 0.1~5h,
It makes it dissolve, forms alkaline calcium hydroxide solution；
（2）Step is added in oxidized coal slime by granularity less than 0.5mm（1）It is formed by calcium hydroxide solution, stirring 0.1~
5h carries out room temperature acid-base neutralization reaction, to neutralize carboxyl, the phenolic hydroxyl group functional group on oxidized coal slime surface；It followed by filters, obtains
Filter cake, and in 50~90 DEG C dry 3~for 24 hours, acid-base neutralization oxidized coal slime filter cake is made；The calcium hydroxide and oxidized coal slime
Mass ratio be 0.1~0.6: 100；
（3）It is 0.022~2: 100 by the mass ratio of organic carboxyl acid and water, organic carboxyl acid is dissolved in water, forms organic carboxyl acid water
Solution, stirring, heating promote the dissolution of organic carboxyl acid；
（4）By step（2）The acid-base neutralization oxidized coal slime filter cake of acquisition is added to step（3）In the organic carboxyl acid solution of formation,
0.1~5h of stirring at normal temperature carries out graft reaction, followed by filters, obtain filter cake in 50~90 DEG C dry 3~for 24 hours, be made and dredge
The modified oxidized slime filter cake of aquation；The mass ratio of the organic carboxyl acid and acid-base neutralization oxidized coal slime filter cake is 0.044~0.5:
100。
2. improving the hydrophobic sur- face modification method of oxidized coal slime flotation effect, the organic carboxyl acid as described in claim 1
It is one of n-caproic acid, positive enanthic acid and caprylic acid.
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| CN100548496C (en) * | 2007-03-02 | 2009-10-14 | 山西焦煤集团有限责任公司 | A kind of floatation method of difficult-to-float coal |
| CN101700491B (en) * | 2009-11-09 | 2011-07-20 | 中国海洋石油总公司 | Method for modifying fly ash |
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