CN1117635C - Floatating, desulfurizing and ash-reducing method for hihg-sulfur fine-particle coal - Google Patents

Floatating, desulfurizing and ash-reducing method for hihg-sulfur fine-particle coal Download PDF

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CN1117635C
CN1117635C CN 01102191 CN01102191A CN1117635C CN 1117635 C CN1117635 C CN 1117635C CN 01102191 CN01102191 CN 01102191 CN 01102191 A CN01102191 A CN 01102191A CN 1117635 C CN1117635 C CN 1117635C
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ash
inhibitor
desulfurizing
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CN1368404A (en
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胡军
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Abstract

The present invention provides a desulfurizing and ash-reducing method for high-sulfur fine-particle coal by the unification of inhibitor ultrasonic strengthening and a high efficiency flotation agent. The desulfurizing and ash-reducing method can effectively obtain ash-reducing effect for coal powder when in desulfurization, and thus, the yield of head coal is improved. The desulfurizing and ash-reducing method comprises the following steps: (1), preparing coal powder of which the grain diameter is smaller than 0.5mm into coal slurry of which the concentration is from 20 g/l to 200 g/l; (2), adding inhibitor into the coal slurry to be stirred, treating the coal slurry by ultrasonic of which the frequency is from 18 to 100kHz and adding a collecting agent to be stirred; (3), inputting into a flotation machine to carry out separation.

Description

A kind of Floatating, desulfurizing and ash-reducing method for hihg-sulfur fine-particle coal
Technical field
The present invention relates to a kind of sulphur coal floatation desulphurization and fall grey method, particularly a kind ofly adopt ultrasound-enhanced inhibitor and efficient floating agent synergy to the desulfurization of high-sulfur Bed for Fine Coal with fall grey method.
Background technology
At present, fall in the gray technology at coal desulfurization both at home and abroad, can carry out washing to lump coal by jigging, dense medium separation, can remove the bigger pyrite of particle and become grey mineral, and very poor to the separating effect of fine slime, desulfurization degree and to fall grey rate all very low, so, effectively remove the pyrite in the Bed for Fine Coal of particle diameter＜0.5mm, it is not enough only utilizing the gravity separation method desulfurization of coal.The fifties former Soviet Union is inhibitor with lime, suppresses pyrite and is used for the coal desulfurization test, and this method desulfurized effect is not obvious, and cleans ash increases to some extent; In coloured, ferrous metal ore dressing, be inhibitor with waterglass, suppress quartz, silicate etc., coal falls ash and does not see application report; Domestic once was foaming agent with the diethyl phthalate, be used for lead-zinc ore floating, can obtain close with terpenic oil, as to be better than ether alcohol foaming agent technical indicator, referring to " principles of chemistry of floating agent " that publishing house of Zhongnan Polytechnic Univ publishes in February, 1987, this foaming agent is not seen application report as being used for the coal floating agent; There is the scholar to carry out the report of desulfurization research with low frequency sound energy abroad.
The coal floatation process of using in the production practices now is: add hydrocarbon collector and size mixing in black water, add the alcohols foaming agent again, feed flotation device then and carry out sorting; Can also in black water, add collecting agent and foaming agent bulk flotation medicament is sized mixing, feed the flotation device sorting then.But the requirement that these two kinds of methods are difficult to reach desulfurization simultaneously and fall ash.
Summary of the invention
The objective of the invention is to: provide a kind of and adopt ultrasound-enhanced inhibitor and efficient floating agent synergy to the desulfurization of high-sulfur Bed for Fine Coal with fall the method for ash, can in desulfurization, play the effect of coal dust being fallen ash effectively, and the productive rate of raising cleaned coal.
The present invention is achieved in that a kind of Floatating, desulfurizing and ash-reducing method for hihg-sulfur fine-particle coal, 1. particle diameter is made the black water that concentration is 20g/l-200g/l less than the 0.5mm coal dust; 2. in black water, add inhibitor and stirred, the black water that has added inhibitor is carried out ultrasound-enhanced processing, add collecting agent and stir with the ultrasonic wave of frequency 18-100kHz; 3. feed flotation device and carry out sorting.
Described inhibitor is that the quick lime of coal dust weight 0.05%-1% and waterglass that weight is coal dust weight 0.01%-1% are formed by weight; Collecting agent is that weight is repefral or diethyl phthalate or dibutyl phthalate or the dioctyl phthalate of coal dust weight 0.005%-0.1%.
Described collecting agent is a diethyl phthalate.
Described ultrasonic wave is to the black water effect of having added inhibitor more than 5 minutes.
Grey floating agent diethyl phthalate and homologue thereof fall in the coal desulfurization that the present invention adopts, and this medicament is few to the flotation consumption of coal, collecting height, selectivity are strong, is that grey floating agent falls in a kind of good coal desulfurization.With the diethyl phthalate is collecting agent, under different pH condition, to the not influence of floatability of coal.Adopt lime and waterglass inhibitor as desulfurization and deashing, very obvious to becoming the inhibition effect of grey mineral in the coal.Lime is divided into quick lime and white lime, and quick lime is met water and just become white lime, and the solubility of white lime in water is minimum, and degree of ionization is very low, can not give full play to desulfidation as inhibitor; After the black water that has added inhibitor carried out ultrasound-enhanced processing, thereby the degree of ionization that has improved inhibitor widely increases and has strengthened Ca 2+Absorption in pyrite surface; Ultrasonic processing simultaneously changes the granularmetric composition, granularity quality of mineral grain in the ore pulp etc., has promoted that the pyrite of fine grained embedding cloth dissociates in the coal, for floatation process to pyritous inhibition, created advantageous conditions.Ultrasonic processing place changes pH value, surface potential, electrical conductivity, dissolved oxygen of ore pulp system etc.To the separation results of high-sulfur dirty coal sample, the pyrite removal efficiency can reach 70%-85%, and ash content is less than 10%.
The specific embodiment
The present invention will be further described below in conjunction with non-limiting embodiment.
Embodiment 1 and embodiment 2 are two kinds of actual coal sample sorting demonstration test results, totally 17 examples, and contrast sees Table 1 and table 2.Experimental condition: 1.5L hanging trough flotator, pulp density 50g/L, diethyl phthalate (BET) consumption 200g/t coal dust, GF consumption 600g/t coal dust, FS202 consumption 900g/t coal dust, CaO consumption 2.0kg/t coal dust, waterglass (Na 2SiO 3) consumption 1.0kg/t coal dust, lignin 0.1kg/t coal dust, sodium humate 0.2kg/t coal dust, ultrasonic processing 10 minutes.
The checking of embodiment 1. Shandong Zibo coal samples
Table 1 Shandong Zibo coal sample separation results data
The test technology condition r％ Aad％ ε％ St，ad％ Sp，ad％ Ts tl％ Ts pl％ The sulphur rate falls in Sp ηs p％
GF 70.35 12.68 86.36 3.62 2.52 50.55 55.34 36.52 37.45
FS202 69.61 11.20 86.90 3.84 2.74 48.10 51.96 30.98 31.54
BET 69.57 9.49 88.52 2.65 1.57 54.75 72.49 60.45 60.46
AET 54.66 8.96 78.26 2.62 1.55 53.67 71.83 60.75 56.14
DET 68.95 10.22 88.17 2.74 1.66 52.74 67.35 57.66 57.43
HET 58.32 9.23 80.06 2.83 1.75 51.31 60.94 54.37 54.19
Lignin 51.74 8.61 69.34 2.45 1.38 53.72 74.39 61.96 43.78
Sodium humate 56.38 8.74 77.85 2.61 1.53 52.35 73.26 61.41 46.39
CaO+Na 2SiO 3 +BET 63.36 8.64 81.38 2.47 1.39 60.58 77.82 64.99 59.04
Ultrasonic processing 10 '+BET 71.38 9.52 90.80 2.58 1.48 53.61 73.39 62.72 64.28
CaO+Na 2SiO 3+ ultrasonic processing 10 '+BET 65.46 9.12 83.64 1.96 0.86 67.68 85.82 78.34 72.98
Annotate: the r rate of recovery; Aad as analysed basis ash content; The body rate of recovery that ε is flammable; St, the full sulphur of ad as analysed basis; Sp, ad as analysed basis pyritic sulfur; Ts tThe full sulphur desulfurization degree of l; Ts pL pyritic sulfur desulfurization degree; η s pPyrite desulfurization sophistication; The Sp pyritic sulfur; BET is the diethyl phthalate code name; AET (repefral), DET (dibutyl phthalate), HET (dioctyl phthalate); GF is a foaming agent; FS202 is a collecting agent; Na 2SiO 3Be waterglass.
Table 1 data show
1) floating agent: three kinds of floating agent consumption differences, the rate of recovery is suitable, and about 70%.Has only ash content＜10% with BET.Compare when using BET, full sulphur content lacks more than 1.0%, pyrite removal efficiency Ts pL increases by 20%, reaches 72.49%.Illustrate that BET is the respond well coal floating agent of a kind of desulfurization and deashing.
2) comparison of inhibitor effect and ultrasound-enhanced desulfurization and deashing:
With CaO is inhibitor, and to the not influence substantially of the rate of recovery (r=69.12%), ash content (A=9.75%), sulphur content (St=2.52%) reduces by 0.13%, pyrite removal efficiency Ts pL increases by 2.5%.
With waterglass is inhibitor, and bigger to the rate of recovery (r=60.86%) influence, the rate of recovery reduces by 9%; Ash content (A=8.46%) reduces by 1%, plays certain ash effect of falling; Sulphur content (St=2.66%) does not change substantially, illustrates that independent use of waterglass do not have inhibitory action to pyrite, pyrite removal efficiency Ts pIt is that the rate of recovery reduces due to 9% that l increases by 3.29%.
Mix use with CaO and waterglass, (r=63.36%) has certain influence to the rate of recovery, and the rate of recovery reduces by 6.2%; It is nearly 1% that ash content (A=8.64%) reduces, and plays certain ash effect of falling; Sulphur content (St=2.47%) reduces by 0.2%, pyrite removal efficiency Ts pL increases by 5.33%, and effect is more obvious.
To carrying out flotation after the ultrasonic processing of ore pulp, there are certain influence, the rate of recovery to increase nearly 2.0% separately to the rate of recovery (r=71.38%); Ash content (A=9.52%) does not change substantially; Sulphur content (St=2.58%) reduces less than 0.1%, pyrite removal efficiency Ts pL increases by 1.0%, and it is nearly 4.0% that the desulfurization sophistication increases, DeGrain.After this was ultrasonic processing, the fine grained mineral increased in the ore pulp, cause medicament selectivity variation, so that produced all increases to some extent of the rate of recovery, ash content.
Carry out flotation after inhibitor and the ultrasound-enhanced synergy, (r=65.46%) has certain influence to the rate of recovery, and the rate of recovery reduces 4.11%; It is not obvious that ash content (A=9.12%) reduces by 0.37% variation; Sulphur content (St=1.96%) has obviously reduced by 0.69%, pyrite removal efficiency Ts pL reaches 85.82%.Compare pyrite removal efficiency Ts with the data of medicament GF and FS202 effect pL has increased more than 30%.This explanation inhibitor and ultrasound-enhanced synergy have been played obvious effects to desulfurization and deashing.
3) floatation clean coal is selected: bigger to the rate of recovery (r=50.11%) influence, the rate of recovery reduces nearly 20%; Ash content (A=6.57%) obviously reduces, and the flammable body rate of recovery has also reduced by 23%; Sulphur content (St=2.51%) has reduced by 0.14%, pyrite removal efficiency Ts pL reaches 82.2%, but the desulfurization sophistication only reaches 46.35%.
Floatation clean coal behind the interpolation inhibitor is selected, and is bigger to the rate of recovery (r=47.35%) influence, and the rate of recovery reduces above 22%; Ash content (A=6.43%) also obviously reduces, and the flammable body rate of recovery has reduced by 26%; Sulphur content (St=2.37%) has only reduced by 0.28%, pyrite removal efficiency Ts pL reaches 84.85%, but the desulfurization sophistication only is 46.1%.Cleaned coal is selected can obviously reduce ash content in this explanation, improves the sulphur content removal efficiency, but this obtains by losing the rate of recovery, is difficult to get the nod in actual production.
4) with standard slime separation method-coal slime flotation substep release test result relatively: when the rate of recovery 70%, ash content reduces by 3%, and it is nearly 1% that sulphur content reduces, and the cleaned coal class has improved nearly 7 ranks.The effect that shows this floating agent and inhibition method is tangible.
5) homologue of diethyl phthalate has been investigated in test: AET (repefral), DET (dibutyl phthalate), HET (dioctyl phthalate) are to the influence of actual coal sample separating effect.
Test shows: DET is suitable to the collecting performance and the phenethyl ester of coal, but simultaneously pyritous collecting performance is also increased.It is bigger that AET compares difference to the floatability of coal and phenethyl ester, and to pyritous float-amount a little more than phenethyl ester.When using HET, the float-amount of coal reduces, and pyritous float-amount increases.
6) result of use of inhibitor lignin, sodium humate etc. is that flotation has certain desulfurization and deashing effect to coal, but the clean coal recovery loss is bigger.
Jiexiu, embodiment 2. Shanxi coal sample demonstration test
Determine that by experimental study BET is a kind of effective desulfurization and deashing coal floating agent, add CaO and waterglass, strengthen, can further reach the positive effect that ash falls in the coal floatation desulphurization through ultrasonic processing.For understanding this medicament and adaptation of methods, verified that with Jiexiu, Shanxi coal sample result of the test sees Table 2.(experimental condition is the same, the medicament mixed proportion: FS202 900g/t+GF200g/t)
Table 2 Shanxi coal sample screening test result
The test technology condition r％ Aad％ ε％ St，ad％ Sp，ad％ Ts tl％ Ts pl％ ηs p％
FS202+GF 71.94 11.98 77.51 2.32 1.56 51.62 58.43 37.91
BET 70.67 9.48 78.32 1.92 1.16 60.67 69.64 50.06
CaO+Na 2SiO 3 +BET 66.28 8.73 74.06 1.71 0.95 67.15 76.68 53.21
Ultrasonic processing 10 '+BET 72.41 9.76 80.00 1.80 1.04 62.22 72.11 55.21
Ultrasonic processing 10 '+BET+CaO+Na 2SiO 3 71.24 9.52 78.92 1.34 0.58 72.33 84.70 68.97
Condition the same (coal sample size-200 order) 67.34 10.03 74.17 1.48 0.72 71.11 82.04 61.00
Annotate: the r rate of recovery; Aad as analysed basis ash content; The body rate of recovery that ε is flammable; St, the full sulphur of ad as analysed basis; Sp, ad as analysed basis pyritic sulfur; Ts tThe full sulphur desulfurization degree of l; Ts pL pyritic sulfur desulfurization degree; η s pPyrite desulfurization sophistication; The Sp pyritic sulfur; BET is the phthalic acid diethyl ester code name; GF is a foaming agent; FS202 is a collecting agent; Na 2SiO 3Be waterglass.
Show by table 2 test data:
1) floating agent: relatively also consumption is different with BET for floating agent FS202+GF, and the rate of recovery is still suitable, and about 71%.Ash content＜10% with BET.Compare when using BET, full sulphur content reduces 0.4%, pyrite removal efficiency Ts pL increases by 11%, reaches 69.64%.
2) comparison of inhibitor effect and ultrasound-enhanced desulfurization and deashing:
With inhibitor C aO and waterglass synergy, (r=66.28%) has certain influence to the rate of recovery, and the rate of recovery reduces by 4.93%; It is nearly 1% that ash content (A=8.73%) reduces, and it is not obvious to fall the ash effect; Sulphur content (St=1.71%) reduces by 0.21%, pyrite removal efficiency Ts pL increases by 7.04%, and effect is more obvious.
To carrying out flotation after the ultrasonic processing of ore pulp, there are certain influence, the rate of recovery to increase nearly 2.0% separately to the rate of recovery (r=72.41%); Ash content (A=9.76%) does not change substantially; Sulphur content (St=1.80%) reduces by 0.12%, pyrite removal efficiency Ts pL increases by 2.74%, and certain effect is arranged.
Carry out flotation after inhibitor and the ultrasound-enhanced acting in conjunction, little to the rate of recovery (r=71.24%) influence, the rate of recovery increases by 0.57%; Ash content (A=9.52%) is suitable; Sulphur content (St=1.34%) has obviously reduced by 0.58%, pyrite removal efficiency Ts pL reaches 84.7%, has increased by 15%.Compare pyrite removal efficiency Ts with the data of medicament GF and FS202 effect pL has increased nearly 20%.
More than explanation floating agent BET, inhibitor and ultrasound-enhanced acting in conjunction method have obvious effects equally to the desulfurization and deashing of Jiexiu, Shanxi coal.
3) sorting after the fine grinding: this research is milled to coal sample in-200 orders under the constant situation of sorting and rejection condition, checking and investigate the effect of this method to the fine grained desulfurization and deashing.Test data (table 8-4) shows that sorting after the coal sample fine grinding has certain influence to the rate of recovery (67.34%), has reduced by 3%, and this and simple ore thing test data match.Show that the fine grained specific surface strengthens, reagent consumption increases.Dosing is constant when in other words being conventional coal flotation, and the rate of recovery of-200 order particles is less than the rate of recovery of+200 order particles.
Sorting after the fine grinding to the reduction of cleans ash (10.03%), is not played the inhibition effect, even the ash content when being higher than former state and not suppressing.For sulphur content (1.48%) tangible reduction is arranged then, but also the sulphur content of the too late not identical rejection condition of fine grinding is low.Pyrite removal efficiency Ts pL has reduced nearly 2.7%.Situation when this produces with actual coal flotation conforms to fine grain sorting selectivity variation.Floating agent, inhibitor and intensified condition all should suitably increase or be adjusted under this situation, and this awaits further studying from now on.
4) with standard slime separation method-coal slime flotation substep release test result relatively: when the rate of recovery 70%, ash content changes little, and it is nearly 1.18% that sulphur content reduces, and the cleaned coal class has improved nearly 6 ranks.
Embodiment 3. different sorting condition test results
1. the floating agent consumption changes
Table 3 Shandong coal sample screening test result
Test technology condition BET consumption ml/t r％ Aad％ S t，ad％ ηst％
100 57.37 7.44 2.41 57.04
200 69.57 9.49 2.65 63.62
300 70.47 10.33 2.84 59.52
Annotate: the table internal symbol is with table 1; BET is 1.2 gram/ml.
Table 4 Shandong coal sample screening test result
Test technology condition GF consumption ml/t r％ Aad％ S t.ad％ ηst％
200 56.73 200 2.8 48.71
400 64.18 400 3.31 43.57
600 70.35 600 3.62 39.97
Annotate: the table internal symbol is with table 1; GF is 0.9 gram/ml.
Table 5 Shandong coal sample screening test result
Test technology condition FS202 consumption ml/t r％ Aad％ S t，ad％ ηst％
300 56.87 8.76 2.65 51.81
600 67.78 10.66 3.73 35.84
900 69.61 11.2 3.84 34.05
Annotate: the table internal symbol is with table 1; FS202 is 0.91 gram/ml.
Result of the test shows: under the essentially identical situation of the rate of recovery, the separating effect of floating agent BET obviously is better than GF and FS202.Consider by coking pit ash requirement＜10%, behind the use BET, the clean coal recovery maximum, sulphur content is minimum, and dosing is minimum.Concrete data analysis is with table 1.
2. the result of different inhibitor conditions
Table 6 Shandong coal sample screening test result
CaO 2.0kg/t BET consumption ml/t r％ Aad％ S t，ad％ ηst％
100 58.67 7.51 2.33 57.93
200 69.12 9.75 2.52 66.33
300 74.46 11.89 2.69 63.05
Annotate: the table internal symbol is with table 1; BET is 1.2 gram/ml.
Table 7 Shandong coal sample screening test result
Na 2SiO 31.0kg/t BET consumption ml/t r％ Aad％ S t，ad％ ηst％
100 51.23 6.73 2.54 47.92
200 60.86 8.46 2.66 55.23
300 63.99 9.66 3.01 50.22
Annotate: the table internal symbol is with table 1; BET is 1.2 gram/ml.
Table 8 Shandong coal sample screening test result
CaO 2.0kg/t Na 2SiO 31.0kg/t BET consumption ml/t r％ Aad％ S t，ad％ ηst％
100 56.74 6.63 2.3 58.57
200 63.36 8.64 2.47 68.34
300 66.67 9.11 2.51 65.98
Annotate: the table internal symbol is with table 1; BET is 1.2 gram/ml.
Test shows: the different amounts of floating agent BET, and inhibitor waterglass is bigger to rate of recovery influence, reduces about 10%, and CaO does not have influence substantially to the rate of recovery, and the two mixing is also little to the influence of the rate of recovery.To the reduction of ash content, the most obvious when waterglass is arranged.To the reduction of sulphur content, more obvious when CaO is arranged, when mixing, the two reduces the amplitude maximum.
3. the result of the test of different inhibitor consumptions
Table 9 Shandong coal sample screening test result
BET 200ml/t CaO consumption kg/t r％ Aad％ S t，ad％ ηst％
1 69.46 9.7 2.61 73.38
2 69.12 9.75 2.52 81.78
3 66.41 10.86 2.48 81.28
Annotate: the table internal symbol is with table 1; BET is 1.2 gram/ml.
Table 10 Shandong coal sample screening test result
BET200ml/t Na 2SiO 3Consumption kg/t r％ Aad％ S t，ad％ ηst％
0.5 65.31 9.47 2.64 64.94
1 63.99 8.49 2.66 70.02
1.5 57.23 8.23 2.65 63.8
2 55.76 7.76 2.64 63.12
Annotate: the table internal symbol is with table 1; BET is 1.2 gram/ml.
Test shows: the consumption of CaO is little to rate of recovery influence; Effect is to decrease to sulphur content; The influence of ash content is had tangible increase when the 3kg/t, and this is because CaO when big consumption, causes ore pulp viscosity to increase, and is unfavorable to falling ash.When the waterglass consumption increases, bigger to rate of recovery influence, also bigger to the ash content reduction, not obvious to the reduction of sulphur content.

Claims (4)

1. 1. a Floatating, desulfurizing and ash-reducing method for hihg-sulfur fine-particle coal makes the black water that concentration is 20g/l-200g/l with particle diameter less than the 0.5mm coal dust; 2. in black water, add inhibitor and stirred, the black water that has added inhibitor is carried out ultrasound-enhanced processing, add collecting agent and stir with the ultrasonic wave of frequency 18-100kHz; 3. feed flotation device and carry out sorting.
2. Floatating, desulfurizing and ash-reducing method for hihg-sulfur fine-particle coal according to claim 1 is characterized in that: described inhibitor is that the lime of coal dust weight 0.05%-1% and waterglass that weight is coal dust weight 0.01%-1% are formed by weight; Collecting agent is that weight is repefral or diethyl phthalate or dibutyl phthalate or the dioctyl phthalate of coal dust weight 0.005%-0.1%.
3. Floatating, desulfurizing and ash-reducing method for hihg-sulfur fine-particle coal according to claim 2 is characterized in that: described collecting agent is a diethyl phthalate.
4. Floatating, desulfurizing and ash-reducing method for hihg-sulfur fine-particle coal according to claim 1 and 2 is characterized in that: described ultrasonic wave is to the black water effect of having added inhibitor more than 5 minutes.
CN 01102191 2001-01-31 2001-01-31 Floatating, desulfurizing and ash-reducing method for hihg-sulfur fine-particle coal Expired - Fee Related CN1117635C (en)

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CN102276027B (en) * 2011-05-30 2013-01-09 太原理工大学 Method for ultrasonic treatment, electrolysis and flocculation of slime water
CN104073318B (en) * 2014-07-10 2015-11-11 北京铱金惠通能源控股有限公司 Sulphur method falls in a kind of high sulphur coal
US20160082446A1 (en) * 2014-09-24 2016-03-24 Omnis Mineral Technologies, Llc Flotation separation of fine coal particles from ash-forming particles
CN104525385B (en) * 2015-01-14 2017-01-25 中南大学 Coal dressing collecting agent and preparing method thereof
CN105331421B (en) * 2015-12-02 2018-10-09 深圳市瑞成世代实业有限公司 A kind of coal floatation desulphurization composite restrainer and its application
CN107127055A (en) * 2017-05-23 2017-09-05 西北矿冶研究院 Separation method and separation device for difficult-to-separate oxidized coal slime
CN109054464B (en) * 2018-08-20 2020-11-06 西安科技大学 Physical deashing process for tire cracking carbon black
CN110560256B (en) * 2019-09-30 2021-06-04 西安科技大学 Comprehensive utilization process for reducing sulfur content of high-sulfur coal ash

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