CN103396777A - Application of chlorine dioxide blocking remover in coal bed modification - Google Patents
Application of chlorine dioxide blocking remover in coal bed modification Download PDFInfo
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- CN103396777A CN103396777A CN2013103086052A CN201310308605A CN103396777A CN 103396777 A CN103396777 A CN 103396777A CN 2013103086052 A CN2013103086052 A CN 2013103086052A CN 201310308605 A CN201310308605 A CN 201310308605A CN 103396777 A CN103396777 A CN 103396777A
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Abstract
The invention relates to an application of a chlorine dioxide blocking remover in coal bed modification and particularly relates to an application of a chlorine dioxide blocking remover for reducing the methane affinity of a coal bed. The coal bed modification process comprises the steps of reducing the adsorption capacity of coal to methane and improving the permeability of the methane in the coal bed. A chlorine dioxide water solution formed after the chlorine dioxide blocking remover enters bed beam cracks has the concentration of 200-6000mg/L. Lots of experiments find that after a blocking remover, namely the chloride dioxide blocking remover (HRS) frequently used in the oil and gas field, interacts with coal, the methane affinity of the coal is reduced and the permeability is remarkably improved. The reduction of the methane affinity of the coal means that the gas saturation and critical storativity of a coal reservoir are improved, and the increase of critical desorption pressure means that the gas production time in the initial mining period is shorted; more importantly, the recovery rate of coalbed methane under the same depletion pressure is increased and the economic benefit of coalbed methane mining is increased.
Description
Technical field
The present invention relates to the purposes of dioxide peroxide unblocking agent, be specially the application of dioxide peroxide unblocking agent aspect the parent's methane ability of reduction coal seam.
Background technology
The exploitation coal-seam gas (mainly contains methane CH
4) can obtain high effect cleaning the energy, reduce the control of coalmine gas cost, also can reduce greenhouse gas emission simultaneously, be subject to for many years the extensive concern of each coal production state of the world always.But the coal-bed gas exploitation of China exists the shortcomings such as gas output per well is low, the stable yields cycle is short, recovery ratio is not high, has seriously hindered China's coal gas industry development.
At present, the guanidine glue laminated of often using in oil recovery industry is split in the exploitation that technology applies to coal-seam gas, and the produced quantity that improves coal-seam gas has been played to positive effect.It is the Main Yield-increasing method in hyposmosis, extra-low permeability oil, gas field that the guanidine glue laminated is split, and is also the main method of cbm development.But there is the situation of " three is low " in China's overwhelming majority coal-seam gas, and namely low permeability, low gas content saturation ratio are faced the storage ratio with low, and ature of coal is softer, belongs to soft seam, coal seam temperature lower (generally at 10～20 ℃).The guanidine glue laminated that this means traditional oils, gas field routine is split technology and when cbm development is applied, is existed very large difficulty, and after adopting guanidine glue to take the sand pressure break, the guanidine glue is sent sand grains into newly-generated crack, and during crack closure, sand grains has been made propping agent, is filled in space.And guanidine glue itself is a kind of high molecular polymer, its existence makes fracture permeability reduce, even blocked, so when pressure break completes, tradition guanidine glue laminated split original fracturing liquid rubber-breaking not in time, not thorough, particularly the fracturing liquid injection pressure is greater than coal seam pressure, fracturing fluid leak, guanidine glue forms filter cake in fracture faces, and the problem that has reduced flow conductivity is more serious.And in order to address the above problem, the patent No. is to put down in writing in 02146452.9 patent document, utilize the effect of dioxide peroxide unblocking agent (HRS) to be " utilize the strong oxidizing property energy of dioxide peroxide; make the high molecular polymer oxygenolysis such as polyacrylamide, sesbania gum, guanidine glue; viscosity degradation, mobility improve and be easy to discharge; Can also kill rapidly various biomasses, reach the purpose of oil, well de-plugging ".Therefore when pressure break completes, need to use effective HRS ?the guanidine glue laminated split technology, HRS can fully degrade guanidine glue, broken glue is effective, in thorough solution hyposmosis soft seam, the guanidine glue laminated is split and in coal seam, is formed the filter cake pollution, by after the degraded of guanidine glue, returning discharge ，Shi crack, ground, is open to traffic.
Yet, in current coal-bed gas exploitation, if adopt a kind of mode of chemical modification to reduce coal seam reservoirs parent methane (CH
4) ability, and then gas saturation and the critical desorption pressures of increase coal seam reservoirs, and finally improve recovery ratio, will greatly improve the economic benefit of coal-bed gas exploitation.
Summary of the invention
The object of the present invention is to provide a kind of new purposes of dioxide peroxide unblocking agent (HRS), the specifically application of dioxide peroxide unblocking agent in the modification of coal seam.
After after many experiments, finding the unblocking agent that oil-gas field is commonly used-dioxide peroxide unblocking agent (HRS) and coal facies mutual effect, the close methane ability of coal descends and perviousness obviously improves.
The concrete using method of dioxide peroxide unblocking agent is the record in 02146452.9 patent document with the patent No., HRS enter behind the crack, coal seam control the concentration that forms aqueous solution of chlorine dioxide be 200 ?6000mg/L, further better must be to the coal seam modification.
Dioxide peroxide unblocking agent (HRS) is as follows to the mechanism of the modifying function on coal surface:
1, the change of coal surface physico-chemical property caused to the impact of coal on the methane adsorptive power
The coal surface adsorption property is by its physical properties (specific surface area and pore structure) and the common decision of chemical property (surface chemical property), and the chemical property on coal surface is determined by classification and the quantity of surface functional group to a great extent, the modal functional group in coal surface is oxygen-containing functional group, it affects wetting ability, surface charge of coal etc., thereby affects the absorption behavior of coal.The functional group on coal surface mainly contains carboxyl, lactone group, carbonyl, phenolic hydroxyl group, acid anhydrides, ether etc.Coal is after the dioxide peroxide unblocking agent is processed, and due to the strong oxidation of dioxide peroxide, change has to a certain degree all occurred for coal surface physics structure and surface chemical property.
Impact on coal surface physics structure:
In the data that the coal surface pore structure is characterized, after discovery HRS modification, specific surface area and the pore volume on coal surface significantly increase.After modification, the coal surface pore structure collapses, and the volume of unit mass obviously reduces, thereby causes the rate of permeation of methane in coal seam to increase.
Impact on the coal surface chemical property:
(1) the coal surface oxygen functional group increases: the elementary cell in texture of coal is arene compounds, as benzene, naphthalene, anthracene, phenanthrene, fluorenes.The surface functional group of coal mainly contains aldehyde, ketone, hydroxyl etc., and hydroxyl reduces along with increasing of metamorphic grade, after the HRS modification, on the coal surface, has mainly increased hydroxyl, carboxyl, carbonyl.
Methyl generation oxidizing reaction generates carboxyl:
Hydroxyl generation oxidizing reaction generates aldehyde radical:
Aldehyde radical generation oxidizing reaction generates carboxyl:
Related experiment proves, after the oxidation modification of HRS, the coal surface oxygen functional group increases, and coal sample reduces the absorption of methane, as table 1, shown in Figure 1.Coal surface oxygen functional group content increases after the HRS modification, and especially carboxyl-content significantly increases.Table 1 is associated with Fig. 1 result, can knows that carboxyl is larger to the methane Adsorption Effect, the increase of carboxyl-content obviously reduces adsorptive capacity, and the impact of lactone group and phenolic hydroxyl group is smaller.The increase of this explanation oxygen-containing functional group content, can reduce the absorption of coal to methane.
The content of table 1 oxidation modification front and rear surfaces oxygen-containing functional group
| Sample | Carboxyl | Lactone group | Phenolic hydroxyl group | Total oxygen-containing functional group |
| Before modification | 0.341 | 0.087 | 0.008 | 0.436 |
| After modification | 1.769 | 0.498 | 0.124 | 2.391 |
(2) the coal surface negative charge increases: raw coal is after peroxidation, the coal sample surface-CH-,-CH2-,-structure divisions such as CH3 change alcoholic extract hydroxyl group, aldehyde radical, ketone group and carboxyl into, the alcoholic extract hydroxyl group that the coal surface exists originally also can change to carboxyl, after oxidation-OH, C=O ,-increase of COOH functional group, coal surface electronegativity increases.After the HRS modification, coal surface negative charge number increases, the active adsorption position of having reduced methane molecule, and oxygen-containing functional group has changed the polarity on coal surface simultaneously, thereby has reduced the adsorptive capacity of methane.
Different functional groups is connected to different condensed-nuclei aromatics formation model compounds, and the coal surface of simulation after oxidation, measure the net charge on the carbon potential that functional group after oxidation is connected to condensed-nuclei aromatics, the results are shown in Table 2.
The surperficial net charge of model compound after table 2 oxidation
As can be seen from Table 2, along with the intensification (Jia Ji of methyl oxidation degree ?Qiang Ji ?Quan Ji ?carboxyl), its surface negative charge increases gradually, that is to say oxide treatment is carried out in the coal surface, can improve its surperficial electronegativity.
In addition, some groups on coal surface such as carbonyl can be used as electron donor provides electronics to organism, form Dian ?be subjected to electronic mechanism to strengthen adsorption, ketonic oxygen changes into carboxyl after oxidation, between sorbent material and adsorbate, can not form Dian ?be subjected to the electron recombination thing, cause the adsorptive capacity of methane to descend, therefore the surface of the coal after the oxide treatment of HRS electron-withdrawing group reduces, and the adsorbed methane amount reduces.
(3) the coal surface hydrophilicity improves: after HRS processed, coal surface oxygen functional group content increased, and has increased the coal surface polarity, has improved the wetting ability on coal surface.Along with the increase of oxygen-containing functional group content, the coal surface hydrophilicity strengthens, and is unfavorable for the absorption of nonpolar organic matter methane, thereby causes the variation of its absorption property.
Increase along with the coal surface hydrophilicity, water molecules by and oxygen-containing functional group between hydrogen bond action be adsorbed on the coal surface (in water, hydrogen bond preferentially is formed between water molecules and coal surface functional group), the water molecules of absorption becomes the secondary absorption site, thereby adsorb more water molecules, form water cluster, stoped the diffusion of methane.
In a word, although coal surface physical properties and chemical property are all influential to the adsorption of methane to coal, oxygen-containing functional group is greater than the impact of specific surface area on the impact of absorption.
2, the impact of the acidification of HRS rate of permeation in coal seam on methane
The pH value of HRS less than 4, have oxidisability, and contain the kinds of surface promoting agent, can play cleanup action to oily matter, the mineral substance on coal surface, thereby increase the perviousness of coal; After acid treatment was carried out in the coal surface, its surface acidity oxygen-containing functional group total amount increased, and specific surface area and pore volume increase, thereby rate of permeation increases.
Along with the reduction of pH value, metal ion such as iron, magnesium, calcium etc. are difficult for existing with precipitation forms, and are soluble in water, promoted the dissolving of metal ion.
The pH value of HRS is less than 4, and under acidic conditions, its surface potential is higher, and as shown in Figure 2, the polarity of HRS strengthens, thereby has reduced the adsorption of coal to non-polar molecule methane.
Mineral substance such as calcium, magnesium etc. in coal seam, with negative charge, can be adsorbed in the coal surface, thus in and Partial charge, reduced the surface potential of coal.But under acidic conditions, coal reduces the adsorptive power of mineral ion, thereby has improved the Surface Permeability of coal.
In addition, in coal, contain the sulphur content that exists with inorganic sulfur and organosulfur form, wherein inorganic sulfur mainly contains vitriol, sulfurous iron ore and a small amount of elementary sulfur.Main component dioxide peroxide in HRS can pH be 2 ?with S, FeS, react rapidly in 10 scope, make the pH value increase slowly, prevent Fe(OH)
2, Fe(OH)
3Colloid forms and stops up, simultaneously by Fe
2+Be oxidized to Fe
3+.Due to Fe
3+Compare Fe
2+Precipitation needs higher pH value, thereby slows down Fe
2+Secondary sedimentation.Reaction equation is as follows:
5S+6ClO
2+8H
2O→6Cl
‐+5SO
4 2‐+16H
+
5FeS+9ClO
2+2H
2O→5Fe
3++9Cl
‐+5SO
4 2‐+4H
+
FeS
2+3ClO
2+2H
2O→Fe
3++3Cl
‐+2SO
4 2‐+4H
+
In sum, coal-seam gas (mainly contains methane CH
4) with absorption, free and water-soluble three kinds of states, compose and be stored in the coal hole, mainly present ADSORPTION STATE.Coal is subject to the impact of metamorphic grade, coal seam temperature, reservoir pressure and the many factors such as moisture in coal type and moisture content of coal on the absorption property of methane.The adsorptive power of coal increases along with the intensity enhancing of incoalation.Polar group on low coalification stage molecular structure of coal unit is more, have wetting ability, and in coal, total moisture content is high, thereby has reduced the adsorptive capacity of coal to methane, i.e. incoalation is lower, and adsorptive capacity is less.The adsorptive power of brown coal is lower than the coal of each metamorphic episode, and long-flame coal, bottle coal, 3 coal rank adsorptive capacitys of rich coal increase slowly; Coking coal stage, the adsorptive capacity of coal starts quick increase; The hard coal adsorptive power is the strongest.The mesometamorphism coal, namely contain more condensed ring structure in the organic structure of rich coal, coking coal, lean coal, these hydrogeneous more condensed ring structures have hydrophobic nature, thereby in coal, total moisture content is obviously on the low side.Namely along with the enhancing of incoalation, coal increases the adsorptive power of methane; Along with the rising of coal seam temperature, coal is regular reduction to the adsorptive capacity of methane; In reservoir, moisture occupies the hole in coal, has reduced the adsorptive power to methane.Moisture in coal is higher, and the active adsorption point that may occupy position is just more, relatively leaves the available point position of methane molecule " delay " for and will reduce, and the saturated extent of adsorption of coal will reduce, thereby along with the increase of matrix of coal moisture, adsorption volume reduces; Coal is to the control that is stressed of the adsorptive capacity of methane, along with pressure increases and becomes large.When the coal seam reservoirs buried depth is larger, corresponding reservoir pressure is larger, and the per-cent that the gas in coal seam reservoirs can be separated the total adsorptive capacity of sucking-off is just less.When pressure is 20MPa, there is 3%～19% coal-seam gas to desorb; After reservoir pressure was less than 20MPa, the coal-seam gas of absorption just started more desorbing; Less than absorption coal-seam gas under the 10MPa pressure condition, account for 55%～85% of total adsorptive capacity.
In the present invention, after dioxide peroxide unblocking agent (HRS) and coal facies mutual effect, the close methane ability of coal descends and perviousness obviously improves.Coal parent methane ability reduces and means the coal seam reservoirs gas saturation and face storage than increasing, and critical desorption pressures increases also just to equal to shorten to arrange adopts the initial stage gas breakthrough time; Recovery ratio that the more important thing is coal-seam gas under identical exhausted pressure increases, and has improved the economic benefit of coal-bed gas exploitation.
The accompanying drawing explanation
Fig. 1 is the methane adsorption curve under 298K.
Fig. 2 is the impact of pH value on the zeta current potential.
Fig. 3 is the rate of permeation test macro.
In figure, 1 ?high pressure N
2Source, 2 ?decompression venting valve, 3 ?gas pressure sensor, 4 ?the static resistance strain gage, 5 ?digital treating meter, 6 ?pressure head of testing machine, 7 ?sealing rubber cover, 8 ?air permeable plate, 9 ?coal sample, 10 ?mass-flow gas meter, 11 ?the gas flow integrating instrument, 12 ?data collecting instrument.
Embodiment
The impact experiment of dioxide peroxide unblocking agent on coal seam parent's methane ability.
The die coal in Han Shankuang, Si Jiazhuan ore deposit, Yangquan and osiery Sha Qu ore deposit of Institutes Of Technology Of He'nan's energy science and engineering college's coal-seam gas engineering experiment chamber focusing, according to the GB/T19560 of the People's Republic of China (PRC) ?2004 " the high pressure isothermal adsorption test method volumetry of coal " regulation, isothermal adsorption parameter to coal is tested, and the results are shown in Table 3.
Table 3 isothermal adsorption experimental result
In upper table 3, data show: Jiaozhuo Gu Han mountain plateau beginning sample V
L=45.73cm
3/ g.daf, after the HRS composite blockage relieving agent is processed 09 ?10 ?the 3# sample be reduced to V
L=38.74cm
3/ g.daf, P
LBy 1.06MPa, bring up to 1.17MPa.Si Jia village coal sample V
L=45.43cm
3/ g.daf is reduced to 41.64cm after processing
3/ g.daf, P
LBy 1.15MPa, bring up to 1.23MPa.The husky bent pit coal sample V of osiery
L=22.74cm
3/ g.daf is reduced to 21.03cm after processing
3/ g.daf, PL brings up to 1.87MPa by 1.61MPa.Lan Shi volume V
LWith the Lan Shi pressure P
LThe index of coal adsorbed gas ability, the blue co-volume V of coal sample after the HRS composite blockage relieving agent is processed
LReduce blue formula pressure P
LRaise, show that the ability of coal adsorbed methane reduces.
The experiment of dioxide peroxide unblocking agent to the anti-reflection property of coal seam reservoirs.
1, sample preparation: according to experiment purpose and requirement, coal sample is processed into to the coal core of Ф 50mm * 50mm.
2, rate of permeation experimental system: comprise sealing rubber cover, trier loading and several parts such as Controlling System, high-pressure air source, gas flow and pressure test, as shown in Figure 3.
3, rate of permeation test, result such as table 4:
Table 4: rate of permeation test result
Table 4 data show, after HRS composite blockage relieving agent solution soaking, the raising of the rate of permeation minimum of coal sample 6.18%, maximum raising 354.65%, antireflective effect is remarkable.If increase the action time of HRS and coal, rate of permeation increases can be more.
Claims (2)
1. the application of dioxide peroxide unblocking agent in the modification of coal seam, the modification of described coal seam comprise the adsorptive power of reduction coal to methane, improve the rate of permeation of methane in coal seam.
2. it is 200-6000mg/L that the application of dioxide peroxide unblocking agent according to claim 1 in the modification of coal seam, described dioxide peroxide unblocking agent enter the concentration that forms aqueous solution of chlorine dioxide behind the crack, coal seam.
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Cited By (3)
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| CN105621823A (en) * | 2014-10-30 | 2016-06-01 | 中国石油天然气股份有限公司 | Treatment process for oil-contained sludge generated by oilfield wastewater treatment |
| CN106867501A (en) * | 2017-02-22 | 2017-06-20 | 山西晋城无烟煤矿业集团有限责任公司 | A kind of coal seam reservoirs transparent agent based on aqueous sodium hypochlorite solution |
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