CN115124978B - Gas drainage borehole gel hole sealing material and preparation method thereof - Google Patents

Gas drainage borehole gel hole sealing material and preparation method thereof Download PDF

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CN115124978B
CN115124978B CN202210749361.0A CN202210749361A CN115124978B CN 115124978 B CN115124978 B CN 115124978B CN 202210749361 A CN202210749361 A CN 202210749361A CN 115124978 B CN115124978 B CN 115124978B
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gel
active
hole sealing
sealing material
acrylamide
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CN115124978A (en
Inventor
李敏
李东雨
鲁义
施式亮
贺珊
叶青
李贺
王正
朱双江
储明浩
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Hunan University of Science and Technology
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Hunan University of Science and Technology
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
    • C09K8/42—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells
    • C09K8/46—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells containing inorganic binders, e.g. Portland cement
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B26/00—Compositions of mortars, concrete or artificial stone, containing only organic binders, e.g. polymer or resin concrete
    • C04B26/02—Macromolecular compounds
    • C04B26/04—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • E—FIXED CONSTRUCTIONS
    • E21—EARTH DRILLING; MINING
    • E21B—EARTH DRILLING, e.g. DEEP DRILLING; OBTAINING OIL, GAS, WATER, SOLUBLE OR MELTABLE MATERIALS OR A SLURRY OF MINERALS FROM WELLS
    • E21B33/00—Sealing or packing boreholes or wells
    • E21B33/10—Sealing or packing boreholes or wells in the borehole
    • E21B33/13—Methods or devices for cementing, for plugging holes, crevices, or the like
    • E—FIXED CONSTRUCTIONS
    • E21—EARTH DRILLING; MINING
    • E21F—SAFETY DEVICES, TRANSPORT, FILLING-UP, RESCUE, VENTILATION, OR DRAINING IN OR OF MINES OR TUNNELS
    • E21F7/00—Methods or devices for drawing- off gases with or without subsequent use of the gas for any purpose
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
    • C04B2111/00724—Uses not provided for elsewhere in C04B2111/00 in mining operations, e.g. for backfilling; in making tunnels or galleries
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00—Technologies for solid waste management
    • Y02W30/50—Reuse, recycling or recovery technologies
    • Y02W30/91—Use of waste materials as fillers for mortars or concrete

Abstract

The application discloses a gas drainage borehole gel hole sealing material and a preparation method thereof. The gel hole sealing material is a composite material and comprises an active gel base material, fly ash, water and a water retaining agent; the fly ash is basic aggregate, and the active gel base material and the fly ash form an active gel material; the active gel base material is three-dimensional network-shaped polyacrylamide gel prepared by the reaction of acrylamide, N- (4-hydroxy-3-methoxy-benzyl) -acrylamide and an active material, and the active material is sodium polydodecyl benzene sulfate. The gel hole sealing material can well fill the drilled holes, and can fill the gaps of the drilled holes by proper pressurization in a reasonable range and fluidity under the action of pressure, so that the requirement of tightness is met; the gel hole sealing material has good flexibility and ductility, deforms along with the deformation of the drilling hole, does not break along with the deformation of the drilling hole, and still has good sealing performance in the long-term gas drainage process.

Description

Gas drainage borehole gel hole sealing material and preparation method thereof
Technical Field
The application belongs to the field of efficient extraction of coal mine gas, and particularly relates to a gas drainage borehole gel hole sealing material and a preparation method thereof.
Background
Under the existing coal resource occurrence condition in China, the coal mine has complex geological conditions, a large amount of coal beds containing gas and large gas reserves of the coal mine, and the gas is used as a coal companion and is an unconventional natural gas with high heat value and no pollution, and is also a greenhouse gas which threatens the underground production safety and the atmospheric environment.
In order to cope with the occurrence of gas accidents, gas extraction is usually carried out on a coal seam of a gas mine, and the gas extraction is used for solving the problem that the gas concentration in a gas mine roadway is too high, so that the gas extraction is a fundamental measure for controlling the gas disasters, fully utilizing resources and reducing environmental pollution. The investigation results of the gas extraction conditions of some main mining areas in China show that the gas concentration is limited in a range of 30 days after about 40% of mine pre-extraction holes are extracted, and the extraction can be continued for several months. The cost of the drainage drilling hole is high, and the drainage concentration is reduced, so that the gas drainage period is prolonged, and the improvement of gas drainage benefits is further hindered. The main reason is that the sealing quality of the extraction drilling hole is poor, so that the initial plugging is invalid, and the drilling hole cannot be plugged effectively. After several months of extraction, the new-born fissures develop and the leakage channels are expanded, so that the underground gas extraction amount and the underground gas extraction concentration are lower. In the gas extraction process, the coal seam is required to be drilled and sealed, the drilling sealing quality is closely related to the gas leakage condition of the drilling, and data show that more than 80% of air enters the extraction system through the drilling to influence the gas extraction amount, and when the air intake amount is reduced by 1/2, the gas extraction amount can be improved by 1.5 times, so that the quality of hole sealing has a direct influence on the gas extraction effect.
In summary, as the coal seam drilling is easy to collapse, the drilling extraction life is short, the drilling hole sealing effect is not ideal, which is a trouble for efficient extraction of coal mine gas, the extraction concentration can be improved by improving the drilling hole sealing quality, and the method for improving the drilling hole sealing quality mainly improves the sealing performance of the hole sealing material and the effectiveness of the hole sealing process, so that the development of the hole sealing material with good performance is important for improving the sealing performance of the pre-extraction drilling hole and the gas extraction effectiveness.
Disclosure of Invention
Aiming at the problems in the prior art, the application provides the gas drainage borehole gel hole sealing material and the preparation method thereof, and the gel hole sealing material not only can form a fluid with certain viscosity to permeate into coal cracks, but also can be well filled to achieve the sealing effect; the gel hole sealing material has certain flexibility and ductility, and the material deforms along with the change of stress in the long-term construction process, so that long-term and efficient tightness is realized; the gel hole sealing material has the excellent properties of environmental protection, no pollution, no toxicity and low price.
In order to achieve the above purpose, the application provides a gas drainage borehole gel hole sealing material, which is a composite material and comprises an active gel base material, fly ash, water and a water retaining agent;
the fly ash is basic aggregate, and the active gel base material and the fly ash form an active gel material;
the active gel base material is three-dimensional network-shaped polyacrylamide gel prepared by the reaction of acrylamide, N- (4-hydroxy-3-methoxy-benzyl) -acrylamide and an active material, and the active material is sodium polydodecyl benzene sulfate.
Further, the gel hole sealing material comprises the following components in parts by mass: 20-30 parts of fly ash, 60-90 parts of water and 1 part of water-retaining agent;
the active gel base material is prepared by reacting 1-2 parts of acrylamide, 1-2 parts of N- (4-hydroxy-3-methoxy-benzyl) -acrylamide, 1-2 parts of sodium dodecyl benzene sulfate and 2-4 parts of sodium dodecyl benzene sulfate.
Further, the mass ratio of the fly ash to the water is 1:3.
Further, the mass ratio of the acrylamide to the N- (4-hydroxy-3-methoxy-benzyl) -acrylamide in the active gel substrate is 1:1-3:2.
Further, the water-retaining agent is carboxymethyl cellulose.
The application also provides a preparation method of the gas drainage borehole gel hole sealing material, which comprises the following steps: firstly, preparing an active gel base material by polymerization reaction of acrylamide, N- (4-hydroxy-3-methoxy-benzyl) -acrylamide and active material sodium polydodecyl benzene sulfate, then uniformly mixing the active gel base material with basic aggregate fly ash to obtain an active gel material, and finally adding water and a water-retaining agent, and stirring at a high speed to obtain the gel hole sealing material.
Further, the preparation method comprises the following steps:
step 1) preparation of an active gel substrate: firstly, sterilizing active material sodium polydodecyl benzene sulfate, then pouring acrylamide, N- (4-hydroxy-3-methoxy-benzyl) -acrylamide and the treated active material into a beaker according to mass proportion, heating to 90 ℃ and stirring, polymerizing to obtain three-dimensional network polyacrylamide gel, cooling to room temperature and preserving for later use;
step 2) preparing an active gel material: adding the fly ash and the active gel base material into a container according to the mass fraction ratio under the normal temperature condition, and stirring and mixing to obtain an active gel material;
step 3) preparing a gel hole sealing material: and adding the active gel material, water and the water-retaining agent into a container according to the mass portion ratio, and uniformly stirring the mixed solution at normal temperature to obtain the gel hole sealing material.
Further, in the step 1), the active material sodium polydodecyl benzene sulfate is sterilized, specifically, the sodium polydodecyl benzene sulfate is sterilized by ultraviolet rays for about 20 to 40 minutes.
Further, the method is characterized in that the step 3) is to stir the mixed solution evenly, specifically: stirring the mixed solution by adopting a constant-temperature magnetic stirrer at the speed of 10r/s for 3-5 min.
Compared with the prior art, the application has the following advantages:
1. the application provides a gas drainage borehole gel hole sealing material, which is a composite material and comprises an active gel base material, fly ash, water and a water retaining agent; the fly ash is basic aggregate, and the active gel base material and the fly ash form an active gel material; the active gel base material is three-dimensional network-shaped polyacrylamide gel prepared by the reaction of acrylamide, N- (4-hydroxy-3-methoxy-benzyl) -acrylamide and an active material, and the active material is sodium polydodecyl benzene sulfate. Through the mutual synergistic effect of the components, the gel hole sealing material not only can form fluid with certain viscosity to permeate into coal cracks, but also can be well filled to achieve the sealing effect; the gel hole sealing material has certain flexibility and ductility, and the material deforms along with the change of stress in the long-term construction process, so that long-term and efficient tightness is realized; the gel hole sealing material has the excellent properties of environmental protection, no pollution, no toxicity and low price.
2. According to the gas drainage borehole gel hole sealing material, the fly ash is used as the basic aggregate, and the fly ash and the active gel base material are organically combined, so that the obtained target material has gel characteristics, and meanwhile, the fly ash can improve the toughness of the gel hole sealing material after being solidified when meeting water, so that the quality after hole sealing is improved, the cost of the material and the hole sealing speed can be ensured, the hole sealing is efficient and quick, the operation is simple and convenient, the production cost can be reduced under the condition that a cross-linking agent is not added, the pollution to the environment can be reduced to the greatest extent, the cost is low, and the gas drainage borehole gel hole sealing material is nontoxic. Meanwhile, under the condition of not adding a cross-linking agent, acrylamide and a monomer N- (4-hydroxy-3-methoxy-benzyl) -acrylamide are subjected to free radical copolymerization reaction, so that three-dimensional network-shaped polyacrylamide gel can be synthesized, and an appropriate amount of active material (sodium polydodecyl benzene sulfate) is added to promote the combination of the two to prepare an active gel substrate; meanwhile, the water-retaining agent carboxymethyl cellulose is added, and because the carboxymethyl cellulose is a fiber derivative, the molecular structure of the carboxymethyl cellulose contains a large number of hydrophilic groups: after water is added, the active gel hole sealing material can be combined with a non-hydrated dispersion medium (water), free moisture is prevented from escaping, the moisture is preserved as much as possible, the water retention of the gel hole sealing material is improved, the active gel hole sealing material has good fluid characteristics, and the hole sealing material can be filled in a drilling rock mass and a fracture field through a certain pressure effect in the grouting process. In addition, when the composite characteristic is ensured, after the water-retaining agent and water are added into the active gel material to be fully mixed, the active gel material can swell when meeting water and is insoluble in water, so that the gel hole sealing material has certain expansibility, the coal cracks are further ensured to be full of, the tightness is ensured, good construction operation under various conditions can be ensured, and the gel hole sealing material has universal applicability.
3. According to the gas drainage borehole gel hole sealing material provided by the application, the acrylamide and N- (4-hydroxy-3-methoxy-benzyl) -acrylamide in the active gel base material undergo free radical copolymerization reaction under the action of the active material sodium polydodecyl benzene sulfate according to the mass ratio of 1:1-3:2 to form a hydrophilic three-dimensional network polymer (polyacrylamide gel), and the produced network polymer is neither compact nor loose, has strength and brittleness not too high, and has good flexibility and ductility. Wherein, the active material of the sodium polydodecyl benzene sulfate can form an adsorption layer on the surfaces of acrylamide and N- (4-hydroxy-3-methoxy-benzyl) -acrylamide monomers, so that the charges on the surfaces of the two monomers are increased to form reaction force among particles with three-dimensional obstruction, thereby having good dispersing effect, preventing the two monomers from agglomerating, better enabling the two monomers to have polymerization reaction under the high temperature condition, and enabling the carbon-carbon double bond to be broken and added to form a catalyst with (-CH) 2 -CH-) n Three-dimensional network of groups (gel). In addition, when the consumption of the acrylamide is large, a large amount of acrylamide homopolymer exists in the obtained product, so that the product becomes hard and brittle after water absorption, the deformability is poor, and the flexibility of the gel hole sealing material is poor; similarly, when N- (4-hydroxy-3-methoxy-benzyl) -acrylamide is excessive, the excessive N- (4-hydroxy-3-methoxy-benzyl) -acrylamide monomer is more prone to agglomeration, the hydrogel brittleness is enhanced after water absorption, so that the deformability of the gel hole sealing material is weakened, the flexibility and the ductility of the gel hole sealing material are further reduced, the gel hole sealing material cannot deform along with deformation of a rock body, and the requirements of crack filling, sealing performance and long-term construction operation cannot be met. Compared with the traditional cement, the application ensures the tightness and the tightness is not damaged by the influence of stress at the same timeThe gel hole sealing material has good flexibility and ductility when the rock mass is deformed by the ground stress, can deform along with the deformation of the rock mass, fills cracks, and meets the requirements of tightness and long-term construction operation.
4. The gas drainage borehole gel hole sealing material provided by the application can well fill the borehole, and can fill the borehole gap by properly pressurizing in a reasonable range and the material has fluidity under the action of pressure, so as to meet the requirement of tightness; the gel hole sealing material has good flexibility and ductility, deforms along with the deformation of the drilling hole, does not break along with the deformation of the drilling hole, and still has good sealing performance in the long-term gas drainage process. In addition, the preparation process of the gas drainage borehole gel hole sealing material provided by the application is simple and is convenient to produce and operate.
In addition to the objects, features and advantages described above, the present application has other objects, features and advantages. The present application will be described in further detail with reference to the drawings
Drawings
The accompanying drawings, which are included to provide a further understanding of the application and are incorporated in and constitute a part of this specification, illustrate embodiments of the application and together with the description serve to explain the application. In the drawings:
fig. 1 is a preparation flow chart of a gas drainage borehole gel hole sealing material provided by the application.
Detailed Description
The present application will be further described with reference to the drawings for the purpose of enhancing the understanding of the present application, and the examples are only for the purpose of illustrating the present application and are not to be construed as limiting the scope of the present application.
The application provides a gas drainage borehole gel hole sealing material, which is a composite material, and is prepared by preparing an active gel base material from a plurality of additives serving as auxiliary materials, uniformly mixing the active gel base material with fly ash basic aggregate to obtain an active gel material, adding water and a water retaining agent, and stirring at a high speed to obtain a target material.
Specifically, the gel hole sealing material comprises an active gel base material, fly ash, water and a water retaining agent; the fly ash is basic aggregate, and the active gel base material and the fly ash form an active gel material; the active gel base material is three-dimensional network-shaped polyacrylamide gel prepared by the reaction of acrylamide, N- (4-hydroxy-3-methoxy-benzyl) -acrylamide and an active material, and the active material is sodium polydodecyl benzene sulfate.
The gel hole sealing material comprises the following components in parts by mass: 20-30 parts of fly ash, 60-90 parts of water and 1 part of water-retaining agent; the active gel base material is prepared by reacting 1-2 parts of acrylamide, 1-2 parts of N- (4-hydroxy-3-methoxy-benzyl) -acrylamide, 1-2 parts of sodium dodecyl benzene sulfate and 2-4 parts of sodium dodecyl benzene sulfate.
Preferably, the mass ratio of the fly ash to the water is 1:3; the mass ratio of the acrylamide to the N- (4-hydroxy-3-methoxy-benzyl) -acrylamide in the active gel substrate is 1:1-3:2. The water-retaining agent is carboxymethyl cellulose.
The application is explained and illustrated below in connection with specific embodiments.
Example 1
As shown in fig. 1, the preparation method of the gas drainage borehole gel hole sealing material comprises the following specific implementation steps:
(1) preparing an active gel base material: firstly, carrying out ultraviolet disinfection treatment on 3g of active material (sodium polydodecyl benzene sulfate) for about 30min, pouring 2g of acrylamide, 2g of N- (4-hydroxy-3-methoxy-benzyl) -acrylamide and the treated active material into a beaker according to mass proportion, heating to 90 ℃, stirring, cooling to room temperature and preserving for later use;
(2) preparing an active gel material: adding 25g of fly ash and the prepared active gel base material into a container at normal temperature, and stirring and mixing to obtain an active gel material;
(3) preparing a gel hole sealing material: adding the prepared active gel material, 75g of water and 1g of water-retaining agent (carboxymethyl cellulose) into a container, uniformly stirring the mixture at normal temperature, stirring the mixture for 5min at a speed of 10r/s by adopting a constant-temperature magnetic stirrer, and placing the mixture in normal temperature to obtain the gel hole sealing material after stirring.
And (3) test verification:
performing experiments on the gel hole sealing material prepared in the embodiment 1 in two sections in an experiment area of a coal mine, and measuring and calculating the accumulated amount and the extraction ratio of gas extraction before and after improvement after a certain period of time, wherein the accumulated amount is the content of the extracted gas in unit time; the extraction ratio is the cumulative amount of gas extraction in unit time, and the cumulative amount is higher than the content of all the gas in the corresponding section. The experimental measurement results are shown in table 1:
TABLE 1
From the above experiments, it can be seen from table 1 that, in each unit time, the extraction ratio of the first section is improved by about 40% compared with the extraction ratio before the improvement, and the extraction effect of the second section is improved by 30%. Such as: the total amount of gas contained in the first section and the second section is 20864m respectively 3 、20366m 3 The first section cumulative amount at 30 (d) was from the original 7425m 3 Lifting to 15049m 3 The second section accumulated amount is 5704m from the original 3 Lifting to 11676m 3 In the same time, the accumulation amount is improved, and the extraction ratio is also improved under the condition that the total gas amount is unchanged, so that the gas extraction efficiency is improved. Therefore, when the open drill hole sealed and pumped by the original hole sealing method can not work any more, the improved measure effect is better. This is because, firstly, acrylamide and N- (4-hydroxy-3-methoxy-benzyl) -acrylamide are mixed according to a proper proportion and undergo a free radical copolymerization reaction under the action of active material sodium polydodecyl benzene sulfate to form a hydrophilic three-dimensional network polymer (polyacrylamide gel), and the produced network polymer is neither compact nor loose, has strength and brittleness not too high, and has good flexibility and ductility. Meanwhile, by adding water-retaining agent carboxymethyl cellulose, because carboxymethyl cellulose is a fiber derivative, the carboxymethyl cellulose is molecularThe structure contains a large number of hydrophilic groups: after water is added, the active gel hole sealing material can be combined with a non-hydrated dispersion medium (water), free moisture is prevented from escaping, the moisture is preserved as much as possible, the water retention of the gel hole sealing material is improved, the active gel hole sealing material has good fluid characteristics, a drilling rock mass and a fracture field can be ensured to be filled with the gel hole sealing material through a certain pressure effect in the grouting process, the gel material is easy to swell when meeting water and has a certain expansibility, the hole sealing material is further ensured to be filled with coal cracks, the sealing performance is ensured, and the gap can be effectively plugged. In addition, the gel hole sealing material takes the fly ash as basic aggregate, and the active gel material is formed by organically combining the fly ash and the active gel base material, so that the obtained target material has gel characteristics, and meanwhile, the fly ash can improve the toughness of the gel hole sealing material after being solidified by water, the quality after hole sealing is improved, the cost of the material and the hole sealing speed can be ensured, the hole sealing is efficient and quick, the operation is simple and convenient, the production cost can be reduced under the condition of not adding a cross-linking agent, the pollution to the environment can be reduced to the greatest extent, the cost is low, and the gel hole sealing material is nontoxic. In addition, when the composite characteristic is ensured, after the water-retaining agent and water are added into the active gel material to be fully mixed, the active gel material can swell when meeting water and is insoluble in water, so that the gel hole sealing material has certain expansibility, the coal cracks are further ensured to be full of, the tightness is ensured, good construction operation under various conditions can be ensured, and the gel hole sealing material has universal applicability.
Example 2
A preparation method of a gas drainage borehole gel hole sealing material comprises the following specific implementation steps:
firstly, carrying out ultraviolet disinfection treatment on 4g of active material (sodium polydodecyl benzene sulfate) for about 30min, pouring 2g of acrylamide, 2g of N- (4-hydroxy-3-methoxy-benzyl) -acrylamide and the treated active material into a beaker according to mass proportion, heating to 90 ℃, stirring, cooling to room temperature and preserving for later use;
adding 30g of fly ash and the prepared active gel base material into a container at normal temperature, and stirring and mixing to obtain an active gel material;
adding the prepared active gel material, 90g of water and 1g of water-retaining agent (carboxymethyl cellulose) into a container, uniformly stirring the mixture at normal temperature, stirring the mixture for 5min at a speed of 10r/s by adopting a constant-temperature magnetic stirrer, and placing the mixture in normal temperature to obtain the gel hole sealing material after stirring.
And (3) test verification:
the gel hole sealing material prepared in the example 2 is subjected to experiments in two sections in an experimental area of a coal mine, and after a certain period of time, the accumulated amount and the extraction ratio of gas extraction before and after improvement are measured and calculated, and experimental measurement results are shown in table 2:
TABLE 2
Example 3
A preparation method of a gas drainage borehole gel hole sealing material comprises the following specific implementation steps:
firstly, carrying out ultraviolet disinfection treatment on 2g of active material (sodium polydodecyl benzene sulfate) for about 30min, pouring 1g of acrylamide, 1.5g of N- (4-hydroxy-3-methoxy-benzyl) -acrylamide and the treated active material into a beaker according to mass proportion, heating to 90 ℃, stirring, cooling to room temperature and preserving for later use;
adding 20g of fly ash and the prepared active gel base material into a container at normal temperature, and stirring and mixing to obtain an active gel material;
adding the prepared active gel material, 60g of water and 1g of water-retaining agent (carboxymethyl cellulose) into a specific container, stirring uniformly at normal temperature, stirring the mixed solution for 3min at a speed of 10r/s by adopting a constant-temperature magnetic stirrer, and placing the mixture into normal temperature to obtain the gel hole sealing material after stirring.
The gel hole sealing material prepared in the embodiment 3 is subjected to experiments in two sections in an experimental area of a coal mine, and after a certain period of time, the accumulated amount and the extraction ratio of gas extraction before and after improvement are measured and calculated, and the specific result is similar to that of the embodiment 2. After the gel hole sealing material provided by the application is used for hole sealing improvement, the gel hole sealing material is obviously improved compared with the gel hole sealing material before improvement. The gel hole sealing material plays an important role in improving the tightness of the pre-extraction drilling hole and improving the gas extraction effectiveness.
Comparative example 1 (without active Material)
A preparation method of a gas drainage borehole gel hole sealing material comprises the following specific implementation steps:
pouring 2g of acrylamide and 2g of N- (4-hydroxy-3-methoxy-benzyl) -acrylamide into a beaker according to mass proportion, heating to 90 ℃, stirring, cooling to room temperature and preserving for later use; adding 25g of fly ash and the prepared active gel base material into a container at normal temperature, and stirring and mixing to obtain an active gel material; adding the prepared active gel material, 75g of water and 1g of water-retaining agent (carboxymethyl cellulose) into a container, uniformly stirring the mixture at normal temperature, stirring the mixture for 5min at a speed of 10r/s by adopting a constant-temperature magnetic stirrer, and placing the mixture in normal temperature to obtain the gel hole sealing material after stirring.
Comparative example 2 (active material excess)
A preparation method of a gas drainage borehole gel hole sealing material comprises the following specific implementation steps:
firstly, 10g of active material (sodium polydodecyl benzene sulfate) is subjected to ultraviolet disinfection treatment for about 30min, 2g of acrylamide, 2g of N- (4-hydroxy-3-methoxy-benzyl) -acrylamide and the treated active material are poured into a beaker according to mass proportion, heated to 90 ℃, stirred, cooled to room temperature and stored for standby; adding 25g of fly ash and the prepared active gel base material into a container at normal temperature, and stirring and mixing to obtain an active gel material; adding the prepared active gel material, 75g of water and 1g of water-retaining agent (carboxymethyl cellulose) into a container, uniformly stirring the mixture at normal temperature, stirring the mixture for 5min at a speed of 10r/s by adopting a constant-temperature magnetic stirrer, and placing the mixture in normal temperature to obtain the gel hole sealing material after stirring.
And (3) test verification:
the gel hole sealing materials prepared in comparative examples 1 and 2 were subjected to experiments in two sections of the coal mine experimental area, and after a certain period of time, the cumulative amount and the extraction ratio of gas extraction before and after improvement were measured and calculated, and the experimental measurement results are shown in table 3. Wherein the first and second sections in Table 3 are the same as those of example 1 in terms of the cumulative amount and extraction ratio of extraction after modification of the gel plugging material prepared in comparative examples 1 and 2, and are omitted from the table.
TABLE 3 Table 3
As can be seen from tables 1 and 3, in the case where the addition amount of other substances was kept unchanged, the gas extraction in the first zone was increased by only 16% as compared with that before improvement in table 1, and the gas extraction in the second zone was increased by only 10% as compared with that before improvement in table 1, when the active material (sodium polydodecyl benzene sulfate) was not added; when the active material is excessive, the gas extraction in the first zone is increased by only 14% compared to that before improvement in table 1, and the gas extraction in the second zone is increased by only 8% compared to that before improvement in table 1. The active material sodium polydodecyl benzene sulfate can form an adsorption layer on the surfaces of acrylamide and N- (4-hydroxy-3-methoxy-benzyl) -acrylamide monomers, so that the charges on the surfaces of the two monomers are increased to form reaction force among particles with three-dimensional obstruction, a good dispersing effect is achieved, the two monomers are prevented from agglomerating, the two monomers are better polymerized under the high temperature condition, and the carbon-carbon double bond is broken and added to form a catalyst with (-CH) 2 -CH-) n Three-dimensional network of groups (gel). However, acrylamide and N- (4-hydroxy-3-methoxy-benzyl) -acrylamide cannot be sufficiently dispersed without adding the active material sodium polydodecylbenzene sulfateThe monomer is agglomerated, polyacrylamide gel cannot be formed by full polymerization, only a small amount of polyacrylamide gel is formed, and cracks of coal and rock cannot be fully plugged, so that the gas extraction ratio is not obviously improved. When an excessive amount of active material is added, sodium polydodecyl benzene sulfate which is an active material ionizes Na + Ions will remain in solution, excessive Na + Ions can compress the double electric layer, so that the absolute value of the Zeta potential is reduced, the stabilizing effect generated by electrostatic repulsion is reduced, the stability of gel is possibly agglomerated, gel cannot be fully polymerized, the swelling rate of the gel material is reduced due to the addition of excessive active materials, the gel material cannot be ensured to be filled in coal cracks, the tightness of the gel material cannot be ensured, and the gas extraction ratio is improved to be lower.
Comparative example 3 (acrylamide excess)
A preparation method of a gas drainage borehole gel hole sealing material comprises the following specific implementation steps:
firstly, carrying out ultraviolet disinfection treatment on 2g of active material (sodium polydodecyl benzene sulfate) for about 30min, pouring 4g of acrylamide, 2g of N- (4-hydroxy-3-methoxy-benzyl) -acrylamide and the treated active material into a beaker according to mass proportion, heating to 90 ℃, stirring, cooling to room temperature and preserving for later use; adding 25g of fly ash and the prepared active gel base material into a container at normal temperature, and stirring and mixing to obtain an active gel material; adding the prepared active gel material, 75g of water and 1g of water-retaining agent (carboxymethyl cellulose) into a container, uniformly stirring the mixture at normal temperature, stirring the mixture for 5min at a speed of 10r/s by adopting a constant-temperature magnetic stirrer, and placing the mixture in normal temperature to obtain the gel hole sealing material after stirring.
Comparative example 4 (N- (4-hydroxy-3-methoxy-benzyl) -acrylamide excess)
A preparation method of a gas drainage borehole gel hole sealing material comprises the following specific implementation steps:
firstly, carrying out ultraviolet disinfection treatment on 2g of active material (sodium polydodecyl benzene sulfate) for about 30min, pouring 2g of acrylamide, 4g of N- (4-hydroxy-3-methoxy-benzyl) -acrylamide and the treated active material into a beaker according to mass proportion, heating to 90 ℃, stirring, cooling to room temperature and preserving for later use; adding 25g of fly ash and the prepared active gel base material into a container at normal temperature, and stirring and mixing to obtain an active gel material; adding the prepared active gel material, 75g of water and 1g of water-retaining agent (carboxymethyl cellulose) into a container, uniformly stirring the mixture at normal temperature, stirring the mixture for 5min at a speed of 10r/s by adopting a constant-temperature magnetic stirrer, and placing the mixture in normal temperature to obtain the gel hole sealing material after stirring.
And (3) test verification:
the gel hole sealing materials prepared in comparative example 3 and comparative example 4 were subjected to experiments in two sections in the experimental area of coal mine, and after a certain period of time, the cumulative amount and the extraction ratio of gas extraction before and after improvement were measured and calculated, and the experimental measurement results are shown in table 4. Wherein the first and second sections in Table 4 are the same as those of example 1 in terms of the cumulative amount and extraction ratio of extraction after modification of the gel plugging materials prepared in comparative examples 3 and 4, and are omitted from the tables.
TABLE 4 Table 4
As can be seen from tables 1 and 4, when an excessive amount of acrylamide, that is, acrylamide and N- (4-hydroxy-3-methoxy-benzyl) -acrylamide were added at a mixing mass ratio of 2: in the case of 1, the gas extraction in the first zone was increased by only 22% as compared with that before improvement in Table 1, and the gas extraction in the second zone was increased by only 11% as compared with that before improvement in Table 1. When an excess of N- (4-hydroxy-3-methoxy-benzyl) -acrylamide, i.e. acrylamide and N- (4-hydroxy-3-methoxy-benzyl) -acrylamide were added, the mixing mass ratio was 1: in the case of 2, the gas extraction in the first zone was increased by 15% as compared with that before improvement in Table 1, and the gas extraction in the second zone was increased by 9% as compared with that before improvement in Table 1. This is because when the amount of acrylamide is large, a large amount of acrylamide homopolymer exists in the obtained product, so that the product becomes hard and brittle after water absorption, the deformability is poor, and the flexibility of the gel hole sealing material is poor, so that the gas extraction ratio is low; similarly, when N- (4-hydroxy-3-methoxy-benzyl) -acrylamide is excessive, the excessive N- (4-hydroxy-3-methoxy-benzyl) -acrylamide monomer is more prone to agglomeration, the hydrogel brittleness is enhanced after water absorption, so that the deformability of the gel hole sealing material is weakened, the flexibility and the ductility of the gel hole sealing material are further reduced, the gel hole sealing material cannot deform along with deformation of a rock body, and the requirements of crack filling, sealing performance and long-term construction operation cannot be met. Only acrylamide and N- (4-hydroxy-3-methoxy-benzyl) -acrylamide in the active gel substrate can form hydrophilic three-dimensional network polymer (gel) under chemical action force according to the mass ratio of 1:1-3:2, the network polymer is neither compact nor loose, the strength and brittleness are not too high, and the network polymer has good flexibility and ductility, so that the gas extraction ratio is improved to a lower extent.
Comparative example 5
The cement mortar hole sealing material is used, and the mass ratio of cement to water is 1:2 and water are fully and uniformly mixed, then are subjected to experiments in two sections in an experimental area of a coal mine, after a certain period of time, the accumulated amount and the extraction ratio of gas extraction before and after improvement are measured and calculated, and experimental measurement results are shown in table 5. Wherein the first section and the second section in Table 5 are the cumulative amount of extraction and the extraction ratio after modification with the cement mortar sealing material of comparative example 5, and the cumulative amount of extraction and the extraction ratio after modification of the first section and the second section are the same as in example 1, and are omitted from the table.
TABLE 5
As can be seen from the comparison of tables 1 and 5, when the cement mortar sealing materials were used, the gas extraction ratios of the first section and the second section of 10 (d) were only 21% and 16%, and compared with the gel sealing materials in Table 1 of example, the gas extraction ratios were reduced by 43% and 29.3%, and the gas extraction ratios of the gel sealing materials were not higher for the other extraction times. The cement mortar hole sealing material is lack of expansibility compared with the gel active material, so that the cement mortar hole sealing material cannot be expanded when the sealing effect is carried out on the coal-rock cracks, and the cracks cannot be sealed in time; the cement mortar hole sealing material lacks flexibility and ductility, cannot deform along with rock mass deformation, and cannot fill cracks; the toughness of the cement mortar hole sealing material is insufficient, the cement mortar hole sealing material can crack when being influenced by external stress, the sealing property of the extraction drilling hole is destroyed, and finally the gas extraction effect is not ideal. Compared with the traditional cement, the gel hole sealing material provided by the application can ensure that the tightness is not influenced by stress and the tightness is damaged at the same time; the rock mass is deformed under the ground stress, and meanwhile, the rock mass has good flexibility and ductility, can deform along with the deformation of the rock mass, fills cracks, and meets the requirements of tightness and long-term construction operation.
In summary, according to the gas drainage borehole gel hole sealing material provided by the application, under the condition that a cross-linking agent is not added, acrylamide and monomer N- (4-hydroxy-3-methoxy-benzyl) -acrylamide containing a capsaicin functional group structure undergo a free radical copolymerization reaction, so that three-dimensional network-shaped polyacrylamide gel can be synthesized, and a proper amount of active material (sodium polydodecyl benzene sulfate) is added to promote the combination of the two to prepare an active gel base material; meanwhile, the water-retaining agent carboxymethyl cellulose is added, and because the carboxymethyl cellulose is a fiber derivative, the molecular structure of the carboxymethyl cellulose contains a large number of hydrophilic groups: after water is added, the active gel hole sealing material can be combined with a non-hydrated dispersion medium (water), free moisture is prevented from escaping, the moisture is preserved as much as possible, the water retention of the gel hole sealing material is improved, the active gel hole sealing material has good fluid characteristics, and the hole sealing material can be filled in a drilling rock mass and a fracture field through a certain pressure effect in the grouting process. In addition, the fly ash is used as basic aggregate, and the active gel material is formed by organically combining the fly ash and the active gel base material, so that the obtained target material has gel characteristics, and meanwhile, the fly ash can improve the toughness of the gel hole sealing material after being solidified by water, so that the quality after hole sealing is improved, the cost of the material and the speed of hole sealing can be ensured, the hole sealing is efficient and quick, the operation is simple and convenient, the production cost can be reduced under the condition of not adding a cross-linking agent, the pollution to the environment can be reduced to the greatest extent, the cost is low, and the method is nontoxic. In addition, when the composite characteristic is ensured, after the water-retaining agent and water are added into the active gel material to be fully mixed, the active gel material can swell when meeting water and is insoluble in water, so that the gel hole sealing material has certain expansibility, the coal cracks are further ensured to be full of, the tightness is ensured, good construction operation under various conditions can be ensured, and the gel hole sealing material has universal applicability.
According to the gas drainage borehole gel hole sealing material, through the mutual synergistic effect of the components, fluid with certain viscosity can be formed to permeate into coal cracks, and the gas drainage borehole gel hole sealing material can be well filled to achieve the sealing effect; the gel hole sealing material has certain flexibility and ductility, and the material deforms along with the change of stress in the long-term construction process, so that long-term and efficient tightness is realized; the gel hole sealing material has the excellent properties of environmental protection, no pollution, no toxicity and low price.
The above description is only of the preferred embodiments of the present application and is not intended to limit the present application, but various modifications and variations can be made to the present application by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application should be included in the protection scope of the present application.

Claims (8)

1. The gel hole sealing material for the gas drainage drill hole is characterized by being a composite material and comprising an active gel base material, fly ash, water and a water retaining agent;
the fly ash is basic aggregate, and the active gel base material and the fly ash form an active gel material;
the active gel base material is three-dimensional network-shaped polyacrylamide gel prepared by the reaction of acrylamide, N- (4-hydroxy-3-methoxy-benzyl) -acrylamide and an active material, and the active material is sodium polydodecyl benzene sulfate;
the gel hole sealing material comprises the following components in parts by mass: 20-30 parts of fly ash, 60-90 parts of water and 1 part of water-retaining agent;
the active gel base material is prepared by reacting 1-2 parts of acrylamide, 1-2 parts of N- (4-hydroxy-3-methoxy-benzyl) -acrylamide and 2-4 parts of sodium polydodecyl benzene sulfate.
2. The gas drainage borehole gel plugging material according to claim 1, wherein the mass ratio of the fly ash to the water is 1:3.
3. The gas drainage borehole gel hole sealing material according to claim 1, wherein the mass ratio of the acrylamide to the N- (4-hydroxy-3-methoxy-benzyl) -acrylamide in the active gel base material is 1:1-3:2.
4. The gas drainage borehole gel plugging material according to claim 1, wherein the water retaining agent is carboxymethyl cellulose.
5. The method for preparing the gas drainage borehole gel hole sealing material according to any one of claims 1 to 4, which is characterized by comprising the following steps: firstly, preparing an active gel base material by polymerization reaction of acrylamide, N- (4-hydroxy-3-methoxy-benzyl) -acrylamide and active material sodium polydodecyl benzene sulfate, then uniformly mixing the active gel base material with basic aggregate fly ash to obtain an active gel material, and finally adding water and a water-retaining agent, and stirring at a high speed to obtain the gel hole sealing material.
6. The method for preparing the gas drainage borehole gel hole sealing material according to claim 5, which is characterized by comprising the following steps:
step 1) preparation of an active gel substrate: firstly, sterilizing active material sodium polydodecyl benzene sulfate, then pouring acrylamide, N- (4-hydroxy-3-methoxy-benzyl) -acrylamide and the treated active material into a beaker according to mass proportion, heating to 90 ℃ and stirring, polymerizing to obtain three-dimensional network-shaped polyacrylamide gel, cooling to room temperature and preserving for later use;
step 2) preparing an active gel material: adding the fly ash and the active gel base material into a container according to the mass fraction ratio under the normal temperature condition, and stirring and mixing to obtain an active gel material;
step 3) preparing a gel hole sealing material: and adding the active gel material, water and the water-retaining agent into a container according to the mass portion ratio, and uniformly stirring the mixed solution at normal temperature to obtain the gel hole sealing material.
7. The method for preparing a gas drainage borehole gel sealing material according to claim 6, wherein in step 1), an active material, namely sodium polydodecyl benzene sulfate, is subjected to a disinfection treatment, specifically: and performing ultraviolet disinfection treatment on the sodium polydodecyl benzene sulfate for 20-40 min.
8. The method for preparing the gas drainage borehole gel sealing material according to claim 6, wherein the step 3) is to stir the mixed solution uniformly, specifically: and stirring the mixed solution by adopting a constant-temperature magnetic stirrer at a speed of 10r/s for 3-5 min.
CN202210749361.0A 2022-06-28 2022-06-28 Gas drainage borehole gel hole sealing material and preparation method thereof Active CN115124978B (en)

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