[go: up one dir, main page]

CN114854097B - Mining environment-friendly degradable gel drilling sealing material and preparation method thereof - Google Patents

Mining environment-friendly degradable gel drilling sealing material and preparation method thereof Download PDF

Info

Publication number
CN114854097B
CN114854097B CN202210426678.0A CN202210426678A CN114854097B CN 114854097 B CN114854097 B CN 114854097B CN 202210426678 A CN202210426678 A CN 202210426678A CN 114854097 B CN114854097 B CN 114854097B
Authority
CN
China
Prior art keywords
cellulose ether
sealing material
water
drilling sealing
gel
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN202210426678.0A
Other languages
Chinese (zh)
Other versions
CN114854097A (en
Inventor
郝晋伟
舒龙勇
杨伟东
霍中刚
李阳
凡永鹏
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
CCTEG China Coal Research Institute
Original Assignee
CCTEG China Coal Research Institute
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by CCTEG China Coal Research Institute filed Critical CCTEG China Coal Research Institute
Priority to CN202210426678.0A priority Critical patent/CN114854097B/en
Publication of CN114854097A publication Critical patent/CN114854097A/en
Application granted granted Critical
Publication of CN114854097B publication Critical patent/CN114854097B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L1/00Compositions of cellulose, modified cellulose or cellulose derivatives
    • C08L1/08Cellulose derivatives
    • C08L1/26Cellulose ethers
    • C08L1/28Alkyl ethers
    • C08L1/284Alkyl ethers with hydroxylated hydrocarbon radicals
    • CCHEMISTRY; METALLURGY
    • C12BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12NMICROORGANISMS OR ENZYMES; COMPOSITIONS THEREOF; PROPAGATING, PRESERVING, OR MAINTAINING MICROORGANISMS; MUTATION OR GENETIC ENGINEERING; CULTURE MEDIA
    • C12N9/00Enzymes; Proenzymes; Compositions thereof; Processes for preparing, activating, inhibiting, separating or purifying enzymes
    • C12N9/14Hydrolases (3)
    • C12N9/24Hydrolases (3) acting on glycosyl compounds (3.2)
    • C12N9/2402Hydrolases (3) acting on glycosyl compounds (3.2) hydrolysing O- and S- glycosyl compounds (3.2.1)
    • C12N9/2405Glucanases
    • C12N9/2408Glucanases acting on alpha -1,4-glucosidic bonds
    • C12N9/2411Amylases
    • C12N9/2414Alpha-amylase (3.2.1.1.)
    • CCHEMISTRY; METALLURGY
    • C12BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12NMICROORGANISMS OR ENZYMES; COMPOSITIONS THEREOF; PROPAGATING, PRESERVING, OR MAINTAINING MICROORGANISMS; MUTATION OR GENETIC ENGINEERING; CULTURE MEDIA
    • C12N9/00Enzymes; Proenzymes; Compositions thereof; Processes for preparing, activating, inhibiting, separating or purifying enzymes
    • C12N9/14Hydrolases (3)
    • C12N9/24Hydrolases (3) acting on glycosyl compounds (3.2)
    • C12N9/2402Hydrolases (3) acting on glycosyl compounds (3.2) hydrolysing O- and S- glycosyl compounds (3.2.1)
    • C12N9/2405Glucanases
    • C12N9/2434Glucanases acting on beta-1,4-glucosidic bonds
    • C12N9/2445Beta-glucosidase (3.2.1.21)
    • CCHEMISTRY; METALLURGY
    • C12BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12NMICROORGANISMS OR ENZYMES; COMPOSITIONS THEREOF; PROPAGATING, PRESERVING, OR MAINTAINING MICROORGANISMS; MUTATION OR GENETIC ENGINEERING; CULTURE MEDIA
    • C12N9/00Enzymes; Proenzymes; Compositions thereof; Processes for preparing, activating, inhibiting, separating or purifying enzymes
    • C12N9/14Hydrolases (3)
    • C12N9/24Hydrolases (3) acting on glycosyl compounds (3.2)
    • C12N9/2402Hydrolases (3) acting on glycosyl compounds (3.2) hydrolysing O- and S- glycosyl compounds (3.2.1)
    • C12N9/2405Glucanases
    • C12N9/2434Glucanases acting on beta-1,4-glucosidic bonds
    • C12N9/2448Licheninase (3.2.1.73)
    • CCHEMISTRY; METALLURGY
    • C12BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12NMICROORGANISMS OR ENZYMES; COMPOSITIONS THEREOF; PROPAGATING, PRESERVING, OR MAINTAINING MICROORGANISMS; MUTATION OR GENETIC ENGINEERING; CULTURE MEDIA
    • C12N9/00Enzymes; Proenzymes; Compositions thereof; Processes for preparing, activating, inhibiting, separating or purifying enzymes
    • C12N9/14Hydrolases (3)
    • C12N9/24Hydrolases (3) acting on glycosyl compounds (3.2)
    • C12N9/2402Hydrolases (3) acting on glycosyl compounds (3.2) hydrolysing O- and S- glycosyl compounds (3.2.1)
    • C12N9/2477Hemicellulases not provided in a preceding group
    • C12N9/248Xylanases
    • CCHEMISTRY; METALLURGY
    • C12BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12YENZYMES
    • C12Y302/00Hydrolases acting on glycosyl compounds, i.e. glycosylases (3.2)
    • C12Y302/01Glycosidases, i.e. enzymes hydrolysing O- and S-glycosyl compounds (3.2.1)
    • C12Y302/01001Alpha-amylase (3.2.1.1)
    • CCHEMISTRY; METALLURGY
    • C12BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12YENZYMES
    • C12Y302/00Hydrolases acting on glycosyl compounds, i.e. glycosylases (3.2)
    • C12Y302/01Glycosidases, i.e. enzymes hydrolysing O- and S-glycosyl compounds (3.2.1)
    • C12Y302/01021Beta-glucosidase (3.2.1.21)
    • CCHEMISTRY; METALLURGY
    • C12BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12YENZYMES
    • C12Y302/00Hydrolases acting on glycosyl compounds, i.e. glycosylases (3.2)
    • C12Y302/01Glycosidases, i.e. enzymes hydrolysing O- and S-glycosyl compounds (3.2.1)
    • C12Y302/01073Licheninase (3.2.1.73)
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/06Biodegradable

Landscapes

  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Zoology (AREA)
  • Wood Science & Technology (AREA)
  • Genetics & Genomics (AREA)
  • Bioinformatics & Cheminformatics (AREA)
  • Engineering & Computer Science (AREA)
  • Biochemistry (AREA)
  • General Engineering & Computer Science (AREA)
  • General Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Molecular Biology (AREA)
  • Biomedical Technology (AREA)
  • Biotechnology (AREA)
  • Microbiology (AREA)
  • Polymers & Plastics (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The invention relates to a mining environment-friendly degradable gel drilling sealing material and a preparation method thereof, wherein the mining environment-friendly degradable gel drilling sealing material comprises water, modified cellulose ether and an additive in mass ratio: 100 (2-3): (0.5 to 0.6); the modified cellulose ether is glyoxal surface-treated nonionic cellulose ether, the additive comprises a suspending agent, the suspending agent is prepared by granulating 40% -80% of ethanol solution and cellulose ether, and the particle size is 40-100 meshes. The mining environment-friendly degradable gel drilling sealing material has the following beneficial effects: the embodiment of the invention eliminates the sedimentation and water separation of the slurry of the existing environment-friendly phase-change gel drilling sealing material along with time, and ensures the uniformity and stability of the gel material.

Description

Mining environment-friendly degradable gel drilling sealing material and preparation method thereof
Technical Field
The invention belongs to the technical field of drilling sealing, and particularly relates to a mining environment-friendly degradable gel drilling sealing material and a preparation method thereof.
Background
The borehole sealing is a core foundation for underground coal mine borehole gas extraction, and directly determines the concentration, cost, efficiency and utilization rate of the extracted gas. The sealing parameters, the sealing materials and the matched equipment are three elements of the drilling sealing, wherein the sealing materials are the most important material guarantee for the drilling sealing quality. At present, the drilling sealing materials widely used in coal mine underground in China mainly comprise two types: cement-based inorganic and chemically reactive urethanes, and both belong to reactive immobilized non-degradable materials. Along with the increase of the mining depth of the coal mine, the problems of high stress, coal construction and low permeability are increased, the problem of dynamic deformation and instability of surrounding rock of a drilled hole is serious, reactants of the conventional drilling sealing material are difficult to adaptively deform the drilled hole and cause difficult recovery of extraction equipment, so that the concentration of gas extracted from the drilled hole is generally low, the utilization cost and the utilization difficulty are increased, the problem of high maintenance of the drilling sealing cost and the like are increasingly remarkable, and the realization of the aims of efficient development and utilization of coal and coal layers in coal mining areas and cost reduction and synergy of coal mine enterprises is seriously restricted.
The publication No. CN111116998A discloses a mining environment-friendly phase-change gel drilling sealing material, and provides a method and a formula for sealing a drilling hole by utilizing the environment-friendly phase-change gel, wherein the material consists of water, a base material and a modifier, wherein the weight part of the water, the base material and the modifier is 100:1-4:0.2-0.5; the base material consists of 80-90 parts by weight of cellulose ether, 5-10 parts by weight of super absorbent resin, 1-10 parts by weight of glyoxal and 1-5 parts by weight of sodium pyrrolidone carboxylate; the modifier consists of 20-30 parts by weight of preservative, 30-40 parts by weight of mildew inhibitor and 30-50 parts by weight of reinforcing agent. In the formula, the composite cellulose ether is used as a base material, and the self-adaptive high-efficiency sealing of the drilling hole is realized through physical and chemical modification. However, there are some problems in the dissolution process of the powder, uniformity of gel formation, water retention and the like, and the specific problems are as follows:
(1) The phase change gel drilling sealing material belongs to a particle type water-soluble polymer material, and forms a uniform gel system after swelling reaction, but because the material is swelled by utilizing a crosslinked network structure and a large amount of water is kept, the molecular mass and the volume of the hydrogel are increased, the phenomenon of water and gel delamination is easily caused by the influence of gravity in the use process, partial water separation on the gel is caused, and finally the whole use performance is reduced;
(2) The phase-change gel drilling sealing material mainly takes cellulose ether as a main material, has strong surface activity, and is easy to generate foam in the use process, so that the field use effect and experience of the material are affected.
Disclosure of Invention
In order to solve the technical problems in the related art, the embodiment of the invention discloses a mining environment-friendly degradable gel drilling sealing material and a preparation method thereof.
The embodiment of the invention discloses a mining environment-friendly degradable gel drilling sealing material, which comprises water, modified cellulose ether and an additive in mass ratio: 100 (2-3): (0.5 to 0.6); the modified cellulose ether is glyoxal surface-treated nonionic cellulose ether (delayed dissolution), the additive comprises a suspending agent, the suspending agent is prepared by granulating 40% -80% ethanol solution and cellulose ether, and the particle size is 40-100 meshes.
The mining environment-friendly degradable gel drilling sealing material has the following beneficial effects: the embodiment of the invention eliminates the sedimentation and water separation of the slurry of the existing environment-friendly phase-change gel drilling sealing material along with time, and ensures the uniformity and stability of the gel material.
In some embodiments, the modified cellulose ether has a gel point of 25 to 30 minutes, a gelation time of 90 to 120 minutes, and a 2% viscosity of greater than 18 thousand mpa.s.
In some embodiments, the nonionic cellulose ether in the preparation of the modified cellulose ether is one or a combination of two of hydroxyethyl cellulose (HEC), hydroxypropyl methylcellulose (HPMC).
In some embodiments, the mass ratio of suspending agent to modified cellulose ether is (0.3 to 0.4): (2-3).
In some embodiments, the suspending agent is prepared by wetting cellulose ether with 40% -80% ethanol solution, forming film, drying, crushing and sieving, wherein the cellulose ether is one or more of carboxymethyl cellulose (CMC), polyanionic cellulose (HV-PAC), hydroxyethyl cellulose (HEC) and hydroxypropyl methyl cellulose (HPMC).
In some embodiments, the additives comprise suspending agents, retarders, accelerators, stabilizers, water-retaining agents, foam inhibitors and filling agents, wherein the mass ratio of each component to water is as follows: 0.3 to 0.4 percent: 0.01 to 0.02 percent, 0.01 to 0.03 percent, 0.08 to 0.1 percent, 0.03 to 0.05 percent, 0.04 to 0.06 percent, 0 to 0.1 percent,
in some embodiments, the particle size of the suspending agent is of the three types 40-60 mesh, 60-80 mesh, or 80-100 mesh. To meet the suspension performance under different gel point conditions.
In some embodiments, the retarder is a weak acid or weak acid salt. Specifically, in some embodiments, the retarder may be one or both of sodium citrate, citric acid.
In some embodiments, the accelerator is a weak base or weak base salt. Specifically, in some embodiments, the accelerator may be selected from NaHCO 3 、Na 2 CO 3 One or two of them.
In some embodiments, the water retaining agent may be selected from one or both of hydroxyethylurea powder or water soluble lanolin particles.
In some embodiments, the suds suppressor comprises a polyether modified silicone defoamer and/or suds suppressor. Preferably, the foam inhibitor is a nonionic neutral powdered foam inhibitor.
In some embodiments, the stabilizer comprises a preservative and/or a bactericide, in particular, the preservative can be one or two of calcium propionate and potassium trichloride, and the bactericide can be one or two of sodium hydroxymethyl glycinate and epsilon-polylysine hydrochloride. When the stabilizer comprises preservative and bactericide, the mass ratio of the preservative to the bactericide is (1-2): 1.
In some embodiments, the filler is a super absorbent resin.
The embodiment of the invention also provides a preparation method of the mining environment-friendly degradable gel drilling sealing material, which comprises the following steps: fully stirring and mixing the modified cellulose ether and the additive according to the proportion, then mixing the mixture with water, and stirring for 3-5 min to obtain the mining environment-friendly degradable gel drilling sealing material, namely, directly grouting, sealing and drilling.
The embodiment of the invention also provides a decomposer matched with the mining environment-friendly degradable gel drilling sealing material, wherein the decomposer comprises the following components: alpha-amylase, beta-glucosidase and xylanase; the mass ratio is as follows: (2-5): (4-10): 20-30): (50-60).
The implementation method of the decomposer is external injection, and comprises the following specific steps: and injecting the prepared decomposer into the gel system through a reserved pipe to finish gel degradation. Wherein the addition amount of the decomposer is determined according to the degradation period, the grouting amount and the like.
The embodiment of the invention overcomes the sedimentation and water separation effects of the swelling process of the phase-change gel drilling sealing material (such as the mining environment-friendly phase-change gel drilling sealing material disclosed by CN 111116998A) in the related technology by developing a novel suspending agent, so that the stability of the slurry generating process is realized; the water retention performance of the gel material is improved, the foam amount in the pulping process of the gel material is reduced, the stability, the environmental protection performance and the experience feel of the material are effectively improved, the gel drilling sealing material with better performance is formed, and the degradation period control of the gel material are realized by configuring the composite decomposer.
The embodiment of the invention has the beneficial effects that:
(1) The embodiment of the invention eliminates sedimentation and water separation of the slurry of the existing environment-friendly phase-change gel drilling sealing material along with time, and ensures uniformity and stability of gel;
(2) According to the embodiment of the invention, through the addition of the water-retaining agent and the foam inhibitor, the water retention performance of the gel is improved, the loss of water is greatly reduced, and the volume filling capacity of the gel is prolonged;
(3) According to the embodiment of the invention, by adding the foam inhibitor, the defoaming performance and the foam inhibition performance of the gel drilling sealing material slurry in the forming process are increased, and the influence of foam on the material performance and the construction experience is greatly reduced;
(4) According to the embodiment of the invention, the degradation of the gel drilling sealing material and the control of the degradation period are realized by configuring the composite decomposer;
(5) The embodiment of the invention realizes the applicability of the gel drilling sealing material to water quality of different sealing environments and the accurate control of the gel forming process;
(6) According to the embodiment of the invention, the selection range of the base material is widened, the acquisition threshold of the raw material is reduced and the aim of reducing the cost and enhancing the efficiency is fulfilled by adjusting the material-water ratio, the surface treatment degree and the suspension characteristic of the raw material.
Drawings
FIG. 1 is a gelation profile of the mining environment-friendly degradable gel borehole sealing material of example 1 of the present invention;
FIG. 2 is a degradation process curve of the mining environment-friendly degradable gel drilling sealing material of the embodiment 1 of the invention;
FIG. 3a is a viscosity test curve for the suspension of example 1 mixed with water (ratio of 3:1000);
FIG. 3b is a viscosity test curve of polyacrylamide mixed with water (feed water ratio 1:100);
fig. 4 is a graph showing the room temperature standing of the gel borehole sealing materials of example 1 and comparative example 1 according to the present invention, wherein the left side is comparative example 1 and the right side is example 1.
Detailed Description
The following detailed description of embodiments of the invention is exemplary and intended to be illustrative of the invention and not to be construed as limiting the invention.
The embodiment of the invention discloses a mining environment-friendly degradable gel drilling sealing material, which consists of water, modified cellulose ether and an additive in mass ratio: 100 (2-3): (0.5 to 0.6); the modified cellulose ether is glyoxal surface-treated nonionic cellulose ether (delayed dissolution), the additive comprises a suspending agent, the suspending agent is prepared by granulating 40% -80% ethanol solution and cellulose ether, and the particle size is 40-100 meshes.
The mining environment-friendly degradable gel drilling sealing material has the following beneficial effects: the embodiment of the invention eliminates the sedimentation and water separation of the slurry of the existing environment-friendly phase-change gel drilling sealing material along with time, and ensures the uniformity and stability of the gel material.
In some embodiments, the modified cellulose ether has a gel point of 25 to 30 minutes, a gelation time of 90 to 120 minutes, and a 2% (aqueous solution, 23 ℃) viscosity of greater than 18 ten thousand mpa.s.
In some embodiments, the nonionic cellulose ether in the preparation of the modified cellulose ether is one or a combination of two of hydroxyethyl cellulose (HEC), hydroxypropyl methylcellulose (HPMC).
In some embodiments, the mass ratio of suspending agent to modified cellulose ether is (0.3 to 0.4): (2-3).
In some embodiments, the suspending agent is prepared by wetting cellulose ether with 40% -80% ethanol solution, forming film, drying, crushing and sieving, wherein the cellulose ether is one or more of carboxymethyl cellulose (CMC), polyanionic cellulose (HV-PAC), hydroxyethyl cellulose (HEC) and hydroxypropyl methyl cellulose (HPMC).
In some embodiments, the additives comprise suspending agents, retarders, accelerators, stabilizers, water-retaining agents, foam inhibitors and filling agents, wherein the mass ratio of each component to water is as follows: 0.3 to 0.4 percent: 0.01 to 0.02 percent, 0.01 to 0.03 percent, 0.08 to 0.1 percent, 0.03 to 0.05 percent, 0.04 to 0.06 percent, 0 to 0.1 percent,
in some embodiments, the particle size of the suspending agent is of the three types 40-60 mesh, 60-80 mesh, or 80-100 mesh. To meet the suspension performance under different gel point conditions.
In some embodiments, the retarder is a weak acid or weak acid salt. Specifically, in some embodiments, the retarder may be one or both of sodium citrate, citric acid.
In some embodiments, the accelerator is a weak base or weak base salt. Specifically, in some embodiments, the accelerator may be selected from NaHCO 3 、Na 2 CO 3 One or two of them.
In some embodiments, the water retaining agent may be selected from one or both of hydroxyethylurea powder or water soluble lanolin particles.
In some embodiments, the suds suppressor comprises a polyether modified silicone defoamer and/or suds suppressor. Preferably, the foam inhibitor is a nonionic neutral powdered foam inhibitor.
Preferably, the foam inhibitor is a composite foam inhibitor, which can be directly purchased, such as W-320 type or W-321 type composite foam inhibitor of Guangzhou Hewanning New materials Co., ltd.
In some embodiments, the stabilizer comprises a preservative and/or a bactericide, in particular, the preservative can be one or two of calcium propionate and potassium trichloride, and the bactericide can be one or two of sodium hydroxymethyl glycinate and epsilon-polylysine hydrochloride. When the stabilizer comprises a preservative and a bactericide, the mass ratio of the preservative to the bactericide is (1-2): 1.
In some embodiments, the filler is a super absorbent resin, which is commercially available directly, such as DS128 super absorbent resin from Yixing Dansen technologies, inc.
The embodiment of the invention also provides a preparation method of the mining environment-friendly degradable gel drilling sealing material, which comprises the following steps: fully stirring and mixing the modified cellulose ether and the additive according to the proportion, then mixing the mixture with water, and stirring for 3-5 min to obtain the mining environment-friendly degradable gel drilling sealing material, namely, directly grouting, sealing and drilling.
The embodiment of the invention also provides a decomposer matched with the mining environment-friendly degradable gel drilling sealing material, wherein the decomposer comprises the following components: alpha-amylase, beta-glucosidase and xylanase; the mass ratio is as follows: (2-5): (4-10): 20-30): (50-60).
The implementation method of the decomposer is external injection, and comprises the following specific steps: and injecting the prepared decomposer into the gel system through a reserved pipe to finish gel degradation. Wherein the addition amount of the decomposer is determined according to the degradation period, the grouting amount and the like.
The embodiment of the invention overcomes the sedimentation and water separation effects of the swelling process of the phase-change gel drilling sealing material (such as the mining environment-friendly phase-change gel drilling sealing material disclosed by CN 111116998A) in the related technology by developing a novel suspending agent, so that the stability of the slurry generating process is realized; the water retention performance of the gel material is improved, the foam amount in the pulping process of the gel material is reduced, the stability, the environmental protection performance and the experience feel of the material are effectively improved, the gel drilling sealing material with better performance is formed, and the degradation period control of the gel material are realized by configuring the composite decomposer.
The viscosity of the preferable cellulose ether water-soluble polymer material is dynamically controlled by utilizing a physical and chemical modification principle, so that the viscosity of the preferable cellulose ether water-soluble polymer material can react in different time periods to adapt to the requirements of sealing material performances in different stages of the sealing process of low-resistance grouting, low-viscosity permeation, high-viscosity bonding, dynamic sealing and environmental-friendly degradation, and finally, the high-efficiency low-consumption environment-friendly sealing of the gas extraction drilling is realized.
Example 1
(1) Preparing a dry material: 2500 parts of modified cellulose ether, 350 parts of suspending agent and NaHCO are taken 3 20 parts of sodium citrate 30 parts, 50 parts of potassium perchlorate, 40 parts of sodium hydroxymethyl glycinate, 50 parts of hydroxyethyl urea powder and 60 parts of foam inhibitor are uniformly mixed to prepare a dry material;
(2) Mixing the dry materials and water in the step (1) according to the proportion of 1:50, and fully stirring for 3-5 min.
(3) And (3) after the dry material in the step (1) is fully dispersed in water and the initial viscosity (40-50 mPa.s) is released, grouting is started.
(4) The total grouting time is not more than 1h.
In this example, the modified cellulose ether is glyoxal surface-treated nonionic cellulose ether (HEC); the suspending agent is prepared by granulating 60% ethanol solution and cellulose ether (HEC), and the particle size is 50-60 meshes.
The environment-friendly degradable gel drilling sealing material obtained after the step (2) is fully stirred for 5min is subjected to viscosity test (23 ℃) by using an NDJ-8S digital display viscometer; example 1 an environment-friendly degradable gel drilling sealing material gelation performance curve is shown in figure 1; on the basis, weighing a decomposer (alpha-amylase: beta-glucanase: beta-glucosidase: xylanase=3:6:23:55) with the dry material proportion of the environment-friendly degradable phase-change gel drilling sealing material of 0.1:0.5; dissolving a decomposer according to the proportion of 1:2 of the water, adding the dissolved mixed solution into the formed gel system, and carrying out gel viscosity test in the degradation process by adopting the same viscosity test method; example 1 degradation performance curves of the environment-friendly degradable gel drilling sealing material are shown in fig. 2, and as can be seen from fig. 2, the degradation agent of the embodiment of the invention realizes degradation of the environment-friendly degradable gel drilling sealing material, and the degradation period can be controlled by controlling the component proportion and the addition amount of the degradation agent in the use process.
In the research and development process, the inventor aims to solve the problems of stability and the like of a material formula in a phase-change gel drilling sealing material (such as a mining environment-friendly phase-change gel drilling sealing material disclosed in CN 111116998A) in the related art. By developing a novel suspending agent, the sedimentation and water separation effects in the swelling process of the material are overcome, so that the stability of the slurry generating process is realized; the inventors tried various suspending agents in the research and development process, and unexpectedly found that the suspending agent adopted in the embodiment of the invention can be used for breaking through the quality, in order to more clearly characterize the performance of the suspending agent adopted in the embodiment of the invention, fig. 3a and 3b respectively show viscosity test curves (NDJ-8S digital display viscometer, 23 ℃) of the suspending agent mixed with water (3:1000 of material-water ratio) (fig. 3 a) and the polyacrylamide mixed with water (1:100 of material-water ratio) (fig. 3 b), and the viscosity performance of the suspending agent mixed with water is stable as can be seen by comparing fig. 3a and 3b, which is also the basis of the uniform and stable viscosity of the environment-friendly degradable gel drilling sealing material for mine in the embodiment of the invention.
Example 2
(1) Preparing a dry material: taking 2300 parts of modified cellulose ether, 350 parts of suspending agent and NaHCO 3 50 parts of citric acid 10 parts, 50 parts of preservative, 40 parts of sodium hydroxymethylglycinate, 50 parts of hydroxyethyl urea powder and 50 parts of foam inhibitor, and uniformly mixing to prepareObtaining a dry material;
(2) Mixing the dry materials and water in the step (1) according to the proportion of 1:40, and fully stirring for 3-5 min.
(3) And (3) after the dry material in the step (1) is fully dispersed in water and the initial viscosity (40-50 mPa.s) is released, grouting is started.
(4) The total grouting time is not more than 1h.
In this example, the modified cellulose ether is glyoxal surface-treated nonionic cellulose ether (HPMC); the suspending agent is prepared by granulating 50% ethanol solution and cellulose ether (HPMC), and the particle size is 50-60 meshes.
Example 3
(1) Preparing a dry material: taking 2500 parts of modified cellulose ether, 350 parts of suspending agent and Na 2 CO 3 20 parts of sodium citrate 30 parts, 50 parts of potassium perchlorate, 40 parts of epsilon-polylysine hydrochloride, 50 parts of water-soluble lanolin particles, 60 parts of foam inhibitor and 10 parts of super absorbent resin, and uniformly mixing to prepare a dry material;
(2) Mixing the dry materials and water in the step (1) according to the proportion of 1:50, and fully stirring for 3-5 min.
(3) And (3) after the dry material in the step (1) is fully dispersed in water and the initial viscosity (40-50 mPa.s) is released, grouting is started.
(4) The total grouting time is not more than 1h.
In this example, the modified cellulose ether is glyoxal surface-treated nonionic cellulose ether (HEC); the suspending agent is prepared by granulating 60% ethanol solution and cellulose ether (HEC), and the particle size is 40-60 meshes.
Example 4
(1) Preparing a dry material: taking 2300 parts of modified cellulose ether, 400 parts of suspending agent and NaHCO 3 20 parts of citric acid 40 parts, 50 parts of calcium propionate, 40 parts of hydroxymethyl sodium glycinate, 50 parts of hydroxyethyl urea powder, 50 parts of foam inhibitor and 10 parts of super absorbent resin, and uniformly mixing to prepare a dry material;
(2) Mixing the dry materials and water in the step (1) according to the proportion of 1:50, and fully stirring for 3-5 min.
(3) And (3) after the dry material in the step (1) is fully dispersed in water and the initial viscosity (40-50 mPa.s) is released, grouting is started.
(4) The total grouting time is not more than 1h.
In this example, the modified cellulose ether is glyoxal surface-treated nonionic cellulose ether (HEC); the suspending agent is prepared by granulating 80% ethanol solution and cellulose ether (HEC), and the particle size is 60-80 meshes.
Comparative example 1 (scheme of example 1 of publication No. CN 111116998A)
Water to base material to modifier=100:2:0.5, wherein the base material comprises composite cellulose ether to super absorbent resin to glyoxal to sodium pyrrolidone carboxylate=90:5:3:2, and the composite cellulose ether comprises hydroxypropyl methylcellulose to polyanionic cellulose to hydroxyethyl cellulose=80:10:20; wherein the composite preservative, the mildew inhibitor and the reinforcing agent in the modifier are respectively equal to or less than 30:40:30, wherein the composite mildew inhibitor is respectively equal to or less than 20:70:10 of potassium sorbate, calcium propionate and D-isoascorbic acid, wherein the mildew inhibitor is respectively equal to or less than 60:40 of calcium benzoate, calcium sulfate, calcium bicarbonate and calcium hydroxide, and the reinforcing agent is respectively equal to or less than 40:30:20:10. The weight ratio of the components is the weight ratio. And (3) uniformly premixing the base material and the modifier in advance, uniformly stirring with water according to the proportion, and drilling, grouting and sealing.
Comparing the embodiment 1 of the present invention with the comparative example 1, fig. 4 is a comparative graph of the gel-drilling sealing materials of the embodiment 1 and the comparative example 1, which is left standing for 1.5 hours at room temperature, and it can be seen from fig. 4 that the gel of the environmentally-friendly degradable gel-drilling sealing material of the embodiment 1 of the present invention is significantly more uniform and stable.
For purposes of this disclosure, the terms "one embodiment," "some embodiments," "example," "a particular example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, schematic representations of the above terms are not necessarily directed to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, the different embodiments or examples described in this specification and the features of the different embodiments or examples may be combined and combined by those skilled in the art without contradiction.
While embodiments of the present invention have been shown and described above, it will be understood that the above embodiments are illustrative and not to be construed as limiting the invention, and that variations, modifications, alternatives and variations may be made to the above embodiments by one of ordinary skill in the art within the scope of the invention.

Claims (3)

1. An environment-friendly degradable gel drilling sealing material for mines, which is characterized in that: the mining environment-friendly degradable gel drilling sealing material comprises water, modified cellulose ether and an additive, wherein the mass ratio is as follows: 100 (2-3): (0.5 to 0.6); the modified cellulose ether is glyoxal surface-treated nonionic cellulose ether, and the additive comprises a suspending agent, a retarder, an accelerator, a stabilizer, a water-retaining agent, a foam inhibitor and a filling agent, wherein the mass percentages of each component and water are respectively as follows: 0.3 to 0.4 percent, 0.01 to 0.02 percent, 0.01 to 0.03 percent, 0.08 to 0.1 percent, 0.03 to 0.05 percent, 0.04 to 0.06 percent and 0 to 0.1 percent;
the suspending agent is prepared by wetting cellulose ether with 40% -80% ethanol solution, then forming a film, drying, crushing and screening, wherein the cellulose ether is one or two of hydroxyethyl cellulose and hydroxypropyl methyl cellulose; the particle size of the suspending agent is 40-60 meshes, 60-80 meshes or 80-100 meshes;
the retarder is sodium citrate; the accelerator is one or two of sodium bicarbonate or sodium carbonate; the water-retaining agent is one or two of hydroxyethyl urea powder or water-soluble lanolin particles; the foam inhibitor comprises a polyether modified organic silicon defoamer and/or a foam inhibitor; the stabilizer comprises a preservative and/or a bactericide, wherein the preservative is one or two of calcium propionate and potassium trichloride, and the bactericide is one or two of sodium hydroxymethyl glycinate and epsilon-polylysine hydrochloride; the filler is super absorbent resin;
the gel point of the modified cellulose ether is 25-30 min, the gelation time is 90-120 min, and the 2% viscosity is more than 18 ten thousand mPa.s.
2. The mining environment-friendly degradable gel drilling sealing material as claimed in claim 1, wherein: the nonionic cellulose ether in the preparation of the modified cellulose ether is one or two of hydroxyethyl cellulose and hydroxypropyl methyl cellulose.
3. The method for preparing the mining environment-friendly degradable gel drilling sealing material as claimed in claim 1 or 2, which is characterized by comprising the following steps: the method comprises the following steps: and fully stirring and mixing the modified cellulose ether and the additive according to the proportion, then mixing the mixture with the water, and stirring for 3-5 min to obtain the mining environment-friendly degradable gel drilling sealing material.
CN202210426678.0A 2022-04-21 2022-04-21 Mining environment-friendly degradable gel drilling sealing material and preparation method thereof Active CN114854097B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202210426678.0A CN114854097B (en) 2022-04-21 2022-04-21 Mining environment-friendly degradable gel drilling sealing material and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202210426678.0A CN114854097B (en) 2022-04-21 2022-04-21 Mining environment-friendly degradable gel drilling sealing material and preparation method thereof

Publications (2)

Publication Number Publication Date
CN114854097A CN114854097A (en) 2022-08-05
CN114854097B true CN114854097B (en) 2023-12-22

Family

ID=82633358

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202210426678.0A Active CN114854097B (en) 2022-04-21 2022-04-21 Mining environment-friendly degradable gel drilling sealing material and preparation method thereof

Country Status (1)

Country Link
CN (1) CN114854097B (en)

Citations (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB767924A (en) * 1954-03-01 1957-02-13 Hercules Powder Co Ltd Improvements in or relating to the manufacture of carboxyalkyl cellulose ether salts
GB780628A (en) * 1954-12-30 1957-08-07 Hercules Powder Co Ltd Improvements in or relating to improved water-soluble salts of carboxyalkyl cellulose ethers and method of converting into granular form
GB1193650A (en) * 1966-11-21 1970-06-03 Courtaulds Ltd Improvements in and relating to Water-Soluble Cellulose Ether Compositions.
US5837864A (en) * 1994-12-15 1998-11-17 Akzo Nobel Nv Method for producing a suspension in water of a cellulose ether, and dry mixture suitable for use in the production of the suspension
JP2000063565A (en) * 1998-08-20 2000-02-29 Shin Etsu Chem Co Ltd Granular water-soluble cellulose ether and method for producing the same
EP1469031A2 (en) * 2003-04-18 2004-10-20 Shin-Etsu Chemical Co., Ltd. Granulation of nonionic cellulose ether
CN103415536A (en) * 2011-03-07 2013-11-27 赫尔克里士公司 Water soluble polymer powder formulation having improved dispersing properties
CN105377959A (en) * 2013-04-22 2016-03-02 赫尔克里士公司 Methods for dispersing water soluble polymer powder
CN106893115A (en) * 2017-03-01 2017-06-27 广东浪淘砂新型材料有限公司 A kind of high concentration non-ionic celluloses ether suspended dispersed liquid and preparation method thereof
CN111116998A (en) * 2019-12-20 2020-05-08 煤炭科学技术研究院有限公司 Mining environment-friendly phase-change gel drilling sealing material
CN112300446A (en) * 2020-09-24 2021-02-02 煤炭科学技术研究院有限公司 Sealing material and method for pressure measurement of underground water-containing gas of coal mine

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE10158488A1 (en) * 2001-11-28 2003-06-12 Wolff Cellulosics Gmbh & Co Kg Solution-delayed cellulose ethers and a process for their preparation

Patent Citations (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB767924A (en) * 1954-03-01 1957-02-13 Hercules Powder Co Ltd Improvements in or relating to the manufacture of carboxyalkyl cellulose ether salts
GB780628A (en) * 1954-12-30 1957-08-07 Hercules Powder Co Ltd Improvements in or relating to improved water-soluble salts of carboxyalkyl cellulose ethers and method of converting into granular form
GB1193650A (en) * 1966-11-21 1970-06-03 Courtaulds Ltd Improvements in and relating to Water-Soluble Cellulose Ether Compositions.
US5837864A (en) * 1994-12-15 1998-11-17 Akzo Nobel Nv Method for producing a suspension in water of a cellulose ether, and dry mixture suitable for use in the production of the suspension
JP2000063565A (en) * 1998-08-20 2000-02-29 Shin Etsu Chem Co Ltd Granular water-soluble cellulose ether and method for producing the same
EP1469031A2 (en) * 2003-04-18 2004-10-20 Shin-Etsu Chemical Co., Ltd. Granulation of nonionic cellulose ether
CN103415536A (en) * 2011-03-07 2013-11-27 赫尔克里士公司 Water soluble polymer powder formulation having improved dispersing properties
CN105377959A (en) * 2013-04-22 2016-03-02 赫尔克里士公司 Methods for dispersing water soluble polymer powder
CN106893115A (en) * 2017-03-01 2017-06-27 广东浪淘砂新型材料有限公司 A kind of high concentration non-ionic celluloses ether suspended dispersed liquid and preparation method thereof
CN111116998A (en) * 2019-12-20 2020-05-08 煤炭科学技术研究院有限公司 Mining environment-friendly phase-change gel drilling sealing material
CN112300446A (en) * 2020-09-24 2021-02-02 煤炭科学技术研究院有限公司 Sealing material and method for pressure measurement of underground water-containing gas of coal mine

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
"松软煤层壁式密封瓦斯抽采技术研究";杨旭等;《世界科技研究与发展》;第37卷(第6期);第658-662页 *

Also Published As

Publication number Publication date
CN114854097A (en) 2022-08-05

Similar Documents

Publication Publication Date Title
CN112723823B (en) Synchronous mortar prepared from shield muck slurry and preparation method
JP2000502032A (en) Composition for producing lightweight gypsum, method for producing foaming agent to be used, and use thereof
CN103626454A (en) Manufacturing method of fast-setting early-strength two-fluid injecting paste material
CN101891445A (en) Back-injected clay slurry of composite lining tunnel and injection method thereof
CN103626452B (en) A kind of ultrahigh water compaction material
CN108046653B (en) External admixture for shield single-liquid synchronous grouting
CN112250412B (en) Method for curing high-viscosity residue soil to be used as backfill material
CN115745526A (en) Coal mine filling material and preparation process thereof
CN114854097B (en) Mining environment-friendly degradable gel drilling sealing material and preparation method thereof
CN114014603A (en) High-water-retention mortar formula
CN114573290B (en) Single-component active synchronous grouting liquid capable of being quickly coagulated and preparation method thereof
CN111116998B (en) Mining environment-friendly phase-change gel drilling sealing material
CN109439303B (en) A kind of inert filling material for shield sharp turning and preparation method thereof
CN115215627A (en) Low-cost light plastering gypsum mortar and preparation method thereof
CN118878240A (en) A green admixture for regulating mud slurry in sandy strata mud-water shield and its preparation method
CN109369073B (en) Soft soil curing agent
CN112142403A (en) Soil-stabilizing grouting material and preparation method thereof
CN112456859A (en) Water reducing agent composition for coal mine paste filling and preparation method and application thereof
CN117209241A (en) Low-strength synchronous grouting material prepared from earth pressure shield muck, and preparation method and application thereof
CN110317006A (en) A kind of architecture construction concrete and preparation method thereof
CN115432979A (en) Large-section tunnel secondary lining self-compacting concrete used in water-rich environment
CN115572112A (en) Anti-cracking dry-mixed plastering mortar and preparation method thereof
CN115353351B (en) Thin-sprayed high-performance polymer mortar for rock protection in tunnels
CN109574554B (en) Slurry suitable for underground diaphragm wall construction
CZ290113B6 (en) Suspension of injection preparation

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant