CN116655281B - Delay coagulant for well drilling plugging cement paste - Google Patents
Delay coagulant for well drilling plugging cement paste Download PDFInfo
- Publication number
- CN116655281B CN116655281B CN202310943242.3A CN202310943242A CN116655281B CN 116655281 B CN116655281 B CN 116655281B CN 202310943242 A CN202310943242 A CN 202310943242A CN 116655281 B CN116655281 B CN 116655281B
- Authority
- CN
- China
- Prior art keywords
- weight
- hydroxyapatite
- stirring
- solution
- parts
- 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
Links
- 239000004568 cement Substances 0.000 title claims abstract description 33
- 238000005553 drilling Methods 0.000 title claims abstract description 18
- 239000000701 coagulant Substances 0.000 title abstract description 7
- 229910052588 hydroxylapatite Inorganic materials 0.000 claims abstract description 87
- XYJRXVWERLGGKC-UHFFFAOYSA-D pentacalcium;hydroxide;triphosphate Chemical compound [OH-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O XYJRXVWERLGGKC-UHFFFAOYSA-D 0.000 claims abstract description 87
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 claims abstract description 47
- 229910052901 montmorillonite Inorganic materials 0.000 claims abstract description 46
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 32
- 239000012188 paraffin wax Substances 0.000 claims abstract description 23
- 239000007787 solid Substances 0.000 claims abstract description 23
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000002002 slurry Substances 0.000 claims abstract description 20
- 230000003111 delayed effect Effects 0.000 claims abstract description 16
- 239000000654 additive Substances 0.000 claims abstract description 9
- 230000000996 additive effect Effects 0.000 claims abstract description 9
- 230000004048 modification Effects 0.000 claims abstract description 5
- 238000012986 modification Methods 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims description 80
- 239000000243 solution Substances 0.000 claims description 75
- 238000000498 ball milling Methods 0.000 claims description 61
- 239000007864 aqueous solution Substances 0.000 claims description 43
- 229920001661 Chitosan Polymers 0.000 claims description 38
- 238000002360 preparation method Methods 0.000 claims description 36
- 230000001105 regulatory effect Effects 0.000 claims description 35
- IWOUKMZUPDVPGQ-UHFFFAOYSA-N barium nitrate Chemical compound [Ba+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O IWOUKMZUPDVPGQ-UHFFFAOYSA-N 0.000 claims description 34
- 239000003795 chemical substances by application Substances 0.000 claims description 33
- 238000001035 drying Methods 0.000 claims description 32
- 238000011282 treatment Methods 0.000 claims description 32
- 238000005406 washing Methods 0.000 claims description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 28
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 27
- 239000007788 liquid Substances 0.000 claims description 25
- VQEHIYWBGOJJDM-UHFFFAOYSA-H lanthanum(3+);trisulfate Chemical compound [La+3].[La+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O VQEHIYWBGOJJDM-UHFFFAOYSA-H 0.000 claims description 20
- NGDQQLAVJWUYSF-UHFFFAOYSA-N 4-methyl-2-phenyl-1,3-thiazole-5-sulfonyl chloride Chemical compound S1C(S(Cl)(=O)=O)=C(C)N=C1C1=CC=CC=C1 NGDQQLAVJWUYSF-UHFFFAOYSA-N 0.000 claims description 19
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 18
- 230000015271 coagulation Effects 0.000 claims description 18
- 238000005345 coagulation Methods 0.000 claims description 18
- 239000004115 Sodium Silicate Substances 0.000 claims description 17
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 17
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 17
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 16
- 238000001816 cooling Methods 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 10
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 9
- YDEXUEFDPVHGHE-GGMCWBHBSA-L disodium;(2r)-3-(2-hydroxy-3-methoxyphenyl)-2-[2-methoxy-4-(3-sulfonatopropyl)phenoxy]propane-1-sulfonate Chemical compound [Na+].[Na+].COC1=CC=CC(C[C@H](CS([O-])(=O)=O)OC=2C(=CC(CCCS([O-])(=O)=O)=CC=2)OC)=C1O YDEXUEFDPVHGHE-GGMCWBHBSA-L 0.000 claims description 9
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 9
- 229910052708 sodium Inorganic materials 0.000 claims description 9
- 239000011734 sodium Substances 0.000 claims description 9
- -1 sodium alkyl sulfonate Chemical class 0.000 claims description 9
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 8
- 239000007853 buffer solution Substances 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 239000006185 dispersion Substances 0.000 claims description 8
- 239000008055 phosphate buffer solution Substances 0.000 claims description 8
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 8
- ZNCPFRVNHGOPAG-UHFFFAOYSA-L sodium oxalate Chemical compound [Na+].[Na+].[O-]C(=O)C([O-])=O ZNCPFRVNHGOPAG-UHFFFAOYSA-L 0.000 claims description 8
- 229940039790 sodium oxalate Drugs 0.000 claims description 8
- 239000003607 modifier Substances 0.000 claims description 7
- 230000000694 effects Effects 0.000 abstract description 8
- 230000000903 blocking effect Effects 0.000 abstract description 3
- 238000007711 solidification Methods 0.000 abstract description 3
- 230000008023 solidification Effects 0.000 abstract description 3
- 239000002253 acid Substances 0.000 abstract 1
- 230000007797 corrosion Effects 0.000 abstract 1
- 238000005260 corrosion Methods 0.000 abstract 1
- 238000007712 rapid solidification Methods 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 9
- 230000006866 deterioration Effects 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 230000004913 activation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000013043 chemical agent Substances 0.000 description 1
- 230000003750 conditioning effect Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000006187 pill Substances 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
Classifications
-
- 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
- C09K8/426—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells for plugging
-
- 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
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
- C04B40/0039—Premixtures of ingredients
-
- 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
- C09K8/467—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 containing additives for specific purposes
-
- 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
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/10—Accelerators; Activators
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Ceramic Engineering (AREA)
- Inorganic Chemistry (AREA)
- Structural Engineering (AREA)
- Dental Preparations (AREA)
- Soil Conditioners And Soil-Stabilizing Materials (AREA)
Abstract
The invention relates to the technical field of coagulants, and particularly discloses a delayed coagulant for plugging cement slurry for drilling, wherein the delayed coagulant comprises triethanolamine, solid paraffin, a hydroxyapatite regulator and a modification auxiliary agent; the mass ratio of the triethanolamine to the solid paraffin to the hydroxyapatite regulator to the modified additive is (2-4): 5-7): 1.5-2.5): 1. The montmorillonite has a lamellar structure, plays a role in slow release and blocking through the lamellar structure, blocks rapid solidification among cements, and the improved montmorillonite and the hydroxyapatite regulator are better cooperated, so that the slow release solidification effect is more excellent, and the acid corrosion resistance stability of the product is more remarkable.
Description
Technical Field
The invention relates to the technical field of drilling, in particular to a delay coagulant for plugging cement paste for drilling.
Background
The setting accelerator acts as a chemical agent that can be used to shorten the thickening time of the cement slurry. By adding the accelerator to the cement slurry, the hydration reaction of the cement can be accelerated, and the early strength of the cement can be improved. The coagulant is mainly suitable for engineering construction requiring rapid cement slurry solidification, such as leakage well cementation, gas well cementation, shallow well cementation, well drilling engineering plugging and the like.
The plugging cement slurry reaches a certain stratum in the well, and the setting accelerator in the delay accelerator is fully released by increasing the ambient temperature, so that the solidification of the plugging cement slurry is promoted.
The existing accelerator has poor delayed coagulation effect, the cement is quickly coagulated in the rise of the ambient temperature, the delayed coagulation efficiency is poor, and the existing accelerator has insufficient stability, so the invention further improves the treatment.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a delay accelerator for a drilling plugging cement slurry, which aims to solve the problems in the prior art.
The invention solves the technical problems by adopting the following technical scheme:
the invention provides a delayed coagulation accelerator for well drilling plugging cement slurry, which comprises triethanolamine, solid paraffin, hydroxyapatite regulator and modified auxiliary agent; the mass ratio of the triethanolamine to the solid paraffin to the hydroxyapatite regulator to the modified additive is (2-4): 5-7): 1.5-2.5): 1.
Preferably, the mass ratio of the triethanolamine to the solid paraffin to the hydroxyapatite regulator to the modification auxiliary agent is 3:6:2:1.
Preferably, the preparation method of the hydroxyapatite regulator comprises the following steps:
s01: adding hydroxyapatite into hydrochloric acid solution with the mass fraction of 2% according to the weight ratio of 1:5, stirring and dispersing uniformly, washing with water, drying, sending into the heat treatment at 140-150 ℃ for 5-10min, cooling to 40 ℃ at the speed of 1-3 ℃/min, and preserving heat;
s02: dissolving 5-10 parts by weight of citric acid in 35-45 parts by weight of deionized water, adding 2-5 parts by weight of sodium alkyl sulfonate, 2-4 parts by weight of barium nitrate aqueous solution and 1-3 parts by weight of lanthanum sulfate solution, and stirring and mixing thoroughly to obtain a modified liquid;
s03: placing the heat-preserving product and the modified liquid of the S01 in the S02 according to the weight ratio of 1:5, stirring and reacting, and washing and drying after stirring is finished to obtain a hydroxyapatite agent;
s04: adding chitosan regulating solution accounting for 10-15% of the total weight of the hydroxyapatite agent into the hydroxyapatite agent, performing ball milling treatment, wherein the ball milling rotating speed is 1000-1500r/min, performing ball milling for 1-2h, and performing water washing and drying after the ball milling is finished to obtain the hydroxyapatite regulating agent.
The inventor of the present invention found that no hydroxyapatite modifier is added, no modified liquid treatment is adopted in the preparation of the hydroxyapatite modifier, no chitosan modifier treatment is adopted in the preparation of the hydroxyapatite modifier, and no lanthanum sulfate solution is added in the preparation of the modified liquid; the performance of the product is in a trend of deterioration, and meanwhile, only the hydroxyapatite regulator prepared by the method has the most obvious performance effect.
Preferably, the mass fraction of the barium nitrate aqueous solution is 10-15%; the mass fraction of the lanthanum sulfate solution is 4-8%.
Preferably, the stirring speed of the stirring reaction treatment is 350-550 r/min, the stirring time is 10-20 min, and the stirring temperature is 46-48 ℃.
Preferably, the preparation method of the chitosan regulating solution comprises the following steps:
adding 4-6 parts by weight of sodium silicate aqueous solution into 20-25 parts by weight of chitosan aqueous solution with mass fraction of 5-8%, uniformly stirring, then adding 1-3 parts by weight of phosphoric acid buffer solution, 2-5 parts by weight of sodium lignin sulfonate and 0.45-0.65 part by weight of silicon nitride, and uniformly stirring to obtain the chitosan regulating solution.
Preferably, the pH of the phosphate buffer solution is 4.5; the mass dispersion of the sodium silicate aqueous solution is 10-15%.
Preferably, the preparation method of the modifying auxiliary agent comprises the following steps:
s11: heat treatment is carried out on montmorillonite for 10-20 min at 130-140 ℃, then the montmorillonite is cooled to 45 ℃ at a speed of 1-3 ℃/min, and the temperature is kept;
s12: and adding silica sol accounting for 5-10% of the total weight of the montmorillonite, yttrium nitrate solution accounting for 10-15% of the total weight of the montmorillonite and sodium oxalate accounting for 1-3% of the total weight of the montmorillonite into the heat-preserving montmorillonite, performing ball milling treatment, washing with water and drying to obtain the modified auxiliary agent.
The inventor of the invention also discovers that the performance of the product is obviously degraded without adding a modifying auxiliary agent, and the performance of the product is prone to be degraded without adding yttrium nitrate solution in the preparation of the modifying auxiliary agent.
Preferably, the yttrium nitrate solution is 1-3% by mass.
Preferably, the ball milling rotating speed is 1000-1200r/min, and the ball milling is performed for 1-2h.
Compared with the prior art, the invention has the following beneficial effects:
the triethanolamine is matched with the solid paraffin as a matrix material, an effective coagulation accelerating effect can be formed after the solid paraffin is prepared into dripping pills and then is matched with cement, the hydroxyapatite regulator and the modified auxiliary agent are mutually coordinated, the delayed coagulation accelerating effect of the product is improved, the hydroxyapatite has adsorptivity and can better participate in cement coagulation, the modified liquid prepared by mixing the citric acid solution, the sodium alkyl sulfonate, the barium nitrate aqueous solution and the lanthanum sulfate solution is matched with the activation improvement under the hydrochloric acid solution and the heat treatment, the obtained hydroxyapatite agent can be better ball-milled and improved with the chitosan regulating solution by modifying the hydroxyapatite, the chitosan regulating solution adopts the chitosan aqueous solution as the matrix material and is matched with the silicon nitride, the sodium lignin sulfonate and the sodium silicate aqueous solution, the stable activity of the hydroxyapatite is optimized, the montmorillonite has a lamellar structure, the slow release blocking effect is achieved through the lamellar structure, the rapid coagulation between the blocking cement is blocked, and the modified montmorillonite and the hydroxyapatite regulator has better synergy, so that the slow release coagulation effect is better.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and fully with reference to the accompanying drawings, in which it is evident that the embodiments described are only some, but not all embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The delayed coagulation accelerator for the plugging cement slurry for drilling comprises triethanolamine, solid paraffin, hydroxyapatite regulator and modified auxiliary agent; the mass ratio of the triethanolamine to the solid paraffin to the hydroxyapatite regulator to the modified additive is (2-4): 5-7): 1.5-2.5): 1.
The mass ratio of the triethanolamine, the solid paraffin, the hydroxyapatite regulator and the modification auxiliary agent in the embodiment is 3:6:2:1.
The preparation method of the hydroxyapatite regulator in the embodiment comprises the following steps:
s01: adding hydroxyapatite into hydrochloric acid solution with the mass fraction of 2% according to the weight ratio of 1:5, stirring and dispersing uniformly, washing with water, drying, sending into the heat treatment at 140-150 ℃ for 5-10min, cooling to 40 ℃ at the speed of 1-3 ℃/min, and preserving heat;
s02: dissolving 5-10 parts by weight of citric acid in 35-45 parts by weight of deionized water, adding 2-5 parts by weight of sodium alkyl sulfonate, 2-4 parts by weight of barium nitrate aqueous solution and 1-3 parts by weight of lanthanum sulfate solution, and stirring and mixing thoroughly to obtain a modified liquid;
s03: placing the heat-preserving product and the modified liquid of the S01 in the S02 according to the weight ratio of 1:5, stirring and reacting, and washing and drying after stirring is finished to obtain a hydroxyapatite agent;
s04: adding chitosan regulating solution accounting for 10-15% of the total weight of the hydroxyapatite agent into the hydroxyapatite agent, performing ball milling treatment, wherein the ball milling rotating speed is 1000-1500r/min, performing ball milling for 1-2h, and performing water washing and drying after the ball milling is finished to obtain the hydroxyapatite regulating agent.
The mass fraction of the barium nitrate aqueous solution in the embodiment is 10-15%; the mass fraction of the lanthanum sulfate solution is 4-8%.
The stirring speed of the stirring reaction treatment is 350-550 r/min, the stirring time is 10-20 min, and the stirring temperature is 46-48 ℃.
The preparation method of the chitosan regulating solution in the embodiment comprises the following steps:
adding 4-6 parts by weight of sodium silicate aqueous solution into 20-25 parts by weight of chitosan aqueous solution with mass fraction of 5-8%, uniformly stirring, then adding 1-3 parts by weight of phosphoric acid buffer solution, 2-5 parts by weight of sodium lignin sulfonate and 0.45-0.65 part by weight of silicon nitride, and uniformly stirring to obtain the chitosan regulating solution.
The pH of the phosphate buffer solution of this example was 4.5; the mass dispersion of the sodium silicate aqueous solution is 10-15%.
The preparation method of the modified auxiliary agent of the embodiment comprises the following steps:
s11: heat treatment is carried out on montmorillonite for 10-20 min at 130-140 ℃, then the montmorillonite is cooled to 45 ℃ at a speed of 1-3 ℃/min, and the temperature is kept;
s12: and adding silica sol accounting for 5-10% of the total weight of the montmorillonite, yttrium nitrate solution accounting for 10-15% of the total weight of the montmorillonite and sodium oxalate accounting for 1-3% of the total weight of the montmorillonite into the heat-preserving montmorillonite, performing ball milling treatment, washing with water and drying to obtain the modified auxiliary agent.
The mass fraction of the yttrium nitrate solution in the embodiment is 1-3%.
The ball milling rotating speed of the embodiment is 1000-1200r/min, and the ball milling is carried out for 1-2h.
Example 1
The delayed coagulation accelerator for the plugging cement slurry for drilling comprises triethanolamine, solid paraffin, hydroxyapatite regulator and modified auxiliary agent; the mass ratio of the triethanolamine to the solid paraffin to the hydroxyapatite regulator to the modified additive is 2:5:1.5:1.
The preparation method of the hydroxyapatite regulator in the embodiment comprises the following steps:
s01: adding hydroxyapatite into hydrochloric acid solution with the mass fraction of 2% according to the weight ratio of 1:5, stirring and dispersing uniformly, washing with water, drying, sending into the temperature of 140 ℃ for heat treatment for 5min, cooling to 40 ℃ at the speed of 1 ℃/min, and preserving heat;
s02: dissolving 5 parts by weight of citric acid in 35 parts by weight of deionized water, adding 2 parts by weight of sodium alkyl sulfonate, 2 parts by weight of barium nitrate aqueous solution and 1 part by weight of lanthanum sulfate solution, and stirring and mixing thoroughly to obtain a modified liquid;
s03: placing the heat-preserving product and the modified liquid of the S01 in the S02 according to the weight ratio of 1:5, stirring and reacting, and washing and drying after stirring is finished to obtain a hydroxyapatite agent;
s04: adding chitosan regulating solution accounting for 10 percent of the total weight of the hydroxyapatite agent into the hydroxyapatite agent, performing ball milling treatment, wherein the ball milling rotating speed is 1000r/min, performing ball milling for 1h, and performing water washing and drying after the ball milling is finished to obtain the hydroxyapatite regulating agent.
The mass fraction of the barium nitrate aqueous solution in the embodiment is 10%; the mass fraction of the lanthanum sulfate solution is 4%.
The stirring speed of the stirring reaction treatment in this example was 350r/min, the stirring time was 10min, and the stirring temperature was 46 ℃.
The preparation method of the chitosan regulating solution in the embodiment comprises the following steps:
adding 4 parts by weight of sodium silicate aqueous solution into 20 parts by weight of chitosan aqueous solution with mass fraction of 5%, uniformly stirring, then adding 1 part by weight of phosphoric acid buffer solution, 2 parts by weight of sodium lignin sulfonate and 0.45 part by weight of silicon nitride, and uniformly stirring to obtain the chitosan regulating solution.
The pH of the phosphate buffer solution of this example was 4.5; the mass dispersion of the sodium silicate aqueous solution was 10%.
The preparation method of the modified auxiliary agent of the embodiment comprises the following steps:
s11: heat-treating montmorillonite at 130deg.C for 10min, cooling to 45deg.C at a rate of 1deg.C/min, and maintaining the temperature;
s12: then adding silica sol accounting for 5 percent of the total weight of the montmorillonite, yttrium nitrate solution accounting for 10 percent of the total weight of the montmorillonite and sodium oxalate accounting for 1 percent of the total weight of the montmorillonite into the heat-preserving montmorillonite, performing ball milling treatment, and washing and drying after the ball milling is finished to obtain the modified auxiliary agent.
The mass fraction of the yttrium nitrate solution of this example was 1%.
The ball milling rotation speed of the embodiment is 1000r/min, and the ball milling is carried out for 1h.
Example 2
The delayed coagulation accelerator for the plugging cement slurry for drilling comprises triethanolamine, solid paraffin, hydroxyapatite regulator and modified auxiliary agent; the mass ratio of the triethanolamine to the solid paraffin to the hydroxyapatite regulator to the modified additive is 4:7:2.5:1.
The preparation method of the hydroxyapatite regulator in the embodiment comprises the following steps:
s01: adding hydroxyapatite into hydrochloric acid solution with the mass fraction of 2% according to the weight ratio of 1:5, stirring and dispersing uniformly, washing with water, drying, sending into a heat treatment device at 150 ℃ for 10min, cooling to 40 ℃ at the speed of 3 ℃/min, and preserving heat;
s02: dissolving 10 parts by weight of citric acid in 45 parts by weight of deionized water, adding 5 parts by weight of sodium alkyl sulfonate, 4 parts by weight of barium nitrate aqueous solution and 3 parts by weight of lanthanum sulfate solution, and stirring and mixing thoroughly to obtain a modified liquid;
s03: placing the heat-preserving product and the modified liquid of the S01 in the S02 according to the weight ratio of 1:5, stirring and reacting, and washing and drying after stirring is finished to obtain a hydroxyapatite agent;
s04: adding chitosan regulating solution accounting for 15 percent of the total weight of the hydroxyapatite agent into the hydroxyapatite agent, performing ball milling treatment, wherein the ball milling rotating speed is 1500r/min, performing ball milling for 2 hours, and performing water washing and drying after the ball milling is finished to obtain the hydroxyapatite regulating agent.
The mass fraction of the barium nitrate aqueous solution in the embodiment is 15%; the mass fraction of the lanthanum sulfate solution is 8%.
The stirring speed of the stirring reaction treatment in this example was 550r/min, the stirring time was 20min, and the stirring temperature was 48 ℃.
The preparation method of the chitosan regulating solution in the embodiment comprises the following steps:
adding 6 parts by weight of sodium silicate aqueous solution into 25 parts by weight of 8% by weight of chitosan aqueous solution, uniformly stirring, adding 3 parts by weight of phosphoric acid buffer solution, 5 parts by weight of sodium lignin sulfonate and 0.65 part by weight of silicon nitride, and uniformly stirring to obtain the chitosan regulating solution.
The pH of the phosphate buffer solution of this example was 4.5; the mass dispersion of the sodium silicate aqueous solution was 15%.
The preparation method of the modified auxiliary agent of the embodiment comprises the following steps:
s11: heat-treating montmorillonite at 140deg.C for 20min, cooling to 45deg.C at a rate of 3deg.C/min, and maintaining the temperature;
s12: then adding silica sol accounting for 10 percent of the total weight of the montmorillonite, yttrium nitrate solution accounting for 15 percent of the total weight of the montmorillonite and sodium oxalate accounting for 3 percent of the total weight of the montmorillonite into the heat-preserving montmorillonite, performing ball milling treatment, and washing and drying after the ball milling is finished to obtain the modified auxiliary agent.
The mass fraction of the yttrium nitrate solution of this example was 3%.
The ball milling rotation speed of the embodiment is 1200r/min, and the ball milling is carried out for 2 hours.
Example 3
The delayed coagulation accelerator for the plugging cement slurry for drilling comprises triethanolamine, solid paraffin, hydroxyapatite regulator and modified auxiliary agent; the mass ratio of the triethanolamine to the solid paraffin to the hydroxyapatite regulator to the modified additive is 3:6:2:1.
The preparation method of the hydroxyapatite regulator in the embodiment comprises the following steps:
s01: adding hydroxyapatite into hydrochloric acid solution with the mass fraction of 2% according to the weight ratio of 1:5, stirring and dispersing uniformly, washing with water, drying, sending into 145 ℃ for heat treatment for 7.5min, cooling to 40 ℃ at the speed of 2 ℃/min, and preserving heat;
s02: dissolving 7.5 parts by weight of citric acid in 40 parts by weight of deionized water, adding 3.5 parts by weight of sodium alkyl sulfonate, 3 parts by weight of barium nitrate aqueous solution and 2 parts by weight of lanthanum sulfate solution, and stirring and mixing fully to obtain a modified liquid;
s03: placing the heat-preserving product and the modified liquid of the S01 in the S02 according to the weight ratio of 1:5, stirring and reacting, and washing and drying after stirring is finished to obtain a hydroxyapatite agent;
s04: adding chitosan regulating solution accounting for 12.5 percent of the total weight of the hydroxyapatite agent into the hydroxyapatite agent, performing ball milling treatment, wherein the ball milling rotating speed is 1250r/min, performing ball milling for 1.5 hours, and performing water washing and drying after the ball milling is finished to obtain the hydroxyapatite regulating agent.
The mass fraction of the barium nitrate aqueous solution in the embodiment is 12%; the mass fraction of the lanthanum sulfate solution is 6%.
The stirring speed of the stirring reaction treatment in this example was 400r/min, the stirring time was 15min, and the stirring temperature was 47 ℃.
The preparation method of the chitosan regulating solution in the embodiment comprises the following steps:
adding 5 parts by weight of sodium silicate aqueous solution into 22.5 parts by weight of chitosan aqueous solution with the mass fraction of 6.5%, uniformly stirring, then adding 2 parts by weight of phosphoric acid buffer solution, 3.5 parts by weight of sodium lignin sulfonate and 0.50 part by weight of silicon nitride, and uniformly stirring to obtain the chitosan regulating solution.
The pH of the phosphate buffer solution of this example was 4.5; the mass dispersion of the sodium silicate aqueous solution is 10-15%.
The preparation method of the modified auxiliary agent of the embodiment comprises the following steps:
s11: heat-treating montmorillonite at 135deg.C for 15min, cooling to 45deg.C at a rate of 2deg.C/min, and maintaining the temperature;
s12: then adding silica sol with the weight of 7.5 percent of the total weight of the montmorillonite, yttrium nitrate solution with the weight of 12.5 percent of the total weight of the montmorillonite and sodium oxalate with the weight of 2 percent of the total weight of the montmorillonite into the heat-preserving montmorillonite, performing ball milling treatment, and washing and drying after the ball milling is finished to obtain the modified auxiliary agent.
The mass fraction of the yttrium nitrate solution of this example was 2%.
The ball milling rotation speed of the embodiment is 1100r/min, and the ball milling is carried out for 1.5 hours.
Example 4
The delayed coagulation accelerator for the plugging cement slurry for drilling comprises triethanolamine, solid paraffin, hydroxyapatite regulator and modified auxiliary agent; the mass ratio of the triethanolamine to the solid paraffin to the hydroxyapatite regulator to the modified additive is 3:6:1.8:1.
The preparation method of the hydroxyapatite regulator in the embodiment comprises the following steps:
s01: adding hydroxyapatite into hydrochloric acid solution with the mass fraction of 2% according to the weight ratio of 1:5, stirring and dispersing uniformly, washing with water, drying, sending into 142 ℃ for heat treatment for 6min, cooling to 40 ℃ at the speed of 2 ℃/min, and preserving heat;
s02: dissolving 6 parts by weight of citric acid in 38 parts by weight of deionized water, adding 3 parts by weight of sodium alkyl sulfonate, 3 parts by weight of barium nitrate aqueous solution and 2 parts by weight of lanthanum sulfate solution, and stirring and mixing thoroughly to obtain a modified liquid;
s03: placing the heat-preserving product and the modified liquid of the S01 in the S02 according to the weight ratio of 1:5, stirring and reacting, and washing and drying after stirring is finished to obtain a hydroxyapatite agent;
s04: adding a chitosan regulating solution accounting for 12% of the total weight of the hydroxyapatite agent into the hydroxyapatite agent, performing ball milling treatment, wherein the ball milling rotating speed is 1200r/min, performing ball milling for 1.2 hours, and performing water washing and drying after the ball milling is finished to obtain the hydroxyapatite regulating agent.
The mass fraction of the barium nitrate aqueous solution in the embodiment is 12%; the mass fraction of the lanthanum sulfate solution is 5%.
The stirring speed of the stirring reaction treatment in this example was 400r/min, the stirring time was 12min, and the stirring temperature was 47 ℃.
The preparation method of the chitosan regulating solution in the embodiment comprises the following steps:
adding 5 parts by weight of sodium silicate aqueous solution into 22 parts by weight of chitosan aqueous solution with the mass fraction of 6%, uniformly stirring, then adding 2 parts by weight of phosphoric acid buffer solution, 3 parts by weight of sodium lignin sulfonate and 0.50 part by weight of silicon nitride, and uniformly stirring to obtain the chitosan regulating solution.
The pH of the phosphate buffer solution of this example was 4.5; the mass dispersion of the sodium silicate aqueous solution was 12%.
The preparation method of the modified auxiliary agent of the embodiment comprises the following steps:
s11: heat-treating montmorillonite at 132 deg.C for 12min, cooling to 45 deg.C at 2 deg.C/min, and maintaining the temperature;
s12: then adding silica sol accounting for 6 percent of the total weight of the montmorillonite, yttrium nitrate solution accounting for 12 percent of the total weight of the montmorillonite and sodium oxalate accounting for 2 percent of the total weight of the montmorillonite into the heat-preserving montmorillonite, performing ball milling treatment, and washing and drying after the ball milling is finished to obtain the modified auxiliary agent.
The mass fraction of the yttrium nitrate solution of this example was 2%.
The ball milling rotation speed of this example is 1050r/min, and ball milling is carried out for 1.2 hours.
Example 5
The delayed coagulation accelerator for the plugging cement slurry for drilling comprises triethanolamine, solid paraffin, hydroxyapatite regulator and modified auxiliary agent; the mass ratio of the triethanolamine to the solid paraffin to the hydroxyapatite regulator to the modified additive is 3:6:2.5:1.
The preparation method of the hydroxyapatite regulator in the embodiment comprises the following steps:
s01: adding hydroxyapatite into hydrochloric acid solution with the mass fraction of 2% according to the weight ratio of 1:5, stirring and dispersing uniformly, washing with water, drying, sending into 148 ℃ for heat treatment for 8min, cooling to 40 ℃ at the speed of 2 ℃/min, and preserving heat;
s02: dissolving 8 parts by weight of citric acid in 42 parts by weight of deionized water, adding 4 parts by weight of sodium alkyl sulfonate, 3 parts by weight of barium nitrate aqueous solution and 2 parts by weight of lanthanum sulfate solution, and stirring and mixing thoroughly to obtain a modified liquid;
s03: placing the heat-preserving product and the modified liquid of the S01 in the S02 according to the weight ratio of 1:5, stirring and reacting, and washing and drying after stirring is finished to obtain a hydroxyapatite agent;
s04: adding chitosan regulating solution accounting for 14% of the total weight of the hydroxyapatite agent into the hydroxyapatite agent, performing ball milling treatment, wherein the ball milling rotating speed is 1400r/min, performing ball milling for 1.8 hours, and performing water washing and drying after the ball milling is finished to obtain the hydroxyapatite regulating agent.
The mass fraction of the barium nitrate aqueous solution in the embodiment is 14%; the mass fraction of the lanthanum sulfate solution is 6%.
The stirring speed of the stirring reaction treatment in this example was 500r/min, the stirring time was 18min, and the stirring temperature was 47 ℃.
The preparation method of the chitosan regulating solution in the embodiment comprises the following steps:
adding 5 parts by weight of sodium silicate aqueous solution into 24 parts by weight of chitosan aqueous solution with mass fraction of 7%, uniformly stirring, then adding 2 parts by weight of phosphoric acid buffer solution, 4 parts by weight of sodium lignin sulfonate and 0.55 part by weight of silicon nitride, and uniformly stirring to obtain the chitosan regulating solution.
The pH of the phosphate buffer solution of this example was 4.5; the mass dispersion of the sodium silicate aqueous solution was 14%.
The preparation method of the modified auxiliary agent of the embodiment comprises the following steps:
s11: heat-treating montmorillonite at 135deg.C for 15min, cooling to 45deg.C at a rate of 2deg.C/min, and maintaining the temperature;
s12: then adding silica sol accounting for 8 percent of the total weight of the montmorillonite, yttrium nitrate solution accounting for 14 percent of the total weight of the montmorillonite and sodium oxalate accounting for 2 percent of the total weight of the montmorillonite into the heat-preserving montmorillonite, performing ball milling treatment, and washing and drying after the ball milling is finished to obtain the modified auxiliary agent.
The mass fraction of the yttrium nitrate solution of this example was 2%.
The ball milling rotation speed of the embodiment is 1100r/min, and the ball milling is carried out for 1.8 hours.
Comparative example 1
Unlike example 3, no hydroxyapatite modifier was added.
Comparative example 2
The difference from example 3 is that no modification liquid treatment was used in the preparation of the hydroxyapatite modifier.
Comparative example 3
The difference from example 3 is that no chitosan conditioning liquid treatment was used in the preparation of the hydroxyapatite conditioner.
Comparative example 4
The difference from example 3 is that no lanthanum sulfate solution was added in the preparation of the modified liquid.
Comparative example 5
The difference from example 3 is that no modifying auxiliary is added.
Comparative example 6
The difference from example 3 is that no yttrium nitrate solution was added in the preparation of the modifying auxiliary.
The cement slurry was obtained by uniformly mixing 800g of cement, 350g of water and 4g of the products of examples 1 to 5 and comparative examples 1 to 6, and the performance test was performed as follows:
as can be seen from comparative examples 1 to 6 and examples 1 to 4;
the product of example 3 has excellent set-accelerating properties with excellent results for the properties of examples 1-2 and examples 4-5;
as shown in comparative examples 1-6 and example 3, the invention does not add hydroxyapatite regulator, does not adopt modified liquid treatment in the preparation of the hydroxyapatite regulator, does not adopt chitosan regulating liquid treatment in the preparation of the hydroxyapatite regulator, and does not add lanthanum sulfate solution in the preparation of the modified liquid; the performance of the product is in a trend of deterioration, and the hydroxyapatite regulator prepared by the method has the most obvious performance effect; the performance of the product is obviously deteriorated without adding the modified auxiliary agent, and the performance of the product is prone to be deteriorated without adding yttrium nitrate solution in the preparation of the modified auxiliary agent.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present disclosure describes embodiments, not every embodiment is provided with a separate embodiment, and that this description is provided for clarity only, and that the disclosure is not limited to the embodiments described in detail below, and that the embodiments described in the examples may be combined as appropriate to form other embodiments that will be apparent to those skilled in the art.
Claims (7)
1. The delay setting accelerator for the plugging cement slurry for drilling is characterized by comprising triethanolamine, solid paraffin, hydroxyapatite regulator and modification auxiliary agent; the mass ratio of the triethanolamine to the solid paraffin to the hydroxyapatite regulator to the modified additive is (2-4): 5-7): 1.5-2.5): 1;
the preparation method of the hydroxyapatite regulator comprises the following steps:
s01: adding hydroxyapatite into hydrochloric acid solution with the mass fraction of 2% according to the weight ratio of 1:5, stirring and dispersing uniformly, washing with water, drying, sending into the heat treatment at 140-150 ℃ for 5-10min, cooling to 40 ℃ at the speed of 1-3 ℃/min, and preserving heat;
s02: dissolving 5-10 parts by weight of citric acid in 35-45 parts by weight of deionized water, adding 2-5 parts by weight of sodium alkyl sulfonate, 2-4 parts by weight of barium nitrate aqueous solution and 1-3 parts by weight of lanthanum sulfate solution, and stirring and mixing thoroughly to obtain a modified liquid;
s03: placing the heat-preserving product and the modified liquid of the S01 in the S02 according to the weight ratio of 1:5, stirring and reacting, and washing and drying after stirring is finished to obtain a hydroxyapatite agent;
s04: adding chitosan regulating solution accounting for 10-15% of the total weight of the hydroxyapatite agent into the hydroxyapatite agent, performing ball milling treatment, wherein the ball milling rotating speed is 1000-1500r/min, performing ball milling for 1-2h, and performing water washing and drying after the ball milling is finished to obtain the hydroxyapatite regulating agent;
the preparation method of the modified auxiliary agent comprises the following steps:
s11: heat treatment is carried out on montmorillonite for 10-20 min at 130-140 ℃, then the montmorillonite is cooled to 45 ℃ at a speed of 1-3 ℃/min, and the temperature is kept;
s12: then adding silica sol accounting for 5-10% of the total weight of the montmorillonite, yttrium nitrate solution accounting for 10-15% of the total weight of the montmorillonite and sodium oxalate accounting for 1-3% of the total weight of the montmorillonite into the heat-preserving montmorillonite, performing ball milling treatment, washing with water and drying to obtain a modified auxiliary agent;
the preparation method of the chitosan regulating solution comprises the following steps:
adding 4-6 parts by weight of sodium silicate aqueous solution into 20-25 parts by weight of chitosan aqueous solution with mass fraction of 5-8%, uniformly stirring, then adding 1-3 parts by weight of phosphoric acid buffer solution, 2-5 parts by weight of sodium lignin sulfonate and 0.45-0.65 part by weight of silicon nitride, and uniformly stirring to obtain the chitosan regulating solution.
2. The delayed coagulation accelerator for well plugging cement paste of claim 1, wherein the mass ratio of triethanolamine, solid paraffin, hydroxyapatite modifier and modifying aid is 3:6:2:1.
3. The delayed coagulation accelerator for well plugging cement slurry of claim 1, wherein the mass fraction of the barium nitrate aqueous solution is 10-15%; the mass fraction of the lanthanum sulfate solution is 4-8%.
4. The delayed coagulation accelerator for plugging cement slurry for drilling according to claim 1, wherein the stirring speed of the stirring reaction treatment is 350-550 r/min, the stirring time is 10-20 min, and the stirring temperature is 46-48 ℃.
5. The drilling lost circulation cement slurry delay accelerator of claim 1, wherein the pH of the phosphate buffer solution is 4.5; the mass dispersion of the sodium silicate aqueous solution is 10-15%.
6. The well plugging cement paste time-delay accelerator according to claim 1, wherein the mass fraction of the yttrium nitrate solution is 1-3%.
7. The delayed coagulation accelerator for plugging cement slurry for well drilling according to claim 1, wherein the rotation speed of the ball milling treatment in the step S12 is 1000-1200r/min, and the ball milling is carried out for 1-2h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310943242.3A CN116655281B (en) | 2023-07-31 | 2023-07-31 | Delay coagulant for well drilling plugging cement paste |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310943242.3A CN116655281B (en) | 2023-07-31 | 2023-07-31 | Delay coagulant for well drilling plugging cement paste |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN116655281A CN116655281A (en) | 2023-08-29 |
| CN116655281B true CN116655281B (en) | 2023-09-26 |
Family
ID=87712155
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310943242.3A Active CN116655281B (en) | 2023-07-31 | 2023-07-31 | Delay coagulant for well drilling plugging cement paste |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116655281B (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105238375A (en) * | 2015-10-23 | 2016-01-13 | 中国石油化工股份有限公司 | High strength auto-expansion plugging agent |
| CN107285723A (en) * | 2017-08-03 | 2017-10-24 | 上海欧卓实业发展有限公司 | A kind of improved loss circulation material |
| CN114574180A (en) * | 2022-03-25 | 2022-06-03 | 西南石油大学 | Delayed-gelling composite leakage-stopping liquid and preparation method thereof |
| CN116218491A (en) * | 2023-05-09 | 2023-06-06 | 山东省地质矿产勘查开发局第二水文地质工程地质大队(山东省鲁北地质工程勘察院) | Hydrogel plugging agent, preparation method of hydrogel plugging agent and water-based drilling fluid |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20180072938A1 (en) * | 2016-09-12 | 2018-03-15 | Baker Hughes Incorporated | Ductile cementing materials and the use thereof in high stress cementing applications |
| AU2018292121A1 (en) * | 2017-06-26 | 2020-01-30 | Baker Hughes Holdings, LLC | Set on demand cement |
-
2023
- 2023-07-31 CN CN202310943242.3A patent/CN116655281B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105238375A (en) * | 2015-10-23 | 2016-01-13 | 中国石油化工股份有限公司 | High strength auto-expansion plugging agent |
| CN107285723A (en) * | 2017-08-03 | 2017-10-24 | 上海欧卓实业发展有限公司 | A kind of improved loss circulation material |
| CN114574180A (en) * | 2022-03-25 | 2022-06-03 | 西南石油大学 | Delayed-gelling composite leakage-stopping liquid and preparation method thereof |
| CN116218491A (en) * | 2023-05-09 | 2023-06-06 | 山东省地质矿产勘查开发局第二水文地质工程地质大队(山东省鲁北地质工程勘察院) | Hydrogel plugging agent, preparation method of hydrogel plugging agent and water-based drilling fluid |
Also Published As
| Publication number | Publication date |
|---|---|
| CN116655281A (en) | 2023-08-29 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN116535940B (en) | Wear-resistant and conductive coordinated metal substrate coating and method thereof | |
| CN111423143A (en) | Liquid accelerator and preparation method and application thereof | |
| CN111056762B (en) | Alkali-free liquid accelerator and preparation method thereof | |
| CN111333362A (en) | Low-dosage high-early-strength alkali-free liquid accelerator and preparation method thereof | |
| CN110734242B (en) | Sprayed concrete alkali-free liquid accelerator for alpine regions and preparation method thereof | |
| CN114276042A (en) | Alkali-free fluorine-free liquid accelerator and preparation method thereof | |
| CN110963732A (en) | Environment-friendly alkali-free liquid accelerator and normal-temperature preparation method thereof | |
| CN115636615A (en) | Alkali-free chlorine-free fluorine-free early strength type liquid accelerator and preparation method thereof | |
| CN116655281B (en) | Delay coagulant for well drilling plugging cement paste | |
| CN113003976A (en) | Alkali-free liquid accelerator containing fluorosilicate and preparation method and application thereof | |
| CN111377651B (en) | Low-alkali liquid accelerator containing microbial polysaccharide and preparation method thereof | |
| CN110627400A (en) | Alkali-free accelerator and preparation method and application thereof | |
| CN112225486B (en) | Stable alkali-free liquid accelerator and preparation method and application thereof | |
| CN113860788A (en) | Composite retarder suitable for magnesium phosphate cement | |
| CN110510912B (en) | Wet-mixed mortar additive and preparation method thereof | |
| CN116769271A (en) | Process method for producing damping backing plate | |
| CN113880487A (en) | Fluoride-free alkali-free liquid accelerator and preparation method thereof | |
| CN112960928B (en) | Stabilizer for alkali-free liquid accelerator, alkali-free liquid accelerator and preparation method of alkali-free liquid accelerator | |
| CN115536300A (en) | Functional admixture for shotcrete and preparation method and application thereof | |
| CN106699002B (en) | A kind of aliphatic water reducing agent and its preparation process | |
| CN115353317A (en) | High-aluminum-content accelerator and preparation method thereof | |
| CN113548826B (en) | Antifreezing alkali-free liquid accelerator and preparation method thereof | |
| CN113307534A (en) | Concrete accelerator | |
| CN112520774A (en) | Preparation method of polyaluminum sulfate solution and alkali-free liquid accelerator | |
| CN111333358A (en) | Concrete antifreezing agent and preparation method and application thereof |
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 |