CN115449037A - Modified polyalcohol drilling flushing fluid - Google Patents
Modified polyalcohol drilling flushing fluid Download PDFInfo
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- CN115449037A CN115449037A CN202210945878.7A CN202210945878A CN115449037A CN 115449037 A CN115449037 A CN 115449037A CN 202210945878 A CN202210945878 A CN 202210945878A CN 115449037 A CN115449037 A CN 115449037A
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- 239000012530 fluid Substances 0.000 title claims abstract description 61
- 238000005553 drilling Methods 0.000 title claims abstract description 46
- 150000005846 sugar alcohols Polymers 0.000 title claims abstract description 26
- 238000011010 flushing procedure Methods 0.000 title abstract description 63
- 229920000642 polymer Polymers 0.000 claims abstract description 65
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 37
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 35
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000001913 cellulose Substances 0.000 claims abstract description 22
- 229920002678 cellulose Polymers 0.000 claims abstract description 22
- 239000002518 antifoaming agent Substances 0.000 claims abstract description 21
- 239000003112 inhibitor Substances 0.000 claims abstract description 20
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 11
- 239000005543 nano-size silicon particle Substances 0.000 claims abstract description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 34
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- 239000002131 composite material Substances 0.000 claims description 19
- 238000006116 polymerization reaction Methods 0.000 claims description 18
- 239000003999 initiator Substances 0.000 claims description 16
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical group [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 12
- 239000000706 filtrate Substances 0.000 claims description 12
- 239000001103 potassium chloride Substances 0.000 claims description 11
- 235000011164 potassium chloride Nutrition 0.000 claims description 11
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 10
- 239000003638 chemical reducing agent Substances 0.000 claims description 9
- 229920002401 polyacrylamide Polymers 0.000 claims description 9
- 239000013530 defoamer Substances 0.000 claims description 8
- -1 hydroxyalkyl ether Chemical compound 0.000 claims description 8
- 229920000609 methyl cellulose Polymers 0.000 claims description 8
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- 239000007864 aqueous solution Substances 0.000 claims description 7
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 claims description 6
- 239000000654 additive Substances 0.000 claims description 6
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 claims description 6
- 230000000996 additive effect Effects 0.000 claims description 5
- 150000001875 compounds Chemical class 0.000 claims description 5
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- 230000005764 inhibitory process Effects 0.000 abstract description 39
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- 238000002474 experimental method Methods 0.000 description 4
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- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 3
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerol Natural products OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- 238000005481 NMR spectroscopy Methods 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 229910010413 TiO 2 Inorganic materials 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
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- KSPIHGBHKVISFI-UHFFFAOYSA-N Diphenylcarbazide Chemical compound C=1C=CC=CC=1NNC(=O)NNC1=CC=CC=C1 KSPIHGBHKVISFI-UHFFFAOYSA-N 0.000 description 1
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- 238000004566 IR spectroscopy Methods 0.000 description 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
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- 238000002441 X-ray diffraction Methods 0.000 description 1
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- 229910052797 bismuth Inorganic materials 0.000 description 1
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- 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 description 1
- SOCTUWSJJQCPFX-UHFFFAOYSA-N dichromate(2-) Chemical compound [O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O SOCTUWSJJQCPFX-UHFFFAOYSA-N 0.000 description 1
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- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
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- VGIBGUSAECPPNB-UHFFFAOYSA-L nonaaluminum;magnesium;tripotassium;1,3-dioxido-2,4,5-trioxa-1,3-disilabicyclo[1.1.1]pentane;iron(2+);oxygen(2-);fluoride;hydroxide Chemical compound [OH-].[O-2].[O-2].[O-2].[O-2].[O-2].[F-].[Mg+2].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[K+].[K+].[K+].[Fe+2].O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2 VGIBGUSAECPPNB-UHFFFAOYSA-L 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
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- 239000003921 oil Substances 0.000 description 1
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 1
- 239000003209 petroleum derivative Substances 0.000 description 1
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- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Images
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-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F299/00—Macromolecular compounds obtained by interreacting polymers involving only carbon-to-carbon unsaturated bond reactions, in the absence of non-macromolecular monomers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L53/00—Compositions of block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers
-
- 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
- C09K8/52—Compositions for preventing, limiting or eliminating depositions, e.g. for cleaning
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K2208/00—Aspects relating to compositions of drilling or well treatment fluids
- C09K2208/10—Nanoparticle-containing well treatment fluids
-
- 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
- C09K2208/00—Aspects relating to compositions of drilling or well treatment fluids
- C09K2208/12—Swell inhibition, i.e. using additives to drilling or well treatment fluids for inhibiting clay or shale swelling or disintegrating
-
- 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
- C09K2208/00—Aspects relating to compositions of drilling or well treatment fluids
- C09K2208/34—Lubricant additives
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- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention provides a modified polyalcohol obtained by polymerizing polyvinyl alcohol and PH-7, and a drilling flushing fluid prepared based on the modified polyalcohol. The modified polyalcohol has excellent tackifying, shear-promoting and rheological properties, is applied to a flushing fluid system, and has better comprehensive effects of carrying rocks, lubricating and protecting walls; the rheological property is further enhanced after the hydrophobic cellulose polymer and the nano silicon dioxide are compounded. And a fluid loss agent, a defoaming agent and an anti-collapse inhibitor are further added, so that the anti-collapse inhibition performance can be improved, the prepared flushing fluid has the advantages of good environmental protection performance, easiness in degradation, no pollution, moderate apparent viscosity, higher shear force, small filter loss and stronger anti-collapse inhibition performance, and can meet the construction requirements of site drilling, particularly rope core-taking directional drilling.
Description
Technical Field
The invention belongs to the field of drilling engineering flushing fluids, and particularly relates to a modified polyalcohol drilling flushing fluid.
Background
With the continuous promotion of the construction of great infrastructures such as roads, railways and electric power of the Qinghai-Tibet plateau, related tunnels and underground engineering enter a high-speed development period, and meanwhile, huge technical challenges are brought to many aspects such as investigation, design and construction. The traditional vertical hole related drilling equipment and the traditional vertical hole related drilling process cannot meet the requirement of refined geological exploration of a deeply buried tunnel, horizontal directional exploration is combined with directional drilling equipment and a coring technology to carry out continuous directional coring along a long-distance exploration hole of a tunnel design axis, the vertical hole point exploration is optimized into the directional hole line exploration, the tunnel geological condition can be accurately and quickly explored, the life and property hazards possibly brought by geological safety risks and the like are reduced, and the urgent requirements on the quality and the efficiency of railway exploration in plateau mountain areas are met.
However, compared with the conventional vertical hole coring technology, the horizontal hole coring technology has higher difficulty, the drilling inclination angle is large, and larger drilling pressure is required to overcome the backing pressure of the drilling tool; the annular space has small clearance, the dynamic pressure of the annular space is difficult to control, and the cuttings bed and the drill bit falling block are easy to generate, even the stratum is leaked, fractured or crushed. The existing coring technology which is widely applied and has higher efficiency is rope coring, and has the obvious technical advantages of preventing blocks from falling in holes, reducing drilling times, reducing drilling cost and the like. However, when the method is applied to areas with severe geological environments, such as structural development, steep terrain and the like, the problems of poor stratum leakage pressure-bearing capacity, unstable and collapse hole walls and the like still easily occur. Therefore, the flushing fluid suitable for the horizontal wire line core directional drilling technology has to put higher requirements on the comprehensive performances of the flushing fluid such as rheology, inhibition, collapse prevention and the like.
Meanwhile, the western high-altitude and high-cold regions are ecologically fragile and sensitive, and exploration engineering activities may have adverse effects on the local environment. Drilling mud is one of the most pollutant sources in drilling engineering, and the environmental requirements are becoming more stringent due to newly promulgated environmental standards.
Therefore, in order to solve key technical problems of poor stability of the well wall, low cleanliness of the well hole, large environmental protection pressure of the stratum and the like in horizontal wire line coring and directional drilling, researchers at home and abroad develop basic research work of a large amount of flushing liquid aiming at shale inhibition, system stability, environmental protection and the like. The polyalcohol treating agent widely applied to oil and gas exploration and exploitation gradually expands the field of geological drilling due to excellent anti-collapse inhibition capability, and most of the polyalcohol is non-toxic and environment-friendly, and is more suitable for environment-friendly high-performance flushing fluid process technology. However, in the field of geological drilling, research on a horizontal wire line coring directional drilling flushing fluid process technology is few, the rheological property of the existing system and the research on corresponding treating agents are lack of pertinence, and due to the fact that most of the treating agents commonly used at present are limited in environmental acceptability, the environmental protection and the anti-collapse performance are difficult to be considered at the same time.
In view of the above, in order to ensure that the flushing fluid system has excellent environmental performance and simultaneously meets the requirements of comprehensive performance such as rheology, collapse prevention and the like, it is necessary to start with environment-friendly raw materials, select the polymeric polyol having excellent performance such as non-toxicity, strong inhibition, simple use and the like, perform polymerization modification on the polymeric polyol to improve the weak rheological performance of the polymeric polyol, and further perform the research on the environment-friendly collapse prevention flushing fluid system of the modified polymeric polyol suitable for horizontal rope coring directional drilling through the synergistic effect of the polymer, the nano material and the environment-friendly treating agent, so as to provide a new solution for constructing a safe, green and efficient rope coring directional drilling technology.
Disclosure of Invention
The invention aims to provide a modified polyalcohol anti-collapse flushing fluid which is suitable for being applied to drilling technology, particularly in rope core-drilling directional drilling technology, is green and environment-friendly and has excellent rheological property and anti-collapse property.
The invention provides a modified polyalcohol which is polymerized by polyvinyl alcohol and PH-7; the PH-7 is partially hydrolyzed polyacrylamide with the hydrolysis degree of 35-50%.
Further, the mass ratio of the polyvinyl alcohol to the pH-7 is 2 (0.01 to 0.02), preferably 2.
Further, the polymerization is carried out in an aqueous solution under the action of an initiator; the using amount of the initiator is not less than 2.25 percent of the total mass of the polyvinyl alcohol and the PH-7; preferably, the initiator is ammonium persulfate and sodium bisulfite, and the mass ratio of the ammonium persulfate to the sodium bisulfite is 2.
The invention also provides a modified polyalcohol composite material, which is compounded by the modified polyalcohol as claimed, cellulose polymer and nano silicon dioxide;
the mass ratio of the modified polyalcohol to the cellulose polymer to the nano-silica is (2.02) - (0.08-0.15) - (0.05-0.2), and preferably (2.02).
Further, the above cellulose-based polymer is a mixture of methylcellulose and a cellulose hydroxyalkyl ether; the mass ratio of the methyl cellulose to the cellulose hydroxyalkyl ether is 1 (0.6-1), preferably 1.
The invention also provides the application of the modified polymer alcohol or the modified polymer alcohol composite material in drilling flushing fluid.
The invention also provides a drilling flushing fluid which is an aqueous solution containing the modified polymer alcohol or the modified polymer alcohol composite material; preferably, the mass fraction of the modified polymeric alcohol in the aqueous solution is 2%, and the mass fraction of the modified polymeric alcohol composite material is 2.02%.
Further, the feed also comprises the following components in percentage by mass:
0.1-0.3 per mill of filtrate reducer, 0.15-0.25 percent of defoamer and 0.8-1.2 percent of anti-collapse inhibitor;
preferably: 0.3 per mill of filtrate reducer, 0.2 percent of defoamer and 0.8 percent of anti-collapse inhibitor.
Furthermore, the filtrate reducer is a starch compound, the defoaming agent is an organic silicon compound, and the anti-collapse inhibitor is an inorganic salt compound.
Furthermore, the drilling flushing fluid consists of the following components in percentage by mass:
2.02% of the modified polyalcohol, 0.5% of methylcellulose, 0.5% of cellulose hydroxyalkyl ether, 0.1% of nano silicon dioxide, 0.3% of modified pregelatinized starch DFD, 70.2% of organosilicon defoamer DU-900.8%, and the balance of water.
The invention has the beneficial effects that: the invention provides a polymer copolymerized and modified by polyacrylamide derivatives and polyvinyl alcohol, which has excellent tackifying, shear-improving and rheological properties, and has better comprehensive effects of carrying rocks, lubricating and protecting walls when being applied to a flushing fluid system; the polymer mixed with the hydrophobic cellulose polymer can synergistically enhance the stability of a polymer structure, and the mixed nano silicon dioxide can enhance the regularity of the polymer structure and enhance the rheological property of a solution. And a fluid loss agent, a defoaming agent and an anti-collapse inhibitor are further added, so that the anti-collapse inhibition performance can be improved, the prepared flushing fluid has the advantages of good environmental protection performance, easiness in degradation, no pollution, moderate apparent viscosity, higher shear force, small filter loss and stronger anti-collapse inhibition performance, and can meet the construction requirements of site drilling, particularly rope core-taking directional drilling.
The term "partially hydrolyzed polyacrylamide" as used herein refers to polyacrylamide having a degree of hydrolysis of less than 100%.
Obviously, many modifications, substitutions, and variations are possible in light of the above teachings of the invention, without departing from the basic technical spirit of the invention, as defined by the following claims.
The present invention will be described in further detail with reference to the following examples. This should not be understood as limiting the scope of the above-described subject matter of the present invention to the following examples. All the technologies realized based on the above contents of the present invention belong to the scope of the present invention.
Drawings
FIG. 1: the effect of PVA addition on viscosity (a) and flow pattern (b).
FIG. 2: the trend chart of the influence of the high molecular polymer on the rheological property of PVA-1788.
FIG. 3: the effect of the cellulose polymer on the performance of the pH-VA solution.
FIG. 4: the variation trend of the compounding performance parameters of the cellulose polymer.
FIG. 5: the trend of the performance parameters after the nano material is compounded.
FIG. 6: the compounding performance trend of the filtrate reducer.
FIG. 7 is a schematic view of: and (4) the compounding performance trend of the defoaming agent.
FIG. 8: the trend of the complex performance of the anti-collapse inhibitor.
Detailed Description
The main experimental raw materials of the present invention are shown in table 1.
TABLE 1
The remaining starting materials and equipment used in the present invention are, unless otherwise stated, known products obtained by purchasing commercially available products. The performance tests of the present invention, such as infrared spectroscopy, nuclear magnetic resonance analysis, X-ray diffraction analysis, environmental scanning electron microscopy analysis, and the like, are performed according to conventional procedures known to those skilled in the art.
The abbreviations referred to in the present invention have the following meanings:
example 1 preparation of modified polymeric alcohol of the invention
1. A reaction polymer solution was prepared. Firstly, weighing polyvinyl alcohol (PVA 1788), stirring and dissolving in a certain amount of deionized water; the addition of the designed amount of pH-7 was continued while the corresponding amount of deionized water was replenished to ensure that the total mass concentration of the reacting polymer was maintained: the total mass concentration of the polyvinyl alcohol is 2 percent, and the PH-7 mass concentration is 0.02 percent; the pH value of the reaction solution was controlled to 7 throughout the process.
2. Ammonium persulfate and sodium hydrogen sulfite (mass ratio 2). Transferring the prepared reaction solution into a reaction beaker, introducing nitrogen to remove dissolved oxygen, and then putting the reaction beaker into a water bath at 60 ℃ for reaction.
3. And (3) keeping the temperature at 60 ℃, continuously heating and stirring at a constant speed of 500r/min to carry out polymerization reaction, and stopping the reaction after 45min to obtain the solution of the modified polyalcohol PH-VA of the invention.
The reaction principle is as follows:
the successful synthesis of the PH-VA polymer is confirmed by infrared spectrum analysis and nuclear magnetic resonance analysis.
Example 2 preparation of modified polymeric alcohol composite materials of the invention
The solution obtained in example 1 was mixed with methylcellulose CM-1 (final concentration: 0.5 ‰), cellulose hydroxyalkyl ether AC-1 (final concentration: 0.5 ‰) and nano-silica (final concentration: 0.1%), and mixed to obtain a modified polyalcohol composite solution of the present invention.
Example 3 preparation of the rinse solution of the invention
DFD-1 (final concentration 0.3 ‰), DU-907 (final concentration 0.2%) and potassium chloride (final concentration 0.8%) were added to the solution obtained in example 2, and mixed well to obtain the final product.
The beneficial effects of the present invention are demonstrated by the following experimental examples.
The test method related by the invention comprises the following steps:
1. rheological Property test
1.1 funnel viscosity
The test adopts a ZLN-1A Su's funnel viscometer, the diameter of the upper opening of a conical funnel is 150mm, the upper part of the conical funnel is provided with a filter screen with the specification of 1.25mm and used for removing redundant impurities and coarse particles in the washing liquid to be tested, the volume of the funnel at the lower part of the filter screen is 700 +/-15 ml, the length of a diversion pipe is 100mm, and the diameter of a pipe opening is 5mm. After checking with distilled water according to the protocol, the measuring cup was placed under the draft tube, and the time required for the flushing liquid to fill the 500ml portion of the measuring cup from the funnel was measured and recorded as the funnel viscosity in seconds.
1.2 rotational viscosity
As the viscosity value of the flushing liquid at a certain fixed shear rate cannot be measured by the viscosity of the funnel, and the reason of viscosity change cannot be judged, in order to measure the rheological property of the flushing liquid in the shear rate range of the annular space, a ZNN-D6 type six-speed rotational viscometer shown in figure 2-1 is adopted to measure rheological parameters, and the main technical parameters of the instrument are shown in a table 2. The viscometer mainly comprises an inner barrel, an outer barrel, a spring assembly and a dial assembly, wherein during measurement, as the flushing liquid has viscosity and acts with the outer barrel rotating at a constant speed, the inner barrel rotates for a certain angle, the size of the rotating angle is in direct proportion to the viscosity of the slurry, and the viscosity value of the slurry can be calculated by measuring the rotating angle of the inner barrel.
TABLE 2 Main technical parameters of six-speed rotational viscometer
Refer to GB/T29170-2012 laboratory test Specification for Petroleum and Natural gas Industrial flushing fluid test. Finally, the experimental data are calculated according to the specification of American Petroleum Institute (API) to obtain rheological parameters such as apparent viscosity, plastic viscosity, dynamic shear force and the like of the measured flushing fluid.
2. Fluid loss performance test
The flush fluid loss was measured using an API fluid loss tester as shown in FIGS. 2-2, with reference to the test methods specified in the American Petroleum institute Standard (API). The percolation area of the instrument is 45.8cm at room temperature 2 The percolation pressure difference is controlled at 6.89MPa.
3. Collapse resistance test
The collapse prevention inhibition performance of the washing liquid is particularly important when the rope core-taking directional drilling well wall is unstable and even collapses, and both the linear expansion experiment and the rolling recovery experiment can be used for evaluating the capability of the slurry for inhibiting the shale hydration and can be used as a reference for regulating and controlling the collapse prevention performance of the washing liquid. The specific test method refers to a standard SY-T5613-2000 shale physical and chemical property test method.
4. Environmental protection Performance test
4.1 biotoxicity assay
The biological toxicity of the sample is evaluated by summarizing the reaction change condition and the reaction rule of the organism under the conditions of different concentrations according to GB/T15441-1994 ' method for measuring acute toxicity of water quality's luminous bacteria '. Common reactions that organisms exhibit are: lethal dose/concentration (LD/LC); effect Concentration (EC).
4.2 biodegradability test
By investigating and evaluating biodegradability of drilling industry, BOD is often adopted 5 /COD Cr The higher the ratio, the better the biodegradability of the material. BOD 5 Represents the five-day Biochemical Oxygen Demand (BOD) of water according to HJ 505-2009 5 ) The measurement dilution and inoculation method of (1); and COD Cr For the chemical oxygen demand, the test is carried out by referring to HJ 828-2017, dichromate determination method for water quality chemical oxygen demand and GB 31571-2015, discharge Standard for pollutants in petrochemical industry.
4.3 chemical toxicity test
The contents of total chromium (Cr), total mercury (Hg), total lead (Pb), total arsenic (As) and total cadmium (Cd) in a sample solution are detected by referring to HJ 786-2016 (flame atomic absorption spectrophotometry for determining lead, zinc and cadmium in solid wastes), HJ 680-2013 (microwave digestion/atomic fluorescence method for determining mercury, arsenic, selenium, bismuth and antimony in soil and sediments) and HJ749-2015 (flame atomic absorption spectrophotometry for determining total chromium in solid wastes).
Wherein, the lead and cadmium selective atomic absorption spectrophotometer adopts a spectrophotometry method to detect; the mercury and arsenic are detected by an atomic fluorescence spectrophotometer by adopting an atomic fluorescence photometry method; chromium was detected by diphenylcarbazide colorimetry (yoga, 2019).
Experimental example 1 preparation of modified Polymer alcohol of the present invention screening test
1. Polymeric alcohol type screening
The polymeric alcohol includes various types of polyhydric alcohols such as polyethylene glycol, polyglycerol, ethylene glycol/glycerol copolymer, etc. In order to select the polymer alcohol types with excellent performance and economic applicability, different types of polymer alcohol types (PEG, PPG, POL, PEO and PVA) with molecular weight and polymerization degree which can be cold-dissolved at normal temperature are comprehensively selected. As the performance of the polymeric alcohol under the same concentration is too large, the final result is unreliable through direct comparison, the funnel viscosity measured by the Su funnel viscometer is used as a first evaluation index, the numerical result is controlled between 18s and 20s to determine the addition of the polymeric alcohol and prepare the solution, the solution is stood for 2 hours at room temperature, and then rheological parameter tests are carried out by adopting a ZNN-D6 type six-speed rotary viscometer, and the specific test data are shown in Table 3.
The data in the analysis table show that the rheological properties of different types of polymeric alcohols are obviously different, and the polymeric alcohols are pseudoplastic fluids close to Newton in a certain concentration, wherein the performances of PEG, PEO and PVA are relatively better. The viscosity of PEG increases along with the increase of molecular weight, the dynamic-plastic ratio is higher, the shear dilutability is better, but the funnel viscosity is approximately equivalent to that of PVA with the concentration of 1% when the concentration of PEG-2000 is 5%, and the addition of materials is overlarge. The PEO has considerable viscosity when the addition amount is small and the viscosity is 0.05 percent, but the PEO has unstable performance due to overlarge molecular weight, the rod climbing phenomenon in the test process is obvious, and the material preparation and the test are difficult. PVA has smaller performance difference under the same polymerization degree, and although PVA-1799 has better dynamic shear performance, the alcoholysis degree is high, so that the water solubility is poor, and the test consumes longer time. Therefore, PVA-1788 which has smaller alcoholysis degree and is easier to dissolve in water is selected as a modification research object in comprehensive contrast.
TABLE 3 rheological Properties of different types of polymeric alcohols
* FV in the Table: funnel viscosity(s), AV: apparent viscosity, PV: plastic viscosity, YP: dynamic shear force, τ 0 /μ p : dynamic-plastic ratio, n: the power law model fluidity index, the same below.
2. Polymer alcohol addition optimization
The early-stage test finds that the rheological properties of polyvinyl alcohols with different polymerization degrees and alcoholysis degrees have certain differences, so that the differences of fluid rheological modes and rheological properties of polyvinyl alcohols with different types under different addition amounts are analyzed through experimental research, and the optimal addition amount range is determined. Since the aqueous PVA solution is an aqueous polymer solution and a pseudoplastic fluid, it is usually studied by a power law fluid model, the rheological parameter values are shown in table 4, and the trend of the related parameters is shown in fig. 1.
TABLE 4 rheological Properties of polyvinyl alcohol (PVA)
* In the table, K: the coefficient of consistency.
As can be seen from the analysis of the data in the table, the viscosity of the polyvinyl alcohol solution continuously increases with the addition amount; under the condition of equal addition, the higher the polymerization degree of the polyvinyl alcohol is, the higher the viscosity is, wherein, the plastic viscosity of the PVA-2488 is about 10 times of that of the PVA-0588 model at 4 percent of addition, and the funnel viscosity changes rapidly and reaches 86s at the maximum at 5 percent of addition. In addition, the dynamic shear force is increased to a certain extent under the condition of small addition change, but after the viscosity is increased by more than 3%, the viscosity increasing speed is obviously accelerated, the dynamic shear force is gradually reduced, and the general trend of increasing first and then reducing is presented.
As can be seen from the comprehensive comparison of the three types of polymeric alcohols in FIG. 1 (a), the PVA-0588 has little viscosity change with the increase of the addition amount, and the plastic viscosity is only 3.8 mPas at the addition amount of 5 percent; when the addition of the 2488 type polyvinyl alcohol is higher than 3%, the viscosity is rapidly increased and the dynamic shear force is reduced due to overhigh polymerization degree, so that the reduction amplitude of the dynamic-plastic ratio is accelerated; compared with PVA-1788, the viscosity is proper, the dynamic shear force is better under the addition of 2% -3%, and the dynamic-plastic ratio is reduced after exceeding 3%, but the performance is the most stable.
The viscosity of the aqueous solution of PVA-1788 at different addition levels was analyzed by the power law model fluidity index n value and the consistency coefficient K value, see FIG. 1 (b). It can be seen that, in the process that the addition of the polyvinyl alcohol is increased to 5% by a concentration gradient of 1%, the molecular structure and association behavior of the polyvinyl alcohol are changed under the influence of the shear rate, the flow pattern index n value of the polyvinyl alcohol is gradually close to 1, certain pseudoplasticity is shown, the characteristics of the near-Newtonian fluid are realized, and the structural discontinuity is increased. The overall trend of the K value is higher, and the maximum value of 0.037 appears at 2% addition. Therefore, for the convenience of subsequent modification, 2% PVA-1788 was selected for rheological property studies (hereinafter, PVA refers to PVA-1788 unless otherwise specified).
3. Preference of modified Polymer
The test was carried out using the product of the zwitterionic synthesis by copolymerization (AM-1, AM-2, DMSA). AM-1 and AM-2 are both formed by copolymerization of anionic monomers AMPS and cationic monomers, and DMSA is an amphoteric hybrid polymer obtained by quaternization. In addition, multi-combination alcohol polymers (HB-1, HB-2, HAP) and polyacrylamide derivatives (PH-7, PH, PDA) in the same system as the polyalcohol were selected for the test.
In a solution with the addition of 2% of PVA-1788, the modified polymer is mixed with the PVA solution according to the molecular weight and the concentration of 0.2 per mill, and tests are carried out to compare the change of performance parameters such as viscosity, dynamic shear force and the like, so that a high molecular polymer capable of effectively improving the rheological property of the polyvinyl alcohol is preferred. The specific test protocol and data are shown in Table 5, and the results are analyzed and compared in FIG. 2.
TABLE 5 influence of high molecular weight polymers on the rheological Properties of PVA-1788
The analysis of the combined chart shows that:
(1) The addition of the polymer can obviously improve the system viscosity, the influence of the zwitterionic polymer on the solution viscosity under the same concentration is smaller, compared with PVA, the solution dynamic shear force and the dynamic-plastic ratio are reduced except AM-1, and AM-2 causes the dynamic shear force to be only 0.255Pa.
(2) The multi-combination alcohol polymer and PVA can effectively form a micelle structure, and the dynamic shear force of the system is obviously increased, the effect is better after HB-2 is compounded, and the dynamic shear force can reach 2.044Pa. However, the hydrogen bonding effect and the hydrophobic association effect of the polymer are enhanced, the viscosity is increased, so the dynamic-plastic ratio influence is a negative effect, the performance of the system is reduced more obviously after the HAP is added, the viscosity of the funnel can reach 59.4s, the plastic viscosity is 39 mPa.s, the dynamic shear force is only 1.022Pa, and the rod climbing phenomenon in the test is also more remarkable. In comparison, HB-2 has better rheological property improvement on PVA, but due to the existence of a large number of hydrophobic groups, the water solubility of the polymer solution in the test process is poor, and the polymer solution needs longer time to be completely dissolved.
(3) The viscosity of the PVA solution is obviously improved by the polyacrylamide derivative, the plastic viscosity is in the range of 12-25 mPa.s, and simultaneously, the dynamic shear force is effectively increased to 2.3Pa after the polyacrylamide derivative is added into the solution, because the derivative simultaneously has a strong polar hydration group-COO - ，-NH 2 Meanwhile, a net structure can be formed through hydrogen bond action, and the influence of molecular structure is larger due to the intermolecular action under small addition, so that the dynamic-plastic ratio is weaker than the negative effect. Therefore, by combining the above analysis, PH-7 is finally selected for subsequent modification research.
4. Copolymerization parameter screening
After the polymerization process, the initiator system and the like are screened and confirmed, on the basis, in the conditions that the total mass concentration of polyvinyl alcohol is 2%, the mass ratio of initiators, namely ammonium persulfate (KPS) and sodium bisulfite (mass ratio is 2.
TABLE 6 PH-7 proportioning design and rheological Property test data
According to the experimental results, the following results are obtained: the solution viscosity value is continuously increased along with the gradual increase of the PH-7 addition, a positive viscosity effect is generated, and the dynamic shear force of the solution with the PH-7 addition of 0.04% reaches a peak value of 3.27Pa.
However, when the pH-7 ratio is increased from 0.02% to 0.03%, the dynamic shear force is rapidly reduced from 2.45Pa to 1.99Pa after being greatly increased, and when the pH-7 is at a higher concentration (0.04%), the viscosity increase is remarkably accelerated, and the growth rates of the funnel viscosity and the plastic viscosity are 32.9% and 29.5% respectively. However, too high a viscosity is not favorable for subsequent studies of the rinse solution system. Therefore, the amount of pH-7 should not exceed 0.02%.
In addition, in order to examine the influence of the amount of the initiator system on the synthesis of the polymer, the amount of the initiator KPS was adjusted to 0.5%, 1%, 1.5%, 2% of the total mass of the reaction polymer, and rheological parameters such as apparent viscosity of the polymer were evaluated, and the test results are shown in Table 7.
TABLE 7 initiator proportioning design and rheological Properties test data
As can be seen from the data in the table, the viscosity of the polymer solution is always reduced along with the increase of the mass concentration of the initiator, when the addition amount of the initiator KPS is higher (1.5 percent), the free radicals of a reaction system are increased, the molecular weight of the synthesized polymer is high, and a chain segment interpenetrating network is formed, so the dynamic shear force can reach 2.56Pa, and the dynamic plastic ratio is 0.32; when the concentration of the initiator is higher, the chain growth radical reaction is gradually weakened, the chain termination speed is accelerated, the free radical activity disappears to form stable polymer molecules, the molecular weight is difficult to increase again, and the optimal addition of the initiator KPS is determined to be 1.5 percent of the total mass of the polymer by comprehensive consideration.
In conclusion, the optimal synthesis conditions for the PH-VA of the polymerization product are determined as follows: initiator (NH) at a reaction polymer PVA addition of 2% and pH-7 of 0.02% 4 ) 2 S 2 O 8 (KPS) with NaHSO 3 The mass ratio of 2, 1 kps added was 1.5% of the total mass of the polymer, the polymerization temperature was 60 ℃, the pH of the reaction solution was 7, and the duration of the polymerization reaction was 45min, the synthesized polymerization product (example 1) had good rheological properties.
Experimental example 2 preparation screening test of modified Polyol composite Material of the present invention
Through the research of the experimental example 1, the modified polymerization product PH-PA has good rheological property, and the rheological parameters such as viscosity, dynamic shear force and the like are greatly improved compared with the original polymer alcohol, and compared with clear water and emulsion, the product is applied to a flushing fluid system and can have better comprehensive effects of carrying rocks, lubricating and protecting walls. However, since formation fluid is in contact with the wall of the rock formation for a long time in horizontal directional drilling, most of the layers contain a certain amount of clay minerals such as montmorillonite, kaolinite, illite or a mixture thereof, the polymer may interact with the formation to cause certain damage, and the lack of solid-phase particles causes weak performance of system-stable clay, which easily causes collapse of the upper hole wall, so that the collapse resistance of the system-stable clay is still to be further improved.
1. Optimization and proportioning of associative polymer-cellulose polymer
In consideration of the applicability of PH-VA and the performance requirements of materials, polymers with the characteristics of no toxicity, easy dissolution and better stability of methylcellulose (CM-1), ethylcellulose (HC-7) and cellulose hydroxyalkyl ether (AC-1) are selected for rheological property and inhibition performance test research. Specific test data and results are shown in table 8 and fig. 3.
TABLE 8 variation of copolymerization Properties of different types of cellulose polymers
Through the tests and analysis, the common cellulose polymer material can effectively improve the rheological property of the original basic solution, and the value of the fluidity index of the solution floats about 0.65-0.85 after the three materials are added, so that the material has the characteristics of pseudoplastic fluid and the rheological property is obviously improved; but may also have some negative impact on the inhibiting properties of the composite solution. As can be seen from an analysis of fig. 3 and table 8:
(1) The viscosity of the solution system is continuously increased along with the increase of the addition amount, the dynamic shear force is also greatly increased, wherein the AC-1 viscosity value and the variation amplitude are higher than those of other two materials, and the plastic viscosity and the dynamic shear force value are respectively maximum under the addition amount of 2 per thousand, and are respectively 25.5mPa & s and 10.22Pa.
(2) The dynamic plastic ratio of the system is increased after the CM-1 and the AC-1 are added, the linear expansion rate is continuously reduced within 16h, as shown in figure 3 (b), the inhibition performance is improved, but when the addition amount is small, namely from 0.5 per thousand to 1 per thousand, the inhibition performance is weakened to a certain extent compared with the original solution; when the addition is increased to more than 1.5 per mill, the system inhibition performance is gradually enhanced, the rheological property is better, but the increase trend of the plastic viscosity is remarkably accelerated, and the CM-1 dynamic-plastic ratio is reduced after reaching the peak value of 0.33, so that the pressure control in a shaft is not facilitated, and the circulation of flushing liquid is influenced. Therefore, the proper adding amount range of CM-1 is not more than 0.15%, and the proper adding amount range of AC-1 is 0.1% -0.15%.
(3) The effect is gradually reflected when the addition of HC-7 is more than 1 per thousand, the viscosity change amplitude is small, the dynamic shear force increase amplitude is slow, and the dynamic-plastic ratio is continuously increased, so the shear dilution performance is relatively more stable. But the linear expansion rate is 18.56% when 0.5% of the addition amount, has a larger difference with 14.92% of the original solution, and the inhibition performance is obviously reduced along with the increase of the addition amount, and reaches 33.26% of the peak value when 2% of the addition amount reaches, so the linear expansion rate is eliminated.
2. Compounding ratio of cellulose polymer
The CM-1 and the AC-1 screened in the previous test can obviously improve the PH-VA performance of the modified polymerization product, but because both are cellulose polymers, the viscosity change amplitude is large under small addition, the subsequent performance regulation and control of a flushing fluid system are not facilitated, and in comparison, the improvement of the rheological performance of the CM-1 is more prominent, and the improvement of the AC-1 performance is mainly reflected in inhibition, so that the CM-1 and the AC-1 are compounded according to a certain proportion on the basis of trying to optimally mix the two materials so as to play the synergistic effect of the materials, and the rheological performance and the inhibition performance can be effectively improved under small addition.
In order to avoid excessive increase of viscosity of a solution system after compounding, the test determines that the addition of the AC-1 is 0.5 per mill and 1 per mill better, the CM-1 is increased from 0.3 per mill to 0.9 per mill by 0.2 per mill gradient, and the optimal proportion of the AC-1 and the CM-1 is determined by comparing test data. The specific experimental design and data are shown in Table 9, and the performance trend is shown in FIG. 4.
TABLE 9 variation of compounding Properties of cellulose polymers
The analysis of the test results by combining the graphs can show that:
(1) The plastic viscosity of the system is 16 mPa.s after the AC-1 addition is 0.5 thousandth and the CM-1 addition is 0.3 thousandth, the viscosity can reach the viscosity when the single addition of the two materials is 1 thousandth, and is twice of the PH-VA viscosity value, which indicates that the viscosity of the system can be better improved by small addition after the two materials are matched. When the addition concentration of CM-1 is less than 0.5 per thousand, the viscosity of the solution is increased slightly, and the dynamic shear force is increased rapidly to 5.62Pa at the peak value, because the intermolecular action of CM-1 and AC-1 is enhanced along with the increase of the concentration, a micelle network structure is gradually formed, and can be used for adsorbing and wrapping clay particles under the synergistic action of PH-VA, and the linear expansion rate of the system is reduced to 13.95 percent at the lowest; meanwhile, when the concentration is increased, the association effect is easier to repair after being damaged by shearing, and the fact that the fluidity index is reduced to 0.67 can also be verified, which indicates that a strong association structure is formed among polymers and the shear thinning property is better.
However, when the addition of CM-1 is more than 0.5 per mill, the viscosity of the system is rapidly increased, the dynamic shear force is greatly reduced, and the inhibition performance is weakened, when the addition is 0.9 per mill, the dynamic shear force is only 4.09Pa, the linear expansion rate is increased to 15.14 percent, and the pH-VA is exceeded. The possible reason is that as the concentration of CM-1 increases and exceeds AC-1, the intermolecular association effect does not change any more, the CM-1 molecular chains gradually gather to carry out intramolecular association, and a dynamic network structure formed under low concentration has certain defects, which shows that the system performance is weakened. That is, when the addition of AC-1 is 0.5%, the addition of CM-1 should not exceed 0.5%.
(2) The addition of AC-1 is 1 per mill, and the viscosity of the system is always greater than 0.5 per mill of the addition of the same CM-1 concentration. With the increase of the concentration of CM-1, the viscosity of the polymer composite solution is continuously increased, the funnel viscosity can reach 58.7s under the concentration of 0.9 per mill, and the plastic viscosity is 23 mPa.s, so that the resistance of a solution system under the shearing action is large, and the water power of a drill bit in the drilling process is not fully utilized. In addition, the dynamic shear force of the system is obviously increased, 5.62Pa is achieved under the condition that the addition amount of 0.7 per thousand, and the addition amount of CM-1 is increased compared with that of an AC-1 system with lower concentration, because the hydrophobic association effect of AC-1 is greater than that of CM-1, and relatively stronger action forms such as electrostatic action, hydrogen bond action and the like exist, CM-1 can begin intermolecular association only when reaching higher concentration, and the viscosity of the system is increased greatly.
Meanwhile, the linear expansion rate of the system is reduced from 14.52% to 12.80%, and the inhibition performance is improved well because the number of AC-1 hydrophobic groups is relatively more, the steric hindrance is small, the intermolecular association is easier, and the inhibition performance is consistent with the stronger inhibition performance shown by independently adding the AC-1 into the PH-VA.
(3) By comparing the performance difference of the PH-VA composite solution with the CM-1 under two different addition amounts of AC-1, the performance of 0.5 thousandth of the CM-1 addition amount is the best when the AC-1 addition amount is 0.5 thousandth; when the addition of the AC-1 is 1 per mill, the CM-1 reaches the peak value at the dynamic shear force of 0.7 per mill, the inhibition performance is also greatly reduced, the linear expansion rate is 13.64 percent and is superior to the random gradient inhibition performance under the other concentration of the AC-1, but the viscosity is overhigh, the fluidity index is over 0.7, the viscosity of the system is strong under the high shear rate, and the resistance is large; low shear rates are not conducive to suspending and carrying debris. Therefore, the optimal performance improvement of the PH-VA solution system is realized when the addition of the CM-1 and the AC-1 is 0.5 per mill in comprehensive consideration.
3. Nano material kind and proportion
Through carrying out the investigation analysis to commonly used nano-material, combine to use convenient degree, with high costs low and in the flush fluid application feasibility three-aspect, the mainly selected and used nano-particle material has: nano silicon dioxide (SiO) 2 ) Nano aluminium oxide (Al) 2 O 3 ) And nano titanium dioxide (TiO) 2 )。
In order to investigate the influence of the nano material on the rheological and inhibiting properties of the polymerization solution under different addition amounts, a scheme is designed and a performance test is carried out, and the results are shown in table 10 and fig. 5.
TABLE 10 different high-activity nanoparticle experimental study data
The data in the analysis table show that the three different types of nano materials can reduce the linear expansion rate of the system to a certain extent, have stable shale and can effectively improve the inhibition performance, but meanwhile, the rheological parameter value of the system is reduced to some extent, and the performance of the system is greatly influenced along with the increase of the addition amount.
In connection with the trend of variation in fig. 5, it can be found that:
(1) Random nano SiO 2 The viscosity of the system was increased as a whole with the increase of the amount added, and the viscosity reached a peak value of 19.7 mPas at 0.5%, but the dynamic shear of the solution tended to decrease, while the viscosity was 15.8 mPas, which was closest to the original polymerization solution, at 0.1% addition, and the dynamic shear was 5.47Pa at the maximum. BodyThe system dynamic plastic ratio is obviously increased firstly and then decreased, and the nano SiO is added in a small amount (0.1 percent) 2 The nano material is easy to uniformly bridge to an original solution structure through the particle size advantage, and can adsorb the shale clay surface due to large specific surface area and high surface energy, the dynamic-plastic ratio value reaches the best 0.35, and the linear expansion rate is remarkably reduced to 9.86%; and the nano SiO is added in an amount of more than 0.1 percent 2 Is easy to self-agglomerate, so that various properties of the solution system are reduced.
(2) Nano Al 2 O 3 After the solution of the original system is added, the viscosity and the dynamic shear force are reduced, and the nano TiO 2 The viscosity of the original system is improved to a certain extent, but the rheological property data of the original system shows a certain reduction trend along with the increase of the addition of the nano material; however, the linear expansion rate value is continuously reduced, and the interaction positions of water molecules and surfaces of shale clay and the like are inevitably reduced due to the adsorption of the nano material, so that the shale hydration can be effectively inhibited. In contrast, nano TiO 2 Has better performance, but is combined with nano SiO 2 Compared with the prior art, the viscosity is higher, the rock debris circulation is not facilitated, and the shear thinning characteristic is weaker. Therefore, the above test analysis is combined, and the nano SiO is selected 2 As a component of the anti-collapse rinse solution system, the optimum addition amount was 0.1%, and a PH-VA/associated nano-copolymer composite material having excellent properties was formed (example 2).
Experimental example 3 component screening and formulation optimization of the rinse solution of the present invention
Basic researches of experimental examples 1 and 2 find that the rheological and inhibiting properties of the modified polyalcohol and the nano copolymerization composite material reach the expected improvement effect, and the environmental protection indexes of the applied materials reach the international standard, but the basic performance indexes of the flushing fluid still have some defects. Such as: the surface activity of the polyalcohol is high, and a large amount of bubbles are easy to appear when the system is stirred at high speed; and the solution viscosity is higher, but the filtration loss is slightly larger. In order to improve the above-mentioned disadvantages, a treating agent may be further added. Based on the analysis of the performance defects of the association copolymerization composite material, the selected treating agents are mainly a filtrate reducer, an inhibitor and a defoaming agent.
The conventional fluid loss additives selected for testing are cellulosics (CMC, PAC), starches (CMS, HPS, DFD), polymers (HPAN, KHPAN, 80A-51), resins (SPNH, SLSP, SMP); the defoaming agent comprises organosilicon (DU-478, DU-907 and DU-908) and self-emulsifying (B-780 and B-5738); the anti-collapse inhibitor is mainly inorganic salts (KCl and NaCl) and paraffin (BSL 7), and the results of biodegradability and toxicity analysis show that the starch fluid loss additive and the organic silicon defoamer are both easy to degrade, have lower chemical toxicity and better environmental protection performance compared with other types, so the anti-collapse inhibitor can be roughly determined as the preferred material type of the subsequent treatment agent.
1. Preference is given to filtrate reducers
Common HPAN, CMS, 80A-51 and DFD-1 with better environmental protection performance are selected to develop a filtration loss experiment, and the API water loss of the system under different dosage conditions is measured. The specific test data are shown in Table 11, and the performance trend is shown in FIG. 6.
TABLE 11 fluid loss additive combination Performance results
Analysis of the data of the test chart shows that the selected material reduces the filtration loss of the API of the composite material, but the effect is different, and besides, the rheological property of the system also changes to a certain extent correspondingly.
(1) The filtration loss after adding both HPAN and 80A-51 is reduced and increased, and the effect of HPAN is better than that of 80A-51 at lower adding amount. When the addition of 80A-51 is 0.3%, the filtration loss is the lowest 31ml, which is not only larger than the filtration loss of the HPAN system with the same addition, but also exceeds the minimum 26ml of the filtration loss of 0.3 per thousand HPAN. Meanwhile, the selected HPAN has low relative molecular mass, the change amplitude of the solution viscosity after the HPAN is added is far less than 80A-51, the dynamic shear force is relatively stable, and the adverse effect on the rheological property of the system is less.
(2) After CMS and DFD-1 are added, the filtrate loss reduction performance is improved more obviously, the total filtrate loss is continuously reduced along with the increase of the addition, and the influence on the rheological property of the system is little; the filtration loss of the DFD-1 system with 0.2 per mill addition is the lowest, 18ml, and the dynamic plastic ratio of the system is improved to 0.38. Because the DFD-1 is a spiral structure different from a linear polymer chain material, has higher relative molecular weight, contains a large amount of hydroxyl and ether bonds, forms a grid structure by hydrogen bond adsorption, improves the viscosity of free water in the flushing fluid and reduces the percolation effect, and the filter loss can be greatly reduced after the flushing fluid is added.
In conclusion, DFD-1 is finally determined as a fluid loss additive, and the addition amount of the DFD-1 is not more than 0.3 per thousand in order to reduce the influence on the rheological property of a system.
2. The antifoam is preferably
Therefore, the environmental protection type defoaming agents such as common organic silicon (DU-478, DU-907) and self-emulsifying (B-780) are selected for testing, the density recovery rate of the solution is tested by referring to the evaluation program of defoaming agent for SY-T5560-92 flushing fluid to evaluate the performance of the defoaming agent, and the test results are shown in Table 12 and figure 7.
TABLE 12 defoamer compounding performance results
Through analyzing data in the table, the defoaming agent has a certain effect on the system, and bubbles generated by stirring after the washing liquid sample is prepared are obviously reduced.
As can be seen from the comparison of the trend change of the density recovery rates of the three antifoaming agents in fig. 7, the density recovery rate of the system increases along with the increase of the addition of the antifoaming agent DU-478, the increase amplitude is remarkably increased when the concentration is greater than 0.2%, and the recovery rate reaches the peak value of 80.65% when the addition of the antifoaming agent is 0.4%; the recovery rate after the addition of B-780 also shows a continuously increasing trend, but the lifting amplitude is smaller, and the maximum value of the recovery rate under the same addition is only 74.29 percent. The performance of the antifoaming agent DU-907 is the most excellent, the recovery rate can reach 75.68% at the minimum concentration of 0.1%, which is far more than the test value of the same concentration of the other two materials, and in addition, as the addition of the DU-907 is increased, the recovery rate of the flushing liquid density is increased firstly and then reduced, and the peak value reaches 91.43% at the concentration of 0.2%. Thus, the three defoamers rank their effectiveness from superior to inferior: DU-907 >.
By combining the test analysis, DU-907 serving as a defoaming agent is screened out, and the effect is optimal when the addition amount is 0.2%.
3. The anti-collapse agent is preferably
Referring to the related research of researchers at home and abroad, the anti-collapse plugging agent KCl, naCl and emulsified paraffin (BSL 7) within the recommended dosage range are respectively added into the system solution, the inhibition performance test is carried out by adopting the linear expansion rate and core recovery rate tests, and the test results are shown in the table 13 and the figure 8.
TABLE 13 results of anti-collapse inhibitor compounding performance
From the graph, it can be seen that:
(1) KCl can remarkably improve the inhibition performance of a polyalcohol solution system, when the addition amount is only 1%, the reduction rate of the linear expansion rate is 25.6%, and the shale recovery rate is more prominent than that of other materials under the same addition amount and is similar to the test value of 4% NaCl and 2% BSL7 concentration. Along with the increase of the addition of KCl, the linear expansion rate of the system is greatly reduced, the recovery rate of the core is gradually increased, when the addition is 3%, the expansion rate of the system is 5.23% at the lowest, and the recovery rate is 88.9% at the highest. The KCl and the polymeric alcohol system have good synergistic effect.
(2) With the increase of NaCl concentration, the anti-collapse inhibition effect of the system is enhanced. The NaCl concentration is less than or equal to 6 percent, the expansion rate is increased by the NaCl concentration, and the recovery rate is not greatly improved; however, when the NaCl concentration is increased from 6% to 8%, the recovery rate is increased rapidly. NaCl plays a main inhibiting role under small addition, and the linear expansion rate is obviously reduced along with the increase of NaCl concentration.
(3) The system inhibition performance is improved to a certain extent after the BSL7 is added; however, under the same 1% concentration addition, the core recovery rate is only 63.2%, and the effect is not obvious enough compared with KCl.
The comprehensive test result shows that the anti-collapse inhibition performance of the system can be greatly improved by adding less KCl, and the anti-collapse inhibition performance is better than that of BSL-7; the improvement of the inhibition performance after the NaCl is added is mainly reflected in large addition, but the increase of the concentration can adversely affect other performances and is not beneficial to the cost control of the system. Therefore, the finally preferred anti-collapse inhibitor is KCl, and the addition amount of the anti-collapse inhibitor can be controlled to be about 1% -2%.
4. Orthogonal tests confirm that the anti-collapse flushing fluid disclosed by the invention is optimized in formula
Based on the approximate addition range of the treating agent explored in the test process, a three-factor three-level orthogonal test is designed, and the influence primary and secondary sequences of different factors on the main performance indexes such as rheological performance, inhibition performance and fluid loss performance are determined, so that an orthogonal table L9 (3) is selected 4 ) And designing and combining 9 groups of tests on the main performance of the flushing system according to orthogonal tests. The orthogonality factor levels are shown in table 14 and the orthogonality test schedule is shown in table 15.
TABLE 14 orthogonal test factor horizon
Table 15 orthogonal experimental design table
Rinse solutions were formulated according to the above orthogonal test design and tested for relevant performance, with specific test results shown in table 16. The results were analyzed by the three-factor variance method to obtain visual data of mean and variance as shown in table 17. Wherein k represents the average value of a certain factor under multiple levels, R is the range of each factor level, and the data of the k and the R are combined to judge the optimal level of the factor and the primary and secondary sequences influencing the performance.
TABLE 16 orthogonal test data
TABLE 17 visual analysis chart of orthogonal test
The analysis shows that:
(1) The fluid loss agent, the anti-collapse inhibitor and the defoaming agent have obvious influence on the system performance, wherein the fluid loss agent enables the viscosity and the dynamic shear k value to show a descending trend overall, and the influence on the fluid loss and the linear expansion rate is stable when the fluid loss agent is at the second level and the third level; therefore, in order to control the overall viscosity of the system, the fluid loss additive is suitable for the third level, the dynamic shear value reaches 3.20Pa, the fluid loss is reduced to 37ml, and the linear expansion rate is 7.53 percent, so that the practical engineering application can be met.
(2) The influence degree of the defoaming agent on the performance index is observed, the influence on the plastic viscosity and the filtration loss is the largest among the three treating agents, the R value of the plastic viscosity reaches 1.87, and the viscosity of the system is continuously reduced along with the increase of the level; the filtration loss R value reaches 9.33, and the filtration loss is the lowest at the second level and is 33ml, and meanwhile, the dynamic shear force and the linear expansion rate performance are optimal; when the level increases with the increase in concentration, the defoaming agent is preferably selected to have a second level because the salt concentration destroys the molecular structure in the system, the dynamic shear force decreases, and the fluid loss and the expansion rate both rapidly increase.
(3) The anti-collapse inhibitor has greatly different influence trends on various performances of the system, and for the rheological performance, the inhibitor can ensure that the dynamic shear force of the system is maximized to 3.97Pa and the plastic viscosity is controlled to be lower than 14.8mPa & s at a first level; as the level is increased, the fluid loss of the system reaches a minimum of 34ml at a third level, but the linear expansion rate is increased compared with the first level, and the rheological property is also reduced. Therefore, the first level is most suitable for the comprehensive consideration of the anti-collapse inhibitor.
Through the analysis, the environment-friendly type of the rope coring modified polyalcohol can be finally obtainedThe optimized formula of the anti-collapse flushing fluid system is as follows: 0.5% o CM-1+ 0.5% o AC-1+0.1% SiO 2 + 0.3% DFD-1+0.2% DU-907+0.8% KCl (example 3) with a concentration of PH-VA of 2.02%.
Experimental example 4 Performance of flushing fluid of the present invention
1. Environmental protection performance of flushing fluid
In order to test the environmental hazard of the optimized formula of the flushing fluid system in example 3 and evaluate the indexes of biological toxicity, biological degradability, chemical toxicity and the like, the test data obtained by the inspection of example 3 are shown in tables 18-20.
Table 18 example 3 flush biotoxicity test data
TABLE 19 example 3 biodegradability in rinse solution test data
The biological toxicity EC50 of the system is more than the set discharge value, BOD 5 /COD Cr 0.088, easy biodegradation, standard heavy metal content and good compatibility of the whole system to the environment.
2. Rheological properties of flushing fluid
According to the design of an environment-friendly flushing fluid system, 1.1g/cm is prepared by referring to conventional test conditions 3 The rheological performance indexes of the flushing liquid of example 3 of the density, such as viscosity and the like before and after hot rolling for 16 hours at 80 ℃, are tested, the rheological properties of the flushing liquid are further discussed, and specific test data are shown in a table 21.
The data in the table show that the apparent viscosity of the flushing fluid is slightly different from that before and after aging, the apparent viscosity is 17.5-19 mPa.s, the plastic viscosity meets the performance requirement of the flushing fluid, the dynamic shear force is still maintained at 4.5Pa after aging, the dynamic-plastic ratio is 0.34, the rock carrying capacity is good, and the rheological property of the flushing fluid is not seriously influenced. The comprehensive rheological parameter data show that the rheological property of the flushing fluid in the example 3 is excellent.
Table 21 example 3 rheological testing data for rinse fluid systems
3. Fluid loss performance of flushing fluid
The fluid loss test was performed on the rinse fluid system before and after aging by hot rolling at 80 ℃ for 16h using an API fluid loss tester, and the test results are shown in table 22.
Table 22 example 3 fluid loss performance test data for rinse solution system
As can be seen from the table, the filtration loss of the system in example 3 is 24ml before hot rolling, and even reduced to 21ml after 16h at high temperature, which can meet the performance requirements of the water-based flushing fluid. This phenomenon occurs because the aging temperature is close to the cloud point of the polymeric alcohol in the system, and part of the polymeric alcohol molecules gradually separate out, so that the pores of the filter paper can be filled during the fluid loss test, and the plastic film formed by aggregation can form plugs in part of the area, so that the fluid loss is reduced. In addition, the density of the polymer alcohol plastic film in unit volume is less than that of water, and the mass of a filter cake is obviously reduced from 1.769g to 1.346g. In conclusion, the flushing fluid system in the embodiment 3 has excellent fluid loss reducing capacity and can better meet the requirements of core drilling construction.
4. Anti-collapse performance of flushing fluid
According to the inhibition performance test method, after the rock core sample and the shale debris are properly treated, the linear expansion and rock core recovery rate test is carried out. Wherein, the linear expansion experiment increases the expansion rate by 2h to evaluate the change of the inhibition performance of the flushing liquid along with the time; in the core recovery rate test, 50g of rock debris is taken and rolled at the constant temperature of 80 ℃ for 16h to measure the first recovery rate R 1 (ii) a Then baking in a 105 ℃ ovenBaking for 4h, standing to normal temperature, performing rolling test again, and recording the second recovery rate R of the core 2 (ii) a Then repeating the previous steps and recording the third recovery rate R of the rock core 3 3 replicates were prepared according to the optimized formulation and averaged, with the experimental data as in table 23.
Table 23 example 3 inhibition performance test data for rinse solution system
The data in the analysis table show that the linear expansion rate of the flushing liquid system in the embodiment 3 is 0.98% in 2h, the expansion amount in clear water is more than 10 times, the vertical expansion amount of the core is gradually reduced along with the time extension, the core change is small after the flushing liquid system is soaked in 16h, the expansion rate of the flushing liquid system in the embodiment 3 is stabilized at 6.43%, and the system has strong anti-collapse inhibition performance. In addition, by combining with the analysis of the rock core rolling recovery test data, the first rock debris recovery rate of the flushing fluid system can reach 89.31 percent, and meanwhile, the system can be observed to be uniformly attached and coated on the surface of rock debris, and the recovered rock debris is complete; the third recovery rate is 88.98%, which shows that the flushing liquid system can better maintain the stability of the well wall, has strong inhibition and has certain positive effect on preventing the occurrence of underground complex accidents.
In conclusion of the research, the modified polyalcohol environment-friendly anti-collapse flushing fluid system has good rheological property, high dynamic-plastic ratio and other parameters meeting the requirements, strong anti-collapse inhibition capability, certain high-temperature stability, good reservoir protection performance, no toxicity, easy degradation and excellent environmental protection performance, and is very suitable for being used as a drilling flushing fluid, especially a flushing fluid for rope coring directional drilling.
In conclusion, the invention provides a polymer copolymerized and modified by polyacrylamide derivatives and polyvinyl alcohol, which has excellent tackifying, shear-improving effect and rheological property, and has better comprehensive effects of carrying rocks, lubricating and protecting walls when being applied to a flushing fluid system; the polymer mixed with the hydrophobic cellulose polymer can synergistically enhance the stability of a polymer structure, and the mixed nano silicon dioxide can enhance the regularity of the polymer structure and enhance the rheological property of a solution. The anti-collapse inhibition performance can be improved by further adding a filtrate reducer, a defoaming agent and an anti-collapse inhibitor, the prepared flushing fluid has the advantages of good environmental protection performance, easy degradation, no pollution, moderate apparent viscosity, higher shearing force, small filtrate loss and stronger anti-collapse inhibition performance, can meet the construction requirements of site drilling, particularly rope core-taking directional drilling, and has popularization and application prospects.
Claims (10)
1. A modified polymeric alcohol, characterized in that it is polymerized from polyvinyl alcohol and pH-7; the PH-7 is partially hydrolyzed polyacrylamide with the hydrolysis degree of 35-50%.
2. The modified polymeric alcohol of claim 1, wherein the mass ratio of polyvinyl alcohol to PH-7 is 2 (0.01 to 0.02), preferably 2.
3. The modified polymeric alcohol of claim 1 or 2, wherein the polymerization is in an aqueous solution with the aid of an initiator; the using amount of the initiator is not less than 2.25 percent of the total mass of the polyvinyl alcohol and the PH-7; preferably, the initiator is ammonium persulfate and sodium bisulfite, and the mass ratio of the ammonium persulfate to the sodium bisulfite is 2.
4. A modified polyalcohol composite material which is characterized in that the modified polyalcohol as claimed in any one of claims 1 to 3 is compounded with cellulose polymer and nano silicon dioxide;
the mass ratio of the modified polyalcohol to the cellulose polymer to the nano-silica is (2.02) - (0.08-0.15) - (0.05-0.2), and preferably (2.02).
5. The modified polymeric alcohol composite of claim 4, wherein the cellulosic polymer is a mixture of methylcellulose and a cellulose hydroxyalkyl ether; the mass ratio of the methyl cellulose to the cellulose hydroxyalkyl ether is 1 (0.6-1), preferably 1.
6. Use of the modified polymeric alcohol according to any one of claims 1 to 3 or the modified polymeric alcohol composite according to claim 5 or 6 in drilling flushes.
7. A drilling fluid which is an aqueous solution containing the modified polymeric alcohol according to any one of claims 1 to 3 or the modified polymeric alcohol composite according to claim 5 or 6; preferably, the mass fraction of the modified polymeric alcohol in the aqueous solution is 2%, and the mass fraction of the modified polymeric alcohol composite material is 2.02%.
8. The drilling fluid of claim 7, further comprising the following components in mass fractions:
0.1-0.3 per mill of filtrate reducer, 0.15-0.25 percent of defoamer and 0.8-1.2 percent of anti-collapse inhibitor;
preferably: 0.3 per mill of filtrate reducer, 0.2 percent of defoamer and 0.8 percent of anti-collapse inhibitor.
9. The drilling flush fluid of claim 8, wherein the fluid loss additive is a starch-based compound, the anti-foaming agent is a silicone-based compound, and the collapse inhibitor is an inorganic salt-based compound.
10. The drilling flush of any one of claims 7 to 9, consisting of, in mass fraction:
2.02% of modified polymeric alcohol as defined in any one of claims 1 to 3, 0.5% o of methyl cellulose, 0.5% o of hydroxyalkyl cellulose ether, 0.1% of nano-silica, 0.3% o of modified pregelatinized starch DFD, 0.2% of silicone defoamer DU-907, 0.8% of potassium chloride, and the balance of water.
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