CN114702941A - Bionic polymer filtrate reducer for drilling fluid - Google Patents
Bionic polymer filtrate reducer for drilling fluid Download PDFInfo
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- CN114702941A CN114702941A CN202210209148.0A CN202210209148A CN114702941A CN 114702941 A CN114702941 A CN 114702941A CN 202210209148 A CN202210209148 A CN 202210209148A CN 114702941 A CN114702941 A CN 114702941A
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- lignin
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- fluid loss
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- 238000005553 drilling Methods 0.000 title claims abstract description 41
- 239000012530 fluid Substances 0.000 title claims abstract description 38
- 229920000642 polymer Polymers 0.000 title claims abstract description 26
- 239000000706 filtrate Substances 0.000 title claims abstract description 25
- 239000003638 chemical reducing agent Substances 0.000 title claims abstract description 20
- 239000011664 nicotinic acid Substances 0.000 title claims abstract description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 99
- 229920005610 lignin Polymers 0.000 claims abstract description 53
- 239000000654 additive Substances 0.000 claims abstract description 19
- UOULCEYHQNCFFH-UHFFFAOYSA-M sodium;hydroxymethanesulfonate Chemical compound [Na+].OCS([O-])(=O)=O UOULCEYHQNCFFH-UHFFFAOYSA-M 0.000 claims abstract description 18
- 239000002994 raw material Substances 0.000 claims abstract description 17
- 230000000996 additive effect Effects 0.000 claims abstract description 16
- 229920002873 Polyethylenimine Polymers 0.000 claims abstract description 14
- 239000002518 antifoaming agent Substances 0.000 claims abstract description 13
- 238000002360 preparation method Methods 0.000 claims abstract description 11
- YCIMNLLNPGFGHC-UHFFFAOYSA-N catechol Chemical group OC1=CC=CC=C1O YCIMNLLNPGFGHC-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000001914 filtration Methods 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 33
- 238000003756 stirring Methods 0.000 claims description 31
- 239000012153 distilled water Substances 0.000 claims description 22
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 18
- 238000010992 reflux Methods 0.000 claims description 15
- 238000006243 chemical reaction Methods 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 9
- 239000012279 sodium borohydride Substances 0.000 claims description 9
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- 238000002474 experimental method Methods 0.000 claims description 7
- 230000003592 biomimetic effect Effects 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 239000012467 final product Substances 0.000 claims description 5
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- 238000001035 drying Methods 0.000 claims description 3
- 230000001376 precipitating effect Effects 0.000 claims description 3
- 239000000725 suspension Substances 0.000 claims description 3
- 239000012065 filter cake Substances 0.000 abstract description 7
- 241000237536 Mytilus edulis Species 0.000 abstract description 2
- 230000003213 activating effect Effects 0.000 abstract description 2
- 235000020638 mussel Nutrition 0.000 abstract description 2
- 230000035699 permeability Effects 0.000 abstract description 2
- 108090000623 proteins and genes Proteins 0.000 abstract description 2
- 102000004169 proteins and genes Human genes 0.000 abstract description 2
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- 239000000243 solution Substances 0.000 description 55
- 239000000523 sample Substances 0.000 description 34
- 238000012360 testing method Methods 0.000 description 34
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 27
- 235000011121 sodium hydroxide Nutrition 0.000 description 24
- 239000002002 slurry Substances 0.000 description 23
- 230000032683 aging Effects 0.000 description 14
- 239000011780 sodium chloride Substances 0.000 description 13
- 238000000034 method Methods 0.000 description 12
- 241000894006 Bacteria Species 0.000 description 7
- 238000004020 luminiscence type Methods 0.000 description 7
- 239000000047 product Substances 0.000 description 7
- VJOUUGUSJOHNRQ-UHFFFAOYSA-N OC[Na] Chemical compound OC[Na] VJOUUGUSJOHNRQ-UHFFFAOYSA-N 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 150000003839 salts Chemical class 0.000 description 6
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 5
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 5
- 239000010428 baryte Substances 0.000 description 5
- 229910052601 baryte Inorganic materials 0.000 description 5
- 239000003814 drug Substances 0.000 description 5
- 239000011521 glass Substances 0.000 description 5
- 238000011085 pressure filtration Methods 0.000 description 5
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- 239000000853 adhesive Substances 0.000 description 4
- 230000001070 adhesive effect Effects 0.000 description 4
- 239000003077 lignite Substances 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
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- 241001411320 Eriogonum inflatum Species 0.000 description 3
- 102100021913 Sperm-associated antigen 8 Human genes 0.000 description 3
- 101710098579 Sperm-associated antigen 8 Proteins 0.000 description 3
- 239000010426 asphalt Substances 0.000 description 3
- 239000000440 bentonite Substances 0.000 description 3
- 229910000278 bentonite Inorganic materials 0.000 description 3
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 3
- 238000012937 correction Methods 0.000 description 3
- 238000009775 high-speed stirring Methods 0.000 description 3
- 238000012417 linear regression Methods 0.000 description 3
- 239000000314 lubricant Substances 0.000 description 3
- 229920001568 phenolic resin Polymers 0.000 description 3
- 239000005011 phenolic resin Substances 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 238000005096 rolling process Methods 0.000 description 3
- 239000012488 sample solution Substances 0.000 description 3
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 3
- -1 sulfomethyl phenolic resin Chemical compound 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000003708 ampul Substances 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
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- 239000012267 brine Substances 0.000 description 2
- 229910000281 calcium bentonite Inorganic materials 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
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- 229910001385 heavy metal Inorganic materials 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
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- 239000004033 plastic Substances 0.000 description 2
- 231100000614 poison Toxicity 0.000 description 2
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- 239000002131 composite material Substances 0.000 description 1
- 239000013068 control sample Substances 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
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- 238000006073 displacement reaction Methods 0.000 description 1
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- 239000003345 natural gas Substances 0.000 description 1
- 229920005615 natural polymer Polymers 0.000 description 1
- 231100000989 no adverse effect Toxicity 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000010979 pH adjustment Methods 0.000 description 1
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- 125000000542 sulfonic acid group Chemical group 0.000 description 1
- 229920001059 synthetic polymer Polymers 0.000 description 1
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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
- C09K8/02—Well-drilling compositions
- C09K8/03—Specific additives for general use in well-drilling compositions
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08H—DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
- C08H6/00—Macromolecular compounds derived from lignin, e.g. tannins, humic acids
-
- 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
- C09K8/02—Well-drilling compositions
- C09K8/04—Aqueous well-drilling compositions
- C09K8/14—Clay-containing compositions
- C09K8/18—Clay-containing compositions characterised by the organic compounds
- C09K8/20—Natural organic compounds or derivatives thereof, e.g. polysaccharides or lignin derivatives
- C09K8/203—Wood derivatives, e.g. lignosulfonate, tannin, tall oil, sulfite liquor
-
- 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
- C09K8/02—Well-drilling compositions
- C09K8/04—Aqueous well-drilling compositions
- C09K8/14—Clay-containing compositions
- C09K8/18—Clay-containing compositions characterised by the organic compounds
- C09K8/22—Synthetic organic compounds
- C09K8/24—Polymers
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Dispersion Chemistry (AREA)
- Wood Science & Technology (AREA)
- Biochemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a bionic polymer fluid loss additive for drilling fluid, which is prepared from the following raw materials in parts by weight: 400-500g of modified lignin, 260-300g of 20% NaOH solution, 400-800g of 60% sodium hydroxymethyl sulfonate solution, 180g of polyethylenimine and a small amount of antifoaming agent. In the preparation process of the filtrate reducer, the super-strong adhesion property of catechol groups in mussel byssus protein is utilized, and the filtrate reducer has the functions of plugging micropores and improving strength. The modified lignin with catechol groups is obtained by activating and modifying brown rot lignin, and can be further crosslinked in the drilling fluid by utilizing the stronger adhesion characteristic of the modified lignin underwater to form a gel membrane with stronger cohesion and adhesion, so that a filter cake formed by the drilling fluid is more compact, micropores are blocked, the toughness and strength of the filter cake are improved, and finally, the filter cake with low permeability, flexibility, thinness and compactness is formed, and the filtration loss of the drilling fluid is effectively reduced.
Description
Technical Field
The invention relates to the technical field of petroleum and natural gas drilling, in particular to a bionic polymer filtrate reducer for drilling fluid.
Background
With the rapid development of the petroleum industry, the difficulty of petroleum drilling is more and more high, the well is drilled deeper and deeper, the well type is more and more complex, the development from a single vertical well to a multi-bottom well, a directional well, a horizontal well and a large displacement well is realized, and the requirement on drilling fluid materials is higher and higher. The filtrate reducer is a chemical additive which needs to be added in the drilling fluid of the oil field, and in the drilling process, the filtrate in the drilling fluid invades into the stratum to cause hydration expansion of shale, which leads to unstable well wall and various underground complex conditions in serious cases.
Water-based drilling fluid filtrate reducers can be currently mainly classified into three main categories: the natural polymer modified products, synthetic resins and polymer fluid loss additives are relatively late in domestic research on the fluid loss additives, and corresponding achievements are obtained through a large amount of recent researches, but the fluid loss additives in the current industry are insufficient in temperature resistance, poor in salt resistance and fluid loss reduction effect, stable in properties, not easy to degrade and harmful to the environment.
Disclosure of Invention
The invention aims to provide a bionic polymer filtrate reducer for drilling fluid, which aims to solve the problems of paying attention to the filtrate reducer performance, temperature resistance, salt resistance and prevention of pollution to stratum and environment. The lignin-based drilling fluid can be applied to the current domestic common drilling fluid systems such as polymers, polysulfonate, organic salts and the like, has good rheological property and fluid loss reduction effect when being applied at 180 ℃, can have good effect when being added in a small amount, has good compatibility with other treating agents, does not have adverse effect of large-scale viscosity increase in the drilling fluid, is biomimetically synthesized by taking lignin as a matrix, does not contain toxic substances such as heavy metals and the like, is easy to degrade, and is environment-friendly.
In order to achieve the purpose, the invention provides the following technical scheme: a bionic polymer fluid loss additive for drilling fluid is prepared from the following raw materials in parts by weight:
400-500g of modified lignin, 300g of 20% NaOH solution, 800g of 60% sodium hydroxymethyl sulfonate solution, 180g of polyethylenimine and 0.5-1.51 g of defoaming agent.
Further, the composition is composed of the following raw materials in parts by weight: 450g of modified lignin, 280g of 20% NaOH solution, 600g of 60% sodium hydroxymethyl sulfonate solution, 150g of polyethylenimine and 1g of defoaming agent.
Furthermore, the lignin can be prepared by changing the modified lignin, wherein the raw materials in parts by weight comprise the following components,
1-3L of 1% NaOH solution, 40-120g of brown rot lignin, 0.22-0.66g of NaBH4 and 2mol/L of hydrochloric acid solution.
Further, the ratio of the modified lignin is changed as follows: 4.2L of 1% NaOH solution, 80g of brown rot lignin, 0.44g of NaBH4 and 2mol/L of hydrochloric acid solution.
Further, the preparation method of the polymer fluid loss agent comprises the following steps:
s1, adding 450g of modified lignin and 280g of 20% NaOH solution into a four-neck flask containing 500mL of distilled water, adding 200g of 60% sodium hydroxymethyl sulfonate solution, and carrying out heating reflux reaction for 1 h;
s2, adding 200g of 60% sodium hydroxymethyl sulfonate solution, carrying out reflux reaction for 1.5h, adding a defoaming agent, adding 100g of distilled water and 150g of polyethylenimine, mixing, carrying out reflux reaction for about 50min,
and S3, adding 100g of distilled water and 200g of 60% sodium hydroxymethyl sulfonate solution, and reacting for half an hour to obtain the final product, namely the filtrate reducer.
Further, the preparation method of the modified lignin comprises the following steps:
s1, preparing 2L 1% NaOH solution, adding 1200mL of the NaOH solution into a four-neck flask with a stirrer, placing the flask in a water bath kettle, weighing 80g of brown rot lignin, adding the brown rot lignin into the flask, starting stirring, heating in a water bath to 70 ℃, and keeping the temperature for 2 hours;
S2, filtering the suspension by using filter paper, washing residues by using 800mL of hot 1% NaOH solution, combining filtrates, concentrating on a rotary evaporator to about 20%, cooling to obtain a raw material solution, and performing multiple experiments for later use;
s3, 500g of 20% concentrated raw material solution is weighed and transferred to a flask, stirring is started, 1g of NaBH4 is added, and reaction is carried out at room temperature for 6 hours.
S4, precipitating lignin from the reaction solution by using a 2mol/L hydrochloric acid solution, and then repeatedly washing and drying by using distilled water to obtain the modified lignin containing catechol groups.
Compared with the prior art, the invention has the beneficial effects that:
1. in the preparation process of the filtrate reducer, the super-strong adhesion property of catechol groups in mussel byssus protein is utilized, and the filtrate reducer has the functions of plugging micropores and improving strength. The modified lignin with catechol groups is obtained by activating and modifying brown rot lignin, and can be further crosslinked in the drilling fluid by utilizing the stronger adhesion characteristic of the modified lignin underwater to form a gel film with stronger cohesion and adhesion, so that a filter cake formed by the drilling fluid is more compact, micropores are blocked, the toughness and strength of the filter cake are improved, and finally, the filter cake with low permeability, flexibility, thinness and compactness is formed, and the filtration loss of the drilling fluid is effectively reduced;
2. The filtrate reducer introduces modified lignin with catechol group into sulfonic acid group through sodium hydroxymethyl sulfonate, improves water solubility of the lignin, improves temperature resistance and salt resistance of the lignin, and simultaneously improves molecular weight of the lignin, enhances adhesion performance and has positive effect on improving filter cake quality through cross-linking polymerization of polyethylenimine;
3. the filtrate reducer has the temperature resistance of over 200 ℃, is suitable for conventional and composite salt polysulfonate system drilling fluid, can resist higher salinity in brine drilling fluid, 4 percent of sample is added into test slurry with 30 percent of NaCl dosage, and after the test slurry is heated and rolled at 180 ℃, the high-temperature high-pressure filtrate loss is less than or equal to 25 mL. The drilling fluid has good compatibility with other treating agents, and has no adverse effect of greatly increasing viscosity in a common drilling fluid system;
4. the bionic polymer filtrate reducer prepared by the invention adopts raw materials such as biological lignin, polyethylenimine, sodium hydroxymethyl sulfonate and the like, and finally synthesized products do not contain toxic substances such as heavy metals and the like, have low biological toxicity and are environment-friendly.
Detailed Description
In the case of the example 1, the following examples are given,
in the embodiment of the invention, the biomimetic polymer fluid loss additive for drilling fluid comprises the following raw materials in parts by weight:
400-500g of modified lignin, 260-300g of 20% NaOH solution, 400-800g of 60% sodium hydroxymethyl sulfonate solution, 100-180g of polyethylenimine and 0.5-1.51 g of defoaming agent.
The composition is prepared from the following raw materials in parts by weight: 450g of modified lignin, 280g of 20% NaOH solution, 600g of 60% sodium hydroxymethyl sulfonate solution, 150g of polyethylenimine and 1g of defoaming agent.
Wherein the defoaming agent is emulsified silicone oil.
Can be prepared by modifying lignin, wherein the raw materials in parts by weight comprise the following components,
1-3L of 1% NaOH solution, 40-120g of brown rot lignin, 0.22-0.66g of NaBH4 and 2mol/L hydrochloric acid solution.
The method comprises the following steps of changing the ratio of modified lignin: 4.2L of 1% NaOH solution, 80g of brown rot lignin, 0.44g of NaBH4 and 2mol/L hydrochloric acid solution.
The preparation method of the polymer fluid loss agent comprises the following steps:
s1, adding 450g of modified lignin and 280g of 20% NaOH solution into a four-neck flask containing 500mL of distilled water,
adding 200g of 60% sodium hydroxymethyl sulfonate solution, and heating and refluxing for reaction for 1 h;
s2, adding 200g of 60% sodium hydroxymethyl sulfonate solution, carrying out reflux reaction for 1.5h, adding a defoaming agent, adding 100g of distilled water and 150g of polyethylenimine, mixing, carrying out reflux reaction for about 50min,
and S3, adding 100g of distilled water and 200g of 60% sodium hydroxymethyl sulfonate solution, and reacting for half an hour to obtain the final product, namely the filtrate reducer.
In the case of the example 2, the following examples are given,
adding 450g of modified lignin and 280g of 20% NaOH solution into a four-necked flask containing 500mL of distilled water, adding 160g of 60% hydroxymethyl sodium sulfonate solution, heating and refluxing for 1h, then adding 160g of 60% hydroxymethyl sodium sulfonate solution, refluxing for 1.5h, adding a defoaming agent, then adding 100g of distilled water and 120g of polyaziridine, mixing and refluxing for about 50min, then adding 160g of 100g of distilled water and 60% hydroxymethyl sodium sulfonate solution, and reacting for half an hour to obtain the final product, namely the filtrate reducer.
In the case of the embodiment 3, the following examples,
adding 450g of modified lignin and 280g of 20% NaOH solution into a four-necked flask containing 500mL of distilled water, adding 200g of 60% hydroxymethyl sodium sulfonate solution, heating and refluxing for 1h, then adding 200g of 60% hydroxymethyl sodium sulfonate solution, refluxing for 1.5h, adding a defoaming agent, then adding 100g of distilled water and 150g of polyaziridine, mixing and refluxing for about 50min, then adding 100g of distilled water and 200g of 60% hydroxymethyl sodium sulfonate solution, and reacting for half an hour to obtain the final product, namely the filtrate reducer.
In the case of the example 4, it is preferred,
the preparation method of the modified lignin comprises the following steps:
s1, preparing 2L 1% NaOH solution, adding 1200mL of the NaOH solution into a four-neck flask with a stirrer, placing the flask in a water bath kettle, weighing 80g of brown rot lignin, adding the brown rot lignin into the flask, starting stirring, heating in a water bath to 70 ℃, and keeping the temperature for 2 hours;
s2, filtering the suspension by using filter paper, washing residues by using 800mL of hot 1% NaOH solution, combining filtrates, concentrating on a rotary evaporator to about 20%, cooling to obtain a raw material solution, and performing multiple experiments for later use;
s3, 500g of 20% concentrated raw material solution is weighed and transferred to a flask, stirring is started, 1g of NaBH4 is added, and reaction is carried out at room temperature for 6 hours.
S4, precipitating lignin from the reaction solution by using a 2mol/L hydrochloric acid solution, and then repeatedly washing and drying by using distilled water to obtain the modified lignin containing catechol groups.
Experimental example 1:
table 1 test of the effects of examples 1, 2 and 3 in fresh water and salt water
According to experimental data, the bionic polymer fluid loss additive is added into a 30% NaCl salt water slurry by 4%, and after hot rolling at 180 ℃, the fluid loss at high temperature and high pressure is measured at 180 ℃, wherein the fluid loss at high temperature and high pressure is less than or equal to 25 mL.
In table 1, the apparent viscosity and high-temperature and high-pressure fluid loss of the brine slurry are measured as follows:
1) preparation of base slurry
350mL of distilled water is added into a high-speed stirring cup, 1.0g of anhydrous sodium carbonate, 21.0g of bentonite for drilling fluid test and 16.0g of evaluation soil are added into the cup, the cup is stirred for 20min by a high-speed stirrer, the stirring is interrupted twice during the stirring to scrape off the adhered substances on the wall of the container, and the cup is sealed and maintained at the temperature of 24 +/-3 ℃ for 24h to prepare the base slurry.
The base slurry was stirred at a high speed for 5min, and the fluid loss of the base slurry was measured as specified in GB/T16783.1-2014 at 7.3.2, which should be within the range of 65 mL. + -. 10 mL. If the filtration loss of the base slurry is not in the range, the addition amount of the two kinds of soil powders can be properly adjusted.
2) Sample slurry
Adding 17.5g (calculated by dry basis) of sulfonated lignite into a high-speed stirring cup containing base slurry, stirring at a high speed for 15min, adding 14.0g (calculated by dry basis) of a sample, stirring at a high speed for 15min, adding 105g of ground sodium chloride, stirring at a high speed for 15min, finally adding 8.75g of anhydrous sodium carbonate, stirring at a high speed for 15min, stirring uniformly by using a glass rod once each medicine is added, and cutting off paste on the wall of the container twice in the high-speed stirring process.
And (3) filling the prepared test slurry into an aging tank, putting the aging tank into a roller furnace, rolling and aging the aging tank for 16h at the constant temperature of 180 +/-5 ℃, taking out the aging tank, cooling the aging tank to room temperature, pouring out the test slurry, stirring the test slurry at a high speed for 5min, and testing the apparent viscosity of the test slurry and the high-temperature high-pressure filtration loss at 180 ℃ according to the regulations of 6.3.2 and 7.3.2 in GB/T16783.1-2014.
The apparent viscosity of the blank slurry and the high-temperature high-pressure filtration loss at 180 ℃ were measured according to the above method without adding a sample.
Experimental example 2:
table 2 examples 1, 2, 3 biotoxicity EC50 test
Experimental data show that the biotoxicity EC50 of the bionic polymer fluid loss additive is more than 30000mg/L, is basically nontoxic and is environment-friendly.
Biotoxicity EC50 detection method
1) Preparation of test sample
Preparing a sample into a 2% concentration sample stock solution by using distilled water; adjusting the pH value of the stock solution of the sample to be tested to 6.50-7.00 by using 1mol/L sulfuric acid solution for later use.
2) Preparation of test samples
The stock solution of the test sample after pH adjustment was diluted with 30g/L sodium chloride solution as a diluent. Taking 1 part of sample stock solution to be tested according to the volume ratio, adding 9 parts of 30g/L sodium chloride solution, stirring for 30min at the rotating speed of 11000r/min, standing for 60min, setting the concentration of the sample solution as 106mg/L, and sequentially diluting into sample solutions with different concentrations (105mg/L, 104mg/L, 103mg/L, 102mg/L, 10mg/L and 1 mg/L). The concentration gradient is set to obtain regular change of luminosity, and the relative luminosity is close to 50%. The concentration of the experimental sample can be calculated by dividing the concentration of the stock solution of the test sample by the dilution factor.
3) Luminous bacteria activation pretreatment
Taking out the ampoule bottle containing 0.5g of luminous bacteria freeze-dried powder and 25g/L of sodium chloride solution from a refrigerator at the temperature of 2-5 ℃, injecting 1mL of 25g/L of sodium chloride solution into the freeze-dried powder ampoule bottle, fully mixing, and placing in an ice-water bath for 2 min. Taking 1 test tube of 2mL, sequentially adding 2mL of 30g/L sodium chloride solution and 10 mu L of resuscitation luminous bacteria liquid, covering a bottle stopper, and uniformly mixing. The bottle stopper is pulled out, and the tube is put into a bioluminescence photometer for luminescence detection. The resuscitation luminescent bacteria with the luminescence quantity larger than 800mV can be used for subsequent inspection; otherwise, replacing the luminescent bacteria freeze-dried powder and recovering again.
4) Experimental procedure
And (3) adding 2mL of prepared experimental samples with certain concentration gradient into 2mL of test sample tubes respectively to serve as experimental groups, and arranging 3 parallel experimental sample tubes with the same concentration.
2mL of 30g/L sodium chloride solution was added to a 2mL test sample tube as a control.
And (3) sucking 10 mu L of resuscitation luminous bacteria liquid by using a micro-pipette gun, sequentially and respectively adding the resuscitation luminous bacteria liquid into the experiment sample tube and the control sample tube, and uniformly mixing. After standing for 15min, the test tube was immediately placed in the instrument test chamber and the amount of luminescence displayed on the recording instrument was read. The measurement was repeated 3 times for each sample tube, and the average value was taken as the measurement value of luminescence amount.
The method for correcting the light emission quantity obtained by the control group is adopted to eliminate the chroma interference, and the specific method is as follows:
a) two 2mL test tubes were taken and 2mL of 30g/L NaCl solution was added.
b) Taking one test tube of 5mL, adding 3.3mL of 30g/L sodium chloride solution, and marking the test tube as a Ta tube; one 5mL test tube, labeled as Tc tube, was added to 3.3mL of the sample solution to be tested.
c) Adding 10 mu L of resuscitation luminous bacterial liquid into two 2mL test tubes in the step a), covering a bottle stopper, and uniformly mixing.
d) After standing for 15min, two 2mL test tubes were placed in a Ta tube and a Tc tube, respectively, and the luminescence amounts M1(Ta tube), M2(Tc tube) were measured with a bioluminescence photometer.
e) A light emission amount correction value due to color is calculated,
ΔM＝M1-M2
in the formula:
Δ M — light emission correction value, mV;
m1-light emission amount of Ta tube, mV;
M2-Tc tube luminescence, mV.
f) The light emission quantity of the control group sample measured in the above steps is corrected by this step by subtracting the correction value Δ M from the light emission quantity measured in the control group to obtain the actually measured light emission quantity of the control group.
5) Calculation of results
Method of regression equation
a) Calculating the relative luminosity of the sample according to a formula,
in the formula:
t-relative luminosity,%;
ESample(s)-sample tube luminescence, mV;
Econtrol ofControl tube luminescence, mV.
a) Calculating the relative luminosity of the sample according to a formula
In the formula:
T1，T2，T3relative luminosity,%, of the three parallel experimental groups.
c) And (3) carrying out unary linear regression analysis on the samples obtained by detection analysis according to the C, establishing a linear regression equation, and solving a (intercept), b (slope) and r (correlation coefficient) of the unary linear regression equation.
In the formula:
if r is more than or equal to 0.997, the correlation equation is established, 50 is substituted into equation (6), and the C sample is calculated, and the concentration is the EC50 value.
Method for drawing curve
If the correlation equation is not verified, the EC50 value is determined according to a curve method. Drawing a T-C sample curve by taking the concentration (C sample) as an abscissa and the relative luminosity (T) as an ordinate; sample EC50 values were determined against the T-C sample curve.
Experimental example 3:
in the experimental example, the sample in example 3 is selected for testing, and the formula of the polysulfonate high-temperature resistant drilling fluid system is as follows: 3% of bentonite + 0.25% of soda + 0.2% of caustic soda + 0.6% of FA-367+ 3% of the sample + 0.6% of PAC-LV + 3% of SMP-1+ 30% of NaCl + 62% of barite.
The experimental method is as follows:
adding 400mL of distilled water into 4 high-stirring cups, adding 12g of calcium bentonite for drilling fluid, stirring at a high speed for 20min, and taking down the scraping cup walls for multiple times in the period; sealing and curing at 25 +/-1 ℃ for 24 h.
Taking two parts, respectively adding 1g of anhydrous sodium carbonate, 0.8g of sodium hydroxide, 2.4gFA-367, 2.4gXY-27, 12g of SMP-1, 120g of sodium chloride and 248g of barite in sequence, uniformly stirring by using a glass rod after each addition of one medicine, then stirring at a high speed for 15min, and interrupting the stirring process twice to scrape off an adhesive stuck on the wall of a container.
And respectively adding 1g of anhydrous sodium carbonate, 0.8g of sodium hydroxide, 2.4gFA-367, 2.4gXY-27, 12g of a polymer filtrate reducer sample, 12g of SMP-1, 120g of sodium chloride and 248g of barite into the other two parts in sequence, uniformly stirring the mixture by using a glass rod after each addition of one medicine, then stirring the mixture at a high speed for 15min, and interrupting the stirring process twice to scrape off an adhesive stuck on the wall of the container.
And (3) filling 4 parts of prepared test slurry into an aging tank, placing the aging tank into a roller furnace, rolling and aging at a constant temperature of (180 +/-5) DEG C for 16h, taking out the aging tank, cooling to room temperature, stirring the test slurry at a high speed for 5min, and measuring the apparent viscosity of the test slurry and the high-temperature high-pressure filtration loss of (180 +/-3) DEG C according to the specification in GB/T16783.1-2014.
The experimental data are shown in table 3:
TABLE 3 polysulfonated brine high temperature resistant drilling fluid system experimental data
As can be seen from Table 3 in the field, before and after the sample of test example 3 is added, the difference between the apparent viscosity and the plastic viscosity is not great, the HTHP FL is obviously reduced, and the reduction rate of the HTHP FL exceeds 75%, which indicates that the addition of the polymer fluid loss additive in a polysulfonate water high-temperature resistant drilling fluid system does not cause great influence on rheological property, the compatibility is good, and the fluid loss reducing effect is excellent.
Experimental example 4
The slurry apparent viscosity and the (200 +/-3) DEG C high-temperature high-pressure filtration loss of the same product are as follows:
the sample of example 3 was selected for testing in this example, polymer-potassium polysulfonate drilling fluid: 3% bentonite + 0.2% caustic soda + 0.3% macromolecular polymer (IND-30) + 3% sample + 0.2% NH4PAN + 0.5% lubricant + 2% sulfomethyl phenolic resin + 2% sulfonated lignite resin + 2% sulfonated asphalt + 5% KCl + weighting agent.
The experimental method is as follows:
adding 400mL of distilled water into 4 high-stirring cups, adding 12g of calcium bentonite for drilling fluid, stirring at a high speed for 20min, and taking down the wall of the scraping cup for multiple times in the period; and (3) sealing and curing for 24 hours at the temperature of (25 +/-1).
0.4g of caustic soda, 1.2g of macromolecular polymer (IND-30), 12g of similar product, 0.8g of NH4PAN, 2g of lubricant, 8g of sulfomethyl phenolic resin, 8g of sulfonated lignite resin, 8g of sulfonated asphalt, 20g of KCl and barite (the density is kept at 1.90g/cm3) are respectively added into two parts in sequence, and after each addition of one medicine, the mixture is firstly stirred by a glass rod and then stirred at high speed for 15min, and the stirring process is interrupted twice to scrape off adhesive stuck on the wall of the container.
And adding 0.4g of caustic soda, 1.2g of macromolecular polymer (IND-30), 12g of the sample of the invention, 0.8g of NH4PAN, 2g of lubricant, 8g of sulfomethyl phenolic resin, 8g of sulfonated lignite resin, 8g of sulfonated asphalt, 20g of KCl and barite (the density is kept at 1.90g/cm3) into the other two parts in sequence, stirring uniformly by using a glass rod after each addition of one medicine, stirring at high speed for 15min, and interrupting twice during stirring to scrape off the adhesive stuck on the wall of the container.
And (3) loading the prepared 4 parts of test slurry into an aging tank, placing the aging tank into a roller furnace, rolling and aging at a constant temperature of (200 +/-5) DEG C for 16h, taking out the aging tank, cooling to room temperature, stirring the test slurry at a high speed for 5min, and measuring the apparent viscosity and the high-temperature and high-pressure filtration loss of (180 +/-3) DEG C of the test slurry according to the specification in GB/T16783.1-2014. The experimental data are shown in table 4:
TABLE 4 Polymer-Potassium polysulfonate drilling fluid System Experimental data
As can be seen from Table 4, the apparent viscosity AV and the plastic viscosity PV of the experimental example 3 are not much different from those of the same type of product, while the HTHP FL of the experimental example 3 is significantly lower than that of the same type of product, as can be seen: compared with the similar products, the polymer fluid loss agent has more excellent fluid loss effect.
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 attributes 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 specification describes embodiments, not every embodiment includes only a single embodiment, and such description is for clarity purposes only, and it is to be understood that all embodiments may be combined as appropriate by one of ordinary skill in the art to form other embodiments as will be apparent to those of skill in the art from the description herein.
Claims (6)
1. A bionic polymer fluid loss additive for drilling fluid is characterized in that: the fluid loss agent is prepared from the following raw materials in parts by weight:
400-500g of modified lignin, 300g of 20% NaOH solution, 800g of 60% sodium hydroxymethyl sulfonate solution, 180g of polyethylenimine and 0.5-1.5 g of defoaming agent.
2. The biomimetic polymer fluid loss additive for drilling fluid as claimed in claim 1, wherein the fluid loss additive is composed of the following raw materials in parts by weight: 450g of modified lignin, 280g of 20% NaOH solution, 600g of 60% sodium hydroxymethyl sulfonate solution, 150g of polyethylenimine and 1g of defoaming agent.
3. The biomimetic polymer fluid loss additive for drilling fluid as recited in claim 1, wherein the fluid loss additive is prepared by modifying lignin, wherein the raw materials in parts by weight are as follows,
1-3L of 1% NaOH solution, 40-120g of brown rot lignin, 0.22-0.66g of NaBH4 and 2mol/L hydrochloric acid solution.
4. The biomimetic polymer fluid loss additive for drilling fluid as claimed in claim 3, wherein the blend ratio of the modified lignin is as follows: 4.2L of 1% NaOH solution, 80g of brown rot lignin, 0.44g of NaBH4 and 2mol/L hydrochloric acid solution.
5. The biomimetic polymer fluid loss additive for drilling fluid as recited in claim 1 or 2, wherein the preparation method of the polymer fluid loss additive comprises the following steps:
s1, adding 450g of modified lignin and 280g of 20% NaOH solution into a four-neck flask containing 500mL of distilled water, adding 200g of 60% sodium hydroxymethyl sulfonate solution, and carrying out heating reflux reaction for 1 h;
s2, adding 200g of 60% sodium hydroxymethyl sulfonate solution, carrying out reflux reaction for 1.5h, adding a defoaming agent, adding 100g of distilled water and 150g of polyethylenimine, mixing, carrying out reflux reaction for about 50min,
and S3, adding 100g of distilled water and 200g of 60% sodium hydroxymethyl sulfonate solution, and reacting for half an hour to obtain the final product, namely the filtrate reducer.
6. The biomimetic polymer fluid loss additive for drilling fluid as recited in claim 3 or 4, characterized in that the preparation method of the modified lignin comprises the following steps:
S1, preparing 2L of 1% NaOH solution, adding 1200mL of the NaOH solution into a four-neck flask with a stirrer, placing the flask into a water bath kettle, weighing 80g of brown rot lignin, adding the brown rot lignin into the flask, starting stirring, heating in a water bath to 70 ℃, and keeping the temperature for 2 hours;
s2, filtering the suspension by using filter paper, washing residues by using 800mL of hot 1% NaOH solution, combining the filtrates, concentrating on a rotary evaporator to about 20%, cooling to obtain a raw material solution, and performing multiple experiments for later use;
s3, weighing 500g of 20% concentrated raw material solution, transferring the solution into a flask, starting stirring, adding 1g of NaBH4, and reacting at room temperature for 6 h.
S4, precipitating lignin from the reaction solution by using a 2mol/L hydrochloric acid solution, and then repeatedly washing and drying by using distilled water to obtain the modified lignin containing catechol groups.
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| CN116355599A (en) * | 2023-06-01 | 2023-06-30 | 四川巨正科技有限公司 | Environment-friendly lignite resin for drilling fluid and preparation method thereof |
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| CN116355599A (en) * | 2023-06-01 | 2023-06-30 | 四川巨正科技有限公司 | Environment-friendly lignite resin for drilling fluid and preparation method thereof |
| CN116355599B (en) * | 2023-06-01 | 2023-08-08 | 四川巨正科技有限公司 | Environment-friendly lignite resin for drilling fluid and preparation method thereof |
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