Preparation method and application of ultra-high temperature biomass synthetic resin filtrate reducer

Abstract

The application provides a preparation method of an ultra-high-temperature biomass synthetic resin fluid loss additive, comprising the following steps: reacting lignin conversion products, cashew nut phenol, formaldehyde, a sulfonating agent and water according to a certain proportion to obtain the ultra-high-temperature biomass synthetic resin fluid loss additive. The ultra-high-temperature biomass synthetic resin fluid loss additive in the application has the advantages of temperature resistance of 220 DEG C, saturation salt resistance, good high-temperature and high-pressure water loss reduction performance, biodegradability, remarkable viscosity reduction effect in high-density drilling fluid, and suitability for various water-based drilling fluid systems, especially high-temperature and high-density drilling fluid systems. Meanwhile, the method provided by the application uses green and low-cost synthetic raw materials, has a simple and mild synthesis process, and has excellent product performance and wide application prospect. The application further provides a drilling fluid.

Description

Technical Field

[0001] This invention belongs to the field of petroleum drilling fluid additive technology, and particularly relates to a preparation method and application of an ultra-high temperature biomass synthetic resin filtration loss reducer. Background Technology

[0002] Biomass is the fourth largest energy source after coal, oil, and natural gas, and the only carbon-based renewable resource. It is characterized by its wide availability and low price, leading to active global development of biomass energy. In the oil exploration sector, as drilling areas in Xinjiang and Southwest China gradually move towards deep and ultra-deep well exploration and development, coupled with environmental requirements such as "dual carbon" (carbon dioxide, sulfur dioxide, and sulfur dioxide), drilling fluid systems are developing towards high-temperature, high-density, salt-resistant, and environmentally friendly characteristics. This necessitates that core treatment agents possess properties such as high-temperature resistance, saturated salt resistance, non-viscosifying properties, and environmental friendliness. Summary of the Invention

[0003] In view of this, the purpose of this invention is to provide a method for preparing and applying an ultra-high temperature biomass synthetic resin filtration loss reducer. The product prepared by the method provided by this invention is resistant to temperature and saturated salt, has good performance in reducing high temperature and high pressure water loss, is biodegradable, and is suitable for various water-based drilling fluid systems, especially high temperature and high density drilling fluid systems.

[0004] This invention provides a method for preparing an ultra-high temperature biomass synthetic resin filtration loss reducer, comprising the following steps:

[0005] 1) Mix the lignin conversion product, cashew phenol, formaldehyde and water to obtain a mixture;

[0006] 2) The mixture and sulfonating agent A are subjected to a first reaction to obtain a first reaction product;

[0007] 3) The first reaction product and water are reacted in a second reaction to obtain the second reaction product;

[0008] 4) The second reaction product, sulfonating agent B and formaldehyde are subjected to a third reaction to obtain an ultra-high temperature biomass synthetic resin filtration loss reducer.

[0009] Preferably, the mass ratio of lignin conversion product, cashew phenol, formaldehyde, water, sulfonating agent A in step 1), water in step 3), sulfonating agent B in step 4) and formaldehyde is (20-30): (20-30): (50-55): (30-40): (10-15): (80-180): (5-10): (50-60).

[0010] Preferably, the mixing time is 20 to 30 minutes.

[0011] Preferably, the temperature of the first reaction is 65–75°C.

[0012] Preferably, the temperature of the second reaction is 100–105°C.

[0013] Preferably, the temperature of the third reaction is 120–130°C.

[0014] Preferably, the hydroxyl content in the lignin conversion product is 0.339–0.941 mmol / g. -1 .

[0015] Preferably, the sulfonating agent A is selected from one or both of sodium metabisulfite and anhydrous sodium sulfite;

[0016] The sulfonating agent B is selected from p-aminobenzenesulfonic acid.

[0017] Preferably, after the third reaction is completed, the process further includes:

[0018] The obtained reaction product was spray-dried to obtain an ultra-high temperature biomass synthetic resin filtration loss reducer.

[0019] This invention provides a drilling fluid, comprising:

[0020] The ultra-high temperature biomass synthetic resin filtration reducer prepared by the method described in the above technical solution.

[0021] This invention uses lignin conversion products as the main raw material. The extraction of this raw material primarily employs enzyme catalysis or supercritical CO2 extraction technology, a gentle process that maximizes the preservation of the highly active structure of lignin, yielding the lignin conversion products. Based on this, an ultra-high temperature biomass synthetic resin filtration reducer is prepared using the lignin conversion products as raw materials. The prepared product is resistant to temperatures up to 220℃, saturated salts, exhibits excellent performance in reducing high-temperature and high-pressure water loss, is biodegradable, and demonstrates a significant viscosity-reducing effect in high-density drilling fluids. It is suitable for various water-based drilling fluid systems, especially high-temperature and high-density drilling fluid systems. Furthermore, the method provided by this invention uses green and inexpensive synthetic raw materials, the synthesis process is simple and gentle, the product has excellent performance, and its application prospects are broad.

[0022] The preparation method of the ultra-high temperature biomass synthetic resin filtration loss reducer provided by this invention uses green and inexpensive raw materials. The main raw material is lignin separated from corn cobs and straw using enzyme catalysis or supercritical CO2 technology. The structure of the lignin itself is well preserved, and its reactivity is high, providing a good foundation for the sulfonation, polycondensation and other synthesis reactions of ultra-high temperature synthetic resin. The ultra-high temperature biomass synthetic resin filtration loss reducer prepared by this invention has excellent performance, with a temperature resistance of 220℃, a salt resistance of 30% (saturated) in the base slurry, an apparent viscosity of 20 mPa·s, and a high-temperature and high-pressure water loss of <25 mL at 220℃ / 16h. It is applicable to various water-based drilling fluid systems, and especially has a significant function in regulating the flow pattern in ultra-high temperature and high-density drilling fluid systems. The preparation conditions of the ultra-high temperature biomass synthetic resin filtration loss reducer provided by this invention are mild, the process is simple, and it is easy to industrialize. Compared with the traditional sulfonated phenolic resin preparation process, the amount of phenol used is greatly reduced, and the temperature resistance and salt resistance are significantly improved. Detailed Implementation

[0023] The technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0024] This invention provides a method for preparing an ultra-high temperature biomass synthetic resin filtration loss reducer, comprising the following steps:

[0025] 1) Mix the lignin conversion product, cashew phenol, formaldehyde and water to obtain a mixture;

[0026] 2) The mixture and sulfonating agent A are subjected to a first reaction to obtain a first reaction product;

[0027] 3) The first reaction product and water are reacted in a second reaction to obtain the second reaction product;

[0028] 4) The second reaction product, sulfonating agent B and formaldehyde are subjected to a third reaction to obtain an ultra-high temperature biomass synthetic resin filtration loss reducer.

[0029] Lignin is a class of aromatic polymers widely found in plants, possessing strong temperature resistance and representing the world's second most abundant biomass resource. Lignin molecules contain a wealth of active functional groups, including aromatic groups, phenolic hydroxyl groups, alcoholic hydroxyl groups, carbonyl groups, methoxy groups, carboxyl groups, and conjugated double bonds, providing broad avenues for the modification of high-temperature resistant materials. This invention utilizes lignin and other biomass conversion products to prepare high-value drilling fluid treatment agents.

[0030] In this invention, the mixing time is preferably 20 to 30 minutes, more preferably 23 to 27 minutes, and most preferably 25 minutes; the mixing is preferably carried out under stirring conditions.

[0031] In this invention, the temperature of the first reaction is preferably 65-75°C, more preferably 68-72°C, and most preferably 70°C; the time of the first reaction is preferably 30-60 min, more preferably 40-50 min, and most preferably 45 min.

[0032] In this invention, the temperature of the second reaction is preferably 100-105°C, more preferably 101-104°C, and most preferably 102-103°C; during the second reaction, water is preferably added once every 20-30 minutes, preferably a total of 4-6 times, and then the reaction continues for 2-3 hours.

[0033] In this invention, the temperature of the third reaction is preferably 120-130°C, more preferably 123-127°C, and most preferably 125°C; the time of the third reaction is preferably 2-3 hours, more preferably 2.5 hours.

[0034] In this invention, after the third reaction is completed, it preferably further includes:

[0035] The obtained reaction product was spray-dried to obtain an ultra-high temperature biomass synthetic resin filtration loss reducer.

[0036] In this invention, it is preferable to cool the obtained reaction product to room temperature before spray drying; the air inlet temperature during the spray drying process is preferably 210-230°C, more preferably 215-225°C, and most preferably 220°C.

[0037] In this invention, the lignin conversion product is preferably lignin extracted from corn cobs, straw, etc., through enzyme catalysis to achieve "three-element separation" or lignin extracted using supercritical CO2 technology; the lignin conversion product contains hydroxyl (OH) groups. - The preferred content is 0.339–0.941 mmol / g. -1 More preferably, it is 0.4–0.8 mmol / g. -1 The optimal value is 0.5–0.7 mmol / g. -1 .

[0038] This invention uses corn cobs and straw as raw materials, and extracts lignin using enzyme catalysis or supercritical CO2 technology. The structure of the lignin is well preserved, with high content of active groups such as phenolic hydroxyl groups, methoxy groups, and ether bonds. The hydroxyl (OH) groups are particularly abundant. - The content ranges from 0.339 to 0.941 mmol / g. -1Its structure exhibits good reactivity, providing a solid foundation for the sulfonation, polycondensation, and other synthetic reactions of ultra-high temperature synthetic resins.

[0039] In this invention, the sulfonating agent A is preferably selected from one or both of sodium metabisulfite and anhydrous sodium sulfite; the sulfonating agent B is preferably selected from p-aminobenzenesulfonic acid.

[0040] In this invention, the preferred mass ratio of lignin conversion product, cashew phenol, formaldehyde, water, sulfonating agent A in step 1), water in step 3), sulfonating agent B in step 4), and formaldehyde is (20-30):(20-30):(50-55):(30-40):(10-15):(80-180):(5-10):(50-60), more preferably (23-27):(23-27):(51-54):(33-37):(11-14):(100-160):(6-9):(53-57), and most preferably 25:25:(52-53):35:(12-13):(120-140):(7-8):55.

[0041] In this invention, the preferred method for preparing the ultra-high temperature biomass synthetic resin filtration loss reducer includes:

[0042] By weight, 20-30 parts of lignin conversion product, 20-30 parts of cashew phenol, 50-55 parts of formaldehyde, and 30-40 parts of water are mixed and stirred for 20-30 minutes; then 10-15 parts of sulfonating agent A are added, heated to 65-75°C, and reacted for 30-60 minutes to obtain mixture 1.

[0043] Mixture 1 is heated to 100-105°C, and 20-30 parts of water are added every 20-30 minutes for a total of 4-6 times. The reaction is continued for 2-3 hours to obtain mixture 2.

[0044] Add 5-10 parts of sulfonating agent B and 50-60 parts of formaldehyde to mixture 2, heat to 120-130℃, and react for 2-3 hours to obtain mixture 3;

[0045] Mixture 3 was cooled to room temperature, and the liquid was spray-dried to obtain ultra-high temperature biomass synthetic resin filtration reducer. The inlet air temperature of the spray dryer was 220℃.

[0046] This invention employs a two-stage sulfonation synthesis process in the preparation of ultra-high temperature biomass synthetic resin filtration loss reducer. The first sulfonation synthesis process involves: mixing 20-30 parts by weight of lignin conversion product, 20-30 parts of cashew phenol, 50-55 parts of formaldehyde, and 30-40 parts of water for 20-30 minutes; then adding 10-15 parts of sulfonating agent A, which is one or both of sodium metabisulfite and anhydrous sodium sulfite; and then heating to 65-75°C and reacting for 30-60 minutes to obtain the first reaction product. This sulfonation process can introduce sulfonic acid groups at the hydroxyl active groups of the lignin conversion product and cashew phenol, achieving salt and temperature resistance. Given that the sulfonation temperature is controlled at 65-75°C and the sulfonation reaction time is 30-60 minutes, the molecular weight of the first reaction product is not high, and there is basically no condensation reaction, resulting in a very low degree of molecular weight increase.

[0047] Then raise the temperature to 100-105℃, add 20-30 parts of water every 20-30 minutes, add water 4-6 times in total, and continue the reaction for 2-3 hours to obtain the second reaction product; at this time, the reaction is mainly condensation polymerization, the purpose of which is to increase the molecular weight and reduce the filtration loss under high temperature and high pressure.

[0048] The second sulfonation synthesis process involves adding 5-10 parts of sulfonating agent B (p-aminobenzenesulfonic acid) and 50-60 parts of formaldehyde to the second reaction product, heating to 120-130°C, and reacting for 2-3 hours to obtain an ultra-high temperature biomass synthetic resin filtration reducer. This sulfonation process further introduces amino and sulfonic acid groups, which not only further improves its temperature and salt resistance but also imparts good viscosity-reducing properties. This allows the ultra-high temperature biomass synthetic resin filtration reducer prepared by this invention to be used in ultra-high temperature and ultra-high density drilling fluids, playing a role in reducing high temperature and high pressure, being environmentally friendly, salt-resistant, and regulating flow pattern.

[0049] The ultra-high temperature biomass synthetic resin filtration reducer prepared by this invention appears as a yellowish-brown free-flowing powder with a dry basis mass fraction ≥94%. Its molecular weight was tested using gel permeation chromatography, and the result was 6100–8500 g / mol. According to the industry standard SY / T 5094-2017 "Drilling Fluid Filtration Reducer Sulfomethylphenolic Resin SMP", the filtration loss after aging at 220℃ for 16 hours under high temperature and pressure was <25 mL, and the apparent viscosity was <20 mPa·s. According to SY / T 6787-2010 "Environmental Protection Technical Requirements for Water-Soluble Oilfield Chemical Agents", the biodegradability of the ultra-high temperature biomass synthetic resin filtration reducer was tested, and the BOD / COD ratio was >0.05.

[0050] This invention provides a drilling fluid, comprising:

[0051] The ultra-high temperature biomass synthetic resin filtration reducer prepared by the method described in the above technical solution.

[0052] In this invention, the drilling fluid is preferably a water-based drilling fluid; the drilling fluid preferably comprises:

[0053] Bentonite, sulfonate copolymer, ultra-high temperature biomass synthetic resin filtration loss reducer, sulfonated lignite, sulfonated pitch, NaCl, KCl, barite and water.

[0054] In this invention, the bentonite content in the drilling fluid is preferably 2-4% by mass, more preferably 2.5-3.5%, and most preferably 3%; the sulfonate copolymer content in the drilling fluid is preferably 0.4-0.6% by mass, more preferably 0.5%; the ultra-high temperature biomass synthetic resin filtration reducer content in the drilling fluid is preferably 5-9% by mass, more preferably 6-8%, and most preferably 7%; the sulfonated lignite content in the drilling fluid is preferably 5-9% by mass, more preferably 6-8%, and most preferably 7%; the sulfonated bitumen content in the drilling fluid is preferably 2-4% by mass, more preferably 2.5-3.5%, and most preferably 3%; the NaCl content in the drilling fluid is preferably 13-17% by mass, more preferably 14-16%, and most preferably 15%; the KCl content in the drilling fluid is preferably 5-9% by mass, more preferably 6-8%, and most preferably 7%; the amount of barite is preferably added according to the required density of the drilling fluid; and the amount of water is the balance.

[0055] In line with the development trend of temperature- and salt-resistant green water-based drilling fluids, this invention provides a method for preparing an ultra-high temperature biomass synthetic resin filtration reducer. The method provided by this invention is simple, environmentally friendly, and easily industrialized. The prepared product is resistant to temperatures up to 220℃, saturated salts, and exhibits excellent performance in reducing high-temperature and high-pressure fluid loss. It is biodegradable and shows significant viscosity-reducing effects in high-density drilling fluids, making it suitable for various water-based drilling fluid systems, especially high-temperature and high-density drilling fluid systems. The ultra-high temperature biomass synthetic resin filtration reducer prepared by this invention possesses excellent high-temperature resistance, salt resistance, filtration reduction properties, and biodegradability. It is environmentally friendly, can replace sulfonated phenolic resin, and is suitable for various water-based drilling fluids.

[0056] To further understand the present invention, the preparation method of ultra-high temperature biomass synthetic resin filtration loss reducer provided by the present invention will be described below with reference to the embodiments. The scope of protection of the present invention is not limited by the following embodiments.

[0057] All raw materials used in the following embodiments of the present invention are commercially available products. Lignin conversion products and cashew phenol were purchased from Jinan Shengquan New Materials Co., Ltd.; formaldehyde was purchased from Linyi Shengyang Chemical Co., Ltd.; sodium metabisulfite was purchased from Shouguang Dinghao Economic and Trade Co., Ltd.; anhydrous sodium sulfite was purchased from Jining Kunfeng Chemical Co., Ltd.; and p-aminobenzenesulfonic acid was purchased from Suzhou Rongzhen Fine Chemical Co., Ltd.

[0058] The hydroxyl content (C-OH) in lignin conversion products was determined by aqueous potentiometric titration. The results are as follows:

[0059]

[0060] Example 1

[0061] By weight, 20 parts of lignin conversion product (product 1), 20 parts of cashew phenol, 50 parts of formaldehyde, and 30 parts of water were added sequentially to a reactor equipped with a stirrer and a reflux condenser, and mixed for 20 minutes; then 10 parts of sodium metabisulfite were added, heated to 65°C, and reacted for 30 minutes to obtain mixture 1.

[0062] The mixture 1 was heated to 100°C, and 20 parts of water were added every 20 minutes for a total of 6 times. The reaction was continued for 2 hours to obtain mixture 2.

[0063] Add 5 parts of p-aminobenzenesulfonic acid and 50 parts of formaldehyde to mixture 2, heat to 120°C, and react for 2 hours to obtain mixture 3.

[0064] Mixture 3 was cooled to room temperature, and the liquid was spray-dried to prepare the target product of ultra-high temperature biomass synthetic resin filtration loss reducer. The inlet air temperature of the spray dryer was 220℃.

[0065] Example 2

[0066] By weight, 30 parts of lignin conversion product (product #2), 30 parts of cashew phenol, 55 parts of formaldehyde, and 40 parts of water were added sequentially to a reactor equipped with a stirrer and a reflux condenser, and mixed for 30 minutes; then 15 parts of anhydrous sodium sulfite were added, heated to 75°C, and reacted for 60 minutes to obtain mixture 1.

[0067] The mixture 1 was heated to 105°C, and 30 parts of water were added every 30 minutes for a total of 4 times. The reaction was continued for 3 hours to obtain mixture 2.

[0068] Add 10 parts of p-aminobenzenesulfonic acid and 60 parts of formaldehyde to mixture 2, heat to 130°C, and react for 3 hours to obtain mixture 3.

[0069] Mixture 3 was cooled to room temperature, and the liquid was spray-dried to prepare the target product of ultra-high temperature biomass synthetic resin filtration loss reducer. The inlet air temperature of the spray dryer was 220℃.

[0070] Example 3

[0071] By weight, 20 parts of lignin conversion product (product #3), 30 parts of cashew phenol, 50 parts of formaldehyde, and 40 parts of water were added sequentially to a reactor equipped with a stirrer and a reflux condenser, and mixed for 20 minutes; then 5 parts of sodium metabisulfite and 10 parts of anhydrous sodium sulfite were added, and the mixture was heated to 75°C and reacted for 30 minutes to obtain mixture 1.

[0072] The mixture 1 was heated to 100°C, and 20 parts of water were added every 30 minutes for a total of 5 times. The reaction was continued for 3 hours to obtain mixture 2.

[0073] Add 5 parts of p-aminobenzenesulfonic acid and 60 parts of formaldehyde to mixture 2, heat to 120°C, react for 3 min, and obtain mixture 3;

[0074] Mixture 3 was cooled to room temperature, and the liquid was spray-dried to prepare the target product of ultra-high temperature biomass synthetic resin filtration loss reducer. The inlet air temperature of the spray dryer was 220℃.

[0075] Example 4

[0076] By weight, 30 parts of lignin conversion product (product #4), 20 parts of cashew phenol, 55 parts of formaldehyde, and 30 parts of water were added sequentially to a reactor equipped with a stirrer and a reflux condenser, and mixed for 25 minutes; then 15 parts of anhydrous sodium sulfite were added, heated to 75°C, and reacted for 45 minutes to obtain mixture 1.

[0077] The mixture 1 was heated to 105°C, and 30 parts of water were added every 20 minutes for a total of 6 times. The reaction was continued for 3 hours to obtain mixture 2.

[0078] Add 10 parts of p-aminobenzenesulfonic acid and 50 parts of formaldehyde to mixture 2, heat to 130°C, and react for 2 hours to obtain mixture 3.

[0079] Mixture 3 was cooled to room temperature, and the liquid was spray-dried to prepare the target product of ultra-high temperature biomass synthetic resin filtration loss reducer. The inlet air temperature of the spray dryer was 220℃.

[0080] Example 5

[0081] By weight, 25 parts of lignin conversion product (product #5), 25 parts of cashew phenol, 52 parts of formaldehyde, and 35 parts of water were added sequentially to a reactor equipped with a stirrer and a reflux condenser, and mixed for 28 minutes; then 13 parts of sodium metabisulfite were added, heated to 70°C, and reacted for 45 minutes to obtain mixture 1.

[0082] The mixture 1 was heated to 102°C, and 25 parts of water were added every 25 minutes for a total of 5 times. The reaction was continued for 2.5 hours to obtain mixture 2.

[0083] Add 7.5 parts of p-aminobenzenesulfonic acid and 55 parts of formaldehyde to mixture 2, heat to 125°C, and react for 2.5 h to obtain mixture 3;

[0084] Mixture 3 was cooled to room temperature, and the liquid was spray-dried to prepare the target product of ultra-high temperature biomass synthetic resin filtration loss reducer. The inlet air temperature of the spray dryer was 220℃.

[0085] Example 6

[0086] By weight, 22 parts of lignin conversion product (product #6), 28 parts of cashew phenol, 52 parts of formaldehyde, and 28 parts of water were added sequentially to a reactor equipped with a stirrer and a reflux condenser, and mixed and stirred for 24 min; then 12.5 parts of anhydrous sodium sulfite were added, heated to 72°C, and reacted for 50 min to obtain mixture 1.

[0087] The mixture 1 was heated to 104°C, and 30 parts of water were added every 20 minutes for a total of 6 times. The reaction was continued for 3 hours to obtain mixture 2.

[0088] Add 6 parts of p-aminobenzenesulfonic acid and 58 parts of formaldehyde to mixture 2, heat to 120°C, and react for 2 hours to obtain mixture 3.

[0089] Mixture 3 was cooled to room temperature, and the liquid was spray-dried to prepare the target product of ultra-high temperature biomass synthetic resin filtration loss reducer. The inlet air temperature of the spray dryer was 220℃.

[0090] Example 7

[0091] By weight, 30 parts of lignin conversion product (product #3), 30 parts of cashew phenol, 50 parts of formaldehyde, and 40 parts of water were added sequentially to a reactor equipped with a stirrer and a reflux condenser, and mixed for 30 minutes; then 7 parts of sodium metabisulfite and 3 parts of anhydrous sodium sulfite were added, and the mixture was heated to 72°C and reacted for 60 minutes to obtain mixture 1.

[0092] The mixture 1 was heated to 102°C, and 30 parts of water were added every 20 minutes for a total of 6 times. The reaction was continued for 3 hours to obtain mixture 2.

[0093] Add 10 parts of p-aminobenzenesulfonic acid and 60 parts of formaldehyde to mixture 2, heat to 125°C, react for 3 min, and obtain mixture 3;

[0094] Mixture 3 was cooled to room temperature, and the liquid was spray-dried to prepare the target product of ultra-high temperature biomass synthetic resin filtration loss reducer. The inlet air temperature of the spray dryer was 220℃.

[0095] Comparative Example 1 without secondary sulfonation

[0096] By weight, 30 parts of lignin conversion product (product #3), 30 parts of cashew phenol, 50 parts of formaldehyde, and 40 parts of water were added sequentially to a reactor equipped with a stirrer and a reflux condenser, and mixed for 30 minutes; then 7 parts of sodium metabisulfite and 3 parts of anhydrous sodium sulfite were added, and the mixture was heated to 72°C and reacted for 60 minutes to obtain mixture 1.

[0097] The mixture 1 was heated to 102°C, and 30 parts of water were added every 20 minutes for a total of 6 times. The reaction was continued for 3 hours to obtain mixture 2.

[0098] Mixture 2 was cooled to room temperature, and the liquid was spray-dried to prepare the target product of ultra-high temperature biomass synthetic resin filtration loss reducer. The inlet air temperature of the spray dryer was 220℃.

[0099] Comparative Example 2

[0100] Commercially available sulfonated phenolic resin supplied by Bazhou Sanyuan Co., Ltd.

[0101] Performance testing

[0102] Preparation of base slurry: Add 1.05g of anhydrous sodium carbonate, 14.0g of drilling fluid test bentonite and 14.0g of drilling fluid evaluation soil to a high-speed stirring cup containing 350mL of distilled water, stir at high speed for 20min, and cure in a sealed container at 25℃ for 24h.

[0103] Preparation of saturated brine slurry: Add 28g of the products prepared in the examples and comparative examples to the base slurry, stir at high speed for 15min, add 28g of sulfonated lignite, stopping at least twice during the process to scrape off the sample adhering to the container wall, add 105g of sodium chloride, stir at high speed for 10min, and add 8.75g of anhydrous sodium carbonate solution. Transfer the prepared drilling fluid to an aging tank and heat it at 220℃ for 16h. Remove the aging tank, cool it, open it, stir it evenly, and use a high temperature and high pressure filtration loss meter to measure its water loss at 180℃.

[0104] Biodegradability test: The test was conducted according to SY / T 6788-2010 "Evaluation Method for Environmental Protection Technology of Water-soluble Oilfield Chemical Agents". BOD / COD ≥ 0.05 is easily biodegradable, BOD / COD ≤ 0.01 is difficult to biodegrade, and 0.01 < BOD / COD < 0.05 is relatively difficult to degrade.

[0105] The performance test results of the biomass synthetic resin filtration loss reducers prepared in the embodiments and comparative examples of this invention are as follows:

[0106]

[0107] The ultra-high temperature biomass synthetic resin filtration reducer prepared in this embodiment of the invention has a dry basis mass fraction of 92.4-96.2%; a BOD / COD ratio of 0.98-1.22, indicating easy biodegradation; and a high-temperature and high-pressure filtration loss of 22.6-24.8 mL after aging at 220℃ for 16 h in saturated base slurry; with an apparent viscosity of 16-19 mPa·s. The ultra-high temperature biomass synthetic resin filtration reducer provided by this invention has good temperature resistance, salt resistance, high-temperature and high-pressure filtration reduction, viscosity reduction, and environmental friendliness, meeting the performance requirements for use as a water-based drilling fluid filtration reducer. The product in Comparative Document 1, which has not undergone secondary sulfonation, exhibits poor high-temperature and high-pressure filtration reduction performance, and a significantly increased apparent viscosity of the base slurry, indicating that secondary sulfonation has a significant effect on improving temperature resistance, filtration loss reduction, and viscosity reduction. Comparative Example 2: The commercially available sulfonated phenolic resin has a temperature resistance of less than 220℃. Its functional groups are relatively simple. At high temperatures, the molecules undergo excessive cross-linking, resulting in reduced solubility and loss of filtration reduction effect. On the other hand, its adsorption capacity on the surface of clay particles is reduced, so it cannot play a protective role and has poor biodegradability.

[0108] To further verify the role of the biomass synthetic resin filtration reducer prepared in this invention in the drilling fluid system, water-based drilling fluid systems of different densities were prepared and their performance was compared with that of drilling fluids prepared in Comparative Examples 1 and 2.

[0109] The drilling fluid formula is as follows:

[0110] 3% Bentonite + 0.5% DSP-1 (sulfonate copolymer) + 7% Ultra-high temperature biomass synthetic resin filtration loss reducer + 7% SMC (sulfonated lignite) + 3% FT-1A (sulfonated bitumen) + 15% NaCl + 7% KCl + barite + water.

[0111] Aging conditions: 220℃ / 16h, high temperature and high pressure filtration loss test temperature is 180℃.

[0112] The test results are as follows:

[0113]

[0114] AV is apparent viscosity, PV is plastic viscosity, YP is dynamic shear force, Gel is initial and final shear, FL is API filtration loss, and HTHP is high temperature and high pressure filtration loss.

[0115] The results above show that the water-based drilling fluid prepared with ultra-high temperature biomass synthetic resin according to the embodiments of the present invention has a density of 1.4 g / cm³ under aging temperature conditions of 220°C. 3 ~2.7g / cm 3Within the specified range, it exhibits good rheological properties, reasonable filtration loss control, and low viscosity effect, meeting the field performance requirements of water-based drilling fluids for deep and ultra-deep wells. Furthermore, the test results of Examples 6 and 7 and Comparative Examples 1-2 show that, under the same density conditions, the drilling fluid formulated with the ultra-high temperature biomass synthetic resin provided by this invention has better flow pattern and filtration loss control than SMP-type resins. This further demonstrates that the ultra-high temperature biomass synthetic resin prepared using the method provided by this invention has good high-temperature stability, and utilizes the dispersion effect of lignin conversion products to form multi-point adsorption on clay, preventing clay aggregation at high temperatures and achieving a viscosity reduction effect.

[0116] The ultra-high temperature biomass synthetic resin filtration reducer prepared by this invention, in terms of temperature resistance, utilizes the high activity of lignin conversion products. On the one hand, sulfonic acid groups are introduced at the active sites, and on the other hand, cashew phenol oligophenols are introduced as rigid groups. This weakens the high-temperature desorption effect of the filtration reducer molecules caused by thermal motion, thereby improving the product's ability to reduce filtration loss, resist temperature, and resist salt under high-temperature conditions. In terms of reducing filtration loss, the spatial structure of lignin conversion products is utilized to enhance adsorption, adsorption thickness, and inhibition on clay, forming a low-permeability, dense mud cake. Containing polar groups such as hydroxyl and carboxyl groups, charged groups, and hydrophobic groups such as alkanes, these products can adsorb clay particles through electrostatic adsorption, hydrogen bonding, and inductive interactions. This polarizes water molecules, forming a hydration layer, maintaining a suitable particle distribution, and reducing water permeation. Simultaneously, the molecules swell upon contact with water, increasing in volume to form a gel-like substance, which blocks the pores of the mud cake, significantly reducing filter cake permeability and forming a low-permeability, dense mud cake. This controls the permeation of drilling fluid into the formation, reducing filtration loss without increasing the charge density of the filter cake, relying on the large molecular swelling to block pores. Regarding viscosity reduction, the invention utilizes the excellent dispersibility of lignin conversion products, dispersing them within the clay. More importantly, the secondary sulfonation synthesis process introduces a large number of sulfonic acid groups, effectively preventing clay aggregation and achieving viscosity reduction and inhibition. In terms of biodegradability, the presence of para groups in the natural phenolic structure of lignin conversion products can significantly improve biochemical properties.

[0117] The ultra-high temperature biomass synthetic resin filtration reducer prepared by this invention has excellent temperature resistance, salt resistance, viscosity reduction, and biodegradability, and is environmentally friendly, belonging to the category of "green" functional products. Under the optimized process conditions of this invention, the obtained product exhibits stable performance and has broad application prospects.

[0118] While the invention has been described and illustrated with reference to specific embodiments thereof, such description and illustration are not intended to limit the invention. It will be readily understood by those skilled in the art that various changes may be made to suit particular circumstances, materials, compositions, substances, methods, or processes to the objectives, spirit, and scope of this application without departing from the true spirit and scope of the invention as defined by the appended claims. All such modifications are intended to be within the scope of the appended claims. Although the methods disclosed herein have been described with reference to specific operations performed in a particular order, it should be understood that these operations may be combined, subdivided, or reordered to form equivalent methods without departing from the teachings of the invention. Therefore, unless specifically indicated herein, the order and grouping of operations are not a limitation of this application.

[0119] The above description is merely a preferred embodiment of the present invention and is not intended to limit the present invention. Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art can still modify the technical solutions described in the foregoing embodiments or make equivalent substitutions for some of the technical features. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A method for preparing an ultra-high temperature biomass synthetic resin filtration loss reducer, comprising the following steps: 1) Mix the lignin conversion product, cashew phenol, formaldehyde, and water for 20-30 minutes to obtain a mixture; the hydroxyl content of the lignin conversion product is 0.5-0.7 mmol / g. -1 ; 2) The mixture and sulfonating agent A are subjected to a first reaction to obtain a first reaction product; the temperature of the first reaction is 65~75℃; the sulfonating agent A is selected from one or both of sodium metabisulfite and anhydrous sodium sulfite; 3) The first reaction product and water are reacted in a second reaction to obtain a second reaction product; the temperature of the second reaction is 100~105℃; 4) The second reaction product, sulfonating agent B, and formaldehyde are subjected to a third reaction, and the resulting reaction product is spray-dried to obtain an ultra-high temperature biomass synthesis resin filtration loss reducer; the temperature of the third reaction is 120~130℃; the sulfonating agent B is selected from p-aminobenzenesulfonic acid; The mass ratio of lignin conversion product, cashew phenol, formaldehyde, water, sulfonating agent A in step 1), water in step 3), sulfonating agent B and formaldehyde in step 4) is 25:25:(52~53):35:(12~13):(120~140):(7~8):

55.

2. A drilling fluid, comprising: The ultra-high temperature biomass synthetic resin filtration loss reducer prepared by the method of claim 1.

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