CN109705824B - Plugging anti-sloughing agent for drilling fluid and preparation method thereof - Google Patents
Plugging anti-sloughing agent for drilling fluid and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a plugging anti-sloughing agent for drilling fluid, which is prepared from the following raw materials of sulfonated asphalt, a chelating agent, lignin fiber, polyethylene powder, modified polyvinyl alcohol, nano calcium carbonate, n-pentane and water. The invention also discloses a method for plugging the anti-collapse agent for the drilling fluid, which comprises the following steps: mixing and stirring lignin fiber, nano calcium carbonate and 4/5 sulfonated asphalt for 10-20min, then adding water and a chelating agent, stirring, carrying out chelation reaction for 3-4h at the temperature of 40-60 ℃, heating to 80 +/-5 ℃, sequentially adding polyethylene powder and modified polyvinyl alcohol, stirring for 40-60min, then adding the rest sulfonated asphalt, stirring for 20min, then adding n-pentane, then reacting for 2.5-3h at the temperature of 45-55 ℃, and drying. The invention has the advantages that the prepared plugging anti-collapse agent has stronger plugging anti-collapse capability, improves the quality of mud cakes, reduces the filter loss, has low fluorescence, is not tackified, can improve the lubricating property of drilling fluid, has good compatibility with the drilling fluid, and has remarkable comprehensive efficacy.
Description
Technical Field
The invention relates to the field of additives for drilling fluid, in particular to a plugging anti-collapse agent for drilling fluid and a preparation method thereof.
Background
Well collapse is one of the most serious complications in oil and gas drilling projects. The borehole wall stability of shale formations in oil and gas drilling has always been an important responsibility for drilling fluids. Years of drilling fluid anti-sloughing technical research have shown that borehole wall instability is closely related to the invasion of wellbore drilling fluid filtrate. The key point of the drilling fluid anti-collapse technology is to prevent the drilling fluid filtrate from infiltrating and invading the shale well wall. Although the filter cake of the drilling fluid can greatly reduce the permeation rate and the percolation quantity of the drilling fluid of a shaft to formation pores or fractures, the filter cake formed by the action of the drilling fluid filtrate reducer can only change the formation or filter cake gravity water pores into capillary water pores, the filter cake permeability can be reduced from 10-4md to 10-5md, if the formation or filter cake pores are further changed from the capillary water pores into combined water pores with extremely low permeability, namely, the filter cake permeability is further reduced, the realization is difficult, and the collapse prevention requirement can be met only by depending on the compact plugging action of the collapse prevention plugging agent for the drilling fluid in the mechanism analysis.
The plugging agent is a treating agent with a large dosage in the drilling fluid, and has the effects of adjusting the hydrodynamic shearing force, static shearing force and fluid loss of the drilling fluid and improving the quality of mud cakes besides the plugging effect, so that the plugging agent has important influences on well wall stability, oil reservoir protection and the like.
The plugging anti-collapse agent mainly takes modified asphalt, emulsified paraffin, polyalcohol, organic aluminum and silicate as main materials, and the emulsified paraffin plugging agent has low softening point and effective content and is easy to demulsify at low temperature. The polyalcohol blocking agent has too few particles generated by cloud point effect phase change, has no solid phase particles, cannot meet the requirement of anti-collapse blocking, and mainly plays roles in lubrication and micropore blocking. Asphalt is an ideal anti-collapse agent which is generally accepted at present, but the asphalt blocking anti-collapse agent has high fluorescence intensity and has great limitation on the application.
Disclosure of Invention
Aiming at the defects in the prior art, the first object of the invention is to provide a plugging anti-collapse agent for drilling fluid, which has the advantages of good plugging effect and low fluorescence intensity.
The second purpose of the invention is to provide a preparation method of the plugging anti-collapse agent for the drilling fluid, which has the advantages of good plugging effect and low fluorescence intensity of the prepared plugging anti-collapse agent.
In order to achieve the first object, the invention provides the following technical scheme: the plugging and anti-sloughing agent for the drilling fluid is prepared from the following raw materials, by weight, 45-65 parts of sulfonated asphalt formed by sulfonating natural asphalt, 5-15 parts of a chelating agent, 15-30 parts of lignin fiber, 10-20 parts of polyethylene powder, 34-55 parts of modified polyvinyl alcohol prepared by modifying epoxy resin, 6-20 parts of nano calcium carbonate, 30-50 parts of n-pentane and 50-80 parts of water, wherein the chelating agent is one or more of sodium metaphosphate, sodium acid pyrophosphate and citric acid or citrate.
By adopting the technical scheme, the asphalt anti-collapse agent contains water-insoluble asphalt particles and has a certain softening point, when the temperature and the pressure in a borehole are high enough, the asphalt anti-collapse agent is softened and deformed and is counted in the microcracks of the borehole wall, and the asphalt anti-collapse agent and the mud cake together effectively block the stratum. The natural asphalt has high stability to water, acid and alkali and high compatibility with drilling fluid, but the natural asphalt has poor dispersibility in the water-based drilling fluid, can not be directly used as a filtrate reducer and an anti-collapse inhibitor in the water-based drilling fluid, is sulfonated, introduces sulfonic groups of clear water and improves the hydration dispersibility of the asphalt. When the clean water end of the sulfonated asphalt is adsorbed on the shale interface, the oleophilic end can cover the shale surface, thereby improving the mud cake quality, reducing the drilling fluid filtration loss, and preventing the hydration and dispersion of shale particles from playing a role in preventing collapse; meanwhile, the oleophylic part can fill pore throats and cracks to play a role in plugging.
The plugging and anti-sloughing agent finally prepared by adding the sulfonated asphalt, the lignin fiber, the nano calcium carbonate, the n-pentane and the chelating agent is used in the drilling fluid, so that the particles and the strength in a drilling fluid system are changed, the plugging and anti-sloughing capability of the drilling fluid is improved, the mud cake quality is improved, the filtration loss is reduced, the prepared plugging and anti-sloughing agent is low in fluorescence, does not tackify, can improve the lubricating property of the drilling fluid, is good in compatibility with the drilling fluid, has an obvious comprehensive effect, is more obvious in plugging and anti-sloughing effect on a hard and brittle shale and a microcrack development bottom layer, and is wide in applicability.
Furthermore, the plugging and anti-collapse agent is prepared from 50-60 parts of sulfonated asphalt formed by sulfonating natural asphalt, 8-13 parts of chelating agent, 20-28 parts of lignin fiber, 12-16 parts of polyethylene powder, 40-45 parts of modified polyvinyl alcohol, 10-16 parts of nano calcium carbonate, 35-46 parts of n-pentane and 60-75 parts of water.
The plugging and anti-collapse agent is further prepared from 55 parts of sulfonated asphalt formed by sulfonating natural asphalt, 10 parts of chelating agent, 24 parts of lignin fiber, 15 parts of polyethylene powder, 43 parts of modified polyvinyl alcohol, 15 parts of nano calcium carbonate, 40 parts of n-pentane and 65 parts of water.
Further, the citrate is one or more of calcium citrate, potassium citrate or sodium citrate.
Further, the chelating agent is prepared from sodium metaphosphate, sodium acid pyrophosphate and calcium citrate in a weight ratio of 1: 0.5: 2-1: 1-3 by mass ratio.
Further, the preparation method of the modified polyvinyl alcohol is as follows: mixing the components in a mass ratio of 1: 5-8 of polyvinyl alcohol and water are mixed and stirred, the temperature is increased to 90 +/-10 ℃, the mixture is stirred for 1.5-2h at the temperature, the stirring is stopped, the temperature is kept at 90 +/-10 ℃ for 1h, then the temperature is reduced to 70 ℃, then epoxy resin is added, the mixture is stirred for 10-20min, the mixture is kept at 70 +/-5 ℃ for reaction for 2h, and the modified polyvinyl alcohol is obtained after drying.
Further, the preparation method of the sulfonated asphalt comprises the following steps: mixing natural asphalt and light oil, stirring for 1.5-2h, introducing sulfur trioxide gas, sulfonating for 3.5-4.5h in sulfur trioxide atmosphere, and stirring for 1.5-2 h;
adding sodium hydroxide for neutralization, stirring for 2h, heating to 80 +/-5 ℃, distilling and drying to obtain sulfonated asphalt, wherein the mass ratio of the natural asphalt to the light oil is 1:5-10, and the pH value of the neutralized product is 8.5-9; the introduction flow of the sulfur trioxide gas is 0.045-0.6m3/h。
In order to achieve the second object, the invention provides the following technical scheme: a preparation method of a plugging anti-collapse agent for well fluid comprises the following steps:
mixing and stirring lignin fiber, nano calcium carbonate and 4/5 sulfonated asphalt for 10-20min, then adding water and a chelating agent, stirring, carrying out chelation reaction for 3-4h at the temperature of 40-60 ℃, heating to 80 +/-5 ℃, sequentially adding polyethylene powder and modified polyvinyl alcohol, stirring for 40-60min, then adding the rest sulfonated asphalt, stirring for 20min, then adding n-pentane, then reacting for 2.5-3h at the temperature of 45-55 ℃, and drying to obtain the plugging and anti-collapse agent.
In conclusion, the invention has the following beneficial effects:
1. when the plugging anti-collapse agent prepared by the invention is used in drilling fluid, the particle and strength in a drilling fluid system are changed, the plugging anti-collapse capability of the drilling fluid is improved, the mud cake quality is improved, and the filter loss is reduced;
2. the addition of the lignin fiber enhances the strength of the plugging anti-collapse agent, further reduces the loss rate, provides a new technical support for solving the problem of stable plugging anti-collapse of the well wall of the oil-gas drilling well, and has important significance for further reducing the complex condition of well collapse, ensuring the underground safety of the oil-gas drilling well and accelerating the exploration and development process of oil-gas resources.
Detailed Description
The present invention will be described in further detail with reference to examples.
Examples of preparation of raw materials
Preparation examples 1 to 3 are modified polyvinyl alcohol preparation examples, and preparation examples 4 to 6 are sulfonated asphalt preparation examples.
Preparation example 1
The preparation method of the modified polyvinyl alcohol comprises the following steps: mixing the components in a mass ratio of 1: 6, mixing and stirring the polyvinyl alcohol and the water, heating to 90 ℃, stirring for 100min at the temperature, stopping stirring, preserving heat for 1h at 90 ℃, then cooling to 70 ℃, then adding the epoxy resin, stirring for 15min, preserving heat for reaction for 2h at 70 ℃, and drying to obtain the modified polyvinyl alcohol.
Preparation example 2
The preparation method of the modified polyvinyl alcohol comprises the following steps: mixing the components in a mass ratio of 1:5, mixing and stirring the polyvinyl alcohol and water, heating to 80 ℃, stirring for 1.5h at the temperature, stopping stirring, preserving heat for 1h at 80 ℃, then cooling to 65 ℃, then adding epoxy resin, stirring for 10min, preserving heat for reaction for 2h at 65 ℃, and drying to obtain the modified polyvinyl alcohol.
Preparation example 3
The preparation method of the modified polyvinyl alcohol comprises the following steps: mixing the components in a mass ratio of 1: and 8, mixing and stirring the polyvinyl alcohol and water, heating to 100 ℃, stirring for 2 hours at the temperature, stopping stirring, preserving heat for 1 hour at 100 ℃, then cooling to 75 ℃, then adding epoxy resin, stirring for 20 minutes, preserving heat for reaction for 2 hours at 75 ℃, and drying to obtain the modified polyvinyl alcohol.
Preparation example 4
The preparation method of the sulfonated asphalt comprises the following steps: mixing natural asphalt and light oil, stirring for 100min, introducing sulfur trioxide gas, sulfonating for 4h in sulfur trioxide atmosphere, and stirring for 100 min;
adding sodium hydroxide for neutralization, stirring for 2h, heating to 80 ℃, distilling and drying to obtain sulfonated asphalt, wherein the mass ratio of the natural asphalt to the light oil is 1:8, and the pH value of the neutralized product is 8.8; the introduction flow of sulfur trioxide gas is 0.5m3/h。
Preparation example 5
The preparation method of the sulfonated asphalt comprises the following steps: mixing and stirring natural asphalt and light oil for 1.5h, then introducing sulfur trioxide gas, sulfonating for 3.5h in sulfur trioxide atmosphere, and stirring for 1.5 h;
adding sodium hydroxide for neutralization, stirring for 2h, heating to 75 ℃, distilling and drying to obtain sulfonated asphalt, wherein the mass ratio of the natural asphalt to the light oil is 1:5, and the pH value of the neutralized product is 8.5; the introduction flow of sulfur trioxide gas is 0.045m3/h。
Preparation example 6
The preparation method of the sulfonated asphalt comprises the following steps: mixing and stirring natural asphalt and light oil for 2 hours, then introducing sulfur trioxide gas, sulfonating for 4.5 hours in sulfur trioxide atmosphere, and stirring for 2 hours;
adding sodium hydroxide for neutralization, stirring for 2h, heating to 85 ℃, distilling and drying to obtain sulfonated asphalt, wherein the mass ratio of the natural asphalt to the light oil is 1:10, and the pH value of the neutralized product is 9; the introduction flow of sulfur trioxide gas is 0.6m3/h。
Examples
In the following examples, all the raw materials used are commercially available.
The plugging and anti-sloughing agent for the drilling fluid is prepared from the following raw materials, by weight, 45-65 parts of sulfonated asphalt formed by sulfonating natural asphalt, 5-15 parts of chelating agent, 15-30 parts of lignin fiber, 10-20 parts of polyethylene powder, 34-55 parts of modified polyvinyl alcohol prepared by modifying epoxy resin, 6-20 parts of nano calcium carbonate, 30-50 parts of n-pentane and 50-80 parts of water.
Wherein the chelating agent is one or more of sodium metaphosphate, acid sodium pyrophosphate and citric acid or citrate;
the citrate is one or more of calcium citrate, potassium citrate or sodium citrate;
preferably, the chelating agent is prepared from sodium metaphosphate, sodium acid pyrophosphate and calcium citrate in a ratio of 1: 0.5: 2-1: 1-3 by mass ratio.
Example 1
A preparation method of a plugging anti-sloughing agent for drilling fluid comprises the following steps in parts by weight: mixing and stirring 24 parts of lignin fiber, 15 parts of nano calcium carbonate and 44 parts of sulfonated asphalt prepared in preparation example 4 for 15min, then adding 65 parts of water and 10 parts of chelating agent, stirring, carrying out chelation reaction at 50 ℃ for 3.5h, heating to 80 ℃, sequentially adding 15 parts of polyethylene powder and 43 parts of modified polyvinyl alcohol prepared in preparation example 1, stirring for 50min, then adding the rest 11 parts of sulfonated asphalt, stirring for 20min, then adding 49 parts of n-pentane, then reacting at 50 ℃ for 170min, and drying to obtain the plugging and anti-collapse agent.
Wherein the lignocellulose is purchased from Yixing Shangpo building materials Co., Ltd, and the brand is Shangpo super-strong lignocellulose;
the chelating agent is sodium metaphosphate, sodium acid pyrophosphate and calcium citrate, and the weight ratio of the chelating agent to the sodium metaphosphate, the sodium acid pyrophosphate and the calcium citrate is 1: 0.8: 2.5 by mass ratio.
Example 2
The preparation method of the plugging anti-sloughing agent for the drilling fluid is carried out according to the method in the embodiment 1, and the difference is that the preparation method comprises the following steps in parts by weight: mixing and stirring 20 parts of lignin fiber, 10 parts of nano calcium carbonate and 40 parts of sulfonated asphalt prepared in preparation example 4 for 15min, then adding 60 parts of water and 8 parts of chelating agent, stirring, carrying out chelation reaction at 50 ℃ for 3.5h, heating to 80 ℃, sequentially adding 12 parts of polyethylene powder and 40 parts of modified polyvinyl alcohol prepared in preparation example 1, stirring for 50min, then adding the rest 10 parts of sulfonated asphalt, stirring for 20min, then adding 35 parts of n-pentane, then reacting at 50 ℃ for 170min, and drying to obtain the plugging and anti-collapse agent.
Wherein the chelating agent is sodium metaphosphate, sodium acid pyrophosphate and calcium citrate, and the ratio of the sodium metaphosphate to the calcium acid pyrophosphate to the calcium citrate is 1: 0.8: 2.5 by mass ratio.
Example 3
The preparation method of the plugging anti-sloughing agent for the drilling fluid is carried out according to the method in the embodiment 1, and the difference is that the preparation method comprises the following steps in parts by weight: mixing 28 parts of lignin fiber, 16 parts of nano calcium carbonate and 48 parts of sulfonated asphalt prepared in preparation example 4, stirring for 15min, then adding 75 parts of water and 13 parts of chelating agent, stirring, carrying out chelation reaction at 50 ℃ for 3.5h, heating to 80 ℃, sequentially adding 15 parts of polyethylene powder and 43 parts of modified polyvinyl alcohol prepared in preparation example 1, stirring for 50min, then adding the rest 12 parts of sulfonated asphalt, stirring for 20min, then adding 46 parts of n-pentane, then reacting at 50 ℃ for 170min, and drying to obtain the plugging and anti-collapse agent.
Wherein the chelating agent is sodium metaphosphate, sodium acid pyrophosphate and calcium citrate, and the ratio of the sodium metaphosphate to the calcium acid pyrophosphate to the calcium citrate is 1: 0.8: 2.5 by mass ratio.
Example 4
The preparation method of the plugging anti-sloughing agent for the drilling fluid is carried out according to the method in the embodiment 1, and the difference is that the preparation method comprises the following steps in parts by weight: mixing and stirring 15 parts of lignin fiber, 6 parts of nano calcium carbonate and 36 parts of sulfonated asphalt prepared in preparation example 4 for 15min, then adding 50 parts of water and 5 parts of chelating agent, stirring, carrying out chelation reaction at 50 ℃ for 3.5h, heating to 80 ℃, sequentially adding 10 parts of polyethylene powder and 34 parts of modified polyvinyl alcohol prepared in preparation example 1, stirring for 50min, then adding the rest 9 parts of sulfonated asphalt, stirring for 20min, then adding 30 parts of n-pentane, then reacting at 50 ℃ for 170min, and drying to obtain the plugging and anti-collapse agent.
Wherein the chelating agent is sodium metaphosphate, sodium acid pyrophosphate and calcium citrate, and the ratio of the sodium metaphosphate to the calcium acid pyrophosphate to the calcium citrate is 1: 0.8: 2.5 by mass ratio.
Example 5
The preparation method of the plugging anti-sloughing agent for the drilling fluid is carried out according to the method in the embodiment 1, and the difference is that the preparation method comprises the following steps in parts by weight: mixing and stirring 30 parts of lignin fiber, 20 parts of nano calcium carbonate and 52 parts of sulfonated asphalt prepared in preparation example 4 for 15min, then adding 80 parts of water and 15 parts of chelating agent, stirring, carrying out chelation reaction at 50 ℃ for 3.5h, heating to 80 ℃, sequentially adding 20 parts of polyethylene powder and 55 parts of modified polyvinyl alcohol prepared in preparation example 1, stirring for 50min, then adding the rest 13 parts of sulfonated asphalt, stirring for 20min, then adding 50 parts of n-pentane, then reacting at 50 ℃ for 170min, and drying to obtain the plugging and anti-collapse agent.
Wherein the chelating agent is sodium metaphosphate, sodium acid pyrophosphate and calcium citrate, and the ratio of the sodium metaphosphate to the calcium acid pyrophosphate to the calcium citrate is 1: 0.8: 2.5 by mass ratio.
Example 6
The preparation method of the plugging and anti-sloughing agent for the drilling fluid is carried out according to the method in the embodiment 1, and is characterized in that the chelating agent is sodium metaphosphate, sodium acid pyrophosphate and calcium citrate, and the weight ratio of the chelating agent to the sodium metaphosphate, the sodium acid pyrophosphate and the calcium citrate is 1: 0.5: 2, and mixing the components in a mass ratio.
Example 7
The preparation method of the plugging and anti-sloughing agent for the drilling fluid is carried out according to the method in the embodiment 1, and is characterized in that the chelating agent is sodium metaphosphate, sodium acid pyrophosphate and calcium citrate, and the weight ratio of the chelating agent to the sodium metaphosphate, the sodium acid pyrophosphate and the calcium citrate is 1: 2: 3, and the components are mixed according to the mass ratio.
Example 8
The preparation method of the plugging and anti-sloughing agent for the drilling fluid is carried out according to the method in the example 1, and the difference is that the chelating agent is citric acid.
Example 9
The preparation method of the plugging and anti-sloughing agent for the drilling fluid is carried out according to the method in the example 1, and the difference is that the modified polyvinyl alcohol is the modified polyvinyl alcohol prepared in the preparation example 2, and the sulfonated asphalt is the sulfonated asphalt prepared in the preparation example 2.
Example 10
The preparation method of the plugging and anti-sloughing agent for the drilling fluid is carried out according to the method in the example 1, and the difference is that the modified polyvinyl alcohol is the modified polyvinyl alcohol prepared in the preparation example 3, and the sulfonated asphalt is the sulfonated asphalt prepared in the preparation example 3.
Example 11
The preparation method of the plugging anti-sloughing agent for the drilling fluid is carried out according to the method in the embodiment 1, and is characterized by comprising the following steps in parts by weight: mixing and stirring 24 parts of lignin fiber, 15 parts of nano calcium carbonate and 44 parts of sulfonated asphalt prepared in preparation example 4 for 10min, then adding 65 parts of water and 10 parts of chelating agent, stirring, carrying out chelation reaction at 40 ℃ for 3h, heating to 75 ℃, sequentially adding 15 parts of polyethylene powder and 43 parts of modified polyvinyl alcohol prepared in preparation example 1, stirring for 40min, then adding the rest 11 parts of sulfonated asphalt, stirring for 20min, then adding 49 parts of n-pentane, then reacting at 45 ℃ for 2.5h, and drying to obtain the plugging and anti-collapse agent.
Wherein the chelating agent is sodium metaphosphate, sodium acid pyrophosphate and calcium citrate, and the ratio of the sodium metaphosphate to the calcium acid pyrophosphate to the calcium citrate is 1: 0.8: 2.5 by mass ratio.
Example 12
The preparation method of the plugging anti-sloughing agent for the drilling fluid is carried out according to the method in the embodiment 1, and is characterized by comprising the following steps in parts by weight: mixing and stirring 24 parts of lignin fiber, 15 parts of nano calcium carbonate and 44 parts of sulfonated asphalt prepared in preparation example 4 for 20min, then adding 65 parts of water and 10 parts of chelating agent, stirring, carrying out chelation reaction at the temperature of 60 ℃ for 4h, heating to 75 ℃, sequentially adding 15 parts of polyethylene powder and 43 parts of modified polyvinyl alcohol prepared in preparation example 1, stirring for 60min, then adding the rest 11 parts of sulfonated asphalt, stirring for 20min, then adding 49 parts of n-pentane, then reacting at the temperature of 55 ℃ for 3h, and drying to obtain the plugging and anti-collapse agent.
Wherein the chelating agent is sodium metaphosphate, sodium acid pyrophosphate and calcium citrate, and the ratio of the sodium metaphosphate to the calcium acid pyrophosphate to the calcium citrate is 1: 0.8: 2.5 by mass ratio.
Comparative example 1
The preparation method of the plugging anti-sloughing agent for the drilling fluid is carried out according to the method in the example 1, and is characterized in that no chelating agent is added in the preparation process.
Comparative example 2
The preparation method of the plugging anti-sloughing agent for the drilling fluid is carried out according to the method in the example 1, and is characterized in that nano calcium carbonate is not added in the preparation process.
Comparative example 3
The preparation method of the plugging and anti-sloughing agent for the drilling fluid is carried out according to the method in the example 1, and is characterized in that no polyethylene powder is added in the preparation process.
Comparative example 4
The preparation method of the plugging and anti-sloughing agent for the drilling fluid is carried out according to the method in the example 1, and is characterized in that modified polyvinyl alcohol is not added in the preparation process.
Comparative example 5
The preparation method of the plugging and anti-sloughing agent for the drilling fluid is carried out according to the method in the example 1, and is characterized in that sulfonated asphalt added in the preparation process is purchased from Mingtai chemical industry Co., Ltd, Henan province, and the brand number is Henan Mingtai/FT-1.
Performance detection
The performance of the plugging and anti-collapse agents prepared in examples 1-12 and comparative examples 1-5 was tested, wherein the test samples were the plugging and anti-collapse agents prepared in examples 1-12 and comparative examples 1-5, and the test items and methods were as follows:
1. appearance detection
Visual inspection was performed under natural light.
2. Determination of the pH value
Weighing 2.0g of sample, placing the sample into a 300ml beaker, adding 200ml of distilled water, stirring for 30min, dripping the solution onto a pH test paper by using a glass rod, and contrasting the color scale reading.
3. Determination of screen allowance of 80-mesh wet screen
Weighing 10g of sample, putting the sample into a standard sieve of 80 meshes, washing the sample by using a hand-operated standard sieve and tap water until the sample is not dyed, putting the screen residue into an oven, drying the screen residue for 2 hours at the temperature of 105 +/-3 ℃, cooling the dried screen residue to the room temperature in a dryer, and weighing the mass of the screen residue.
The 80 mesh wet sieve residue is equal to the mass of the residue (g)/the mass of the sample (g) × 100%
4. Determination of moisture
Weighing 10g (standard to 0.01g) of the sample in a weighing bottle with constant temperature of 105 +/-3 ℃, putting the weighing bottle into a constant temperature drying box, drying the weighing bottle for 2 hours at 105 +/-3 ℃, taking the weighing bottle out, putting the weighing bottle into a dryer, cooling the weighing bottle to room temperature, and weighing the weighing bottle.
Moisture (M)1-M2)/(M1-M)*100％
In the formula, M1-weighing the vial and sample mass, g;
M2-weighing the bottle and sample mass after drying, g;
m-weigh the mass of the vial, g.
5. Determination of oil-soluble matter content
Removing 0.2-0.3g of absorbent cotton, putting into a roll of lens wiping paper, and drying at 105 +/-3 ℃ for 2h for later use;
accurately weighing 0.5g (accurate to 0.1g) of sample by using an analytical balance, putting the sample on the paper roll, weighing the sample, putting the weighed sample into a sample cup in an extractor, and hanging the cup below a miniature condenser pipe in the extractor;
300ml of carbon tetrachloride was injected into the extractor. The extractor is placed in an electric heating jacket to be heated and kept in a boiling state until the outflow is colorless. Taking out the sample cup, putting the paper roll into a drying oven, drying for 2h at 105 +/-3 ℃, taking out and putting into the drying oven, cooling for 30min, and weighing the residue.
Content of oil-soluble substance (M)2-M1)/M*100％
In the formula, M1-amount of absorbent cotton lens-wiping paper and residues, g;
M2-absorbent cotton lens wiping paper and sample mass, g;
m-sample mass, g.
6. Determination of filtration loss reduction rate at high temperature and high pressure of 200 DEG C
(1) Preparation of base slurry
And (3) distilled water: slurry preparation soil for test: anhydrous sodium carbonate 400: preparing base slurry at a ratio of 20:1, stirring at high speed for 20min, stopping at least twice during the stirring, scraping off clay adhered to the wall of the container, and sealing and maintaining at room temperature for 24h to obtain the base slurry;
(2) determination of base stock Properties
Taking 400ml of the base slurry prepared in the step (1), stirring at a high speed for 5min, measuring the filtration loss of the base slurry, wherein the measurement result is within the range of 50 +/-10 ml, and otherwise, adjusting the addition amount of the slurry-preparing soil for the test;
(3) test pulp 200 ℃ performance measurement
Taking 400ml of the base slurry adjusted in the step (2), adding a 12.0g sample under stirring, stirring at high speed for 20min, stopping at least twice in the period, scraping off a sample piece adhered to the wall of a container, and measuring the filtration loss reduction rate of 3450KPa at 200 ℃.
The filtration loss reduction rate at high temperature and high pressure of 200 ═ A-B)/A ═ 100%
In the formula, the high-temperature high-pressure filtration loss of the base slurry in A- (2) is ml; and (B- (3) adding the sample, and then, filtering out the sample at high temperature and high pressure, wherein the sample is ml.
7. Evaluation of fluorescence level
Weighing 2.5g (accurate to 0.0001g) of dehydrated crude oil in a 250ml volumetric flask, dissolving the dehydrated crude oil with trichloromethane and diluting the dehydrated crude oil to a scale mark, namely 15-grade fluorescence standard solution;
absorbing 50.0ml of 15-grade fluorescent standard solution into a 100ml volumetric flask by using a 50ml pipette, diluting the 15-grade fluorescent standard solution to a scale by using trichloromethane, namely 14-grade silver standard solution, and gradually diluting the 14-grade silver standard solution to 1 grade according to the method;
adding 20ml of chloroform into a cleaned and dried 50ml beaker, adding 0.50g of sample, shaking uniformly, filtering by using medium-speed qualitative filter paper, pouring the obtained clear liquid into a clean test tube, observing fluorescence under an ultraviolet sightseeing instrument, and comparing with a standard series to determine the fluorescence level.
The results of the measurements are shown in Table 1 below.
Table 1:
the present embodiment is only for explaining the present invention, and it is not limited to the present invention, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present invention.
Claims (9)
1. The plugging and anti-sloughing agent for the drilling fluid is characterized by being prepared from the following raw materials, by weight, 45-65 parts of sulfonated asphalt formed by sulfonating natural asphalt, 5-15 parts of chelating agent, 15-30 parts of lignin fiber, 10-20 parts of polyethylene powder, 34-55 parts of modified polyvinyl alcohol prepared by modifying epoxy resin, 6-20 parts of nano calcium carbonate, 30-50 parts of n-pentane and 50-80 parts of water;
the method for preparing the plugging anti-sloughing agent for the drilling fluid comprises the following steps:
mixing and stirring lignin fiber, nano calcium carbonate and 4/5 sulfonated asphalt for 10-20min, then adding water and a chelating agent, stirring, carrying out chelation reaction for 3-4h at the temperature of 40-60 ℃, heating to 80 +/-5 ℃, sequentially adding polyethylene powder and modified polyvinyl alcohol, stirring for 40-60min, then adding the rest sulfonated asphalt, stirring for 20min, then adding n-pentane, then reacting for 2.5-3h at the temperature of 45-55 ℃, and drying to obtain the plugging and anti-collapse agent.
2. The plugging and anti-sloughing agent for drilling fluid as claimed in claim 1, wherein the plugging and anti-sloughing agent is prepared from 50-60 parts of sulfonated asphalt formed by sulfonating natural asphalt, 8-13 parts of chelating agent, 20-28 parts of lignin fiber, 12-16 parts of polyethylene powder, 40-45 parts of modified polyvinyl alcohol, 10-16 parts of nano calcium carbonate, 35-46 parts of n-pentane and 60-75 parts of water.
3. The plugging and anti-sloughing agent for drilling fluid is prepared from 55 parts of sulfonated asphalt formed by sulfonating natural asphalt, 10 parts of chelating agent, 24 parts of lignin fiber, 15 parts of polyethylene powder, 43 parts of modified polyvinyl alcohol, 15 parts of nano calcium carbonate, 40 parts of n-pentane and 65 parts of water.
4. The plugging and anti-sloughing agent for drilling fluid as claimed in claim 1, wherein the chelating agent is one or more of sodium metaphosphate, sodium acid pyrophosphate and citric acid or citrate.
5. The plugging and anti-sloughing agent for drilling fluid as claimed in claim 4, wherein the citrate is one or more of calcium citrate, potassium citrate or sodium citrate.
6. The plugging and anti-sloughing agent for drilling fluid as claimed in claim 5, wherein the chelating agent is prepared from sodium metaphosphate, sodium acid pyrophosphate and calcium citrate in a weight ratio of 1: 0.5: 2-1: 1-3 by mass ratio.
7. The plugging and anti-sloughing agent for drilling fluid as claimed in claim 1, wherein the preparation method of the modified polyvinyl alcohol is as follows: mixing the components in a mass ratio of 1: 5-8 of polyvinyl alcohol and water are mixed and stirred, the temperature is increased to 90 +/-10 ℃, the mixture is stirred for 1.5-2h at the temperature, the stirring is stopped, the temperature is kept at 90 +/-10 ℃ for 1h, then the temperature is reduced to 70 ℃, then epoxy resin is added, the mixture is stirred for 10-20min, the mixture is kept at 70 +/-5 ℃ for reaction for 2h, and the modified polyvinyl alcohol is obtained after drying.
8. The plugging and anti-sloughing agent for drilling fluid as claimed in claim 1, wherein the preparation method of the sulfonated asphalt is as follows: mixing natural asphalt and light oil, stirring for 1.5-2h, introducing sulfur trioxide gas, sulfonating for 3.5-4.5h in sulfur trioxide atmosphere, and stirring for 1.5-2 h;
adding sodium hydroxide for neutralization, stirring for 2h, heating to 80 +/-5 ℃, distilling and drying to obtain sulfonated asphalt, wherein the mass ratio of the natural asphalt to the light oil is 1:5-10, and the pH value of the neutralized product is 8.5-9; the introduction flow rate of the sulfur trioxide gas is 0.045-0.6m 3/h.
9. A method for preparing the plugging and anti-sloughing agent for drilling fluid as claimed in any one of claims 1 to 8, which comprises the following steps:
mixing and stirring lignin fiber, nano calcium carbonate and 4/5 sulfonated asphalt for 10-20min, then adding water and a chelating agent, stirring, carrying out chelation reaction for 3-4h at the temperature of 40-60 ℃, heating to 80 +/-5 ℃, sequentially adding polyethylene powder and modified polyvinyl alcohol, stirring for 40-60min, then adding the rest sulfonated asphalt, stirring for 20min, then adding n-pentane, then reacting for 2.5-3h at the temperature of 45-55 ℃, and drying to obtain the plugging and anti-collapse agent.
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| CN110330952A (en) * | 2019-07-03 | 2019-10-15 | 济源市宏鑫实业有限公司 | A kind of film forming sealing agent |
| CN111303844B (en) * | 2020-04-11 | 2022-03-08 | 北京宏勤石油助剂有限公司 | Asphalt resin anti-sloughing agent for drilling fluid and preparation method thereof |
| CN111777997B (en) * | 2020-09-07 | 2021-01-05 | 胜利油田胜利化工有限责任公司 | Preparation method of drilling fluid inhibiting anti-sloughing agent |
| CN114716701A (en) * | 2022-04-20 | 2022-07-08 | 湖南骏泰新材料科技有限责任公司 | Preparation method and application of modified lignin-based gel water shutoff agent |
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