CN109852353B - High-temperature-resistant fluid loss additive for drilling fluid and preparation method thereof - Google Patents
High-temperature-resistant fluid loss additive for drilling fluid and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a high-temperature resistant fluid loss additive for drilling fluid, which is prepared from the following raw materials, by weight, 35-55 parts of synthetic resin, 15-25 parts of aldehyde ketone resin, 45-65 parts of sulfonated asphalt formed by sulfonating natural asphalt, 5-15 parts of initiator B, 10-20 parts of nano calcium carbonate and 60-80 parts of vinyl monomer polymer. The invention also discloses a preparation method of the high-temperature-resistant fluid loss additive, which comprises the following steps: stirring sulfonated asphalt and vinyl monomer polymer for 30-40min at 45-60 ℃, adding an initiator B, stirring for 2-3h, then adding nano calcium carbonate, heating to 95-120 ℃, then adding synthetic resin and aldehyde ketone resin, stirring, reacting for 4-5h at the temperature of 100 ℃ and 110 ℃, and drying to obtain the high-temperature resistant fluid loss additive. The high-temperature-resistant filtrate reducer has the advantages of excellent filtrate reduction performance, strong crack plugging capability, stable slurry rheological property, well wall stability and excellent high-temperature-resistant and salt-resistant performance.
Description
Technical Field
The invention relates to the field of additives for drilling fluid, in particular to a high-temperature-resistant fluid loss additive for drilling fluid and a preparation method thereof.
Background
The filtrate reducer is a chemical additive which needs to be added in the oil field drilling fluid, and is also called a filtrate reducer and a filtrate reducer. During drilling, the invasion of the filtrate of the drilling fluid into the formation can cause hydration and expansion of shale, and in severe cases, the wellbore is unstable and various downhole complications are caused. The purpose of adding the fluid loss additive is to reduce the fluid loss of the drilling fluid as much as possible by forming a low-permeability, flexible, thin and compact filter cake on the well wall, and the fluid loss additive is an important drilling fluid treating agent for ensuring the stable performance of the drilling fluid, reducing the filtration loss of harmful liquid to a stratum, stabilizing the well wall and ensuring the well diameter regulation.
The addition of the filtrate reducer can obviously reduce the filtration loss of the drilling fluid, maintain and stabilize the well wall and ensure that the drilling is carried out quickly and safely. With the increasing drilling depth and the increasing complexity of the drilling bottom layer, higher requirements are put on the drilling fluid, and the drilling fluid treating agent is required to have corresponding functions, particularly higher requirements on temperature resistance and salt resistance.
The existing filtrate reducers are mainly divided into the following categories: cellulose, humic acid, acrylic polymer, resin and starch. The fiber product comprises sodium carboxymethyl cellulose, polyanionic cellulose, sodium carboxyethyl cellulose and the like, has excellent filtrate loss reduction performance and wide application system range, but obviously improves the viscosity of the drilling fluid, and has high price and poor temperature resistance;
humic acid products comprise lignite alkali liquor, sodium nitrohumate, chromium humic acid, sulfomethyl lignite and the like, the products can reduce filtration loss and viscosity at the same time, and have certain temperature resistance, but the filtrate pollutes the environment, damages an oil gas reservoir, has harsh production process conditions and has great damage to the bodies of operators;
the acrylic acid polymer comprises hydrolyzed polyacrylonitrile ammonium salt, polyacrylate polymer and the like, propionate multipolymer and the like, the product has the functions of resisting salt, increasing viscosity and improving cutting simultaneously, thereby inhibiting shale expansion, the process is simple, but the calcium resistance is weaker, the temperature resistance is poor, and the raw materials and the product have sour taste;
the resin products comprise petroleum resin, sulfonated lignite resin, sulfonated lignin petroleum resin condensate and the like, and the products have good high-temperature resistance, lubricity and collapse resistance, but relatively poor filtration loss reduction performance and environmental pollution;
starch products comprise carboxymethyl starch, carboxypropyl starch, pregelatinized starch, high temperature resistant starch, modified starch and the like, belong to natural polymers and derivatives thereof, are easy to degrade and have good environmental protection performance, but have poor high temperature resistance, complex modification process and easy fermentation and deterioration, and cannot be used and stored for a long time.
Therefore, the research on the filtrate reducer with good comprehensive effect, which is demanded by the market, has great significance for the research on the filtrate reducer with strong crack plugging capability, stable slurry rheology, good filtrate reduction performance and good high-temperature resistance and salt resistance.
Disclosure of Invention
Aiming at the defects in the prior art, the first object of the invention is to provide a high-temperature-resistant fluid loss additive for drilling fluid, which has the advantages of excellent fluid loss reducing performance, stronger capability of plugging cracks, stable slurry rheological property, well wall stability and excellent high-temperature-resistant and salt-resistant performance.
The second purpose of the invention is to provide a preparation method of the high-temperature-resistant fluid loss additive for the drilling fluid, which has the advantages that the prepared high-temperature-resistant fluid loss additive has excellent fluid loss performance, stronger capability of plugging cracks, stable slurry rheological property, well wall stability and excellent high-temperature-resistant and salt-resistant performance.
In order to achieve the first object, the invention provides the following technical scheme: the high-temperature resistant fluid loss additive for the drilling fluid is prepared from, by weight, 35-55 parts of synthetic resin, 15-25 parts of aldehyde ketone resin, 45-65 parts of sulfonated asphalt formed by sulfonating natural asphalt, 5-15 parts of an initiator B, 10-20 parts of nano calcium carbonate and 60-80 parts of a vinyl monomer polymer, wherein the vinyl monomer polymer is prepared by polymerizing 2-acrylamide-2-methylpropanesulfonic acid, acrylonitrile and N, N' -dimethylacrylamide under the condition of an initiator A ammonium persulfate.
By adopting the technical scheme, the alkene monomer polymer has excellent high temperature resistance and filtration loss reduction performance, and when the clean water end of the sulfonated asphalt is adsorbed on the shale interface, the oleophilic end can cover the shale surface, so that the mud cake quality is improved, the filtration loss of the drilling fluid is reduced, and the hydration dispersion of shale particles is prevented to play a role in preventing collapse; meanwhile, the oleophylic part can fill pore throats and cracks to play a role in plugging. The synthetic resin and the aldehyde ketone resin have good thermal stability and good salt resistance and filtrate loss reduction performance, and the aldehyde ketone resin does not contain benzene, ketone and other substances and has good environmental protection performance. The finally prepared high-temperature resistant fluid loss additive has excellent fluid loss performance, strong capability of plugging cracks, stable mud rheology, improved mud cake quality, stable shale bottom layer and stable well wall. Besides, the materials are nontoxic, do not pollute the environment, do not pollute the stratum, are suitable for exploratory well operation and marine drilling operation, have good compatibility with drilling fluid, and simultaneously have the functions of preventing collapse, preventing swelling and the like, and have excellent comprehensive effect.
Furthermore, the high-temperature resistant fluid loss additive for the drilling fluid is prepared from the following raw materials, by weight, 38-45 parts of synthetic resin, 17-23 parts of aldehyde ketone resin, 47-60 parts of sulfonated asphalt formed by sulfonating natural asphalt, 7-13 parts of an initiator B, 12-17 parts of nano calcium carbonate and 65-75 parts of an alkene monomer polymer.
Furthermore, the high-temperature resistant fluid loss additive for the drilling fluid is prepared from the following raw materials, by weight, 42 parts of synthetic resin, 20 parts of aldehyde ketone resin, 50 parts of sulfonated asphalt formed by sulfonating natural asphalt, 10 parts of an initiator B, 15 parts of nano calcium carbonate and 70 parts of an alkene monomer polymer.
Further, the preparation method of the vinyl monomer polymer comprises the following steps: dissolving sodium hydroxide in water until the pH value of the aqueous solution is 9-10, adding 2-acrylamide-2-methylpropanesulfonic acid under the stirring condition, stirring at the temperature of 40-50 ℃, stirring for 15-20min to dissolve, then adding acrylonitrile and N, N' -dimethylacrylamide, stirring, adjusting the pH value of the solution to 8.5-9 during the stirring process, stirring at the temperature of 75-90 ℃ for 30-40min, adding an initiator A ammonium persulfate, and stirring and reacting for 40-60min under the condition that the rotating speed is 3000 and 4500 r/min;
then granulating in a double-screw extruder at the extrusion temperature of 120-140 ℃ and the screw rotation speed of 300-450r/min, drying and crushing at the temperature of 100-120 ℃ after granulation, and sieving by a sieve of 60-80 meshes to obtain the vinyl monomer polymer.
Furthermore, in the preparation method of the vinyl monomer polymer, 50-70 parts of 2-acrylamide-2-methylpropanesulfonic acid, 40-65 parts of acrylonitrile, 25-30 parts of N, N' -dimethylacrylamide and 3-5 parts of ammonium persulfate are added.
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 rate of the sulfur trioxide gas is 0.045-0.6m 3/h.
Further, the initiator B is azobisisobutyronitrile or dimethyl azobisisobutyrate.
Further, the synthetic resin comprises petroleum resin and synthetic acrylic resin, and the mass ratio of the petroleum resin to the synthetic acrylic resin is 1: 5-8.
In order to achieve the second object, the invention provides the following technical scheme: a preparation method of a high-temperature resistant fluid loss additive for drilling fluid comprises the following steps:
stirring sulfonated asphalt and vinyl monomer polymer for 30-40min at 45-60 ℃, adding an initiator B, stirring for 2-3h, then adding nano calcium carbonate, heating to 95-120 ℃, then adding synthetic resin and aldehyde ketone resin, stirring, reacting for 4-5h at the temperature of 100 ℃ and 110 ℃, and drying to obtain the high-temperature resistant fluid loss additive.
In conclusion, the invention has the following beneficial effects:
1. according to the invention, through adding the synthetic resin, the aldehyde ketone resin, the sulfonated asphalt and the vinyl monomer polymer, the finally prepared high-temperature resistant fluid loss additive has excellent fluid loss performance, stronger crack plugging capability, stable slurry rheological property, well wall stability and excellent high-temperature resistance and salt resistance;
2. the high-temperature resistant filtrate reducer prepared by the invention is nontoxic, does not pollute the environment, does not pollute the stratum, is suitable for exploratory well operation and marine drilling operation, has good compatibility with drilling fluid, and simultaneously has the functions of preventing collapse, preventing swelling and the like, and has excellent comprehensive effect;
3. 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;
4. the synthetic resin and the aldehyde ketone resin have good thermal stability and good salt resistance and filtrate loss reduction performance, and the aldehyde ketone resin does not contain benzene, ketone and other substances and has good environmental protection performance.
Detailed Description
The present invention will be described in further detail with reference to examples.
The starting materials in the following preparations and examples are commercially available.
Examples of preparation of raw materials
Preparation examples 1 to 3 are examples of vinyl monomer polymers, and preparation examples 4 to 6 are examples of sulfonated asphalts.
Preparation example 1
The preparation method of the vinyl monomer polymer comprises the following steps: dissolving sodium hydroxide in water in parts by weight until the pH value of an aqueous solution is 9.5, adding 60 parts of 2-acrylamide-2-methylpropanesulfonic acid under the stirring condition, stirring at 45 ℃ for 18min to dissolve, then adding 50 parts of acrylonitrile and 28 parts of N, N-dimethylacrylamide, stirring, adjusting the pH value of the solution to 8.5 in the stirring process, stirring at 80 ℃ for 35min, adding 4 parts of initiator A ammonium persulfate, and stirring at the rotation speed of 4000r/min for reacting for 50 min;
then granulating in a double-screw extruder at 130 ℃ and a screw rotating speed of 400r/min, drying and crushing at 110 ℃ after granulation, and sieving with a 70-mesh sieve to obtain the alkene monomer polymer.
Preparation example 2
The preparation method of the vinyl monomer polymer is carried out according to the method in preparation example 1, except that sodium hydroxide is dissolved in water until the pH value of the aqueous solution is 9, 50 parts of 2-acrylamido-2-methylpropanesulfonic acid is added under the stirring condition, the stirring temperature is 40 ℃, the stirring is carried out for 15min to dissolve the aqueous solution, then 40 parts of acrylonitrile and 25 parts of N, N, -dimethylacrylamide are added, the stirring is carried out, the pH value of the solution is adjusted to be 8.5 in the stirring process, the stirring is carried out for 30min at 75 ℃, 3 parts of initiator A ammonium persulfate is added, and the stirring reaction is carried out for 40min under the condition that the rotating speed is 3000 r/min;
then granulating in a double-screw extruder at the extrusion temperature of 120 ℃ and the screw rotating speed of 300r/min, drying and crushing at the temperature of 100 ℃ after granulation, and sieving by a 60-mesh sieve to obtain the alkene monomer polymer.
Preparation example 3
The vinyl monomer polymer was prepared by the method of preparation example 1, except that sodium hydroxide was dissolved in water until the pH of the aqueous solution was 10, 70 parts of 2-acrylamido-2-methylpropanesulfonic acid was added under stirring at 50 ℃ for 20min, followed by addition of 65 parts of acrylonitrile and 30 parts of N, -dimethylacrylamide, followed by stirring, wherein the pH of the solution was adjusted to 9 during stirring, stirring at 90 ℃ for 40min, addition of 5 parts of initiator a ammonium persulfate, and stirring at 4500r/min for 60 min;
then granulating in a double-screw extruder at the extrusion temperature of 140 ℃ and the screw rotation speed of 450r/min, drying and crushing at 120 ℃ after granulation, and sieving with a 80-mesh sieve to obtain the alkene monomer polymer.
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 rate of sulfur trioxide gas was 0.5m 3/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 rate of sulfur trioxide gas was 0.045m 3/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 rate of sulfur trioxide gas was 0.6m 3/h.
Examples
The high temperature resistant filtrate reducer for drilling fluid is prepared with the material including synthetic resin 35-55 weight portions, aldehyde ketone resin 15-25 weight portions, sulfonated asphalt formed through sulfonation of natural asphalt 45-65 weight portions, initiator B5-15 weight portions, nanometer calcium carbonate 10-20 weight portions and vinyl monomer polymer 60-80 weight portions.
Wherein the initiator B is azobisisobutyronitrile or dimethyl azobisisobutyrate;
the synthetic resin comprises petroleum resin (obtained from Chilo-Ci-Gong-trade company, Inc. of Laizhou, model number M4100) and synthetic acrylic resin (obtained from Kelison resin, Inc. of Guangdong, model number KN1076F), and the mass ratio of the petroleum resin to the synthetic acrylic resin is 1: 5-8;
the sulfonated asphalt is the sulfonated asphalt prepared in preparation examples 4-6, and the vinyl monomer polymer is the vinyl monomer polymer prepared in preparation examples 1-3;
the aldehyde ketone resin was purchased from Jinan remote aldehyde ketone resin, Inc. under the brand name advocate Tai, model number KR-120.
Example 1
A preparation method of a high-temperature-resistant fluid loss additive for drilling fluid comprises the following steps in parts by weight:
stirring 50 parts of sulfonated asphalt and 70 parts of vinyl monomer polymer for 35min at 50 ℃, adding 10 parts of initiator B, stirring for 2.5h, then adding 15 parts of nano calcium carbonate, heating to 110 ℃, then adding 42 parts of synthetic resin and 20 parts of aldehyde ketone resin, stirring, carrying out heat preservation reaction for 4.5h at 105 ℃, and drying to obtain the high-temperature-resistant filtrate reducer.
Wherein the sulfonated asphalt is the sulfonated asphalt prepared in preparation example 4, and the vinyl monomer polymer is the vinyl monomer polymer prepared in preparation example 1;
the initiator B is azobisisobutyronitrile; the synthetic resin is formed by mixing petroleum resin and synthetic acrylic resin according to the mass ratio of 1: 6.
Example 2
A preparation method of a high-temperature-resistant filtrate reducer for drilling fluid is carried out according to the method in example 1, and is characterized in that 47 parts of sulfonated asphalt and 65 parts of vinyl monomer polymer are stirred for 35min at 50 ℃, 7 parts of initiator B are added, stirring is carried out for 2.5h, then 12 parts of nano calcium carbonate is added, the temperature is raised to 110 ℃, then 38 parts of synthetic resin and 17 parts of aldehyde ketone resin are added, stirring is carried out, heat preservation reaction is carried out for 4.5h at 105 ℃, and drying is carried out, so that the high-temperature-resistant filtrate reducer is obtained.
Example 3
The preparation method of the high-temperature-resistant filtrate reducer for the drilling fluid is carried out according to the method in the embodiment 1, and is characterized in that 60 parts of sulfonated asphalt and 75 parts of vinyl monomer polymer are stirred for 35min at 50 ℃, 13 parts of initiator B are added, the stirring is carried out for 2.5h, then 17 parts of nano calcium carbonate is added, the temperature is raised to 110 ℃, then 45 parts of synthetic resin and 23 parts of aldehyde ketone resin are added, the stirring is carried out, the heat preservation reaction is carried out for 4.5h at 105 ℃, and the drying is carried out, so that the high-temperature-resistant filtrate reducer is obtained.
Example 4
The preparation method of the high-temperature-resistant filtrate reducer for the drilling fluid is carried out according to the method in the embodiment 1, and is characterized in that 45 parts of sulfonated asphalt and 60 parts of vinyl monomer polymer are stirred for 35min at 50 ℃, 5 parts of initiator B are added, stirring is carried out for 2.5h, then 10 parts of nano calcium carbonate is added, the temperature is raised to 110 ℃, then 35 parts of synthetic resin and 15 parts of aldehyde ketone resin are added, stirring is carried out, heat preservation reaction is carried out for 4.5h at 105 ℃, and drying is carried out, so that the high-temperature-resistant filtrate reducer is obtained.
Example 5
The preparation method of the high-temperature-resistant filtrate reducer for the drilling fluid is carried out according to the method in the embodiment 1, and is characterized in that 65 parts of sulfonated asphalt and 80 parts of vinyl monomer polymer are stirred for 35min at 50 ℃, 15 parts of initiator B are added, stirring is carried out for 2.5h, then 20 parts of nano calcium carbonate is added, the temperature is raised to 110 ℃, 55 parts of synthetic resin and 25 parts of aldehyde ketone resin are added, stirring is carried out, heat preservation reaction is carried out for 4.5h at 105 ℃, and drying is carried out, so that the high-temperature-resistant filtrate reducer is obtained.
Example 6
The preparation method of the high-temperature-resistant fluid loss additive for the drilling fluid is carried out according to the method in the example 1, and the difference is that the vinyl monomer polymer is the vinyl monomer polymer prepared in the preparation example 2.
Example 7
The preparation method of the high-temperature-resistant fluid loss additive for the drilling fluid is carried out according to the method in the example 1, and the difference is that the vinyl monomer polymer is the vinyl monomer polymer prepared in the preparation example 3.
Example 8
The preparation method of the high-temperature-resistant fluid loss additive for the drilling fluid is carried out according to the method in the example 1, except that the sulfonated asphalt is the sulfonated asphalt prepared in the preparation example 5.
Example 9
The preparation method of the high-temperature-resistant fluid loss additive for the drilling fluid is carried out according to the method in the example 1, except that the sulfonated asphalt is the sulfonated asphalt prepared in the preparation example 6.
Example 10
The preparation method of the high-temperature-resistant fluid loss additive for the drilling fluid is carried out according to the method in the example 1, except that the initiator B is dimethyl azodiisobutyrate.
Example 11
The preparation method of the high-temperature-resistant fluid loss additive for the drilling fluid is carried out according to the method in the example 1, and is characterized in that the synthetic resin is formed by mixing petroleum resin and synthetic acrylic resin according to the mass ratio of 1: 5.
Example 12
The preparation method of the high-temperature-resistant fluid loss additive for the drilling fluid is carried out according to the method in the example 1, and is characterized in that synthetic resin is formed by mixing petroleum resin and synthetic acrylic resin according to the mass ratio of 1: 8.
Example 13
The preparation method of the high-temperature-resistant fluid loss additive for the drilling fluid is carried out according to the method in the embodiment 1, and is characterized in that 50 parts of sulfonated asphalt and 70 parts of vinyl monomer polymer are stirred for 30min at 45 ℃, 10 parts of initiator B are added and stirred for 2h, then 15 parts of nano calcium carbonate are added, the temperature is raised to 95 ℃, then 42 parts of synthetic resin and 20 parts of aldehyde ketone resin are added and stirred, the reaction is carried out for 4h at 100 ℃, and drying is carried out, so as to obtain the high-temperature-resistant fluid loss additive.
Example 14
The preparation method of the high-temperature-resistant fluid loss additive for the drilling fluid is carried out according to the method in the embodiment 1, and is characterized in that 50 parts of sulfonated asphalt and 70 parts of vinyl monomer polymer are stirred for 40min at 60 ℃, 10 parts of initiator B are added and stirred for 3h, then 15 parts of nano calcium carbonate are added, the temperature is raised to 120 ℃, then 42 parts of synthetic resin and 20 parts of aldehyde ketone resin are added and stirred, the reaction is carried out for 5h at 110 ℃, and drying is carried out, so as to obtain the high-temperature-resistant fluid loss additive.
Comparative example 1
The preparation method of the high-temperature-resistant fluid loss additive for the drilling fluid is carried out according to the method in the example 1, and the difference is that the sulfonated asphalt added in the preparation process is purchased from Mingtai chemical industry Co., Ltd, Henan province, and the brand is Mingtai/FT-1.
Comparative example 2
The preparation method of the high-temperature-resistant fluid loss additive for the drilling fluid is carried out according to the method in the example 1, and is characterized in that vinyl monomer polymers are not added.
Comparative example 3
The preparation method of the high-temperature-resistant fluid loss additive for the drilling fluid is carried out according to the method in the example 1, except that the initiator B is not added.
Performance detection
The performance of the high-temperature-resistant fluid loss additive prepared in the examples 1 to 14 and the comparative examples 1 to 3 is tested, the samples in the following test methods are the high-temperature-resistant fluid loss additives prepared in the examples 1 to 14 and the comparative examples 1 to 3, and the test items and the test methods are 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. Apparent viscosity measurement of 1% aqueous solution
Measuring 400ml tap water, adding 4g sample under high speed stirring, stirring for 5min, and measuring with six-speed viscometer
Read the values and calculate their apparent viscosity.
6. Determination of high-temperature high-pressure filtration loss reduction rate
6.1 base stock preparation
According to the proportion of 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;
6.2 determination of base stock Properties
Taking 400ml of the prepared base slurry in 6.1, 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-mixing soil for the test;
6.3 determination of 200 ℃ Properties of the test slurries
Taking 400ml of the adjusted base slurry in 6.2, stirring and adding 12.0g of the sample, stirring at high speed for 20min, stopping at least twice in the period, scraping off the sample piece adhered to the wall of the container, and measuring the filtration loss reduction rate of 3450KPa at 200 ℃.
The filtrate loss reduction rate at high temperature and high pressure is (A-B)/A100%
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. 10% NaCl API assay
7.1 base stock preparation
According to the proportion of distilled water: sodium chloride: slurry preparation soil for test: preparing base slurry by the anhydrous sodium carbonate in a ratio of 400:40:20:1, stirring at high speed for 20min, stopping stirring at least twice during the stirring, scraping off clay adhered to the wall of a container, and sealing and maintaining at room temperature for 24h to obtain the base slurry;
7.2 base stock Performance determination
Taking 400ml of the prepared base slurry in 7.1, stirring at a high speed for 5min, measuring the filtration loss of the base slurry, wherein the measurement result is within the range of 120 +/-10 ml, and otherwise, adjusting the addition amount of the slurry-preparing soil for the test;
7.3 determination of 200 ℃ Performance of the test slurries
Taking 400ml of the adjusted base slurry in 7.3, stirring and adding 16.0g of sample, stirring at high speed for 20min, stopping at least twice in the period, scraping off the sample piece adhered to the wall of the container, transferring to an aging tank, aging at 200 ℃ for 16h, taking out, and measuring the API value at room temperature.
8. 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.
9. 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 (6)
1. The high-temperature-resistant fluid loss additive for the drilling fluid is characterized by being prepared from the following raw materials, by weight, 35-55 parts of synthetic resin, 15-25 parts of aldehyde ketone resin, 45-65 parts of sulfonated asphalt formed by sulfonating natural asphalt, 5-15 parts of initiator B, 10-20 parts of nano calcium carbonate and 60-80 parts of vinyl monomer polymer, wherein the vinyl monomer polymer is formed by polymerizing 2-acrylamide-2-methylpropanesulfonic acid, acrylonitrile and N, N-dimethylacrylamide under the condition of ammonium persulfate as the initiator A;
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；
The initiator B is azobisisobutyronitrile or dimethyl azobisisobutyrate;
the synthetic resin comprises petroleum resin and synthetic acrylic resin, and the mass ratio of the petroleum resin to the synthetic acrylic resin is 1: 5-8.
2. The high-temperature-resistant fluid loss additive for drilling fluid as claimed in claim 1, which is prepared from the following raw materials, by weight, 38-45 parts of synthetic resin, 17-23 parts of aldehyde ketone resin, 47-60 parts of sulfonated asphalt formed by sulfonating natural asphalt, 7-13 parts of an initiator B, 12-17 parts of nano calcium carbonate and 65-75 parts of an alkene monomer polymer.
3. The high-temperature-resistant fluid loss additive for drilling fluid as claimed in claim 1, which is prepared from 42 parts of synthetic resin, 20 parts of aldehyde ketone resin, 50 parts of sulfonated asphalt formed by sulfonating natural asphalt, 10 parts of initiator B, 15 parts of nano calcium carbonate and 70 parts of vinyl monomer polymer.
4. The high-temperature-resistant fluid loss additive for drilling fluid as claimed in claim 1, wherein the preparation method of the vinyl monomer polymer comprises the following steps: dissolving sodium hydroxide in water until the pH value of the aqueous solution is 9-10, adding 2-acrylamide-2-methylpropanesulfonic acid under the stirring condition, stirring at the temperature of 40-50 ℃, stirring for 15-20min to dissolve, then adding acrylonitrile and N, N-dimethylacrylamide, stirring, adjusting the pH value of the solution to 8.5-9 during the stirring process, stirring at the temperature of 75-90 ℃ for 30-40min, adding an initiator A ammonium persulfate, and stirring and reacting for 40-60min under the condition that the rotating speed is 3000 and 4500 r/min;
then granulating in a double-screw extruder at the extrusion temperature of 120-140 ℃ and the screw rotation speed of 300-450r/min, drying and crushing at the temperature of 100-120 ℃ after granulation, and sieving by a sieve of 60-80 meshes to obtain the vinyl monomer polymer.
5. The high-temperature-resistant fluid loss additive for drilling fluid according to claim 1, wherein 50-70 parts of 2-acrylamido-2-methylpropanesulfonic acid, 40-65 parts of acrylonitrile, 25-30 parts of N, N-dimethylacrylamide and 3-5 parts of ammonium persulfate are added in the preparation method of the vinyl monomer polymer in parts by weight.
6. The preparation method of the high-temperature-resistant fluid loss additive for the drilling fluid as claimed in any one of claims 1 to 5, wherein the preparation method comprises the following steps:
stirring sulfonated asphalt and vinyl monomer polymer for 30-40min at 45-60 ℃, adding an initiator B, stirring for 2-3h, then adding nano calcium carbonate, heating to 95-120 ℃, then adding synthetic resin and aldehyde ketone resin, stirring, reacting for 4-5h at the temperature of 100 ℃ and 110 ℃, and drying to obtain the high-temperature resistant fluid loss additive.
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| CN110699052B (en) * | 2019-10-11 | 2021-10-15 | 北京宏勤石油助剂有限公司 | Temperature-resistant salt-resistant fluid loss agent for drilling fluid and preparation method thereof |
| CN110684513A (en) * | 2019-10-11 | 2020-01-14 | 北京宏勤石油助剂有限公司 | Plugging fluid loss additive for drilling fluid and preparation method thereof |
| CN111454392A (en) * | 2020-03-18 | 2020-07-28 | 滨州德润化工有限责任公司 | Temperature-resistant composite salt-resistant fluid loss agent for drilling fluid |
| CN114106791B (en) * | 2021-12-01 | 2023-01-17 | 北京宏勤石油助剂有限公司 | Oil-based asphalt resin anti-collapse agent and preparation method thereof |
| CN114605970B (en) * | 2022-03-24 | 2023-09-26 | 长江大学 | Humic acid resin filtrate reducer for drilling fluid and preparation method thereof |
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