CN114805680A - Environment-friendly high-temperature-resistant salt-resistant tackifier for water-based drilling fluid and preparation method and application thereof - Google Patents
Environment-friendly high-temperature-resistant salt-resistant tackifier for water-based drilling fluid and preparation method and application thereof Download PDFInfo
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Abstract
The invention provides an environment-friendly high-temperature-resistant salt-resistant tackifier for water-based drilling fluid and a preparation method and application thereof. The preparation method comprises the following steps: adding an alkene monomer, an anion monomer and a cation monomer into water, and uniformly stirring to obtain a water phase A; adding a crosslinking monomer, an emulsifier and an ester monomer into white oil, and emulsifying to obtain an oil phase B; mixing the water phase A and the oil phase B, emulsifying, and adjusting the pH of the system to 6-9 to obtain an emulsion; adding an initiator aqueous solution in a nitrogen atmosphere to perform reaction; after the reaction is finished, acetone is used for precipitation, and the product is obtained after filtration, washing and drying. The water-soluble high-temperature-resistant polymer tackifier with a certain network structure is prepared by an inverse emulsion polymerization method, has excellent tackifying performance on water-based drilling fluid in a high-temperature environment of 180 ℃, is non-toxic and easy to biodegrade, and overcomes the defect of insufficient high-temperature stability of the existing water-based drilling fluid polymer tackifier.
Description
Technical Field
The invention relates to an environment-friendly high-temperature-resistant salt-resistant tackifier for water-based drilling fluid and a preparation method and application thereof, belonging to the field of oilfield chemistry of petroleum industry.
Background
With the continuous increase of the energy demand of economic development in China, the exploration and development of petroleum and natural gas begin to develop from a middle shallow layer to a deep layer. The bottom temperature of the deep stratum is high, and a salt-gypsum layer is generally drilled, so that the drilling fluid has higher and higher requirements on temperature resistance and salt resistance. The water-based drilling fluid is one of the key technologies for drilling high-temperature stratum, however, when deep oil reservoir is drilled, various components in the drilling fluid in the well are easily degraded under the high-temperature condition along with the rise of the stratum temperature, and the drilling quality is seriously influenced. Therefore, the excellent stability of the water-based drilling fluid under high temperature conditions plays a crucial role in safe and efficient oil and gas drilling.
Under high temperature and high salt conditions, the viscosity and shear force of the drilling fluid are kept in appropriate ranges in order to keep the well bore clean and safe drilling. When the viscosity is too low, the viscosity can be improved by increasing the content of bentonite, but the method can increase the solid content in the drilling fluid, and is not beneficial to improving the mechanical drilling rate and protecting hydrocarbon reservoirs. It is therefore often desirable to add a viscosifier to increase the viscosity of the drilling fluid and improve its rheological properties. The tackifier is one of high temperature resistant drilling fluid core treating agents, the type of the conventional tackifier is mainly high molecular polymer, and the main tackifying mechanism is that polymer molecules form a grid structure through a bridging effect to improve the viscosity of the drilling fluid. The temperature resistance of the polymer tackifier is closely related to the molecular structure of the polymer tackifier, the temperature resistance of the tackifier can be obviously improved by optimizing the molecular structure of the polymer, and the method can be realized by the following steps: (1) increasing the molecular weight of the polymer; (2) the primary structure of the molecule should select monomers with good thermal stability and with C-C, C-N and C-S bonds as main chains; (3) the molecular secondary structure has certain branched chain type and body type structures; (4) monomers incorporating specific molecular structures such as hydrolysis and rigid groups.
Chinese patent document CN110643335A provides a modified vegetable gum tackifier, which is composed of the following components in parts by weight: 7-11 parts of guar gum, 0.6-1 part of hydrolyzed polyacrylamide, 1.1-1.3 parts of borax, 0.8-1.5 parts of sodium hydroxide aqueous solution, 1.2-1.5 parts of ethylene oxide and 6-6.5 parts of polyurethane. Although the modified vegetable gum tackifier has better viscosity and certain environmental protection performance, the modified vegetable gum tackifier has limited temperature resistance in oil field application and generally cannot meet the temperature resistance requirement of a drilling construction site, so that the modified vegetable gum tackifier cannot be widely applied.
Chinese patent document CN111662690A provides a tackifier, which comprises the following raw materials in parts by mass: 26-32 parts of acrylamide, 8-10 parts of sodium acrylate, 25-34 parts of xanthan gum, 31-37 parts of polyanionic cellulose, 8-16 parts of emulsion stabilizer, 1-3 parts of initiator and 60-120 parts of water. The tackifier has obvious temperature and viscosity resistant effect, but is not comprehensive in salt resistance performance test, has limited salt resistance performance and is difficult to be widely applied.
Chinese patent document CN113583191A provides a preparation method of an environment-friendly high-temperature-resistant salt-resistant tackifier for water-based drilling fluid, which comprises the following steps: 1) dissolving an emulsifier and an ester monomer in water together, and fully shearing and emulsifying to obtain emulsion A; 2) mixing an alkene monomer, an ether monomer and a cross-linking agent monomer, and uniformly stirring and mixing at a low speed to obtain a water phase B; 3) mixing the emulsion A and the water phase B, stirring and emulsifying, and adjusting the pH value to 6-9 to obtain a mixed reaction solution; 4) and (2) adding an initiator into the mixed reaction liquid in an inert atmosphere and in an environment with the temperature of 60-80 ℃, stirring at a low speed for reaction, and obtaining the polymer tackifier after the reaction is finished, wherein the synthesized product of the tackifier is emulsion, is unstable in performance, is static and easy to layer, and cannot be directly applied to the oil field in a large range.
Currently, viscosifiers for water-based drilling fluids have the following disadvantages: (1) the high temperature resistance is insufficient, the current common tackifier can be degraded at high temperature under the high temperature condition, and the tackifying performance can be obviously reduced; (2) insufficient salt resistance, reduced tackifying performance under high salt conditions; (3) the environmental protection performance is insufficient, and along with the improvement of the environmental protection requirement of the oil field, the environmental protection performance of various treating agents is higher and higher.
Therefore, the development of the environment-friendly high-temperature-resistant salt-resistant tackifier for the water-based drilling fluid is of great significance.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides an environment-friendly high-temperature-resistant salt-resistant tackifier for water-based drilling fluid and a preparation method and application thereof. The water-soluble high-temperature-resistant polymer tackifier with a certain network structure is prepared by using different alkenyl-containing monomers as main raw materials through an inverse emulsion polymerization method, has excellent tackifying performance on water-based drilling fluid in a high-temperature environment of 180 ℃, is non-toxic and easy to biodegrade, and overcomes the defect of insufficient high-temperature stability of the conventional water-based drilling fluid polymer tackifier.
The technical scheme of the invention is as follows:
a preparation method of an environment-friendly high-temperature-resistant salt-resistant tackifier for water-based drilling fluid comprises the following steps:
(1) adding an alkene monomer, an anion monomer and a cation monomer into water, and uniformly stirring to obtain a water phase A;
(2) adding a crosslinking monomer, an emulsifier and an ester monomer into white oil, and emulsifying to obtain an oil phase B;
(3) mixing the water phase A and the oil phase B, emulsifying, and adjusting the pH of the system to 6-9 to obtain an emulsion; adding an initiator aqueous solution in a nitrogen atmosphere to perform reaction; after the reaction is finished, acetone is used for precipitation, and the environment-friendly high-temperature-resistant salt-resistant tackifier for the water-based drilling fluid is obtained after filtration, washing and drying.
Preferably according to the invention, the olefinic monomer in step (1) is acrylamide, acrylic acid, N-dimethylacrylamide or N- (3-dimethylaminopropyl) methacrylamide; the ratio of the mass of the vinyl monomer to the volume of water is 1-15g:100mL, and more preferably 5-10g:100 mL.
According to the invention, the anionic monomer in the step (1) is one or the combination of more than two of 2-acrylamido-2-methyl propane sulfonic Acid (AMPS), 2-acryloyloxy-2-methyl propane sulfonic acid (MAOPS), sodium vinyl sulfonate and sodium allyl sulfonate; the mass ratio of the anionic monomer to the ethylenic monomer is 1.5 to 5:1, and more preferably 3 to 4: 1.
According to the invention, the cationic monomer in the step (1) is one or the combination of more than two of dimethyl diallyl ammonium chloride (DMDAAC), methacryloxyethyl trimethyl ammonium chloride (DMC) and dimethyl octadecyl [ 3-trimethoxysilylpropyl ] ammonium chloride; the mass ratio of the cationic monomer to the ethylenic monomer is 0.1 to 1:1, and more preferably 0.3 to 0.6: 1.
Preferably, according to the present invention, the stirring rate in step (1) is 200-400r/min, and the stirring time is 10-30 min.
Preferably according to the invention, the crosslinking monomer in step (2) is hydroxyethyl acrylate, triallylamine, ethylene glycol dimethacrylate or N-methylolacrylamide; the volume ratio of the crosslinking monomer to the white oil is 0.05 to 0.5 g/100 mL, and more preferably 0.1 to 0.2 g/100 mL.
Preferably according to the invention, the emulsifier in step (2) is Span80, Tween80 or OP-10; the ratio of the mass of the emulsifier to the volume of the white oil is 0.5-2g:100mL, more preferably 1-1.5g:100 mL.
Preferably according to the present invention, the ester monomer in step (2) is butyl acrylate, ethyl methacrylate or triallyl isocyanurate; the ratio of the mass of the ester monomer to the volume of the white oil is 1-10g:100mL, and more preferably 2-5g:100 mL.
According to the invention, the emulsification in the step (2) is preferably shear emulsification for 5-20min at a stirring speed of 2000r/min by using a shear emulsifying machine.
According to the present invention, the mass ratio of the ester monomer in the oil phase B to the vinyl monomer in the water phase A in step (3) is preferably 0.1 to 1.5:1, and more preferably 0.4 to 0.9: 1.
According to the invention, the emulsification in the step (3) is preferably shear emulsification for 15-20min at a stirring speed of 2000r/min by using a shear emulsifying machine.
According to the invention, in the step (3), NaOH solution with the mass fraction of 40% is used for adjusting the pH of the system to be 6-9.
Preferably according to the invention, the initiator in step (3) is ammonium persulfate, potassium persulfate or tert-butyl hydroperoxide; the mass fraction of the initiator aqueous solution is 0.5-1%; the addition mass of the initiator is 0.1-1% of the total mass of the alkene monomer, the temperature-resistant monomer and the cationic monomer.
Preferably according to the invention, the temperature of the reaction in step (3) is 40-60 ℃; the reaction time is 4-6 h.
According to the present invention, it is preferable that the ratio of the addition volume of acetone to the volume of the reaction solution in the step (3) is 1 to 3: 1.
According to the invention, the washing in the step (3) is preferably 3 to 5 times by using a mixed solvent of ethanol and water, wherein the volume ratio of ethanol to water in the mixed solvent is 1.5 to 2.5: 1; the drying is carried out for 16-24h at 80-90 ℃.
An environment-friendly high-temperature-resistant salt-resistant tackifier for water-based drilling fluid, which is prepared by adopting the preparation method.
According to the invention, the environment-friendly high-temperature-resistant salt-resistant tackifier for the water-based drilling fluid is applied to the water-based drilling fluid; preferably, the addition amount in the water-based drilling fluid is 5-10 g/L.
The invention has the following technical characteristics and beneficial effects:
1. the tackifier disclosed by the invention is excellent in temperature and salt resistance, and still has stable performance at a high temperature of 180 ℃ under the condition of 15% of salt addition. The molecular structure of the tackifier synthesized by the invention contains a carbon-carbon long chain, a double-bond structure, a sulfonic acid group and an amino group, so that the long chain structure is stably extended under the synergistic action of the sulfonic acid group, the thermal stability and rigidity of the tackifier can be increased, the copolymer is prevented from being hydrolyzed under the conditions of high temperature and high salt, and the temperature resistance and salt tolerance of the tackifier are improved. Particularly, when the vinyl monomer is N, N-dimethylacrylamide, tertiary amino on the long chain of the obtained tackifier effectively increases the steric hindrance of the copolymer under the protection of two methyl groups, and the temperature and salt resistance is more excellent.
2. In the synthetic process of the tackifier, a specific kind of ester monomer is introduced, a polar hydrophobic chain can enable a macromolecular chain of the tackifier to be in a stretching state, and hydrophobic association among product molecules is enhanced by a hydrophobic group, so that the macromolecular chain is physically crosslinked to form a spatial network structure with certain strength, the tackifier has strong tackifying capability, and meanwhile, the hydrophobic group can also increase the thermal stability of the tackifier and can resist the high temperature of 200 ℃; and the hydrophobic chain of the ester monomer is not too much or too long, the solubility and CMC are correspondingly reduced along with the increase of the number of carbon atoms in the hydrophobic group, spherical micelles are easy to form, the gyration radius of micelle particles is increased, the hydrophobic monomer is easy to generate excessive self-polymerization, products are easy to separate oil from water when the polymerization reaction is incomplete, the performance of the products is reduced, and even the failure of the polymerization experiment is caused, so that target products cannot be obtained.
3. The tackifier disclosed by the invention uses a specific kind of cross-linking agent and a specific amount of cross-linking agent in the synthetic process, so that different alkenyl monomers can be subjected to slight cross-linking, the polymerization degree of a molecular chain can be increased on one hand, and the molecular structural strength is increased by introducing a hydrophobic group to improve the temperature and salt resistance of the tackifier on the other hand; and simultaneously, the tackifier is ensured not to generate excessive crosslinking, so that the performance is reduced.
Detailed Description
The present invention is further illustrated by, but not limited to, the following examples.
Meanwhile, the experimental methods described in the following examples are all conventional methods unless otherwise specified; the reagents, materials and equipment are commercially available, unless otherwise specified.
The white oil used in the examples was # 5 white oil.
Example 1
A preparation method of an environment-friendly high-temperature-resistant salt-resistant tackifier for water-based drilling fluid comprises the following steps:
(1) 5g N, N-dimethylacrylamide, 17g 2-acrylamido-2-methylpropanesulfonic Acid (AMPS), 3g methacryloyloxyethyl trimethylammonium chloride (DMC), and 100mL of water were sequentially added to a 250mL beaker, and stirred for 20min at a stirring speed of 300r/min using a magnetic stirrer, to prepare an aqueous phase A.
(2) 0.1g N-methylolacrylamide, 1g of emulsifier Tween80 and 100mL of white oil were added to a 250mL beaker, followed by weighing 4.25g of butyl acrylate into the beaker and shearing and emulsifying for 20min at a stirring speed of 2000r/min using a shearing and emulsifying machine to obtain oil phase B.
(3) Mixing the water phase A obtained in the step (1) and the oil phase B obtained in the step (2), continuously emulsifying for 15min at the stirring speed of 2000r/min by using a shearing emulsifying machine, adjusting the pH of the system to 7 by using a NaOH solution with the mass fraction of 40%, finally transferring to a reaction device, and heating to 50 ℃ in a water bath kettle; adding 12.5g of ammonium persulfate aqueous solution with the mass fraction of 1% in a nitrogen environment, and reacting at 50 ℃ for 4 hours, wherein the stirring speed in the reaction process is 300 r/min; after the reaction is finished, adding 300mL of acetone into the reaction solution for precipitation, filtering, washing the obtained solid for 3 times by using a mixed solvent of ethanol and water (ethanol: water: 2:1, v/v), and drying at 80 ℃ for 16h to obtain the environment-friendly high-temperature-resistant salt-resistant tackifier for the water-based drilling fluid.
Example 2
A preparation method of an environment-friendly high-temperature-resistant salt-resistant tackifier for water-based drilling fluid comprises the following steps:
(1) 10g N, N-dimethylacrylamide, 17g 2-acrylamido-2-methylpropanesulfonic Acid (AMPS), 3g methacryloyloxyethyl trimethylammonium chloride (DMC), and 100mL of water were sequentially added to a 250mL beaker, and stirred for 20min at a stirring speed of 300r/min using a magnetic stirrer, to prepare an aqueous phase A.
(2) 0.1g N-methylolacrylamide, 1g of emulsifier Tween80 and 100mL of white oil were added to a 250mL beaker, followed by weighing 4.25g of butyl acrylate into the beaker and shearing and emulsifying for 20min at a stirring speed of 2000r/min using a shearing and emulsifying machine to obtain oil phase B.
(3) Mixing the water phase A obtained in the step (1) and the oil phase B obtained in the step (2), continuously emulsifying for 15min at the stirring speed of 2000r/min by using a shearing emulsifying machine, adjusting the pH of the system to 7 by using a NaOH solution with the mass fraction of 40%, finally transferring to a reaction device, and heating to 50 ℃ in a water bath kettle; adding 12.5g of ammonium persulfate aqueous solution with the mass fraction of 1% in a nitrogen environment, and reacting at 50 ℃ for 4 hours, wherein the stirring speed in the reaction process is 300 r/min; after the reaction is finished, adding 300mL of acetone into the reaction solution for precipitation, filtering, washing the obtained solid for 3 times by using a mixed solvent of ethanol and water (ethanol: water: 2:1, v/v), and drying at 80 ℃ for 16h to obtain the environment-friendly high-temperature-resistant salt-resistant tackifier for the water-based drilling fluid.
Example 3
A preparation method of an environment-friendly high-temperature-resistant salt-resistant tackifier for water-based drilling fluid comprises the following steps:
(1) 5g of acrylamide, 22g of 2-acrylamido-2-methylpropanesulfonic Acid (AMPS), 3g of methacryloyloxyethyl trimethylammonium chloride (DMC), and 100mL of water were sequentially added to a 250mL beaker, and stirred for 20min at a stirring speed of 300r/min using a magnetic stirrer, to prepare an aqueous phase A.
(2) 0.1g N-methylolacrylamide, 1g of emulsifier Tween80 and 100mL of white oil were added to a 250mL beaker, followed by weighing 4.25g of butyl acrylate into the beaker and shearing and emulsifying for 20min at a stirring speed of 2000r/min using a shearing and emulsifying machine to obtain oil phase B.
(3) Mixing the water phase A obtained in the step (1) and the oil phase B obtained in the step (2), continuously emulsifying for 15min at the stirring speed of 2000r/min by using a shearing emulsifying machine, adjusting the pH of the system to 7 by using a NaOH solution with the mass fraction of 40%, finally transferring to a reaction device, and heating to 50 ℃ in a water bath kettle; adding 12.5g of ammonium persulfate aqueous solution with the mass fraction of 1% in a nitrogen environment, and reacting at 50 ℃ for 4 hours, wherein the stirring speed in the reaction process is 300 r/min; after the reaction is finished, adding 300mL of acetone into the reaction solution for precipitation, filtering, washing the obtained solid for 3 times by using a mixed solvent of ethanol and water (ethanol: water: 2:1, v/v), and drying at 80 ℃ for 16h to obtain the environment-friendly high-temperature-resistant salt-resistant tackifier for the water-based drilling fluid.
Example 4
The preparation method of the environment-friendly high-temperature-resistant salt-resistant tackifier for the water-based drilling fluid is as described in example 1, except that: the amount of butyl acrylate added in step (2) was 2.25 g.
Example 5
The preparation method of the environment-friendly high-temperature-resistant salt-resistant tackifier for the water-based drilling fluid is as described in example 1, except that: and (3) changing butyl acrylate into ethyl methacrylate in the step (2).
Example 6
The preparation method of the environment-friendly high-temperature-resistant salt-resistant tackifier for the water-based drilling fluid is as described in example 1, except that: in the step (2), butyl acrylate is changed into triallyl isocyanurate.
Comparative example 1
The preparation method of the environment-friendly tackifier for the water-based drilling fluid is as in example 1, except that: tween80 was replaced with 1g of emulsifier OS in step (2).
Comparative example 2
The preparation method of the environment-friendly tackifier for the water-based drilling fluid is as in example 1, except that: step (3) is carried out at 80 ℃.
Comparative example 3
The preparation method of the environment-friendly tackifier for the water-based drilling fluid is as in example 1, except that: and (3) adjusting the pH value of the system to 11.
Comparative example 4
The preparation method of the environment-friendly tackifier for the water-based drilling fluid is as in example 1, except that: butyl acrylate is not added in the step (2).
Comparative example 5
The preparation method of the environment-friendly tackifier for the water-based drilling fluid is as in example 1, except that: n-methylol acrylamide is not added in the step (2).
Comparative example 6
The preparation method of the environment-friendly tackifier for the water-based drilling fluid is as in example 1, except that: adding 1.2g N-hydroxymethyl acrylamide in the step (2).
Comparative example 7
The preparation method of the environment-friendly tackifier for the water-based drilling fluid is as in example 1, except that: in the step (1), 30g of N, N-dimethylacrylamide is added, and 2-acrylamido-2-methylpropanesulfonic acid is not added.
Comparative example 8
The monomer proportion and the addition amount of the cross-linking agent of the environment-friendly tackifier for the water-based drilling fluid are the same as those in example 1, but an inverse emulsion polymerization method is not used. The adopted technical scheme is as follows:
(1) adding 100mL of water, 5g N, N-dimethylacrylamide, 17g of 2-acrylamido-2-methylpropanesulfonic Acid (AMPS), 3g of methacryloxyethyl trimethyl ammonium chloride (DMC) and 0.1g N-hydroxymethyl acrylamide into a 250mL beaker in sequence, dispersing and dissolving for 15min at a stirring speed of 300r/min by using a stirrer, and adjusting the pH of the system to 7 by using a NaOH solution with the mass fraction of 40%;
(2) weighing 4.25g of butyl acrylate and 1g of emulsifier Tween80, adding into the beaker in the step (1), and continuously carrying out shearing emulsification for 20min at the stirring speed of 2000r/min by using a shearing emulsifying machine;
(3) transferring the reaction solution into a reaction device, and heating the reaction solution to 50 ℃ in a water bath kettle; adding 12.5g of ammonium persulfate aqueous solution with the mass fraction of 1% in a nitrogen environment, and reacting at 50 ℃ for 4 hours, wherein the stirring speed in the reaction process is 300 r/min; after the reaction is completed, 300mL of acetone is added to the reaction solution for precipitation, then filtration is performed, and the obtained solid is washed 3 times with a mixed solvent of ethanol and water (ethanol: water: 2:1, v/v), and then dried at 80 ℃ for 16 hours, so that the environment-friendly tackifier for the water-based drilling fluid is obtained.
Test examples
The tackifier agents prepared in the examples and comparative examples were subjected to the following performance evaluations:
(1) influence of tackifier on drilling fluid rheological parameters and normal temperature and pressure filtration loss
Preparing base slurry: adding 16g of bentonite slowly into 400mL of distilled water while stirring, and aging for 24h at room temperature to prepare bentonite-based slurry.
Preparing a drilling fluid sample: 2g of the tackifier prepared in the example and the tackifier prepared in the comparative example are respectively added into 400mL of base slurry, and the mixture is stirred for 20min under the condition of 5000r/min, so that a drilling fluid sample is obtained.
And (4) performance testing: the formulated drilling fluids were tested for rheological parameters (apparent viscosity AV, plastic viscosity PV, and dynamic shear YP) and normal temperature and pressure fluid loss according to the American Petroleum Institute (API) standards (API RP 13B-1,2009).
Aging treatment of drilling fluid: and (3) aging the drilling fluid sample by using a roller heating furnace, wherein the treatment temperature is 180 ℃, and the treatment time is 16 h.
And (3) testing the performance after aging: after the aging is finished, the drilling fluid is cooled to room temperature, stirred for 30min under the condition of 5000r/min, and the rheological parameters (apparent viscosity AV, plastic viscosity PV and dynamic shear force YP) and the normal temperature and pressure fluid loss of the prepared drilling fluid are tested according to the American Petroleum Institute (API) standard (API RP 13B-1,2009), and the rheological and fluid loss test results before and after the aging are shown in the table 1.
TABLE 1
Table 1 reports the changes in rheological parameters and fluid loss at room temperature and pressure of the base slurry, the drilling fluid samples of the viscosifiers prepared in the examples and comparative examples before and after aging. As can be seen from Table 1, compared with base slurry, the apparent viscosity, plastic viscosity and dynamic shear force of the tackifier drilling fluid sample prepared by adding the embodiment before and after aging are obviously increased, and the rheological parameter changes in a small range after aging at 180 ℃; the changes of the apparent viscosity, the plastic viscosity and the dynamic shear force of the tackifier drilling fluid sample prepared by the comparative example before and after aging are smaller than those of the example; the fluid loss under pressure at normal temperature of the tackifier drilling fluid sample prepared in the example before and after aging is obviously reduced. Wherein, the drilling fluid sample added with the tackifier in the embodiment 1 has the minimum filtration loss, the filtration loss at normal temperature is 9.5mL before aging, the filtration loss at normal temperature is only 17.2mL after aging, and the performance is the most excellent.
(2) Influence of tackifier on rheological property and normal temperature and pressure filtration loss before and after aging of base slurry added with 15% NaCl
In the preparation step of the drilling fluid sample, 400mL of base slurry was added with 2g of each of the examples and comparative examples, followed by 15% NaCl (60g NaCl), and the mixture was stirred at 5000r/min for 20min, and the rest of the operation method was the same as that in (1), and the experimental results are shown in Table 2.
TABLE 2
Table 2 records the changes of the rheological parameters and the filtration loss at normal temperature of the base slurry, the tackifier prepared in the addition example and the comparative example and the drilling fluid sample of 15% NaCl before and after aging, and as can be seen from table 2, compared with the experimental results in table 1, the rheological parameters and the filtration loss of the drilling fluid sample after adding salt are reduced to different degrees, which is because the diffusion double electric layer of bentonite is seriously compressed by adding salt in the system, so that certain coalescence and delamination phenomena occur in the system; the addition of 15% NaCl has less effect on the changes of the rheological parameters and the fluid loss of the examples, wherein the tackifier prepared in example 1 has the most excellent performance.
(3) Environmental protection Performance test
Preparing a tackifier aqueous solution with the mass concentration of 2 wt%, testing the biological toxicity of the tackifier by a luminous bacteria method, and taking the concentration EC50 of the substance to be evaluated as an evaluation index when the luminous capacity of luminous bacteria is weakened by half, wherein the larger the EC50 value is, the lower the toxicity of the substance to be evaluated is. The tester is LUMIStox300 type biotoxicity tester, and the testing concentration is 2%. And testing the Chemical Oxygen Demand (COD) and the biological oxygen demand (BOD5) of the sample by using a COD tester and a BOD5 tester, and calculating the ratio of BOD 5/CODCr. The higher the BOD5/CODCr value, the better the biodegradability of the evaluated substance. The testing instruments are a Hash DR1010 COD rapid tester and a model LY-05 BOD automatic rapid tester of Qingdao Green science and technology Limited. The results are shown in Table 3.
TABLE 3
| Examples | EC50/ppm | Grade of toxicity | BOD5/CODCr | Degradability |
| Example 1 | 49334 | Is non-toxic | 32.50％ | Is easy to degrade |
| Example 2 | 47366 | Is non-toxic | 30.12％ | Is easy to degrade |
| Example 3 | 43362 | Is non-toxic | 28.63％ | Is easy to degrade |
| Example 4 | 44554 | Is non-toxic | 29.34％ | Is easy to degrade |
| Example 5 | 42125 | Is non-toxic | 27.65％ | Is easy to degrade |
| Example 6 | 39766 | Is non-toxic | 25.48％ | Is easy to degrade |
The EC50 of the products of each example is more than 30000ppm, and BOD5/CODCr is more than 25 percent, which shows that the products are nontoxic, easy to biodegrade and good in environmental protection performance.
In conclusion, the high temperature resistant tackifier for the water-based drilling fluid has remarkable advantages. The method has the advantages that: the temperature and salt resistance is excellent, and the product still has stable performance at the high temperature of 180 ℃ and under the condition of 15 percent of salt addition; the method has the advantages that: has certain fluid loss reducing capacity, good environmental protection performance and EC 50 ＞30000ppm，BOD5/COD Cr More than 25%, which indicates that the composition is non-toxic and easy to biodegrade; the method has the advantages that: the hydrophobic ester monomer is introduced in the synthesis process, the hydrophobic chain can make the macromolecular chain of the tackifier in a stretching state while improving the thermal stability of the molecule, and the hydrophobic association effect among molecules makes the macromolecular chain physically cross-linked to form a spatial network structure with certain strength, so that the tackifier has strong tackifying capability; the advantages are that: a small amount of cross-linking agent is added in the synthesis process, so that light cross-linking between different monomers can be promoted in the polymerization process, on one hand, the polymerization degree of a molecular chain can be increased, and on the other hand, the structural strength between molecules can be increased to improve the temperature resistance of the synthesized molecules.
Claims (10)
1. A preparation method of an environment-friendly high-temperature-resistant salt-resistant tackifier for water-based drilling fluid comprises the following steps:
(1) adding an alkene monomer, an anion monomer and a cation monomer into water, and uniformly stirring to obtain a water phase A;
(2) adding a crosslinking monomer, an emulsifier and an ester monomer into white oil, and emulsifying to obtain an oil phase B;
(3) mixing the water phase A and the oil phase B, emulsifying, and adjusting the pH of the system to 6-9 to obtain an emulsion; adding an initiator aqueous solution in a nitrogen atmosphere to perform reaction; after the reaction is finished, acetone is used for precipitation, and the environment-friendly high-temperature-resistant salt-resistant tackifier for the water-based drilling fluid is obtained after filtration, washing and drying.
2. The preparation method of the environment-friendly high-temperature-resistant salt-resistant tackifier for water-based drilling fluid according to claim 1, wherein the vinyl monomer in the step (1) is acrylamide, acrylic acid, N-dimethylacrylamide or N- (3-dimethylaminopropyl) methacrylamide; the ratio of the mass of the vinyl monomer to the volume of water is 1-15g:100mL, preferably 5-10g:100 mL.
3. The preparation method of the environment-friendly high temperature and salt resistant tackifier for water-based drilling fluid according to claim 1, wherein the anionic monomer in the step (1) is one or a combination of more than two of 2-acrylamido-2-methylpropanesulfonic acid, 2-acryloyloxy-2-methylpropanesulfonic acid, sodium vinylsulfonate and sodium allylsulfonate; the mass ratio of the anionic monomer to the olefinic monomer is 1.5-5:1, preferably 3-4: 1.
4. The preparation method of the environment-friendly high-temperature-resistant salt-resistant tackifier for water-based drilling fluid according to claim 1, wherein the cationic monomer in the step (1) is one or a combination of more than two of dimethyldiallylammonium chloride, methacryloyloxyethyl trimethyl ammonium chloride and dimethyloctadecyl [ 3-trimethoxysilylpropyl ] ammonium chloride; the mass ratio of the cationic monomer to the vinyl monomer is 0.1-1:1, preferably 0.3-0.6: 1;
the stirring speed in the step (1) is 200-400r/min, and the stirring time is 10-30 min.
5. The preparation method of the environment-friendly high temperature and salt resistant tackifier for water-based drilling fluid according to claim 1, wherein the crosslinking monomer in the step (2) is hydroxyethyl acrylate, triallylamine, ethylene glycol dimethacrylate or N-methylol acrylamide; the volume ratio of the crosslinking monomer to the white oil is 0.05-0.5g:100mL, preferably 0.1-0.2g:100 mL;
the emulsifier is Span80, Tween80 or OP-10; the ratio of the mass of the emulsifier to the volume of the white oil is 0.5-2.0g:100mL, preferably 1-1.5g:100 mL.
6. The preparation method of the environment-friendly high-temperature-resistant salt-resistant tackifier for water-based drilling fluid according to claim 1, wherein the ester monomer in the step (2) is butyl acrylate, ethyl methacrylate or triallyl isocyanurate; the mass ratio of the ester monomer to the volume of the white oil is 1-10g:100mL, preferably 2-5g:100 mL;
the emulsification in the step (2) is shear emulsification for 5-20min at the stirring speed of 2000r/min by using a shear emulsifying machine.
7. The preparation method of the environment-friendly high temperature and salt resistant tackifier for water-based drilling fluid according to claim 1, wherein the mass ratio of the ester monomer in the oil phase B to the alkene monomer in the water phase A in the step (3) is 0.1-1.5:1, preferably 0.4-0.9: 1; the emulsification is shearing emulsification for 15-20min at the stirring speed of 2000r/min by using a shearing emulsifying machine;
in the step (3), NaOH solution with the mass fraction of 40% is used for adjusting the pH value of the system to 6-9.
8. The preparation method of the environment-friendly high temperature and salt resistant tackifier for water-based drilling fluid according to claim 1, wherein the initiator in the step (3) is ammonium persulfate, potassium persulfate or tert-butyl hydroperoxide; the mass fraction of the initiator aqueous solution is 0.5-1%; the adding mass of the initiator is 0.1-1% of the total mass of the alkene monomer, the temperature-resistant monomer and the cationic monomer;
the reaction temperature is 40-60 ℃; the reaction time is 4-6 h;
the ratio of the adding volume of the acetone to the volume of the reaction liquid is 1-3: 1; the washing is carried out for 3-5 times by using a mixed solvent of ethanol and water, wherein the volume ratio of the ethanol to the water in the mixed solvent is 1.5-2.5: 1; the drying is carried out for 16-24h at 80-90 ℃.
9. An environment-friendly high-temperature-resistant salt-resistant tackifier for water-based drilling fluid, which is prepared by the preparation method of claim 1.
10. The use of the environmentally friendly high temperature and salt resistant tackifier for water-based drilling fluids of claim 9 in water-based drilling fluids; preferably, the addition amount in the water-based drilling fluid is 5-10 g/L.
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