CN114805680B - 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 emulsifying agent and an ester monomer into the white oil, and emulsifying to obtain an oil phase B; mixing the water phase A and the oil phase B, emulsifying, and regulating the pH of the system to 6-9 to obtain emulsion; under the nitrogen atmosphere, adding an initiator aqueous solution to react; and after the reaction is finished, precipitating by using acetone, filtering, washing and drying to obtain the catalyst. The invention prepares the water-soluble high-temperature resistant polymer tackifier with a certain network structure by an inverse emulsion polymerization method, and the obtained tackifier has excellent tackifying performance on water-based drilling fluid in a high-temperature environment of 180 ℃ and is nontoxic and easy to biodegrade, thereby overcoming the defect of insufficient high-temperature stability of the polymer tackifier of the existing water-based drilling fluid.
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 in petroleum industry.
Background
Along with the continuous increase of the economic development of China on the energy demand, the exploration and development of petroleum and natural gas begin to develop from the middle shallow layer to the deep layer. The bottom hole temperature of the deep stratum is high, a salt paste layer is commonly drilled, and higher requirements are put on the temperature resistance and the salt resistance of drilling fluid. Water-based drilling fluid is one of the key technologies for drilling high-temperature stratum, however, during deep oil reservoir drilling, various components in the well drilling fluid are easy to degrade under high-temperature conditions along with the increase of stratum temperature, and the drilling quality is seriously affected. Therefore, maintaining excellent stability of water-based drilling fluids at high temperatures plays a critical role in safe and efficient drilling of oil and gas.
Under high temperature and high salt conditions, the viscosity and shear of the drilling fluid are maintained in the proper ranges for maintaining the borehole clean and safe drilling. When the viscosity is too low, the viscosity can be increased by increasing the bentonite content, but the method can increase the solid phase content in the drilling fluid, which is not beneficial to improving the mechanical drilling speed and protecting the hydrocarbon reservoir. It is therefore often desirable to add viscosifiers to increase the viscosity of the drilling fluid and improve its rheological properties. The tackifier is one of the core treatment agents of the high-temperature-resistant drilling fluid, the type of the tackifier commonly used at present is mainly high-molecular polymers, and the main tackifying mechanism is that net frame structures are formed among polymer molecules through bridging action 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, and 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 molecular structure should be selected from monomers with good thermal stability and C-C, C-N and C-S bonds as main chains; (3) The molecular secondary structure has a certain branched structure and a certain body type structure; (4) Monomers incorporating specific molecular structures such as hydrolysis and stiffening groups.
The Chinese patent document CN110643335A provides a modified vegetable gum tackifier which comprises the following components in parts by weight: 7 to 11 parts of guar gum, 0.6 to 1 part of hydrolyzed polyacrylamide, 1.1 to 1.3 parts of borax, 0.8 to 1.5 parts of sodium hydroxide aqueous solution, 1.2 to 1.5 parts of ethylene oxide and 6 to 6.5 parts of polyurethane. Although the modified vegetable gum tackifier has good viscosity and certain environmental protection performance, in oilfield application, the temperature resistance performance is limited, and the temperature resistance requirement of a drilling construction site is generally not met, so that the modified vegetable gum tackifier cannot be widely applied.
Chinese patent document CN111662690a provides a tackifier comprising 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 remarkable temperature resistance and tackifying effect, but is not comprehensive in the aspect of salt resistance test, and has limited salt resistance and is difficult to widely apply.
The 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) The emulsifier and the ester monomer are dissolved in water together, and the emulsion A is obtained after full shearing and emulsification; 2) Mixing vinyl monomer, ether monomer and cross-linking agent monomer, and stirring at low speed to obtain water phase B; 3) Mixing the emulsion A with the water phase B, stirring and emulsifying, and then adjusting the pH value to 6-9 to obtain a mixed reaction solution; 4) And (3) adding an initiator into the mixed reaction liquid in an inert atmosphere at the temperature of 60-80 ℃, stirring at a low speed for reaction, and obtaining the polymer tackifier after the reaction is finished, wherein the synthetic product of the tackifier is emulsion, has unstable performance, is static and is easy to delaminate, and can not be directly applied to oil fields in a large range.
Currently, the following disadvantages exist in the tackifier for water-based drilling fluids: (1) The high temperature resistance is insufficient, the conventional tackifier can be degraded at high temperature, and the tackifying performance can be obviously reduced; (2) Insufficient salt resistance, reduced viscosity under high salt conditions; (3) The environmental protection performance is insufficient, and the environmental protection performance of various treating agents is higher and higher along with the improvement of the environmental protection requirements of oil fields.
Therefore, the development of the environment-friendly high-temperature-resistant and salt-resistant tackifier for the water-based drilling fluid has important 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 invention uses different alkenyl-containing monomers as main raw materials, prepares the water-soluble high-temperature resistant polymer tackifier with a certain network structure by an inverse emulsion polymerization method, and the obtained tackifier has excellent tackifying performance on water-based drilling fluid in a high-temperature environment of 180 ℃ and is nontoxic and easy to biodegrade, thereby overcoming the defect of insufficient high-temperature stability of the traditional water-based drilling fluid polymer tackifier.
The technical scheme of the invention is as follows:
the preparation method of the environment-friendly high-temperature-resistant salt-resistant tackifier for the 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 emulsifying agent and an ester monomer into the white oil, and emulsifying to obtain an oil phase B;
(3) Mixing the water phase A and the oil phase B, emulsifying, and regulating the pH of the system to 6-9 to obtain emulsion; under the nitrogen atmosphere, adding an initiator aqueous solution to react; after the reaction is finished, acetone is used for precipitation, and the environment-friendly high-temperature-resistant salt-resistant tackifier for water-based drilling fluid is obtained after filtering, washing and drying.
According to a preferred embodiment of the present invention, the vinyl 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 1-15 g/100 mL, more preferably 5-10 g/100 mL.
According to a preferred embodiment of the present invention, the anionic monomer in step (1) is one or a combination of two or more of 2-acrylamido-2-methylpropanesulfonic Acid (AMPS), 2-acryloyloxy-2-Methylpropanesulfonic Acid (MAOPS), sodium vinylsulfonate, sodium allylsulfonate; the mass ratio of the anionic monomer to the vinyl monomer is 1.5-5:1, and more preferably 3-4:1.
According to a preferred embodiment of the present invention, the cationic monomer in step (1) is one or a combination of two or more of dimethyldiallylammonium chloride (DMDAAC), methacryloxyethyl trimethylammonium chloride (DMC), dimethyloctadecyl [ 3-trimethoxysilylpropyl ] ammonium chloride; the mass ratio of the cationic monomer to the vinyl monomer is 0.1-1:1, and more preferably 0.3-0.6:1.
According to the invention, the stirring speed in the step (1) is 200-400r/min, and the stirring time is 10-30min.
According to a preferred embodiment of the present 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 0.05-0.5 g/100 mL, more preferably 0.1-0.2 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 0.5-2 g/100 mL, and more preferably 1-1.5 g/100 mL.
According to a preferred embodiment of 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 1-10 g/100 mL, and more preferably 2-5 g/100 mL.
According to the invention, the emulsification in the step (2) is shearing emulsification for 5-20min at a stirring speed of 2000r/min by using a shearing emulsifying machine.
According to the invention, the mass ratio of the ester monomer in the oil phase B to the vinyl monomer in the water phase A in the step (3) is preferably 0.1-1.5:1, more preferably 0.4-0.9:1.
According to the invention, the emulsification in the step (3) is shear emulsification for 15-20min at a stirring speed of 2000r/min using a shear emulsifier.
According to the invention, in the step (3), the pH of the system is adjusted to 6-9 by using a NaOH solution with the mass fraction of 40%.
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 vinyl monomer, the temperature-resistant monomer and the cationic monomer.
According to a preferred embodiment of the present invention, the temperature of the reaction in step (3) is 40-60 ℃; the reaction time is 4-6h.
According to the invention, the ratio of the added volume of the acetone to the volume of the reaction solution in the step (3) is preferably 1-3:1.
According to the invention, the washing in the step (3) is carried out 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 at 80-90 ℃ for 16-24h.
The environment-friendly high-temperature-resistant salt-resistant tackifier for water-based drilling fluid 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 amount of the additive in the water-based drilling fluid is 5-10g/L.
The invention has the technical characteristics and beneficial effects that:
1. the tackifier of the invention has excellent temperature resistance and salt resistance, and still has stable performance under the condition of high temperature of 180 ℃ and 15% salt addition. The synthesized tackifier has a molecular structure containing a carbon-carbon long chain, a double bond structure, a sulfonic acid group and an amine group, and the long chain structure is stably stretched under the synergistic effect of the sulfonic acid group, so that the thermal stability and rigidity of the tackifier can be increased, the hydrolysis of the copolymer under the conditions of high temperature and high salt can be resisted, and the temperature resistance and the salt resistance of the tackifier are improved. Especially when the vinyl monomer is N, N-dimethylacrylamide, tertiary amine groups on long chains of the obtained tackifier effectively increase steric hindrance of the copolymer under the protection of two methyl groups, and the heat resistance and the salt resistance are more excellent.
2. The specific types of ester monomers are introduced in the synthesis process of the tackifier, the polar hydrophobic chain can enable the macromolecular chain of the tackifier to be in an extended state, hydrophobic groups enable hydrophobic association among product molecules to be enhanced, so that the macromolecular chain is physically crosslinked to form a space network structure with certain strength, the tackifier can have stronger tackifying capability, and meanwhile, the hydrophobic groups can also increase the thermal stability of the tackifier and can resist high temperature of 200 ℃; the hydrophobic chain of the ester monomer is not too much or too long, the solubility and CMC of the ester monomer are correspondingly reduced along with the increase of the number of carbon atoms in the hydrophobic group, spherical micelle is easy to form, the radius of gyration of micelle particles is increased, the hydrophobic monomer is easy to excessively self-polymerize, the product is easy to separate oil from water when the polymerization reaction is incomplete, the performance of the product is reduced, and even the polymerization experiment fails, so that the target product cannot be obtained.
3. The specific type and the specific amount of the cross-linking agent are used in the synthesis process of the tackifier, so that different alkenyl monomers can be subjected to light cross-linking, on one hand, the polymerization degree of a molecular chain can be increased, and on the other hand, the molecular structural strength is increased through the introduction of a hydrophobic group, and the temperature resistance and salt resistance of the tackifier are improved; while ensuring that the tackifier does not excessively crosslink, thereby degrading performance.
Detailed Description
The invention is further illustrated, but not limited, by the following examples.
Meanwhile, the experimental methods described in the following examples are all conventional methods unless otherwise specified; the reagents, materials, and apparatus, unless otherwise specified, are all commercially available.
The white oil used in the examples is # 5 white oil.
Example 1
The preparation method of the environment-friendly high-temperature-resistant salt-resistant tackifier for the water-based drilling fluid comprises the following steps:
(1) To a 250mL beaker were successively added 5g of N, N-dimethylacrylamide, 17g of 2-acrylamido-2-methylpropanesulfonic Acid (AMPS), 3g of methacryloyloxyethyl trimethyl ammonium chloride (DMC) and 100mL of water, and stirred using a magnetic stirrer at a stirring speed of 300r/min for 20min to prepare a water phase A.
(2) To a 250mL beaker was added 0.1-g N-methylolacrylamide, 1g of emulsifier Tween80 and 100mL of white oil, followed by weighing 4.25g of butyl acrylate, adding to the beaker, and shearing and emulsifying for 20min using a shearing and emulsifying machine at a stirring speed of 2000r/min to prepare an 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 a stirring speed of 2000r/min by using a shearing emulsifying machine, regulating the pH value of the system to 7 by using a NaOH solution with the mass fraction of 40%, and finally transferring to a reaction device, and heating to 50 ℃ in a water bath kettle; in a nitrogen environment, adding 12.5g of ammonium persulfate aqueous solution with the mass fraction of 1%, and reacting for 4 hours at 50 ℃, wherein the stirring speed is 300r/min in the reaction process; after the reaction is finished, 300mL of acetone is added into the reaction solution for precipitation, then the reaction solution is filtered, the obtained solid is washed for 3 times by using a mixed solvent of ethanol and water (ethanol: water=2:1, v/v), and then the reaction solution is dried for 16 hours at 80 ℃, so that the environment-friendly high-temperature-resistant salt-resistant tackifier for water-based drilling fluid is obtained.
Example 2
The preparation method of the environment-friendly high-temperature-resistant salt-resistant tackifier for the water-based drilling fluid comprises the following steps:
(1) To a 250mL beaker were successively added 10g of N, N-dimethylacrylamide, 17g of 2-acrylamido-2-methylpropanesulfonic Acid (AMPS), 3g of methacryloyloxyethyl trimethyl ammonium chloride (DMC) and 100mL of water, and stirred using a magnetic stirrer at a stirring speed of 300r/min for 20min to prepare a water phase A.
(2) To a 250mL beaker was added 0.1-g N-methylolacrylamide, 1g of emulsifier Tween80 and 100mL of white oil, followed by weighing 4.25g of butyl acrylate, adding to the beaker, and shearing and emulsifying for 20min using a shearing and emulsifying machine at a stirring speed of 2000r/min to prepare an 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 a stirring speed of 2000r/min by using a shearing emulsifying machine, regulating the pH value of the system to 7 by using a NaOH solution with the mass fraction of 40%, and finally transferring to a reaction device, and heating to 50 ℃ in a water bath kettle; in a nitrogen environment, adding 12.5g of ammonium persulfate aqueous solution with the mass fraction of 1%, and reacting for 4 hours at 50 ℃, wherein the stirring speed is 300r/min in the reaction process; after the reaction is finished, 300mL of acetone is added into the reaction solution for precipitation, then the reaction solution is filtered, the obtained solid is washed for 3 times by using a mixed solvent of ethanol and water (ethanol: water=2:1, v/v), and then the reaction solution is dried for 16 hours at 80 ℃, so that the environment-friendly high-temperature-resistant salt-resistant tackifier for water-based drilling fluid is obtained.
Example 3
The preparation method of the environment-friendly high-temperature-resistant salt-resistant tackifier for the water-based drilling fluid comprises the following steps:
(1) To a 250mL beaker were successively added 5g of acrylamide, 22g of 2-acrylamido-2-methylpropanesulfonic Acid (AMPS), 3g of methacryloyloxyethyl trimethyl ammonium chloride (DMC) and 100mL of water, and stirred using a magnetic stirrer at a stirring speed of 300r/min for 20min to prepare a water phase A.
(2) To a 250mL beaker was added 0.1-g N-methylolacrylamide, 1g of emulsifier Tween80 and 100mL of white oil, followed by weighing 4.25g of butyl acrylate, adding to the beaker, and shearing and emulsifying for 20min using a shearing and emulsifying machine at a stirring speed of 2000r/min to prepare an 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 a stirring speed of 2000r/min by using a shearing emulsifying machine, regulating the pH value of the system to 7 by using a NaOH solution with the mass fraction of 40%, and finally transferring to a reaction device, and heating to 50 ℃ in a water bath kettle; in a nitrogen environment, adding 12.5g of ammonium persulfate aqueous solution with the mass fraction of 1%, and reacting for 4 hours at 50 ℃, wherein the stirring speed is 300r/min in the reaction process; after the reaction is finished, 300mL of acetone is added into the reaction solution for precipitation, then the reaction solution is filtered, the obtained solid is washed for 3 times by using a mixed solvent of ethanol and water (ethanol: water=2:1, v/v), and then the reaction solution is dried for 16 hours at 80 ℃, so that the environment-friendly high-temperature-resistant salt-resistant tackifier for water-based drilling fluid is obtained.
Example 4
The preparation method of the environment-friendly high-temperature-resistant and salt-resistant tackifier for water-based drilling fluid is as described in example 1, except that: the butyl acrylate addition in step (2) was 2.25g.
Example 5
The preparation method of the environment-friendly high-temperature-resistant and salt-resistant tackifier for water-based drilling fluid is as described in example 1, except that: in the step (2), butyl acrylate is changed into ethyl methacrylate.
Example 6
The preparation method of the environment-friendly high-temperature-resistant and salt-resistant tackifier for water-based drilling fluid is as described in example 1, except that: butyl acrylate is changed to triallyl isocyanurate in step (2).
Comparative example 1
The preparation method of the environment-friendly tackifier for water-based drilling fluid is as described in example 1, except that: in step (2), tween80 was replaced with 1g of emulsifier OS.
Comparative example 2
The preparation method of the environment-friendly tackifier for water-based drilling fluid is as described in example 1, except that: in step (3), the reaction is carried out at 80 ℃.
Comparative example 3
The preparation method of the environment-friendly tackifier for water-based drilling fluid is as described in example 1, except that: in the step (3), the pH of the system is adjusted to 11.
Comparative example 4
The preparation method of the environment-friendly tackifier for water-based drilling fluid is as described 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 water-based drilling fluid is as described in example 1, except that: in the step (2), N-methylolacrylamide is not added.
Comparative example 6
The preparation method of the environment-friendly tackifier for water-based drilling fluid is as described in example 1, except that: in the step (2), 1.2-g N-methylolacrylamide was added.
Comparative example 7
The preparation method of the environment-friendly tackifier for water-based drilling fluid is as described in example 1, except that: in the step (1), 30g of N, N-dimethylacrylamide was added without adding 2-acrylamido-2-methylpropanesulfonic acid.
Comparative example 8
An environment-friendly tackifier for water-based drilling fluid, which has the same monomer proportion and crosslinking agent addition amount as in example 1, but does not use an inverse emulsion polymerization method. The adopted technical scheme is as follows:
(1) 100mL of water, 5g of N, N-dimethylacrylamide, 17g of 2-acrylamido-2-methylpropanesulfonic Acid (AMPS), 3g of methacryloyloxyethyl trimethyl ammonium chloride (DMC) and 0.1-g N-methylolacrylamide are sequentially added into a 250mL beaker, and after dispersing and dissolving for 15min at a stirring speed of 300r/min by using a stirrer, the pH of the system is adjusted to 7 by using a NaOH solution with a mass fraction of 40%;
(2) Weighing 4.25g of butyl acrylate and 1g of emulsifier Tween80, adding into the beaker of the step (1), and continuing to perform shearing and emulsification for 20min at a stirring speed of 2000r/min by using a shearing emulsifying machine;
(3) Transferring the reaction solution into a reaction device, and heating to 50 ℃ in a water bath kettle; in a nitrogen environment, adding 12.5g of ammonium persulfate aqueous solution with the mass fraction of 1%, and reacting for 4 hours at 50 ℃, wherein the stirring speed is 300r/min in the reaction process; after the reaction was completed, 300mL of acetone was added to the reaction solution to precipitate, followed by filtration, and the obtained solid was washed 3 times with a mixed solvent of ethanol and water (ethanol: water=2:1, v/v), followed by drying at 80 ℃ for 16 hours, to obtain an environment-friendly tackifier for water-based drilling fluids.
Test examples
The following performance evaluations were performed on the tackifier agents prepared in examples and comparative examples:
(1) Influence of tackifier on rheological parameters of drilling fluid and filtration loss at normal temperature and pressure
Preparing base slurry: 16g of bentonite was slowly added to 400mL of distilled water with stirring, and then aged at room temperature for 24 hours to prepare a bentonite-based slurry.
Preparing drilling fluid samples: to 400mL of the base slurry, 2g of the tackifiers prepared in examples and comparative examples were added, respectively, and the mixture was stirred at 5000r/min for 20min to obtain drilling fluid samples.
Performance test: the rheological parameters (apparent viscosity AV, plastic viscosity PV and dynamic shear force YP) and normal temperature and pressure fluid loss of the formulated drilling fluids were tested according to the American Petroleum Institute (API) standard (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 hours.
Performance test after aging: after cooling to room temperature after aging, stirring for 30min at 5000r/min, and testing rheological parameters (apparent viscosity AV, plastic viscosity PV and dynamic shear force YP) and normal temperature and normal pressure fluid loss of the prepared drilling fluid according to American Petroleum Institute (API) standard (API RP 13B-1,2009), wherein the rheological and fluid loss test results before and after aging are shown in Table 1.
TABLE 1
Table 1 records the changes in rheological parameters and normal temperature and pressure fluid loss of the base stock before and after aging, and the viscosifier drilling fluid samples prepared in the examples and comparative examples. As can be seen from Table 1, compared with the base slurry, the apparent viscosity, the plastic viscosity and the dynamic shear force of the viscosifier drilling fluid sample prepared by adding the examples before and after aging are all obviously increased, and the rheological parameter change is floated in a small range after aging at 180 ℃; the apparent viscosity, plastic viscosity and dynamic shear force of the tackifier drilling fluid sample prepared by the comparative example are less than those of the examples before and after aging; the normal temperature medium pressure fluid loss of the tackifier drilling fluid sample prepared in the example is obviously reduced after the addition before and after aging. Wherein, the filtrate loss of the sample of the drilling fluid added with the tackifier of the embodiment 1 is minimum, the pressure filtration loss is 9.5mL at normal temperature before aging, the pressure filtration loss is only 17.2mL at normal temperature after aging, and the performance is most excellent.
(2) Effect of tackifier on rheological properties before and after aging and filtration loss at normal temperature and pressure of base slurry added with 15% NaCl
In the preparation step of drilling fluid samples, 400mL of base slurry was taken, 2g of the products of the examples and the comparative examples were added respectively, followed by 15% NaCl (60 g of NaCl) and stirring at 5000r/min for 20min, and the rest of the operation method was the same as in (1), and the experimental results are shown in Table 2.
TABLE 2
Table 2 records the changes of rheological parameters and normal temperature medium pressure fluid loss of the base slurry before and after aging, the tackifier prepared by the examples and the comparative examples and the 15% nacl drilling fluid sample, and it can be seen from table 2 that, compared with the experimental results in table 1, the rheological parameters and the fluid loss of the drilling fluid sample are reduced to different degrees after salt addition, because the diffusion double layers of bentonite are severely compressed by salt addition in the system, so that certain coalescence and layering phenomena occur in the system; the addition of 15% NaCl had less effect on the variation of the rheological parameters and the fluid loss of the examples, the most excellent of which was the adhesion promoter prepared in example 1.
(3) Environmental protection performance test
Preparing an aqueous solution of the tackifier with the mass concentration of 2wt%, testing the biotoxicity of the tackifier by a luminous bacteria method, taking the concentration EC50 of the substance to be evaluated when the luminous capability of the luminous bacteria is reduced by half as an evaluation index, and indicating that the toxicity of the substance to be evaluated is lower as the EC50 value is larger. The test instrument is a LUMISTox300 type biotoxicity tester, and the test concentration is 2%. The chemical oxygen demand (CODCr) and biological oxygen demand (BOD 5) testers were used to test the chemical oxygen demand and biological oxygen demand of the samples, and the BOD5/CODCr ratio was calculated. The greater BOD5/CODCr value indicates that the better the biodegradability of the substance being evaluated. The testing instrument is a Hash DR1010 COD rapid tester and a Qingdao Lvyu environmental protection technology Co., ltd LY-05 type BOD automatic rapid tester. The results are shown in Table 3.
TABLE 3 Table 3
| Examples | EC50/ppm | Toxicity grade | BOD5/CODCr | Degradability of |
| Example 1 | 49334 | Nontoxic | 32.50％ | Is easy to degrade |
| Example 2 | 47366 | Nontoxic | 30.12％ | Is easy to degrade |
| Example 3 | 43362 | Nontoxic | 28.63％ | Is easy to degrade |
| Example 4 | 44554 | Nontoxic | 29.34％ | Is easy to degrade |
| Example 5 | 42125 | Nontoxic | 27.65％ | Is easy to degrade |
| Example 6 | 39766 | Nontoxic | 25.48％ | Is easy to degrade |
The EC50 of the products of each embodiment is more than 30000ppm, and BOD5/CODCr is more than 25%, which shows that the products are nontoxic, easy to biodegrade and good in environmental protection performance.
In summary, it can be seen that the high temperature resistant tackifier for water-based drilling fluids of the present invention has significant advantages. Advantage 1: the heat resistance and salt resistance are excellent, and the heat resistance and salt resistance still have stable performance under the condition of adding 15 percent of salt at the high temperature of 180 ℃; advantage 2: has certain filtration reducing capability, good environmental protection performance and EC 50 ＞30000ppm，BOD5/COD Cr More than 25%, which indicates that the material is nontoxic and easy to be biodegraded; advantage 3: the hydrophobic ester monomer is introduced in the synthesis process, the hydrophobic chain can enable the macromolecular chain of the tackifier to be in an extended state while improving the thermal stability of molecules, and the macromolecular chain is physically crosslinked by hydrophobic association among molecules to form a space network structure with certain strength, so that the tackifier has strong tackifying capability; advantage 4: and a small amount of cross-linking agent is added in the synthesis process, so that light cross-linking can be promoted to occur between different monomers in the polymerization process, on one hand, the polymerization degree of a molecular chain can be increased, and on the other hand, the intermolecular structural strength can be increased to improve the temperature resistance of the synthesized molecule.
Claims (10)
1. The preparation method of the environment-friendly high-temperature-resistant salt-resistant tackifier for the 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; the vinyl monomer is acrylamide, N-dimethylacrylamide or N- (3-dimethylaminopropyl) methacrylamide; the ratio of the mass of the vinyl monomer to the volume of water is 1-15 g/100 mL; the anionic monomer is one or the combination of more than two of 2-acrylamide-2-methylpropanesulfonic acid, 2-acryloyloxy-2-methylpropanesulfonic acid, sodium vinylsulfonate and sodium allylsulfonate; the mass ratio of the anionic monomer to the vinyl monomer is 1.5-5:1; the cationic monomer is one or the combination of two of dimethyl diallyl ammonium chloride and methacryloyloxyethyl trimethyl ammonium chloride; the mass ratio of the cationic monomer to the vinyl monomer is 0.1-1:1;
(2) Adding a crosslinking monomer, an emulsifying agent and an ester monomer into the white oil, and emulsifying to obtain an oil phase B; the crosslinking monomer is hydroxyethyl acrylate, triallylamine, ethylene glycol dimethacrylate or N-methylolacrylamide; the volume ratio of the crosslinking monomer to the white oil is 0.05-0.5 g/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 0.5-2.0 g/100 mL; the ester monomer is butyl acrylate or ethyl methacrylate; the ratio of the mass of the ester monomer to the volume of the white oil is 1-10 g/100 mL;
(3) Mixing the water phase A and the oil phase B, emulsifying, and regulating the pH of the system to 6-9 to obtain emulsion; under the nitrogen atmosphere, adding an initiator aqueous solution to react; after the reaction is finished, acetone is used for precipitation, and the environment-friendly high-temperature-resistant salt-resistant tackifier for water-based drilling fluid is obtained after filtration, washing and drying; the mass ratio of the ester monomer in the oil phase B to the vinyl monomer in the water phase A is 0.1-1.5:1; the temperature of the reaction is 40-60 ℃; the reaction time is 4-6h.
2. The method for preparing an environment-friendly high-temperature-resistant and salt-resistant tackifier for water-based drilling fluids according to claim 1, wherein the ratio of the mass of the vinyl monomer to the volume of water in the step (1) is 5-10 g/100 ml.
3. The method for preparing an environment-friendly high-temperature-resistant and salt-resistant tackifier for water-based drilling fluids according to claim 1, wherein the mass ratio of the anionic monomer to the vinyl monomer in the step (1) is 3-4:1.
4. The method for preparing an environment-friendly high-temperature-resistant and salt-resistant tackifier for water-based drilling fluids according to claim 1, wherein the mass ratio of the cationic monomer to the vinyl monomer in the step (1) is 0.3-0.6:1;
the stirring speed in the step (1) is 200-400r/min, and the stirring time is 10-30min.
5. The method for preparing an environment-friendly high temperature resistant and salt resistant tackifier for water-based drilling fluids according to claim 1, wherein the volume ratio of the crosslinking monomer to white oil in step (2) is 0.1-0.2g:100ml; the ratio of the mass of the emulsifier to the volume of the white oil is 1-1.5 g/100 mL.
6. The method for preparing an environment-friendly high-temperature-resistant and salt-resistant tackifier for water-based drilling fluids according to claim 1, wherein the ratio of the mass of the ester monomer to the volume of the white oil in the step (2) is 2-5 g/100 ml;
the emulsification in the step (2) is shearing emulsification for 5-20min at a stirring speed of 2000r/min by using a shearing emulsifying machine.
7. The method for preparing the environment-friendly high-temperature-resistant and salt-resistant tackifier for water-based drilling fluids 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 0.4-0.9:1; the emulsification is shearing emulsification for 15-20min at a 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 regulating the pH value of the system to 6-9.
8. The method for preparing an environment-friendly high-temperature-resistant and salt-resistant tackifier for water-based drilling fluids 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 ratio of the added volume of the acetone to the volume of the reaction solution 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 at 80-90 ℃ for 16-24h.
9. An environment-friendly high-temperature-resistant and 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 viscosifier for water-based drilling fluids of claim 9 in water-based drilling fluids; the addition amount of the water-based drilling fluid is 5-10g/L.
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