A kind of heat-resistant anti-expansion clay stabilizer and preparation method thereof
By forming oligomeric tertiary amines with piperazine and 1,12-dibromododecane and reacting with sodium chloride ethyl sulfonate, clay stabilizers with high anti-swelling and temperature resistance were prepared, which solved the problem of poor anti-swelling effect of clay stabilizers in the prior art under high temperature environments and achieved more efficient oil layer protection.
Patent Information
- Application Number
- CN202310360393.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-04-06
- Publication Date
- 2025-04-15
- Estimated Expiration
- 2043-04-06
AI Technical Summary
The existing clay stabilizers have shortcomings in their anti-swelling effect and temperature resistance, especially in high-temperature environments, which cannot effectively prevent the hydration and expansion of clay, affecting the protection effect of the oil and gas layer.
Pipezine and 1,12-dibromododecane were used to perform tertiary amination reaction to form oligomeric tertiary amines, and then quaternization reaction with sodium ethyl chloride sulfonate to obtain a temperature-resistant anti-swelling clay stabilizer with amphoteric surfactant properties. This stabilizer prevents water molecules from infiltration through quaternary ammonium cation adsorption and neutralizes the negative charge on the clay surface, thereby achieving the dual effects of anti-swelling and temperature resistance.
The clay stabilizer has an anti-swelling rate of more than 97% at a concentration of 1 wt%, and is maintained at an anti-swelling rate of more than 96% in an environment of 350°C, which significantly improves the effect of oil layer protection.
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Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of oil field development, and particularly relates to a temperature-resistant anti-swelling clay stabilizer and a preparation method thereof. Background Art
[0002] With the continuous development of oil fields, people are paying more and more attention to reservoir protection technology. Clay minerals are widely present in oil reservoirs. When clay minerals in the reservoirs come into contact with incompatible external fluids, they will hydrate, swell, disperse and migrate, blocking the reservoir channels, resulting in a decrease in permeability and damage to the oil and gas layers. Therefore, clay stabilizers must be used to protect the oil layer to ensure the smooth development of the oil reservoir.
[0003] Clay stabilizers are increasingly widely used and there are more and more types of them. According to their different chemical compositions, they can be divided into inorganic salts, inorganic polymers, cationic surfactants, nonionic and cationic organic polymers. Among them, cationic organic polymer clay stabilizers have developed rapidly in recent years. Their ability to stabilize clay far exceeds that of inorganic salts and water-soluble non-electrolyte polymers, and they have the characteristics of low dosage, high efficiency, and strong adaptability to formations.
[0004] Hu Xingqi et al. published "Synthesis and Evaluation of Small Molecule Polyamine Clay Stabilizer EM", which synthesized a polyamine clay stabilizer EM using epichlorohydrin and methylamine. It has good inhibition of clay hydration expansion. When used alone, the optimal mass concentration range is 1-2%, and the anti-swelling rate is 86%. 4 When C1 is compounded, the anti-swelling rate is only 91%, which cannot meet the requirements for reservoirs with higher anti-swelling requirements.
[0005] CN114106795A discloses a clay stabilizer and its preparation method and application, belonging to the technical field of clay stabilizers. The clay stabilizer, by weight, comprises: 2-8 parts of bisindolylmethane compounds, 2-8 parts of quinazolinone compounds, 5-15 parts of methanol and 80-85 parts of water. The clay stabilizer has a small molecular weight, which is conducive to dispersion on the clay surface, has high anti-swelling efficiency, and is easy to discharge. After fracturing or mining operations, it can reduce residues and reduce damage to the formation. However, from the perspective of molecular structure, the invention belongs to non-ionic organic matter, and has limited adsorption effect on negatively charged clay, thus affecting the anti-swelling effect to some extent. Summary of the invention
[0006] The invention aims at solving the problems in the prior art and provides a heat-resistant anti-swelling clay stabilizer and a preparation method thereof. The clay stabilizer has the characteristics of simple preparation process, low cost, good anti-swelling effect and good temperature resistance.
[0007] In order to achieve the above objectives, the first aspect of the present invention provides a temperature-resistant anti-swelling clay stabilizer, the molecular structure of the clay stabilizer is as follows:
[0008]
[0009] Wherein: n=2-10, n is a natural number.
[0010] Another aspect of the present invention provides a method for preparing the above-mentioned temperature-resistant anti-swelling clay stabilizer, and the preparation method specifically comprises the following steps:
[0011] (1) piperazine, solvent and 1,12-dibromododecane were added to a four-necked flask equipped with a condenser, a stirrer and a dropping funnel, and the mixture was stirred to dissolve. The stirring speed was maintained at 200-250 rpm, and the oil bath was heated to 55-60° C. Within 1 hour after the reaction started, the pH was tested every 10 minutes. If the pH was lower than 7, the pH was adjusted to 8 with 1 mol / L sodium hydroxide solution. After 1 hour after the reaction started, the pH was tested every 30 minutes. If the pH was lower than 7, the pH was adjusted to 8 with 1 mol / L sodium hydroxide solution. The pH was always maintained between 7 and 8 during the reaction. After the reaction was completed, the temperature was lowered to below 40° C.
[0012] (2) adding sodium chloroethylsulfonate to the above four-necked flask, stirring to dissolve, maintaining the stirring speed at 200-250 rpm, heating to reflux, and distilling under reduced pressure to obtain a reddish brown solid as a crude product;
[0013] (3) Recrystallize with ethyl acetate to obtain a light yellow solid, and dry at 90-105° C. for 8-10 h to obtain a clay stabilizer product.
[0014] In the present invention, preferably, the molar ratio of 1,12-dibromododecane, sodium chloroethylsulfonate and piperazine is 0.8-1.2:1.5-2.5:1, more preferably 0.9-1.1:2-2.3:1.
[0015] In the present invention, preferably, the solvent in step (1) is one of methanol, ethanol, propanol, isopropanol, butanol and isobutanol; more preferably, the solvent is ethanol or isobutanol.
[0016] Preferably, the mass ratio of the solvent to piperazine in step (1) is 30-40:1.
[0017] Preferably, the reaction time in step (1) is 3-6 h.
[0018] In the present invention, preferably, the heating reflux time in step (2) is 12-48h.
[0019] In the present invention, preferably, the mass ratio of ethyl acetate to piperazine in step (3) is 6-8:1.
[0020] The heat-resistant anti-swelling clay stabilizer synthesis reaction equation of the present invention is as follows:
[0021]
[0022]
[0023] The heat-resistant anti-swelling clay stabilizer of the present invention is obtained by tertiary amination reaction of piperazine with 1,12-dibromododecane in a solvent to obtain an oligomeric tertiary amine; the generated tertiary amine is further subjected to quaternization reaction with sodium chloroethylsulfonate. It belongs to an oligomeric amphoteric surfactant, each monomer contains two quaternary ammonium salts and two sulfonic acid groups, which are hydrophilic groups, and the dodecyl group is a lipophilic group. The quaternary ammonium cation can adsorb and neutralize the negative charge on the surface of the clay, reduce the repulsion between the crystal layers, and play an anti-swelling role; at the same time, after adsorption, the clay surface changes from hydrophilic to lipophilic, and the dodecyl group can effectively prevent water molecules from infiltrating the clay particles, and inhibit the hydration expansion of the clay by avoiding contact between water molecules and the clay; the ring structure makes the molecule have a certain rigid structure and good temperature resistance; the characteristics of the polymer can form multi-point adsorption with multiple clay particles, and after adsorption, an adsorption film is formed on the surface of the clay particles to prevent the expansion and migration of the clay particles. Due to the multi-point ionization of the molecules, the use concentration can be greatly reduced.
[0024] Compared with the prior art, the present invention has the following advantages and beneficial effects:
[0025] (1) The raw material sources of the heat-resistant anti-swelling clay stabilizer of the present invention are wide, the synthesis process is simple, and the cost is low;
[0026] (2) The heat-resistant anti-swelling clay stabilizer of the present invention has a high anti-swelling rate. When the concentration is 1 wt%, the anti-swelling rate reaches more than 97%;
[0027] (3) The heat-resistant anti-swelling clay stabilizer of the present invention has good heat resistance and is adapted to the high-temperature characteristics of the strata. In an environment of 350°C, the anti-swelling rate reaches more than 96%. DETAILED DESCRIPTION
[0028] The present invention will be further described in detail below in conjunction with specific examples and with reference to data. It should be understood that these examples are only intended to illustrate the present invention and are not intended to limit the scope of the present invention in any way.
[0029] Example 1
[0030] (1) Add 0.2 mol of
[0031] Piperazine, 688g methanol, 0.16mol 1,12-dibromododecane, stir to dissolve, maintain stirring speed at 200rpm, heat oil bath to 55℃, test pH every 10min within 1h after reaction, if pH is lower than 7, adjust pH to 8 with 1mol / L sodium hydroxide solution, test pH every 30min after 1h after reaction, if pH is lower than 7, adjust pH to 8 with 1mol / L sodium hydroxide solution, always maintain pH between 7-8 during reaction, complete reaction for 3h, cool to below 40℃;
[0032] (2) Add 0.3 mol of sodium chloroethylsulfonate to the above four-necked flask, stir to dissolve, maintain the stirring speed at 200 rpm, heat to reflux for 12 h, and distill under reduced pressure to obtain a reddish brown solid as the crude product;
[0033] (3) Recrystallize with 103.2 g of ethyl acetate to obtain a light yellow solid, which is dried at 95 °C for 8 h to obtain the product clay stabilizer N 1 .
[0034] Example 2
[0035] (1) Add 0.2 mol piperazine, 516 g propanol, and 0.24 mol 1,12-dibromododecane to a four-necked flask equipped with a condenser, a stirrer, and a dropping funnel, stir to dissolve, maintain the stirring speed at 250 rpm, and heat to 56°C in an oil bath. Within 1 hour after the start of the reaction, test the pH every 10 minutes. If the pH is lower than 7, adjust it to pH 8 with 1 mol / L sodium hydroxide solution. After 1 hour after the start of the reaction, test the pH every 30 minutes. If the pH is lower than 7, adjust it to pH 8 with 1 mol / L sodium hydroxide solution. Maintain the pH between 7 and 8 during the reaction. After the reaction is completed for 3.5 hours, cool to below 40°C.
[0036] (2) Add 0.35 mol of sodium chloroethylsulfonate to the above four-necked flask, stir to dissolve, maintain the stirring speed at 220 rpm, heat to reflux for 16 h, and distill under reduced pressure to obtain a reddish brown solid as the crude product;
[0037] (3) Recrystallize with 108.6 g of ethyl acetate to obtain a light yellow solid, which is then dried at 105° C. for 10 h to obtain the product clay stabilizer N 2 .
[0038] Example 3
[0039] (1) Add 0.2 mol piperazine, 640 g butanol, and 0.17 mol 1,12-dibromododecane to a four-necked flask equipped with a condenser, a stirrer, and a dropping funnel, stir to dissolve, maintain the stirring speed at 220 rpm, heat to 60°C in an oil bath, test the pH every 10 minutes within 1 hour after the start of the reaction, if the pH is lower than 7, adjust it to pH 8 with 1 mol / L sodium hydroxide solution, test the pH every 30 minutes after 1 hour after the start of the reaction, if the pH is lower than 7, adjust it to pH 8 with 1 mol / L sodium hydroxide solution, and always maintain the pH between 7 and 8 during the reaction. After the reaction is completed for 4 hours, cool down to below 40°C;
[0040] (2) Add 0.5 mol of sodium chloroethylsulfonate to the above four-necked flask, stir to dissolve, maintain the stirring speed at 250 rpm, heat to reflux for 20 h, and distill under reduced pressure to obtain a reddish brown solid as the crude product;
[0041] (3) Recrystallize with 110.5 g of ethyl acetate to obtain a light yellow solid, which is dried at 90 ° C for 9 h to obtain the product clay stabilizer N 3 .
[0042] Example 4
[0043] (1) Add 0.2 mol piperazine, 600 g isopropanol and 0.23 mol 1,12-dibromododecane to a four-necked flask equipped with a condenser, a stirrer and a dropping funnel, stir to dissolve, maintain the stirring speed at 230 rpm, heat to 57°C in an oil bath, test the pH every 10 minutes within 1 hour after the start of the reaction, if the pH is lower than 7, adjust it to pH 8 with 1 mol / L sodium hydroxide solution, test the pH every 30 minutes after the start of the reaction, if the pH is lower than 7, adjust it to pH 8 with 1 mol / L sodium hydroxide solution, and always maintain the pH between 7 and 8 during the reaction. The reaction is completed after 4.5 hours, and the temperature is lowered to below 40°C;
[0044] (2) Add 0.48 mol of sodium chloroethylsulfonate to the above four-necked flask, stir to dissolve, maintain the stirring speed at 210 rpm, heat to reflux for 24 h, and distill under reduced pressure to obtain a reddish brown solid as the crude product;
[0045] (3) Recrystallize with 123 g of ethyl acetate to obtain a light yellow solid, which is dried at 100 ° C for 9 h to obtain the product clay stabilizer N 4 .
[0046] Example 5
[0047] (1) Add 0.2 mol piperazine, 590 g ethanol and 0.18 mol 1,12-dibromododecane to a four-necked flask equipped with a condenser, a stirrer and a dropping funnel, stir to dissolve, maintain the stirring speed at 210 rpm, heat to 58°C in an oil bath, test the pH every 10 minutes within 1 hour after the start of the reaction, if the pH is lower than 7, adjust it to pH 8 with 1 mol / L sodium hydroxide solution, test the pH every 30 minutes after 1 hour after the start of the reaction, if the pH is lower than 7, adjust it to pH 8 with 1 mol / L sodium hydroxide solution, and always maintain the pH between 7 and 8 during the reaction. After the reaction is completed for 4 hours, cool down to below 40°C;
[0048] (2) Add 0.38 mol of sodium chloroethylsulfonate to the above four-necked flask, stir to dissolve, maintain the stirring speed at 230 rpm, heat to reflux for 30 h, and distill under reduced pressure to obtain a reddish brown solid as the crude product;
[0049] (3) Recrystallize with 130 g of ethyl acetate to obtain a light yellow solid, which is then dried at 105 °C for 10 h to obtain the product clay stabilizer N 5 .
[0050] Example 6
[0051] (1) Add 0.2 mol piperazine, 526 g isobutyl alcohol and 0.19 mol 1,12-dibromododecane to a four-necked flask equipped with a condenser, a stirrer and a dropping funnel, stir to dissolve, maintain the stirring speed at 220 rpm, heat to 60°C in an oil bath, test the pH every 10 minutes within 1 hour after the start of the reaction, if the pH is lower than 7, adjust the pH to 8 with 1 mol / L sodium hydroxide solution, test the pH every 30 minutes after 1 hour after the start of the reaction, if the pH is lower than 7, adjust the pH to 8 with 1 mol / L sodium hydroxide solution, and always maintain the pH between 7 and 8 during the reaction. After the reaction is completed for 6 hours, cool down to below 40°C;
[0052] (2) Add 0.41 mol of sodium chloroethylsulfonate to the above four-necked flask, stir to dissolve, maintain the stirring speed at 250 rpm, heat to reflux for 48 h, and distill under reduced pressure to obtain a reddish brown solid as the crude product;
[0053] (3) Recrystallize with 136.6 g of ethyl acetate to obtain a light yellow solid, which is dried at 98° C. for 8 h to obtain the product clay stabilizer N 6 .
[0054] Example 7
[0055] (1) Add 0.2 mol piperazine, 570 g ethanol and 0.21 mol 1,12-dibromododecane to a four-necked flask equipped with a condenser, a stirrer and a dropping funnel, stir to dissolve, maintain the stirring speed at 250 rpm, heat to 55°C in an oil bath, test the pH every 10 minutes within 1 hour after the start of the reaction, if the pH is lower than 7, adjust it to pH 8 with 1 mol / L sodium hydroxide solution, test the pH every 30 minutes after 1 hour after the start of the reaction, if the pH is lower than 7, adjust it to pH 8 with 1 mol / L sodium hydroxide solution, and always maintain the pH between 7 and 8 during the reaction. After the reaction is completed for 5 hours, cool down to below 40°C;
[0056] (2) Add 0.39 mol of sodium chloroethylsulfonate to the above four-necked flask, stir to dissolve, maintain the stirring speed at 240 rpm, heat to reflux for 40 h, and distill under reduced pressure to obtain a reddish brown solid as the crude product;
[0057] (3) Recrystallize with 129.4 g of ethyl acetate to obtain a light yellow solid, which is dried at 100 ° C for 9 h to obtain the product clay stabilizer N 7 .
[0058] Example 8
[0059] (1) Add 0.2 mol piperazine, 670 g ethanol and 0.2 mol 1,12-dibromododecane to a four-necked flask equipped with a condenser, a stirrer and a dropping funnel, stir to dissolve, maintain the stirring speed at 200 rpm, heat the oil bath to 57°C, test the pH every 10 minutes within 1 hour after the start of the reaction, if the pH is lower than 7, adjust it to pH 8 with 1 mol / L sodium hydroxide solution, test the pH every 30 minutes after 1 hour after the start of the reaction, if the pH is lower than 7, adjust it to pH 8 with 1 mol / L sodium hydroxide solution, and always maintain the pH between 7 and 8 during the reaction. After the reaction is completed for 6 hours, cool down to below 40°C;
[0060] (2) Add 0.46 mol of sodium chloroethylsulfonate to the above four-necked flask, stir to dissolve, maintain the stirring speed at 210 rpm, heat to reflux for 48 h, and distill under reduced pressure to obtain a reddish brown solid as the crude product;
[0061] (3) Recrystallize with 130.8 g of ethyl acetate to obtain a light yellow solid, which is dried at 95 °C for 9 h to obtain the product clay stabilizer N 8 .
[0062] Example 9
[0063] (1) Add 0.2 mol piperazine, 646 g isobutyl alcohol and 0.205 mol 1,12-dibromododecane to a four-necked flask equipped with a condenser, a stirrer and a dropping funnel, stir and dissolve, maintain the stirring speed at 230 rpm, heat the oil bath to 59°C, test the pH every 10 minutes within 1 hour after the reaction starts, if the pH is lower than 7, adjust the pH to 8 with 1 mol / L sodium hydroxide solution, test the pH every 30 minutes after the reaction starts 1 hour, if the pH is lower than 7, adjust the pH to 8 with 1 mol / L sodium hydroxide solution, and always maintain the pH between 7 and 8 during the reaction. After the reaction is completed for 5 hours, cool down to below 40°C;
[0064] (2) Add 0.46 mol of sodium chloroethylsulfonate to the above four-necked flask, stir to dissolve, maintain the stirring speed at 220 rpm, heat to reflux for 48 h, and distill under reduced pressure to obtain a reddish brown solid as the crude product;
[0065] (3) Recrystallize with 132.3 g of ethyl acetate to obtain a light yellow solid, which is then dried at 105° C. for 10 h to obtain the product clay stabilizer N 9 .
[0066] Example 10
[0067] (1) Add 0.2 mol piperazine, 596 g isobutyl alcohol and 0.195 mol 1,12-dibromododecane to a four-necked flask equipped with a condenser, a stirrer and a dropping funnel, stir and dissolve, maintain the stirring speed at 210 rpm, heat the oil bath to 57°C, test the pH every 10 minutes within 1 hour after the start of the reaction, if the pH is lower than 7, adjust the pH to 8 with 1 mol / L sodium hydroxide solution, test the pH every 30 minutes after 1 hour after the start of the reaction, if the pH is lower than 7, adjust the pH to 8 with 1 mol / L sodium hydroxide solution, and always maintain the pH between 7 and 8 during the reaction. After the reaction is completed for 6 hours, cool down to below 40°C;
[0068] (2) Add 0.44 mol of sodium chloroethylsulfonate to the above four-necked flask, stir to dissolve, maintain the stirring speed at 250 rpm, heat to reflux for 44 h, and distill under reduced pressure to obtain a reddish brown solid as the crude product;
[0069] (3) Recrystallize with 137.6 g of ethyl acetate to obtain a light yellow solid, which is dried at 90 ° C for 9 h to obtain the product clay stabilizer N 10 .
[0070] Example 11 Evaluation of the Anti-swelling Capacity of Clay Stabilizer
[0071] Refer to method 7.5 in SY / T5971-2016 "Performance Evaluation Method of Clay Stabilizer for Oil and Gas Field Fracturing Acidification and Water Injection", and use the centrifugal method to test the anti-swelling rate.
[0072] Take 0.5 g of clay stabilizer, add 49.5 g of distilled water and shake well to obtain a clay stabilizer solution.
[0073] Weigh 0.50g sodium bentonite, put it into a 10mL centrifuge tube, add 10mL clay stabilizer solution, shake well, leave it at room temperature for 2h, put it into a centrifuge, centrifuge at a speed of 1500r / min for 15min, and read the volume V of the sodium bentonite after expansion. 1 .
[0074] When the clay stabilizer solution is replaced by distilled water, the volume of sodium bentonite after expansion is V 2 .
[0075] When kerosene is used to replace the clay stabilizer solution, the volume of sodium bentonite after expansion is V 0 .
[0076] Calculation method of anti-swelling rate
[0077] B=(V 2 -V 1 ) / (V 2 -V 0 )×100%
[0078] The clay stabilizer of Huainan Kedi Chemical Technology Co., Ltd. was used as a comparative sample. The test results of the anti-swelling rate of the clay stabilizer are shown in Table 1.
[0079] From Table 1 we can see that:
[0080] Clay stabilizer N of the present invention 1 、N 2 、N 3 、N 4 、N 5 、N 6 、N 7 、N 8 、N 9 、N 10 When the mass concentration is 1%, the anti-swelling rate is greater than 97%, and the highest reaches 99.0% (N 10 ); while the oil removal rate of the comparative sample is 90.8%, which is significantly lower than that of the present invention.
[0081] Example 12 Evaluation of Temperature Resistance of Clay Stabilizer
[0082] The clay stabilizer solution was placed in a sealed high-pressure tank, placed in a 350°C oven, taken out after 24 hours, and the anti-swelling rate was tested according to the method of Example 11.
[0083] The clay stabilizer of Huainan Kedi Chemical Technology Co., Ltd. was used as a comparative sample. The test results of the anti-swelling rate of the clay stabilizer are shown in Table 1.
[0084] Table 1 Test results of anti-swelling rate, temperature resistance and water washing resistance
[0085]
[0086] Clay stabilizer N of the present invention 1 、N 2 、N 3 、N 4 、N 5 、N 6 、N 7 、N 8 、N 9 、N 10 In an environment of 350℃, the anti-swelling rate reaches over 96%, with the highest reaching 98.2% (N 10 ); while the anti-swelling rate of the comparative sample is 84.2%, which is significantly lower than that of the present invention.
[0087] The heat-resistant anti-swelling clay stabilizer of the present invention has a wide range of raw material sources, a simple synthesis process and low cost; the heat-resistant anti-swelling clay stabilizer of the present invention has a high anti-swelling rate, and the anti-swelling rate reaches more than 97% under the condition of a use concentration of 1wt%; and the heat-resistant anti-swelling clay stabilizer has good temperature resistance and is adapted to the high temperature characteristics of the formation. In an environment of 350°C, the anti-swelling rate reaches more than 96%. Therefore, the heat-resistant anti-swelling clay stabilizer of the present invention can be widely used in the field of oil layer protection technology.
Claims
1. A method for preparing a heat-resistant anti-swelling clay stabilizer, characterized in that: The preparation method specifically comprises the following steps: (1) piperazine, solvent and 1,12-dibromododecane were added to a four-necked flask equipped with a condenser, a stirrer and a dropping funnel, and the mixture was stirred to dissolve. The stirring speed was maintained at 200-250 rpm, and the oil bath was heated to 55-60° C. Within 1 hour after the reaction started, the pH was tested every 10 minutes. If the pH was lower than 7, the pH was adjusted to 8 with 1 mol / L sodium hydroxide solution. After 1 hour after the reaction started, the pH was tested every 30 minutes. If the pH was lower than 7, the pH was adjusted to 8 with 1 mol / L sodium hydroxide solution. The pH was always maintained between 7 and 8 during the reaction. After the reaction was completed, the temperature was lowered to below 40° C. (2) adding sodium chloroethylsulfonate to the above four-necked flask, stirring to dissolve, maintaining the stirring speed at 200-250 rpm, heating to reflux, and distilling under reduced pressure to obtain a reddish brown solid as a crude product; (3) recrystallizing from ethyl acetate to obtain a light yellow solid, drying at 90-105° C. for 8-10 h to obtain a clay stabilizer product; The molar ratio of 1,12-dibromododecane, sodium chloroethylsulfonate and piperazine is 0.8-1.2:1.5-2.5:
1.
2. The method for preparing a heat-resistant anti-swelling clay stabilizer according to claim 1, characterized in that: The molar ratio of the 1,12-dibromododecane, sodium chloroethylsulfonate and piperazine is 0.9-1.1:2-2.3:
1.
3. The method for preparing a heat-resistant anti-swelling clay stabilizer according to claim 1, characterized in that: The solvent described in step (1) is one of methanol, ethanol, propanol, isopropanol, butanol and isobutanol.
4. The method for preparing a heat-resistant anti-swelling clay stabilizer according to claim 3, characterized in that: The solvent is ethanol or isobutanol.
5. The method for preparing a heat-resistant anti-swelling clay stabilizer according to claim 3 or 4, characterized in that: The mass ratio of the solvent to piperazine in step (1) is 30-40:
1.
6. The method for preparing a heat-resistant anti-swelling clay stabilizer according to claim 1, characterized in that: The reaction time in step (1) is 3-6 hours.
7. The method for preparing a heat-resistant anti-swelling clay stabilizer according to claim 1, characterized in that: The heating reflux time described in step (2) is 12-48h.
8. The method for preparing a heat-resistant anti-swelling clay stabilizer according to claim 1, characterized in that: The mass ratio of ethyl acetate to piperazine in step (3) is 6-8:
1.
9. The clay stabilizer prepared by the method for preparing a heat-resistant anti-swelling clay stabilizer according to any one of claims 1 to 8, characterized in that: The molecular structure of the clay stabilizer is as follows: Wherein: n=2-10, n is a natural number.
Citation Information
Patent Citations
Expandable elastomeric material in presence of water or oil
CN102844401A
Temperature-resistant and salt-resistant type anti-swelling clay stabilizer and synthetic method thereof
CN106675534A