CN115819655B - Underground self-synthesis swelling shrinking agent and preparation method thereof - Google Patents
Underground self-synthesis swelling shrinking agent and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a preparation method of an underground self-synthesis swelling agent, which comprises the following steps: s1, adding 2-8 parts of micromolecular cationic compound into 90-96 parts of sodium bentonite solution A which is already swelled and saturated under the stirring condition, and continuously stirring at the same stirring speed to obtain an intermediate reaction solution; s2, dropwise adding 2-3 parts of peroxide solution B with controllable reaction speed into the intermediate reaction solution obtained in the step S1 to obtain an intermediate reaction solution; and S3, stirring the intermediate reaction liquid obtained in the step S2, and then standing for reaction to obtain the underground self-synthesis swelling agent. The invention also discloses a downhole self-synthesis swelling reducer prepared by the preparation method. The invention has the following beneficial effects: 1. all the chemical agents are compounds with small molecular weight, and displace free water and adsorb clay crystal layers; 2. the reaction occurs in the clay crystal layer; 3. the shrinkage reaction pulls the distance of the smectic layer to realize shrinkage and expansion.
Description
Technical Field
The invention belongs to the field of oilfield exploitation, and particularly relates to an underground self-synthesis swelling agent and a preparation method thereof.
Background
At present, the reserves of high-clay oil reservoirs in victory oil fields exceed 3.2 hundred million tons, so that about 80% of the high-clay oil reservoirs at present enter the middle and later stages of development, clay expansion and blockage cause that oil wells cannot be produced and water wells cannot be injected.
The swelling inhibitor is adopted in the high-clay oil reservoir to inhibit the swelling of clay, but as the development proceeds, the stratum clay is already swelled to block the seepage channel, and meanwhile, the swelling inhibitor is injected again to be unable to effectively restore to the original state because the distance between the crystal layers is too large.
At present, the exploitation of high-clay reservoirs mainly has two problems: 1. under long-term flushing, the swelling inhibitor ions are easily hydrated by ions (Na + 、Ca 2+ 、Mg 2+ ) The mud is expanded again to block the channel, and the effective period of the current anti-swelling agent is generally shorter and is only about 3 months; 2. at present, the oil reservoirs enter the development middle stage, the clay is expanded and blocked, and the shrinkage-expansion recovery seepage channel is the basis for realizing efficient development.
Therefore, for the already expanded high-clay oil reservoir, development of a shrinkage-expansion system suitable for the high-clay oil reservoir is necessary to be pursued, so as to restore a seepage channel and realize the re-economic utilization of the oil reservoir.
Disclosure of Invention
The invention aims to: aiming at the defects of the prior art, the invention discloses an underground self-synthesis swelling reducer and a preparation method thereof. The invention is applied to the field of the shrinkage and expansion recovery seepage channels of high-clay oil reservoirs in the oilfield production process, and aims to compress the spacing between clay crystal layers and displace free water between crystal layers, improve stratum blockage caused by expansion and recover the normal production of an oil-water well.
The invention adopts the strong-adsorptivity micromolecular cationic compound to be firstly and stably adsorbed between montmorillonite crystal layers to displace free water, then improves the underground environment condition, takes peroxide as an initiator to realize the underground polycondensation of olefin groups, and draws in and compresses the spacing between the crystal layers to realize the shrinkage, expansion, unblocking and recovering a seepage channel. The small molecular cationic compounds used in the invention comprise dimethyl dodecyl allyl ammonium chloride, dimethyl hexadecyl allyl ammonium chloride, dimethyl octadecyl allyl ammonium chloride, trimethyl allyl ammonium chloride, diallyl dimethyl ammonium chloride and the like, and the peroxides used in the invention comprise di-tert-butyl peroxide, dibenzoyl peroxide, tert-butyl peroxybenzoate and the like, and the corresponding N-vinyl pyrrolidone is added as a regulator according to the needs to control the reaction speed and degree, so that the optimal polymerization under the well bottom environment is realized.
The technical scheme is as follows: the preparation method of the underground self-synthesis swelling agent comprises the following steps in parts by mass:
s1, adding 2-8 parts of micromolecular cationic compound into 90-96 parts of sodium bentonite solution A which is already swelled and saturated while stirring, and continuously stirring at the same stirring speed to obtain an intermediate reaction solution;
s2, dropwise adding 2-3 parts of peroxide solution B with controllable reaction speed into the intermediate reaction solution obtained in the step S1 to obtain an intermediate reaction solution;
and S3, continuously stirring the intermediate reaction liquid obtained in the step S2 for a period of time, and then standing for reaction, thus obtaining the underground self-synthesis swelling agent.
Further, the small molecule cationic compound in the step S1 is one or a mixture of several of dimethyl dodecyl allyl ammonium chloride, dimethyl hexadecyl allyl ammonium chloride, dimethyl octadecyl allyl ammonium chloride, allyl trimethyl ammonium chloride and dimethyl diallyl ammonium chloride.
Further, the preparation method of the sodium bentonite solution A which is already swelled and saturated in the step S1 is as follows:
0.5 part of sodium bentonite is dissolved in 49.5 parts of water, then stirred for 25-35 min at 800-1200 r/min, and kept stand for 110-130 min to form sodium bentonite solution A which is already swelled and saturated.
Further, the adding speed of the micromolecular cationic compound in the step S1 is 5-10 mL/min, the stirring speed in the step S1 is 800-1000 r/min, and after the micromolecular cationic compound is added into the sodium bentonite solution A which is already swelled and saturated, the stirring is continued for 25-35 minutes, so that an intermediate reaction solution is obtained.
Further, the peroxide solution B with controllable reaction rate in step S2 is a solution formed by dissolving peroxide with a regulator, and the preparation process thereof is as follows, in parts by mass:
and (3) dropwise adding 0.2-0.5 part of peroxide into 4-6 times of the peroxide regulator, controlling the dropwise adding speed to be 10-15 drops/min, controlling the reaction temperature to be 20-30 ℃, continuously stirring under the condition of 800-1200 r/min, continuously stirring for 25-35 min while keeping the stirring speed unchanged after the dropwise adding is completed, and standing for 100-140 min to obtain the peroxide solution B with controllable reaction speed.
Further, the peroxide is one or a mixture of a plurality of di-tert-butyl peroxide, dibenzoyl peroxide and tert-butyl peroxybenzoate.
Further, the regulator is one of N-vinyl pyrrolidone, polyvinylpyrrolidone and nonylphenol polyoxyethylene ether.
Further, the dropping speed of the peroxide solution B with controllable reaction speed in the step S2 is 20-30 drops/min;
further, the reaction temperature of the reaction in the step S3 is 50-120 ℃, the intermediate reaction liquid obtained in the step S2 is stirred for 25-35 min at the stirring speed of 800-1200 r/min in the step S3, and then the reaction mixture is kept stand for 7-9 h to obtain the downhole self-synthesis swelling reducer.
The underground self-synthesis swelling agent is prepared by the preparation method of any underground self-synthesis swelling agent.
The invention has the following effects: the downhole self-synthesis swelling agent disclosed by the invention can realize a swelling rate of more than 30%, can more effectively improve pore blocking of the bottom of a well caused by clay swelling, and can restore the original permeability.
Compared with the conventional anti-swelling and shrinking swelling agent at present, the invention has the following beneficial effects:
1. all the chemical agents are compounds with small molecular weight, and displace free water and adsorb clay crystal layers;
2. the reaction occurs in the clay crystal layer;
3. the shrinkage reaction pulls the distance of the smectic layer to realize shrinkage and expansion.
The specific embodiment is as follows:
the following detailed description of specific embodiments of the invention.
Example 1:
5g of sodium bentonite is dissolved in 495g of water, stirred for 30min at 1000r/min, and kept stand for 2h to form a stable saturated expansion sodium bentonite solution A;
2g of di-tert-butyl peroxide is dropwise added into 10g of N-vinyl pyrrolidone, the dropwise adding speed is 10 drops/min, the temperature is controlled to be 25 ℃, the mixture is continuously stirred under the condition of 1000r/min, after all dropwise adding is finished, the mixture is continuously stirred for 30min, and a peroxide solution B with controllable reaction speed is formed after standing for 2 h;
adding 2 parts of trimethyl allyl ammonium chloride into a saturated expansion sodium bentonite solution A at a speed of 5mL/min in a reaction kettle at 120 ℃, and stirring at 1000r/min for 30min to obtain a solution D;
and (3) dripping the prepared peroxide solution B with controllable reaction speed into the solution D at the speed of 20-30 drops/min, continuously stirring for 30min at 1000r/min, and standing for reaction for 8h to obtain a stable swelling agent system C.
Evaluation of performance: dissolving 0.5g of sodium bentonite in 49.5g of water, stirring for 30min at 1000r/min, standing for 2h to form a stable saturated swelling sodium bentonite solution E, transferring the solution into a centrifuge tube, centrifuging for 30min at a speed of 3000r/min, taking out the centrifuge tube, pouring out supernatant, and measuring that the swelling height is 4.6mm. Taking 50mL of the stable swelling agent system C, placing into a centrifuge tube, centrifuging for 30min at a speed of 3000r/min, taking out the centrifuge tube, pouring out supernatant, and measuring the swelling height to be 2.9mm. The swelling ratio of the swelling agent system= (4.6-2.9)/4.6 x 100% = 36.96%.
Example 2:
5g of sodium bentonite is dissolved in 495g of water, stirred for 30min at 1000r/min, and kept stand for 2h to form a stable saturated expansion sodium bentonite solution A; 5g of dibenzoyl peroxide is dropwise added into 25g of N-vinyl pyrrolidone, the dropwise adding speed is 10 drops/min, the temperature is controlled to be 25 ℃, the mixture is continuously stirred under the condition of 1000r/min, after all dropwise adding is finished, the mixture is continuously stirred for 30min, and a peroxide solution B with controllable reaction speed is formed after standing for 2 h. Adding 8 parts of diallyl dimethyl ammonium chloride into a saturated sodium bentonite solution A at a speed of 5mL/min in a reaction kettle at 90 ℃ and stirring at 1000r/min for 30min to obtain a solution D; and (3) dripping the prepared peroxide solution B with controllable reaction speed into the solution D at the speed of 20-30 drops/min, continuously stirring for 30min at 1000r/min, and standing for reaction for 8h to obtain a stable swelling agent system C.
Evaluation of performance: dissolving 0.5g of sodium bentonite in 49.5g of water, stirring for 30min at 1000r/min, standing for 2h to form a stable saturated swelling sodium bentonite solution E, transferring the solution into a centrifuge tube, centrifuging for 30min at a speed of 3000r/min, taking out the centrifuge tube, pouring out supernatant, and measuring that the swelling height is 4.6mm. Taking 50mL of the stable swelling agent system C, placing into a centrifuge tube, centrifuging for 30min at a speed of 3000r/min, taking out the centrifuge tube, pouring out supernatant, and measuring the swelling height to be 2.3mm. The shrinkage of the shrinkage and expansion agent system is = (4.6-2.1)/4.6 x 100% = 54.35%.
Example 3:
5g of sodium bentonite is dissolved in 495g of water, stirred for 30min at 1000r/min, and kept stand for 2h to form a stable saturated expansion sodium bentonite solution A; 3g of tert-butyl peroxybenzoate is dripped into 25g of N-vinyl pyrrolidone, the dripping speed is 10 drops/min, the temperature is controlled to be 25 ℃, the mixture is continuously stirred under the condition of 1000r/min, after all dripping is finished, the mixture is continuously stirred for 30min, and the peroxide solution B with controllable reaction speed is formed after standing for 2 h. In a reaction kettle at 50 ℃, 1 part of dimethyl dodecyl allyl ammonium chloride, 1 part of dimethyl hexadecyl allyl ammonium chloride and 3 dimethyl octadecyl allyl ammonium chloride are respectively added into a saturated expansion sodium bentonite solution A at a speed of 5mL/min, and stirred at 1000r/min for 30min to obtain a solution D; and (3) dripping the prepared peroxide solution B with controllable reaction speed into the solution D at the speed of 20-30 drops/min, continuously stirring for 30min at 1000r/min, and standing for reaction for 8h to obtain a stable swelling agent system C.
Evaluation of performance: dissolving 0.5g of sodium bentonite in 49.5g of water, stirring for 30min at 1000r/min, standing for 2h to form a stable saturated swelling sodium bentonite solution E, transferring the solution into a centrifuge tube, centrifuging for 30min at a speed of 3000r/min, taking out the centrifuge tube, pouring out supernatant, and measuring that the swelling height is 4.6mm. Taking 50mL of the stable swelling agent system C, placing into a centrifuge tube, centrifuging for 30min at a speed of 3000r/min, taking out the centrifuge tube, pouring out supernatant, and measuring the swelling height to be 2.6mm. The swelling ratio of the swelling agent system= (4.6-2.6)/4.6 x 100% = 43.48%.
Verification test:
(1) Dissolving 0.5g of sodium bentonite in 49.5g of water, stirring for 30min at 1000r/min, and standing for 2h to form a stable saturated swelling sodium bentonite solution E;
(2) Transferring the saturated expansion sodium bentonite solution E into a centrifuge tube, centrifuging for 30min at a speed of 3000r/min, taking out the centrifuge tube, pouring out supernatant, and measuring the expansion height to be L1mm;
(3) Placing 50ml of an anti-swelling agent with the concentration of 2wt% into the centrifuge tube, centrifuging for 30min at the speed of 3000r/min, taking out the centrifuge tube, pouring out supernatant, and measuring the swelling height to be L2mm;
(4) Calculate the shrinkage and expansion ratio = (L1-L2)/L1 x 100%
Respectively selecting different anti-swelling agents: KCl, NH 4 Cl, trimethylammonium chloride and the downhole self-synthesized swelling agent prepared in specific example 3 are shown in the following specific test data:
as can be seen from the table, the downhole self-synthesized swelling agent disclosed by the invention has a better swelling rate than the general swelling agents.
Example 4
The preparation method of the underground self-synthesis swelling agent comprises the following steps in parts by mass:
s1, adding 2 parts of micromolecular cationic compound into 90 parts of sodium bentonite solution A which is already expanded and saturated at a stirring speed of 800r/min, and continuously stirring for 25-35 min at the same stirring speed to obtain an intermediate reaction solution;
s2, dropwise adding 2 parts of peroxide solution B with controllable reaction speed into the intermediate reaction solution obtained in the step S1 to obtain the intermediate reaction solution;
and S3, stirring the intermediate reaction liquid obtained in the step S2 at a stirring speed of 800r/min for 25min, and then standing for 7h to obtain the downhole self-synthesis swelling agent.
Further, the small molecule cationic compound in step S1 is dimethyldodecylallyl ammonium chloride.
Further, the preparation method of the sodium bentonite solution A which is already swelled and saturated in the step S1 is as follows:
0.5 part of sodium bentonite is dissolved in 49.5 parts of water, then stirred at 800r/min for 25min, and the mixture is left to stand for 130min to form a sodium bentonite solution A which is already swelled and saturated.
Further, the adding speed of the small molecule cationic compound in the step S1 is 5mL/min.
Further, the peroxide solution B with controllable reaction rate in step S2 is a solution formed by dissolving peroxide with a regulator, and the preparation process thereof is as follows, in parts by mass:
and (3) dropwise adding 0.2 part of peroxide into a regulator which is 4 times of the peroxide, controlling the dropwise adding speed to be 10 drops/min, controlling the reaction temperature to be 20 ℃, continuously stirring under the condition of 1200r/min, continuously stirring for 25min after all dropwise adding is completed, continuously maintaining the stirring speed unchanged, and standing for 140min to obtain the peroxide solution B with controllable reaction speed.
Still further, the peroxide is di-t-butyl peroxide.
Still further, the modulator is N-vinylpyrrolidone.
Further, the dropping speed of the peroxide solution B with controllable reaction speed in the step S2 is 20 drops/min;
further, the reaction temperature of the reaction described in step S3 is 50 ℃.
The underground self-synthesis swelling agent is prepared by the preparation method of any underground self-synthesis swelling agent.
Example 5
The preparation method of the underground self-synthesis swelling agent comprises the following steps in parts by mass:
s1, adding 8 parts of small molecular cationic compound into 96 parts of sodium bentonite solution A which is already expanded and saturated at a stirring speed of 1000r/min, and continuously stirring for 35min at the same stirring speed to obtain an intermediate reaction solution;
s2, dropwise adding 3 parts of peroxide solution B with controllable reaction speed into the intermediate reaction solution obtained in the step S1 to obtain the intermediate reaction solution;
and S3, stirring the intermediate reaction liquid obtained in the step S2 for 35min at a stirring speed of 1200r/min, and then standing for 9h to obtain the downhole self-synthesis swelling agent.
Further, the small molecular cationic compound in the step S1 is a mixture of dimethyl dodecyl allyl ammonium chloride and dimethyl hexadecyl allyl ammonium chloride with equal mass ratio.
Further, the preparation method of the sodium bentonite solution A which is already swelled and saturated in the step S1 is as follows:
0.5 part of sodium bentonite is dissolved in 49.5 parts of water, then stirred for 35min at 1200r/min, and the mixture is left to stand for 110min to form a sodium bentonite solution A which is already swelled and saturated.
Further, the adding speed of the small molecule cationic compound in the step S1 is 10mL/min.
Further, the peroxide solution B with controllable reaction rate in step S2 is a solution formed by dissolving peroxide with a regulator, and the preparation process thereof is as follows, in parts by mass:
and (3) dropwise adding 0.5 part of peroxide into a regulator which is 6 times of the peroxide, controlling the dropwise adding speed to be 15 drops/min, controlling the reaction temperature to be 30 ℃, continuously stirring under the condition of 800r/min, continuously stirring for 35min after all dropwise adding is finished, continuously maintaining the stirring speed unchanged, and standing for 100 min to obtain the peroxide solution B with controllable reaction speed.
Further, the peroxide is a mixture of dibenzoyl peroxide and tert-butyl peroxybenzoate with equal mass.
Still further, the modulator is polyvinylpyrrolidone.
Further, the dropping speed of the peroxide solution B with controllable reaction speed in the step S2 is 30 drops/min;
further, the reaction temperature of the reaction described in step S3 is 120 ℃.
The underground self-synthesis swelling agent is prepared by the preparation method of any underground self-synthesis swelling agent.
Example 6
The preparation method of the underground self-synthesis swelling agent comprises the following steps in parts by mass:
s1, adding 4 parts of micromolecular cationic compound into 92 parts of sodium bentonite solution A which is already expanded and saturated at the stirring speed of 900r/min, and continuously stirring for 30min at the same stirring speed to obtain an intermediate reaction solution;
s2, dropwise adding 2.5 parts of peroxide solution B with controllable reaction speed into the intermediate reaction solution obtained in the step S1 to obtain the intermediate reaction solution;
and S3, stirring the intermediate reaction liquid obtained in the step S2 for 30min at a stirring speed of 1000r/min, and then standing for reaction for 8h to obtain the downhole self-synthesis swelling agent.
Further, the small molecule cationic compound in step S1 is dimethyl hexadecylallylammonium chloride.
Further, the preparation method of the sodium bentonite solution A which is already swelled and saturated in the step S1 is as follows:
0.5 part of sodium bentonite is dissolved in 49.5 parts of water, then stirred for 30min at 1000r/min, and the mixture is left to stand for 120min to form a sodium bentonite solution A which is already swelled and saturated.
Further, the adding speed of the small molecule cationic compound in the step S1 is 8mL/min.
Further, the peroxide solution B with controllable reaction rate in step S2 is a solution formed by dissolving peroxide with a regulator, and the preparation process thereof is as follows, in parts by mass:
and (3) dropwise adding 0.3 part of peroxide into a regulator which is 5 times of the peroxide, controlling the dropwise adding speed to be 12 drops/min, controlling the reaction temperature to be 25 ℃, continuously stirring under the condition of 1000r/min, continuously stirring for 30min after all dropwise adding is completed, continuously maintaining the stirring speed unchanged, and standing for 120min to obtain the peroxide solution B with controllable reaction speed.
Still further, the peroxide is dibenzoyl peroxide.
Still further, the regulator is nonylphenol polyoxyethylene ether.
Further, the dropping speed of the peroxide solution B with controllable reaction speed in the step S2 is 25 drops/min;
further, the reaction temperature of the reaction described in step S3 is 80 ℃.
The underground self-synthesis swelling agent is prepared by the preparation method of any underground self-synthesis swelling agent.
Examples 7 to 11
Substantially the same as in example 4, the difference is only that: small molecule cationic compounds differ:
further, the small molecule cationic compound in the step S1 is one or a mixture of several of dimethyl dodecyl allyl ammonium chloride, dimethyl hexadecyl allyl ammonium chloride, dimethyl octadecyl allyl ammonium chloride, allyl trimethyl ammonium chloride and dimethyl diallyl ammonium chloride.
Examples 12 to 15
Substantially the same as in example 4, except that the peroxide was different
The embodiments of the present invention have been described in detail. However, the present invention is not limited to the above-described embodiments, and various modifications may be made within the knowledge of those skilled in the art without departing from the spirit of the present invention.
Claims (10)
1. The preparation method of the downhole self-synthesis swelling reducer is characterized by comprising the following steps of:
s1, adding 2-8 parts of micromolecular cationic compound into 90-96 parts of sodium bentonite solution A which is already swelled and saturated while stirring, and continuously stirring for a period of time at the same stirring speed to obtain an intermediate reaction solution;
s2, dropwise adding 2-3 parts of peroxide solution B with controllable reaction speed into the intermediate reaction solution obtained in the step S1 to obtain an intermediate reaction solution;
and S3, continuously stirring the intermediate reaction liquid obtained in the step S2 for a period of time, and then standing for reaction, thus obtaining the underground self-synthesis swelling agent.
2. The method for preparing a downhole self-synthesized swelling agent according to claim 1, wherein the small molecule cationic compound in the step S1 is one or a mixture of several of dimethyldodecylallyl ammonium chloride, dimethylhexadecylallyl ammonium chloride, dimethyloctadecylallyl ammonium chloride, allyltrimethyl ammonium chloride, dimethyldiallyl ammonium chloride.
3. The method for preparing a downhole self-synthesized swelling agent according to claim 1, wherein the method for preparing the sodium bentonite solution a which is already swelled and saturated in the step S1 comprises the following steps:
0.5 part of sodium bentonite is dissolved in 49.5 parts of water, then stirred for 25-35 min at 800-1200 r/min, and kept stand for 110-130 min to form sodium bentonite solution A which is already swelled and saturated.
4. The method for preparing the downhole self-synthesis swelling agent according to claim 1, wherein the adding speed of the small molecular cationic compound in the step S1 is 5-10 mL/min, the stirring speed in the step S1 is 800-1000 r/min, and after the small molecular cationic compound is added into the sodium bentonite solution A which is already swelled and saturated, stirring is continued for 25-35 minutes, so as to obtain an intermediate reaction solution.
5. The method of claim 1, wherein the peroxide solution B with controllable reaction rate in step S2 is a solution formed by dissolving peroxide in a regulator, and the preparation process comprises the following steps in parts by mass:
and (3) dropwise adding 0.2-0.5 part of peroxide into 4-6 times of the peroxide regulator, controlling the dropwise adding speed to be 10-15 drops/min, controlling the reaction temperature to be 20-30 ℃, continuously stirring under the condition of 800-1200 r/min, continuously stirring for 25-35 min while keeping the stirring speed unchanged after the dropwise adding is completed, and standing for 100-140 min to obtain the peroxide solution B with controllable reaction speed.
6. The method of claim 5, wherein the peroxide is one or more of di-t-butyl peroxide, dibenzoyl peroxide and t-butyl peroxybenzoate.
7. The method for preparing a downhole self-synthesized swelling agent according to claim 5, wherein the regulator is one of N-vinyl pyrrolidone, polyvinylpyrrolidone and polyoxyethylene nonylphenol ether.
8. The method for preparing a downhole self-synthesized swelling agent according to claim 1, wherein the dropping speed of the peroxide solution B with controllable reaction rate in the step S2 is 20 to 30 drops/min.
9. The method for preparing an underground self-synthesis swelling agent according to claim 1, wherein the reaction temperature of the reaction in the step S3 is 50-120 ℃, the intermediate reaction liquid obtained in the step S2 is stirred for 25-35 min at a stirring speed of 800-1200 r/min in the step S3, and then the reaction is allowed to stand for 7-9 h, so that the underground self-synthesis swelling agent is obtained.
10. A downhole self-synthesizing swelling agent prepared by the method of preparing a downhole self-synthesizing swelling agent according to any one of claims 1 to 9.
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