CN114989799B - Oligomeric cationic shrinking and swelling agent composition, oligomeric cationic shrinking and swelling agent, and preparation method and application thereof - Google Patents
Oligomeric cationic shrinking and swelling agent composition, oligomeric cationic shrinking and swelling agent, and preparation method and application thereof Download PDFInfo
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- CN114989799B CN114989799B CN202210840548.1A CN202210840548A CN114989799B CN 114989799 B CN114989799 B CN 114989799B CN 202210840548 A CN202210840548 A CN 202210840548A CN 114989799 B CN114989799 B CN 114989799B
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
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- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/58—Compositions for enhanced recovery methods for obtaining hydrocarbons, i.e. for improving the mobility of the oil, e.g. displacing fluids
- C09K8/588—Compositions for enhanced recovery methods for obtaining hydrocarbons, i.e. for improving the mobility of the oil, e.g. displacing fluids characterised by the use of specific polymers
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- C09K2208/00—Aspects relating to compositions of drilling or well treatment fluids
- C09K2208/12—Swell inhibition, i.e. using additives to drilling or well treatment fluids for inhibiting clay or shale swelling or disintegrating
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Abstract
The invention relates to the technical field of oil field chemicals, and discloses an oligomeric cationic type swelling and shrinking agent composition, an oligomeric cationic type swelling and shrinking agent, and a preparation method and application thereof. The composition contains the following components which are stored in a mixing way or independently: epichlorohydrin, dimethylamine, dodecyl dimethyl benzyl ammonium chloride, ammonium persulfate and a solvent; in the oligomeric cationic type shrinking and swelling agent composition, relative to 100 parts by weight of the solvent, the content of epichlorohydrin is 10-50 parts by weight, the content of dimethylamine is 10-60 parts by weight, the content of dodecyl dimethyl benzyl ammonium chloride is 1.6-6.4 parts by weight, and the content of ammonium persulfate is 0.03-0.12 part by weight. According to the invention, a specific amount of epichlorohydrin, dimethylamine, dodecyl dimethyl benzyl ammonium chloride, ammonium persulfate and a solvent are synergistically compounded to prepare the shrinking and swelling agent with high shrinking and swelling rate.
Description
Technical Field
The invention relates to the technical field of oilfield chemicals, in particular to an oligomeric cationic type shrinking-swelling agent composition, an oligomeric cationic type shrinking-swelling agent, and a preparation method and application thereof.
Background
In the process of oilfield flooding, because oil reservoirs usually contain many clay minerals, such as montmorillonite, illite, chlorite and kaolinite, the components can expand, disperse and migrate in water, so that the permeability of the stratum is reduced, the flooding pressure is increased, and the oil and gas exploitation effect is seriously affected.
The swelling shrinkage agent is a chemically synthesized macromolecular cationic compound, and the swelling shrinkage agent is used for modifying the crystal lattice of clay through the physical and chemical reaction with clay minerals so that the clay does not swell after meeting water; the expanded clay crystal lattice releases water molecules after being modified through chemical reaction, the crystal lattice is reduced, and the modified clay substances are firmly combined with in-situ layer minerals through the multi-point adsorption effect, so that the damage to the stratum caused by the expansion and the migration of the clay minerals in water is avoided.
In addition, the swelling shrinkage agent also has the anti-swelling function of the traditional clay stabilizer, can dehydrate and shrink the clay which is already hydrated and swelled, recover the permeability of a reservoir, improve the oil and gas development effect and save a large amount of stratum reconstruction cost.
However, from the research of the existing expansion-contraction agent, the expansion-contraction rate of the expansion-contraction agent produced by the existing manufacturer is only 25% at most; and the current expansion-reducing agents are all high polymers with the molecular weight of more than millions, and have single function.
Therefore, there is still a need for an improvement in the existing texturizing agents to provide an anti-texturizing agent with a higher texturizing ratio.
Disclosure of Invention
The invention aims to overcome the defect of low expansion ratio of the anti-swelling and anti-swelling agent in the prior art.
In order to achieve the above object, a first aspect of the present invention provides an oligomeric cationic type swelling agent composition, which comprises the following components stored in a mixed manner or independently:
epichlorohydrin, dimethylamine, dodecyl dimethyl benzyl ammonium chloride, ammonium persulfate and a solvent;
in the oligomeric cationic type shrinking and swelling agent composition, relative to 100 parts by weight of the solvent, the content of the epichlorohydrin is 10-50 parts by weight, the content of the dimethylamine is 10-60 parts by weight, the content of the dodecyl dimethyl benzyl ammonium chloride is 1.6-6.4 parts by weight, and the content of the ammonium persulfate is 0.03-0.12 part by weight;
the epichlorohydrin has a structure shown in a formula (1), and the dimethylamine has a structure shown in a formula (2).
In a second aspect, the invention provides a method of making an oligomeric cationic swelling and shrinking agent, the method comprising: mixing the components of the composition according to the first aspect.
In a third aspect, the invention provides an oligomeric cationic swelling and shrinking agent prepared by the method of the second aspect.
In a fourth aspect, the invention provides the use of the oligomeric cationic swelling agent of the third aspect in oil and gas development.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, a specific amount of epichlorohydrin, dimethylamine, dodecyl dimethyl benzyl ammonium chloride, ammonium persulfate and a solvent are cooperatively compounded, so that the shrinking and swelling agent with high shrinking and swelling rate can be prepared, the shrinking and swelling agent has good compatibility with the stratum, and the shrinking and swelling agent can effectively inhibit stratum clay minerals from swelling, dispersing and migrating when encountering water, thereby dehydrating and shrinking and swelling the swelled clay.
The product produced by the preparation method provided by the invention has low residual monomer content, simple preparation process, low cost, easy operation, less pollution and easy industrial production.
Detailed Description
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and these ranges or values should be understood to encompass values close to these ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
It should be noted that in each aspect of the present invention, the present invention is described only once in one aspect thereof without repeated descriptions with respect to the same components in each aspect, and those skilled in the art should not be construed as limiting the present invention.
It should be noted that in the present invention, the raw materials that are not described can be obtained from general commercial sources, and those skilled in the art can purchase the raw materials according to needs, and in the present invention, detailed description is omitted.
In the present invention, unless otherwise specified, the room temperature or the ambient temperature both indicate 25. + -. 2 ℃.
As described above, the first aspect of the present invention provides an oligomeric cationic type swelling agent composition, which contains the following components stored in a mixed manner or independently:
epichlorohydrin, dimethylamine, dodecyl dimethyl benzyl ammonium chloride, ammonium persulfate and a solvent;
in the low cationic swelling agent composition, relative to 100 parts by weight of the solvent, the content of the epichlorohydrin is 10-50 parts by weight, the content of the dimethylamine is 10-60 parts by weight, the content of the dodecyl dimethyl benzyl ammonium chloride is 1.6-6.4 parts by weight, and the content of the ammonium persulfate is 0.03-0.12 part by weight;
the epichlorohydrin has a structure shown in a formula (1), and the dimethylamine has a structure shown in a formula (2).
Preferably, in the oligomeric cationic swelling agent composition, relative to 100 parts by weight of the solvent, the content of the epichlorohydrin is 10-40 parts by weight, the content of the dimethylamine is 15-60 parts by weight, the content of the dodecyl dimethyl benzyl ammonium chloride is 3.2-6.4 parts by weight, and the content of the ammonium persulfate is 0.06-0.12 part by weight. The inventors have found that a swelling agent having a higher swelling ratio can be obtained by the specific embodiment in the preferred case.
According to a particularly preferred embodiment, the dimethylamine is an aqueous dimethylamine solution having a concentration of from 35 to 45 wt%.
According to a particularly preferred embodiment, the dodecyldimethylbenzylammonium chloride is benzalkonium chloride with a concentration of 70 to 80 wt.%.
Preferably, the solvent is selected from at least one of water, ethanol, propylene glycol.
As previously mentioned, a second aspect of the invention provides a method of making an oligomeric cationic heave agent, the method comprising: mixing the components of the composition according to the first aspect.
Preferably, the operation of mixing the components of the oligomeric cationic swelling agent composition comprises the following steps:
(1) In the presence of a first part of solvent, mixing dimethylamine and epichlorohydrin for the first time to obtain a first mixed solution; and
carrying out first contact on dodecyl dimethyl benzyl ammonium chloride and a second part of solvent to dissolve so as to obtain a solution I;
(2) Carrying out second mixing on the first mixed solution and the solution I to obtain a second mixed solution; and
carrying out second contact on ammonium persulfate and a third part of solvent to dissolve to obtain a solution II;
(3) Carrying out contact reaction on the second mixed solution and the solution II;
the weight ratio of the first part of solvent to the second part of solvent to the third part of solvent is 1-3.
The operation of the first contact and the second contact is not particularly required, and the ammonium dodecyl dimethyl benzyl chloride and the ammonium persulfate can be respectively dissolved, and the conditions of the first contact and the second contact respectively and independently comprise: the stirring speed is 50-60rpm, and the temperature is 20-30 ℃.
Preferably, the conditions of the first mixing and the second mixing each independently comprise: stirring speed is 50-60rpm, temperature is 20-30 deg.C, and time is 5-10min.
Preferably, in step (3), the conditions of the contact reaction at least include: the temperature is 80-85 ℃, and the time is 4-6h.
As previously mentioned, a third aspect of the present invention provides an oligomeric cationic Pan-shrinking agent prepared by the method of the second aspect.
As previously mentioned, a fourth aspect of the invention provides the use of the oligomeric cationic swelling agent of the third aspect in oil and gas development.
The present invention will be described in detail below by way of examples. In the following examples, various raw materials used are commercially available unless otherwise specified.
Epichlorohydrin: from basf corporation;
dimethylamine: from basf corporation;
trimethylbenzene: purchased from basf;
dodecyl dimethyl benzyl ammonium chloride: purchased from basf;
dodecyl methyl benzyl ammonium chloride: purchased from basf;
ammonium persulfate: from basf corporation;
in the following examples, the solvents were deionized water.
Example 1
The embodiment provides a preparation method of an oligomeric cationic swelling agent, which comprises the following steps:
(1) Adding 15g of dimethylamine aqueous solution (with the concentration of 40 wt%) and 20g of deionized water into a reaction kettle at the temperature of 30 ℃, then adding 10g of epichlorohydrin (with the concentration of 80 wt%), and stirring for 10min at 50rpm to obtain a first mixed solution; and
weighing 1.6g of dodecyl dimethyl benzyl ammonium chloride, and dissolving in 20g of deionized water to obtain a solution I;
(2) Stirring all the obtained first mixed solution and the solution I at the temperature of 30 ℃ for 5min at 60rpm to obtain a second mixed solution; and
weighing 0.03g of ammonium persulfate to dissolve in 10g of deionized water to obtain a solution II;
(3) And (3) reacting all the obtained second mixed solution and the solution II in a reaction kettle at the temperature of 80 ℃ for 6 hours to obtain the oligomeric cationic type swelling shrinking agent S1.
Example 2
The embodiment provides a preparation method of an oligomeric cationic swelling and shrinking agent, which comprises the following steps:
(1) Adding 15g of dimethylamine aqueous solution (with the concentration of 40 wt%) and 40g of deionized water into a reaction kettle at the temperature of 30 ℃, then adding 10g of epichlorohydrin (with the concentration of 80 wt%), and stirring for 10min at 50rpm to obtain a first mixed solution; and
weighing 3.2g of dodecyl dimethyl benzyl ammonium chloride, and dissolving in 40g of deionized water to obtain a solution I;
(2) Stirring all the obtained first mixed solution and the solution I at the temperature of 30 ℃ for 8min at 60rpm to obtain a second mixed solution; and
weighing 0.06g of ammonium persulfate to dissolve in 20g of deionized water to obtain a solution II;
(3) And (3) reacting all the obtained second mixed solution and the solution II in a reaction kettle at the temperature of 80 ℃ for 6 hours to obtain the oligomeric cationic type swelling shrinking agent S2.
Example 3
The embodiment provides a preparation method of an oligomeric cationic swelling agent, which comprises the following steps:
(1) Adding 30g of dimethylamine aqueous solution (with the concentration of 40 wt%) and 20g of deionized water into a reaction kettle at the temperature of 30 ℃, then adding 20g of epichlorohydrin (with the concentration of 80 wt%), and stirring for 8min at 55rpm to obtain a first mixed solution; and
weighing 3.2g of dodecyl dimethyl benzyl ammonium chloride, and dissolving in 20g of deionized water to obtain a solution I;
(2) Stirring all the obtained first mixed solution and the solution I at the temperature of 30 ℃ for 5min at 60rpm to obtain a second mixed solution; and
weighing 0.06g of ammonium persulfate to dissolve in 20g of deionized water to obtain a solution II;
(3) And (3) reacting all the obtained second mixed solution with the solution II in a reaction kettle at the temperature of 80 ℃ for 6 hours to obtain the low-polymer cationic swelling agent S3.
Example 4
This example prepared an oligomeric cationic swelling agent similar to that of example 3, except that 1.6g of dodecyldimethylbenzylammonium chloride was used.
The remaining procedure was the same as in example 3.
And obtaining the oligomeric cationic type shrinking and swelling agent S4.
Example 5
This example prepared an oligomeric cationic swelling agent in a similar manner to example 3, except that 0.03g of ammonium persulfate was used.
The remaining procedure was the same as in example 3.
To obtain the oligomeric cationic swelling agent S5.
Comparative example 1
This comparative example an oligomeric cationic swelling agent was prepared similar to example 3, except that dimethylamine was replaced by an equal mass of trimethylbenzene.
The remaining procedure was the same as in example 3.
Obtaining the low-polymer cationic swelling agent DS1.
Comparative example 2
This comparative example an oligomeric cationic swelling agent was prepared similar to example 3, except that dodecyl dimethyl benzyl ammonium chloride was replaced with an equal mass of dodecyl methyl benzyl ammonium chloride.
The remaining procedure was the same as in example 3.
Obtaining the low-polymer cationic shrinkage-expansion agent DS2.
Comparative example 3
This comparative example an oligomeric cationic swelling agent was prepared in a similar manner to example 3, except that 8g of dodecyldimethylbenzylammonium chloride was used.
The remaining procedure was the same as in example 3.
Obtaining the low-polymer cationic shrinkage-expansion agent DS3.
Comparative example 4
This comparative example an oligomeric cationic swelling agent was prepared in a similar manner to example 3, except that 75g of dimethylamine were used.
The remaining procedure was the same as in example 3.
Obtaining the low-polymer cationic swelling agent DS4.
Test example
The shrinkage-swelling rate of the low-polymer cationic shrinkage-swelling agent prepared in the examples and the comparative examples is detected, and the specific results are shown in table 1.
Wherein the shrinkage-expansion rate is detected by a centrifugation method of the anti-expansion rate in a standard SY/T5971-2016;
the specific detection method comprises the following steps:
(1) Weighing 0.50g of sodium bentonite, accurately weighing to 0.01g, loading into a 10mL centrifuge tube, adding 10mL of clay stabilizer solution, shaking thoroughly, standing at room temperature for 2h, loading into a centrifuge, centrifuging at 1500r/min for 15min, and measuring the swelling volume V of the sodium bentonite in the clay stabilizer solution 1 ；
(2) Weighing 0.50g of sodium bentonite, accurately weighing to 0.01g, loading into a 10mL centrifuge tube, adding 10mL of water, fully shaking, standing at room temperature for 2h, loading into a centrifuge, centrifuging at a rotation speed of 1500r/min for 15min, and measuring the expansion volume V of the sodium bentonite in the test water 2 ；
(3) Weighing 0.50g of sodium bentonite, accurately weighing to 0.01g, loading into a 10mL centrifuge tube, adding 10mL kerosene, shaking thoroughly, standing at room temperature for 2h, loading into a centrifuge, centrifuging at 1500r/min for 15min, and measuring the expansion volume V of the sodium bentonite in the kerosene 0 。
Calculating the shrinkage-expansion ratio of the shrinkage-expansion agent according to the following formula:
in formula (3):
x-shrinkage-expansion ratio,%;
V 2 the swelling volume of sodium bentonite in experimental water, mL;
V 1 the swelling volume of sodium bentonite in clay stabilizer solution, mL;
V 0 swelling volume of sodium bentonite in kerosene, mL.
TABLE 1
As can be seen from Table 1, a swelling agent with high swelling shrinkage can be prepared by using the oligomeric cationic swelling agent composition provided by the invention.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including various technical features being combined in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
Claims (10)
1. An oligomeric cationic type shrinking and swelling agent composition is characterized by comprising the following components which are stored in a mixing way or independently:
epichlorohydrin, dimethylamine, dodecyl dimethyl benzyl ammonium chloride, ammonium persulfate and a solvent;
in the oligomeric cationic type shrinking and swelling agent composition, relative to 100 parts by weight of the solvent, the content of the epichlorohydrin is 10-50 parts by weight, the content of the dimethylamine is 10-60 parts by weight, the content of the dodecyl dimethyl benzyl ammonium chloride is 1.6-6.4 parts by weight, and the content of the ammonium persulfate is 0.03-0.12 part by weight;
the epichlorohydrin has a structure shown in a formula (1), and the dimethylamine has a structure shown in a formula (2).
2. The composition according to claim 1, wherein in the oligomeric cationic swelling agent composition, the content of epichlorohydrin is 10 to 40 parts by weight, the content of dimethylamine is 15 to 60 parts by weight, the content of dodecyldimethylbenzylammonium chloride is 3.2 to 6.4 parts by weight, and the content of ammonium persulfate is 0.06 to 0.12 parts by weight, relative to 100 parts by weight of the solvent.
3. The composition of claim 1 or 2, wherein the dimethylamine is an aqueous dimethylamine solution having a concentration of 35-45 wt%.
4. The composition of claim 1 or 2, wherein the solvent is selected from at least one of water, ethanol, propylene glycol.
5. A method of making an oligomeric cationic swelling agent, comprising: mixing the components of the composition of any one of claims 1-4.
6. The method of claim 5, wherein mixing the components of the oligomeric cationic heave agent composition comprises the steps of:
(1) In the presence of a first part of solvent, mixing dimethylamine and epichlorohydrin for the first time to obtain a first mixed solution; and
carrying out first contact on dodecyl dimethyl benzyl ammonium chloride and a second part of solvent to dissolve to obtain a solution I;
(2) Carrying out second mixing on the first mixed solution and the solution I to obtain a second mixed solution; and
carrying out second contact on ammonium persulfate and a third part of solvent to dissolve to obtain a solution II;
(3) Carrying out contact reaction on the second mixed solution and the solution II;
the weight ratio of the first part of solvent to the second part of solvent to the third part of solvent is 1-3.
7. The process of claim 6, wherein the conditions for first mixing dimethylamine and epichlorohydrin, and for second mixing the first mixed solution with solution I, each independently, comprise: stirring speed is 50-60rpm, temperature is 20-30 deg.C, and time is 5-10min.
8. The process according to claim 6 or 7, wherein in step (3), the conditions of the contact reaction comprise at least: the temperature is 80-85 ℃ and the time is 4-6h.
9. An oligomeric cationic swelling agent prepared by the method of any one of claims 5 to 8.
10. Use of the oligomeric cationic swelling agent of claim 9 in oil and gas development.
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| US4158521A (en) * | 1978-06-26 | 1979-06-19 | The Western Company Of North America | Method of stabilizing clay formations |
| CN102703045A (en) * | 2012-06-18 | 2012-10-03 | 长江大学 | Multi-slug composite pressure decreasing and injection increasing agent for ultra-low permeability oil field |
| CN104418984A (en) * | 2013-09-04 | 2015-03-18 | 中国石油化工股份有限公司 | High-temperature resistant clay stabilizer and preparation method thereof |
| CN106608949A (en) * | 2015-10-26 | 2017-05-03 | 中国石油化工股份有限公司 | Clay stabilizer and preparation method thereof |
| CN109439292A (en) * | 2018-10-22 | 2019-03-08 | 新疆水处理工程技术研究中心有限公司 | Clay stabilizer |
| CN113150765A (en) * | 2021-04-25 | 2021-07-23 | 陕西科技大学 | Expansion shrinkage agent for acidizing and fracturing and preparation method thereof |
-
2022
- 2022-07-18 CN CN202210840548.1A patent/CN114989799B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4158521A (en) * | 1978-06-26 | 1979-06-19 | The Western Company Of North America | Method of stabilizing clay formations |
| CN102703045A (en) * | 2012-06-18 | 2012-10-03 | 长江大学 | Multi-slug composite pressure decreasing and injection increasing agent for ultra-low permeability oil field |
| CN104418984A (en) * | 2013-09-04 | 2015-03-18 | 中国石油化工股份有限公司 | High-temperature resistant clay stabilizer and preparation method thereof |
| CN106608949A (en) * | 2015-10-26 | 2017-05-03 | 中国石油化工股份有限公司 | Clay stabilizer and preparation method thereof |
| CN109439292A (en) * | 2018-10-22 | 2019-03-08 | 新疆水处理工程技术研究中心有限公司 | Clay stabilizer |
| CN113150765A (en) * | 2021-04-25 | 2021-07-23 | 陕西科技大学 | Expansion shrinkage agent for acidizing and fracturing and preparation method thereof |
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