CN114315937B - Biomass nanometer permeability enhancer for pressure flooding and fracturing and preparation method and application thereof - Google Patents
Biomass nanometer permeability enhancer for pressure flooding and fracturing and preparation method and application thereof Download PDFInfo
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- 230000035699 permeability Effects 0.000 title claims abstract description 72
- 239000003623 enhancer Substances 0.000 title claims abstract description 55
- 239000002028 Biomass Substances 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- XHXFXVLFKHQFAL-UHFFFAOYSA-N phosphoryl trichloride Chemical compound ClP(Cl)(Cl)=O XHXFXVLFKHQFAL-UHFFFAOYSA-N 0.000 claims abstract description 42
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims abstract description 36
- 238000006243 chemical reaction Methods 0.000 claims abstract description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims abstract description 20
- 229930006000 Sucrose Natural products 0.000 claims abstract description 20
- 239000005720 sucrose Substances 0.000 claims abstract description 20
- 239000002253 acid Substances 0.000 claims abstract description 14
- 239000011230 binding agent Substances 0.000 claims abstract description 14
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical group CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 27
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 24
- 239000011259 mixed solution Substances 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 13
- 230000035484 reaction time Effects 0.000 claims description 9
- 238000004440 column chromatography Methods 0.000 claims description 8
- 239000000243 solution Substances 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 4
- 239000013043 chemical agent Substances 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 239000003961 penetration enhancing agent Substances 0.000 claims description 2
- 238000000746 purification Methods 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims description 2
- 239000012295 chemical reaction liquid Substances 0.000 abstract description 11
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 abstract description 10
- 238000009736 wetting Methods 0.000 abstract description 9
- 230000002708 enhancing effect Effects 0.000 abstract description 6
- 229910000147 aluminium phosphate Inorganic materials 0.000 abstract description 5
- 239000007864 aqueous solution Substances 0.000 abstract description 3
- 239000012466 permeate Substances 0.000 abstract description 2
- 239000003921 oil Substances 0.000 description 10
- 239000000047 product Substances 0.000 description 7
- 239000012467 final product Substances 0.000 description 6
- 239000002904 solvent Substances 0.000 description 6
- 238000001291 vacuum drying Methods 0.000 description 5
- 239000012530 fluid Substances 0.000 description 4
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- 230000003000 nontoxic effect Effects 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
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- 239000010779 crude oil Substances 0.000 description 1
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Abstract
The invention discloses a biomass nano permeability enhancer for pressure flooding and fracturing, and a preparation method and application thereof, belongs to the technical field of exploitation of pressure flooding and fracturing oil gas resources, and solves the technical problems that the permeability enhancer in the field of exploitation pressure flooding and fracturing of most of the existing oil gas resources has weak permeability enhancing capability, serious pollution and the like. During preparation, sucrose is dissolved in water, ethyl acetate and an acid binding agent are added, phosphorus oxychloride is slowly added dropwise under the low-temperature condition, the temperature is controlled to continue to react for a period of time after the dropwise addition is finished, and the reaction liquid is concentrated, purified and separated and dried in vacuum after the reaction is finished to obtain the biomass nano permeability enhancer for pressure flooding and fracturing. The biomass nano permeability enhancer can decompose phosphoric acid and sucrose at high temperature, can fully permeate into stratum environment, and can prepare a water wetting environment which is used for reducing resistance for the advancing of aqueous solution in stratum micropore environment, and has good temperature resistance and high permeability enhancing rate, and the biomass nano permeability enhancer is free from biotoxicity and biodegradable.
Description
Technical Field
The invention belongs to the technical field of exploitation of oil gas resources by pressure flooding and fracturing, and particularly relates to a biomass nano permeability enhancer for pressure flooding and fracturing, and a preparation method and application thereof.
Background
The development of unconventional oil and gas has made a major breakthrough in the last decade, with the most representative technologies being a combination of hydraulic fracturing and horizontal drilling technologies. Nevertheless, the amount of crude oil that can be produced by the current depletion mode of natural energy is still low, and there is still a large amount of residual oil available for production in tight reservoirs. But the unconventional oil gas has low overall resource grade, compact reservoir, more complex geological structure and low pore and low permeability, and the characteristics greatly influence the exploitation efficiency of oil gas resources.
The primary flow path of unconventional low permeability reservoirs is fractures, and therefore, produced (or injected) fluids flow mostly through hydraulically fractured fractures, and production of hydrocarbons is also mostly limited to low permeability reservoirs near the fracture network. In recent years, various chemical components such as a surfactant are often added in the fracturing process, a synthesized nano permeability enhancer is added into a fracturing fluid pre-fluid, the fracturing fluid is utilized to fracture a stratum into a plurality of cracks, and the nano permeability enhancer enters larger crack pores of the stratum under the residual fracturing pressure. However, most of the current permeability enhancers in the field of exploitation and pressure flooding and fracturing applying oil and gas resources have the problems of weak permeability enhancement capability, serious pollution and the like.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a biomass nano permeability enhancer for fracturing and flooding, and a preparation method and application thereof, which are used for solving the technical problems of weak permeability enhancing capability, serious pollution and the like of the permeability enhancers in the field of exploitation, fracturing and flooding of most of oil and gas resources at present.
In order to achieve the above purpose, the invention is realized by adopting the following technical scheme:
The invention discloses a biomass nano permeability enhancer for pressure flooding and fracturing, which has the following structural formula:
。
the invention also discloses a preparation method of the biomass nano permeability enhancer for pressure flooding and fracturing, which comprises the following steps:
Dissolving sucrose in water, adding ethyl acetate and an acid binding agent to form a mixed solution, dropwise adding phosphorus oxychloride into the mixed solution to react, controlling the temperature to continue the reaction after the dropwise adding is finished, obtaining a reaction solution after the reaction is finished, concentrating the reaction solution, purifying and separating, and drying in vacuum to obtain the biomass nano permeability enhancer for pressure flooding and fracturing.
Further, the reaction time of dropwise adding phosphorus oxychloride into the mixed solution for reaction is 0.5-1 h.
Further, after the dripping is completed, the temperature is controlled to be 25-35 ℃, and the reaction time for continuous reaction is 4-6 hours.
Further, the purification and separation method is toluene column chromatography.
Further, the mol ratio of the sucrose to the phosphorus oxychloride to the water is 1 (4-4.3): 10-15.
Further, the mol ratio of the phosphorus oxychloride to the acid binding agent is 1 (2-3); the acid binding agent is triethylamine.
Further, the adding amount of the ethyl acetate is 3-8 times of the total mass of the sucrose, the phosphorus oxychloride and the water.
The invention also discloses application of the biomass nano permeability enhancer for fracturing, which is used as a chemical agent in the process of fracturing or fracturing of oil and gas resource exploitation.
Compared with the prior art, the invention has the following beneficial effects:
the invention discloses a biomass nano permeability enhancer for pressure flooding and fracturing, which is synthesized by taking sucrose and phosphorus oxychloride as main raw materials. According to the related experimental result table, the biomass nano permeability enhancer for pressure flooding and fracturing disclosed by the invention can decompose phosphoric acid at high temperature, and erode cracks so as to further increase permeability; meanwhile, sucrose can be decomposed and fully permeated into stratum environment, and the manufactured water wetting environment is that the water solution advances in stratum micropore environment to reduce resistance; the biomass nano permeability enhancer for pressure flooding and fracturing has good temperature resistance, is non-biotoxic, biodegradable, environment-friendly, has high permeability enhancing capability, and is excellent in function.
The invention also discloses a preparation method of the biomass nano permeability enhancer for the pressure flooding and fracturing, which is simple to operate, only needs simple mixing reaction, does not need extra large-scale instruments, is nontoxic and harmless, is environment-friendly, has good economic benefit, can be produced in a large scale, and has wide application prospect.
The invention also discloses application of the biomass nano permeability enhancer for pressure flooding and fracturing as a chemical agent in the pressure flooding or fracturing process of oil and gas resource exploitation, and the biomass nano permeability enhancer for pressure flooding and fracturing can decompose phosphoric acid and sucrose at high temperature, so that the biomass nano permeability enhancer has high permeability enhancing capability and high permeability absorbing capability, and the manufactured water wetting environment is good in temperature resistance and nontoxic and non-radioactive, can effectively solve the technical problems of weak permeability enhancing capability, serious pollution and the like of the permeability enhancer in the existing oil and gas resource exploitation pressure flooding and fracturing field, and has wide application prospect.
Drawings
Fig. 1 is a diagram of synthesis and application mechanism of a biomass nano permeability enhancer for pressure flooding and fracturing disclosed by the invention.
Detailed Description
So that those skilled in the art can appreciate the features and effects of the present invention, a general description and definition of the terms and expressions set forth in the specification and claims follows. Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs, and in the event of a conflict, the present specification shall control.
The theory or mechanism described and disclosed herein, whether right or wrong, is not meant to limit the scope of the invention in any way, i.e., the present disclosure may be practiced without limitation to any particular theory or mechanism.
All features such as values, amounts, and concentrations that are defined herein in the numerical or percent ranges are for brevity and convenience only. Accordingly, the description of a numerical range or percentage range should be considered to cover and specifically disclose all possible sub-ranges and individual values (including integers and fractions) within the range.
Herein, unless otherwise indicated, the terms "comprising," including, "" containing, "" having, "or the like are intended to cover the meanings of" consisting of … … "and" consisting essentially of … …, "e.g.," a includes a "is intended to cover" a includes a and the other "and" a includes a only.
In this context, not all possible combinations of the individual technical features in the individual embodiments or examples are described in order to simplify the description. Accordingly, as long as there is no contradiction between the combinations of these technical features, any combination of the technical features in the respective embodiments or examples is possible, and all possible combinations should be considered as being within the scope of the present specification.
The application will be further illustrated with reference to specific examples. It is to be understood that these examples are illustrative of the present application and are not intended to limit the scope of the present application. Furthermore, it should be understood that various changes and modifications can be made by one skilled in the art after reading the teachings of the present application, and such equivalents are intended to fall within the scope of the application as defined in the appended claims.
The following examples use instrumentation conventional in the art. The experimental methods, in which specific conditions are not noted in the following examples, are generally conducted under conventional conditions or under conditions recommended by the manufacturer. The following examples used various starting materials, unless otherwise indicated, were conventional commercial products, the specifications of which are conventional in the art. In the description of the present invention and the following examples, "%" means weight percent, and "parts" means parts by weight, and ratios means weight ratio, unless otherwise specified.
The invention discloses a biomass nano permeability enhancer for pressure flooding and fracturing, and a preparation method and application thereof, wherein the biomass nano permeability enhancer for pressure flooding and fracturing has the following structural formula:
Fig. 1 shows a diagram of synthesis and application mechanism of a biomass nano permeability enhancer for pressure flooding and fracturing, which is disclosed by the invention, wherein during preparation, a certain amount of sucrose is dissolved in water, then ethyl acetate and triethylamine serving as acid binding agents are added, phosphorus oxychloride is slowly added dropwise under an ice bath condition, and the control time is 0.5-1 h. And after the dripping is finished, controlling the reaction temperature to be 25-35 ℃ and reacting for 4-6 hours. Wherein the mol ratio of sucrose, phosphorus oxychloride and water is 1 (4-4.3): (10-15), the mol ratio of phosphorus oxychloride and triethylamine serving as an acid binding agent is 1 (2-3), and the addition amount of ethyl acetate serving as a solvent is 3-8 times of the total mass of sucrose, phosphorus oxychloride and water. After the reaction is finished, concentrating the reaction solution, purifying and separating out a product by using a toluene column chromatography, and drying in vacuum until the weight is constant to obtain a final product, namely the biomass nano permeability enhancer for pressure flooding and fracturing.
The biomass nano permeability enhancer for pressure flooding and fracturing can decompose phosphoric acid at high temperature, and erode cracks so as to further increase permeability; the decomposed sucrose can fully permeate into stratum environment, so that the water wetting environment is produced, the resistance is reduced for the aqueous solution to advance in stratum micropore environment, the water wetting environment has good temperature resistance, and the water wetting environment is non-biotoxic and biodegradable, so that the water wetting environment is environment-friendly, and is a biomass nano permeation enhancer for pressure flooding and fracturing with excellent functions.
The specific decomposition reaction equation is:
Example 1
The preparation method of the biomass nano permeability enhancer for the pressure flooding and fracturing comprises the following steps:
17.1g of sucrose is dissolved in 10.8g of water, 296.5g of solvent ethyl acetate and 45.6g of acid-binding agent triethylamine are added to form a mixed solution, 31.4g of phosphorus oxychloride is slowly added dropwise into the mixed solution under ice bath condition for reaction, and the reaction time is controlled to be 1h. And (3) controlling the reaction temperature to 25 ℃ after the dripping is finished, continuing to react for 6 hours, obtaining a reaction liquid after the reaction is finished, concentrating the reaction liquid, purifying and separating a product by using a toluene column chromatography, and vacuum drying to constant weight to obtain a final product, namely the biomass nano permeability enhancer for pressure flooding and fracturing.
Example 2
The preparation method of the biomass nano permeability enhancer for the pressure flooding and fracturing comprises the following steps:
20.5g of sucrose is dissolved in 15.1g of water, then 300.0g of solvent ethyl acetate and 54.7g of acid-binding agent triethylamine are added to form a mixed solution, 37.7g of phosphorus oxychloride is slowly added dropwise into the mixed solution under the ice bath condition for reaction, and the reaction time is controlled to be 0.8h. And (3) controlling the reaction temperature to be 30 ℃ after the dripping is finished, continuing to react for 6 hours, obtaining a reaction liquid after the reaction is finished, concentrating the reaction liquid, purifying and separating a product by using a toluene column chromatography, and vacuum drying to constant weight to obtain a final product, namely the biomass nano permeability enhancer for pressure flooding and fracturing.
Example 3
The preparation method of the biomass nano permeability enhancer for the pressure flooding and fracturing comprises the following steps:
13.7g of sucrose is dissolved in 10.0g of water, then 320.0g of solvent ethyl acetate and 36.5g of acid-binding agent triethylamine are added to form a mixed solution, 25.1g of phosphorus oxychloride is slowly added dropwise into the mixed solution under the ice bath condition for reaction, and the reaction time is controlled to be 0.5h. And (3) controlling the reaction temperature to 35 ℃ after the dripping is finished, continuing to react for 4 hours, obtaining a reaction liquid after the reaction is finished, concentrating the reaction liquid, purifying and separating a product by using a toluene column chromatography, and vacuum drying to constant weight to obtain a final product, namely the biomass nano permeability enhancer for pressure flooding and fracturing.
Example 4
The preparation method of the biomass nano permeability enhancer for the pressure flooding and fracturing comprises the following steps:
18.8g of sucrose is dissolved in 13.8g of water, then 204.0g of solvent ethyl acetate and 58.3g of acid-binding agent triethylamine are added to form a mixed solution, 35.3g of phosphorus oxychloride is slowly added dropwise into the mixed solution under the ice bath condition for reaction, and the reaction time is controlled to be 1h. And (3) controlling the reaction temperature to be 30 ℃ after the dripping is finished, continuing to react for 5 hours, obtaining a reaction liquid after the reaction is finished, concentrating the reaction liquid, purifying and separating a product by using a toluene column chromatography, and vacuum drying to constant weight to obtain a final product, namely the biomass nano permeability enhancer for pressure flooding and fracturing.
Example 5
The preparation method of the biomass nano permeability enhancer for the pressure flooding and fracturing comprises the following steps:
23.9g of sucrose is dissolved in 17.6g of water, 341.6g of solvent ethyl acetate and 72.5g of acid-binding agent triethylamine are added to form a mixed solution, 43.9g of phosphorus oxychloride is slowly added dropwise into the mixed solution under the ice bath condition for reaction, and the reaction time is controlled to be 0.8h. And (3) controlling the reaction temperature to 25 ℃ after the dripping is finished, continuing to react for 6 hours, obtaining a reaction liquid after the reaction is finished, concentrating the reaction liquid, purifying and separating a product by using a toluene column chromatography, and vacuum drying to constant weight to obtain a final product, namely the biomass nano permeability enhancer for pressure flooding and fracturing.
In order to characterize each performance of the biomass nano permeability enhancer for pressure flooding and fracturing, the interfacial tension, wettability, self-priming capability and core permeability of the biomass nano permeability enhancer for pressure flooding and fracturing synthesized in examples 1-5 are tested, and the results are shown in table 1. As shown in Table 1, the biomass nano permeability enhancer for pressure flooding and fracturing has lower interfacial tension, can play a wetting role, and has obvious capillary self-absorption capacity in 0.3% aqueous solution. When the core is soaked at 80 ℃, the permeability of the core is obviously increased, because the biomass nano permeability enhancer can decompose phosphoric acid at high temperature, and cracks are eroded, so that the permeability is further increased. The comprehensive evaluation is a biomass nano permeability enhancer with excellent functions for pressure flooding and fracturing.
Wherein the test reference criteria are:
Interfacial tension reference GB/T38022-2020 surfactant interfacial tension measurement (pull-up liquid film method);
Wettability test reference GB/T11983-2008 method for determining the wetting force of surfactants (immersion method);
Self-priming capability referring to part 3 of the JB/T6664.3-2004 self-priming pump, namely self-priming performance test method;
core permeability reference SY/T5802-1993 tight rock permeability assay (steady state method).
TABLE 1 Performance of Biomass nanopenetration enhancers for pressure flooding and fracturing
The above is only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited by this, and any modification made on the basis of the technical scheme according to the technical idea of the present invention falls within the protection scope of the claims of the present invention.
Claims (7)
1. The biomass nano permeability enhancer for the pressure flooding and the fracturing is characterized by comprising the following structural formula:
。
2. The method for preparing the biomass nano permeability enhancer for pressure flooding and fracturing, which is disclosed in claim 1, is characterized by comprising the following steps:
Dissolving sucrose in water, adding ethyl acetate and an acid binding agent to form a mixed solution, dropwise adding phosphorus oxychloride into the mixed solution to react, controlling the temperature to continue the reaction after the dropwise adding is finished, obtaining a reaction solution after the reaction is finished, concentrating the reaction solution, purifying and separating, and drying in vacuum to obtain the biomass nano permeation enhancer for pressure flooding and fracturing;
The mol ratio of the sucrose to the phosphorus oxychloride to the water is 1 (4-4.3) (10-15);
the mol ratio of the phosphorus oxychloride to the acid binding agent is 1 (2-3); the acid binding agent is triethylamine.
3. The method for preparing the biomass nano permeability enhancer for pressure flooding and fracturing according to claim 2, wherein the reaction time of dropwise adding phosphorus oxychloride into the mixed solution for reaction is 0.5-1 h.
4. The method for preparing the biomass nano permeability enhancer for pressure flooding and fracturing according to claim 2, wherein the temperature is controlled to be 25-35 ℃ after the completion of the dropwise addition, and the reaction time for continuous reaction is 4-6 h.
5. The method for preparing the biomass nano permeability enhancer for pressure flooding and fracturing according to claim 2, wherein the purification and separation method is toluene column chromatography.
6. The preparation method of the biomass nano permeability enhancer for pressure flooding and fracturing, which is disclosed in claim 2, is characterized in that the adding amount of ethyl acetate is 3-8 times of the total amount of sucrose, phosphorus oxychloride and water.
7. The application of the biomass nano permeability enhancer for fracturing, flooding and fracturing of claim 1, wherein the biomass nano permeability enhancer for fracturing, flooding and fracturing is used as a chemical agent in the process of fracturing, flooding or fracturing of oil and gas resource exploitation.
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| CN105860948A (en) * | 2015-05-25 | 2016-08-17 | 成都能生材科技开发有限责任公司 | Preparation method of polymer viscosity-reducing profile-control resistance-reducing physical dissolution agent PSR |
| CN111022011A (en) * | 2019-12-03 | 2020-04-17 | 中国石油化工股份有限公司 | Construction method of foamable resin sand consolidation agent for argillaceous fine silt oil reservoir |
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| WO2012045009A2 (en) * | 2010-09-30 | 2012-04-05 | Normoxys, Inc. | Polyphosphate and pyrophosphate derivative of saccharides |
| JP6004594B2 (en) * | 2011-11-15 | 2016-10-12 | ジ ウォルター アンド エリザ ホール インスティテュート オブ メディカル リサーチ | Soluble mediator |
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| CN105860948A (en) * | 2015-05-25 | 2016-08-17 | 成都能生材科技开发有限责任公司 | Preparation method of polymer viscosity-reducing profile-control resistance-reducing physical dissolution agent PSR |
| CN111022011A (en) * | 2019-12-03 | 2020-04-17 | 中国石油化工股份有限公司 | Construction method of foamable resin sand consolidation agent for argillaceous fine silt oil reservoir |
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