CN112111263B - Preparation method of high-temperature-resistant clean fracturing fluid - Google Patents
Preparation method of high-temperature-resistant clean fracturing fluid Download PDFInfo
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- C09K8/62—Compositions for forming crevices or fractures
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- C07C303/32—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of salts of sulfonic acids
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- C07C309/02—Sulfonic acids having sulfo groups bound to acyclic carbon atoms
- C07C309/03—Sulfonic acids having sulfo groups bound to acyclic carbon atoms of an acyclic saturated carbon skeleton
- C07C309/13—Sulfonic acids having sulfo groups bound to acyclic carbon atoms of an acyclic saturated carbon skeleton containing nitrogen atoms, not being part of nitro or nitroso groups, bound to the carbon skeleton
- C07C309/14—Sulfonic acids having sulfo groups bound to acyclic carbon atoms of an acyclic saturated carbon skeleton containing nitrogen atoms, not being part of nitro or nitroso groups, bound to the carbon skeleton containing amino groups bound to the carbon skeleton
- C07C309/15—Sulfonic acids having sulfo groups bound to acyclic carbon atoms of an acyclic saturated carbon skeleton containing nitrogen atoms, not being part of nitro or nitroso groups, bound to the carbon skeleton containing amino groups bound to the carbon skeleton the nitrogen atom of at least one of the amino groups being part of any of the groups, X being a hetero atom, Y being any atom
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- C07D295/16—Heterocyclic compounds containing polymethylene-imine rings with at least five ring members, 3-azabicyclo [3.2.2] nonane, piperazine, morpholine or thiomorpholine rings, having only hydrogen atoms directly attached to the ring carbon atoms acylated on ring nitrogen atoms
- C07D295/18—Heterocyclic compounds containing polymethylene-imine rings with at least five ring members, 3-azabicyclo [3.2.2] nonane, piperazine, morpholine or thiomorpholine rings, having only hydrogen atoms directly attached to the ring carbon atoms acylated on ring nitrogen atoms by radicals derived from carboxylic acids, or sulfur or nitrogen analogues thereof
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- C09K8/60—Compositions for stimulating production by acting on the underground formation
- C09K8/62—Compositions for forming crevices or fractures
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- C09K8/60—Compositions for stimulating production by acting on the underground formation
- C09K8/84—Compositions based on water or polar solvents
- C09K8/86—Compositions based on water or polar solvents containing organic compounds
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- C09K2208/00—Aspects relating to compositions of drilling or well treatment fluids
- C09K2208/30—Viscoelastic surfactants [VES]
Abstract
The invention relates to a preparation method of a high-temperature-resistant clean fracturing fluid, belonging to the technical field of oilfield chemistry. Preparing an amidation product by reacting a piperazine compound having a hydroxyl group with an organic acid, and reacting the amidation product with a sulfonating agent to prepare a viscoelastic surfactant; the high temperature stabilizer is prepared by reacting trimethyl borate with a diamino compound. The clean fracturing fluid is prepared by taking a viscoelastic surfactant and a high-temperature stabilizer as raw materials, has good dissolving, tackifying, temperature resistance, salt resistance and sand carrying performances, and can be used as a working fluid for fracturing construction under high temperature and high salt.
Description
Technical Field
The invention relates to a preparation method of a high-temperature-resistant clean fracturing fluid, belonging to the technical field of oilfield chemistry.
Background
Petroleum is an important strategic resource, and the exploitation and utilization of petroleum play an important role in the development of national economy. With the increasing difficulty of oil-gas field exploitation, low-permeability and unconventional oil reservoirs are the main direction of future oil field development. The stratum condition of the low-permeability reservoir is complex, the exploitation effect is poor, the production degree is low, and the hydraulic fracturing is a yield-increasing means with higher efficiency as one of the main measures for the development of the low-permeability reservoir. The fracturing fluid plays a role in transferring pressure, generating and extending fractures and suspending a propping agent in hydraulic fracturing operation, and the performance of the fracturing fluid plays a decisive role in fracturing construction and yield increasing effect of an oil-gas well after the construction. For low-permeability oil reservoirs, the conventional guanidine gum fracturing fluid has a lot of residues, great damage to the reservoir and a lot of defects in use, so that the research and application of the novel fracturing fluid gradually become hot spots.
The clean fracturing fluid is also called as viscoelastic surfactant fracturing fluid, has the advantages of simple preparation, good viscoelasticity, no need of a cross-linking agent, automatic gel breaking when encountering oil and formation water, easy flowback, small damage to the formation and the like, and is more and more widely applied. Spherical micelles of viscoelastic surfactants grow in one dimension to form rod-like or wire-like aggregates, called worm-like micelles. The network structure of the wormlike micelles is formed by intermolecular forces such as electrostatic interaction, hydrophobic interaction, hydrogen bonding and the like of the surfactant. These networks are also known as living polymers, since they can be restored by intermolecular interactions after being destroyed by shearing.
The current clean fracturing fluid has the following defects in the field use process of the oil field: the use concentration of the surfactant is large, and the cost is high; (2) The viscosity of the system is obviously reduced along with the temperature rise, and the tackifying effect under the high-temperature resistant condition is poor; (3) The self-assembled structure of the system is easy to be damaged under high shear conditions, and the shear resistance is to be improved. Therefore, it is necessary to develop a novel viscoelastic surfactant and construct a clean fracturing fluid system with low use concentration, high temperature resistance and excellent anti-shearing performance.
Disclosure of Invention
The invention provides a preparation method of a high-temperature-resistant clean fracturing fluid.
Summary of The Invention
The preparation method comprises the steps of reacting piperazine compound containing hydroxyl with organic acid to prepare amidation product, and reacting the amidation product with a sulfonation reagent to prepare the viscoelastic surfactant; trimethyl borate reacts with diamino compound to prepare amino boron type high temperature stabilizer; the high-temperature resistant clean fracturing fluid is prepared by taking a viscoelastic surfactant and a high-temperature stabilizer as raw materials. Through tests, the fracturing fluid system has good dissolving, tackifying, temperature resisting, salt resisting and sand carrying performances, and can be used as a working fluid for fracturing construction under high temperature and high salt.
Detailed Description
The technical scheme of the invention is as follows:
(1) Preparation of viscoelastic surfactants
(1) Preparation of amidated products
Adding the compound-1, the compound-2 and sodium fluoride into a four-neck glass bottle provided with a stirrer, a nitrogen introducing pipe, a drying pipe and a thermometer, heating and stirring until all raw materials are dissolved, introducing nitrogen for 20min, controlling the reaction temperature at 120-190 ℃, reacting for 3-48 h, and distilling under reduced pressure at 180 ℃ to remove volatile components to obtain the compound-2; the mass ratio of the compound-1 to the compound-2 is 1 (0.3-1), and the mass ratio of the compound-2 to the sodium fluoride is 1 (0.003-0.02);
(2) viscoelastic surfactant preparation
Adding the amidated product, ethyl acetate and the compound-3 into a three-neck glass bottle provided with a stirrer, a spherical condenser tube and a thermometer, heating and stirring until all raw materials are dissolved, controlling the reaction temperature at 60-130 ℃, reacting for 4-24 h, cooling, filtering and drying to obtain the compound; the mass ratio of amidation product, compound-3 and ethyl acetate is 1 (0.3-2) to 1.5-10;
(2) Preparation of high temperature stabilizers
Adding trimethyl borate, compound-4 and ethanol into a three-neck glass bottle provided with a stirrer, a spherical condenser tube and a thermometer, controlling the temperature at 50-80 ℃, reacting for 1-10 h, and distilling under reduced pressure at 60 ℃ to remove volatile components to obtain the compound; the mass ratio of trimethyl borate to compound-4 to ethanol is 1 (0.2-0.7) to 1-6;
(3) Preparation of fracturing fluid system
Adding tap water, sodium chloride, calcium chloride and a viscoelastic surfactant into a beaker provided with a stirrer, heating and stirring until all the surfactant is dissolved, adding a high-temperature stabilizer aqueous solution with the mass fraction of 20%, and uniformly stirring to obtain the high-temperature stabilizer aqueous solution; the mass ratio of tap water, sodium chloride, calcium chloride and viscoelastic surfactant is 1 (0.005-0.1) to 0.0001-0.02 to 0.002-0.04), and the mass ratio of viscoelastic surfactant to high-temperature stabilizer aqueous solution is 1 (0.002-0.25).
According to the present invention, preferably, the compound-1 in the preparation of amidation product in step (1) is one of hexadecanoic acid, octadecanoic acid, eicosanoic acid, docosanoic acid, palmitoleic acid, oleic acid and erucic acid;
preferably, the compound-2 is one of 1- (2-hydroxyethyl) piperazine and 1- (4-hydroxyphenyl) piperazine;
preferably, the mass ratio of the compound-1 to the compound-2 is 1 (0.4-0.8), and the mass ratio of the compound-2 to the sodium fluoride is 1 (0.005-0.015);
preferably, the reaction temperature is controlled to be 150-190 ℃, and the reaction is carried out for 6-24 h.
According to the present invention, preferably, the compound-3 in the preparation of the viscoelastic surfactant in step (1) is one of sodium 3-chloropropanesulfonate and sodium 3-chloro-2-hydroxypropanesulfonate;
preferably, the mass ratio of the amidation product to the compound-3 to the ethyl acetate is 1 (0.45-1.2) to 2-6;
preferably, the reaction temperature is controlled to be 65-85 ℃, and the reaction is carried out for 8-15 h.
According to the present invention, preferably, the compound-4 in the step (2) is one of ethylenediamine, 1, 3-propylenediamine, 1, 4-butylenediamine, and 1, 6-hexylenediamine;
preferably, the mass ratio of the trimethyl borate to the compound-4 to the ethanol is 1 (0.2-0.55) to 1-5;
preferably, the reaction temperature is controlled to be 65-80 ℃, and the reaction is carried out for 2-6 h.
According to the present invention, it is preferable that in the step (3), the mass ratio of the tap water, the sodium chloride, the calcium chloride and the viscoelastic surfactant is 1 (0.01 to 0.05): (0.001 to 0.01): 0.004 to 0.025), and the mass ratio of the viscoelastic surfactant to the aqueous solution of the high-temperature stabilizer is 1 (0.005 to 0.15).
The invention has the following excellent effects:
1. the surfactant structure with anions and cations in the molecule is used, so that the product has good performances of dissolution, salt resistance and the like, and in addition, the anion and cation structure can also control the adsorption capacity of the product in the injection process.
2. Piperazine groups are introduced into the molecules of the surfactant, so that the rigidity of the molecules is enhanced, the molecules can form a stronger aggregate structure in a solution, the tackifying performance of the product is improved, and the using amount of the product is reduced.
3. The interaction between hydrophilic groups of the surfactant is improved through the dynamic covalent reaction between the amino boron compound and the hydroxyl, and the tackifying capability of the product at high temperature is enhanced.
4. The molecules of the surfactant do not contain easily hydrolyzed groups, and the product has excellent high-temperature aging resistance.
5. The preparation process is simple and easy to realize industrial production.
6. The product prepared by the invention has good compatibility with the conventional auxiliary agent for clean fracturing fluid and construction process.
Detailed Description
The experimental procedures used in the following examples are all conventional procedures unless otherwise specified.
Materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
The invention will be further illustrated with reference to specific examples, without however restricting its scope to these examples.
Example 1:
(1) Preparation of viscoelastic surfactants
(1) Preparation of amidated products
Adding 100g of eicosanoic acid, 60g of 1- (2-hydroxyethyl) piperazine and 0.6g of sodium fluoride into a four-neck glass bottle provided with a stirrer, a nitrogen introducing pipe, a drying pipe and a thermometer, heating and stirring until all raw materials are dissolved, introducing nitrogen for 20min, controlling the reaction temperature at 180 ℃, reacting for 12h, and distilling under reduced pressure at 180 ℃ to remove volatile components to obtain an amidated product;
(2) viscoelastic surfactant preparation
Adding 100g of amidation product, 400g of ethyl acetate and 65g of 3-chloro-2-hydroxypropanesulfonic acid sodium salt into a three-neck glass bottle provided with a stirrer, a spherical condenser tube and a thermometer, heating and stirring until all raw materials are dissolved, controlling the reaction temperature at 75 ℃, reacting for 10 hours, cooling, filtering and drying to obtain a viscoelastic surfactant product;
(2) Preparation of high temperature stabilizers
Adding 100g of trimethyl borate, 36g of 1, 4-butanediamine and 400g of ethanol into a three-neck glass bottle provided with a stirrer, a spherical condenser tube and a thermometer, controlling the temperature at 70 ℃, reacting for 3 hours, and distilling under reduced pressure at 60 ℃ to remove volatile components to obtain a high-temperature stabilizer;
(3) Preparation of fracturing fluid system
1000g of tap water, 20g of sodium chloride, 4g of calcium chloride and 10g of viscoelastic surfactant are added into a container
And (3) heating and stirring in a beaker with a stirrer, adding 0.5g of 20% high-temperature stabilizer aqueous solution after all the surfactant is dissolved, and uniformly stirring to obtain the fracturing fluid system.
Example 2:
as described in example 1, except that the amidation product of step (1) is prepared such that compound-1 is erucic acid.
Example 3:
as described in example 1, except that Compound-1 in the amidation product preparation of step (1) is hexadecanoic acid.
Example 4:
as described in example 1, except that 75g of 1- (2-hydroxyethyl) piperazine was used in the preparation of the amidation product of step (1).
Example 5:
as described in example 1, except that the amidation product of step (1) is prepared wherein compound-2 is 1- (4-hydroxyphenyl) piperazine.
Example 6:
as described in example 1, except that the reaction temperature in the preparation of the amidated product of step (1) was 165 ℃ and the time was 10 hours.
Example 7:
the procedure is as described in example 1, except that 300g of ethyl acetate is used in the preparation of the viscoelastic surfactant in step (1).
Example 8:
the procedure was as described in example 1, except that 90g of sodium 3-chloro-2-hydroxypropanesulfonate was used in the preparation of the viscoelastic surfactant in step (1).
Example 9:
the procedure is as described in example 1, except that the reaction temperature in the preparation of the viscoelastic surfactant in step (1) is 65 ℃ and the reaction time is 12 hours.
Example 10:
as described in example 1, except that 48g of 1, 4-butanediamine was used in step (2).
Example 11:
as described in example 1, except that 30g of 1, 4-butanediamine was used in step (2).
Example 12:
as described in example 1, except that the compound-4 in the step (2) was 1, 6-hexanediamine, and the amount added was 42g.
Example 13:
the procedure is as described in example 1, except that the reaction temperature in step (2) is 80 ℃ and the reaction time is 2 hours.
Example 14:
as described in example 1, except that the amount of the viscoelastic surfactant in step (3) was 6g.
Example 15:
as described in example 1, except that the amount of viscoelastic surfactant in step (3) was 15g.
Example 16:
as described in example 1, except that the 20% by mass aqueous solution of the high-temperature stabilizer in the step (3) was 0.25g.
Example 17:
as described in example 1, except that the 20% by mass aqueous solution of the high-temperature stabilizer in step (3) was 0.8g.
Example 18:
as described in example 1, except that 45g of sodium chloride was used in step (3).
Comparative example 1:
industrial products of clean fracturing fluids produced by seiania bang oil science and technology limited.
Comparative example 2:
the Shanxi Senri oil technology development company Limited produces clean fracturing fluid industrial products.
Evaluation of Properties
Comparative example 1 and comparative example 2 fracturing fluid preparation process: 1000g of tap water, 20g of sodium chloride, 4g of calcium chloride and 25g of sample are added into a beaker provided with a stirrer, and the temperature is raised and the mixture is stirred until all the components are dissolved for later use.
The tackifying performance and the sand suspending performance of examples 1 to 18 and comparative example were evaluated by the following test methods.
1. Evaluation of thickening Performance
Heating the prepared fracturing fluid in a high-temperature high-pressure rheometer at the initial temperature of 25 ℃ and the rotor shear rate of 170s at the initial temperature of 3 +/-0.2℃/min -1 . After the temperature had risen to 90 ℃, the temperature and the shear rate were kept constant for a total test time of 2h.
2. Evaluation of imbibition Properties
(1) Putting 100mL of fracturing fluid into a measuring cylinder, and heating the fracturing fluid to 90 ℃ by using constant-temperature water bath;
(2) Selecting ceramsite with the grain size of 20-40 meshes, and putting one ceramsite 2cm below the liquid level by using tweezers;
(3) And loosening the tweezers to allow the porcelain granules to naturally settle, recording the time required for the porcelain granules to uniformly settle for a certain distance (more than 20 cm), and calculating the settling velocity.
The evaluation results are shown in table 1.
TABLE 1 evaluation results of Properties
The experimental result shows that compared with an industrial clean fracturing fluid product, the clean fracturing fluid system prepared by the invention has the advantages of small using amount, excellent tackifying effect and good temperature resistance, and in addition, the system also has a good sand carrying effect at high temperature.
Claims (8)
1. A preparation method of high-temperature-resistant clean fracturing fluid comprises the following steps:
(1) Preparation of viscoelastic surfactants
(1) Preparation of amidated products
Adding the compound-1, the compound-2 and sodium fluoride into a four-neck glass bottle provided with a stirrer, a nitrogen introducing pipe, a drying pipe and a thermometer, heating and stirring until all raw materials are dissolved, introducing nitrogen for 20min, controlling the reaction temperature at 120-190 ℃, reacting for 3-48 h, and distilling under reduced pressure at 180 ℃ to remove volatile components to obtain the compound-2; the mass ratio of the compound-1 to the compound-2 is 1 (0.3-1), and the mass ratio of the compound-2 to the sodium fluoride is 1 (0.003-0.02);
(2) viscoelastic surfactant preparation
Adding the amidated product, ethyl acetate and the compound-3 into a three-neck glass bottle provided with a stirrer, a spherical condenser tube and a thermometer, heating and stirring until all raw materials are dissolved, controlling the reaction temperature at 60-130 ℃, reacting for 4-24 h, cooling, filtering and drying to obtain the compound; the mass ratio of the amidation product to the compound-3 to the ethyl acetate is 1 (0.3-2) to 1.5-10;
the compound-1 is one of hexadecanoic acid, octadecanoic acid, eicosanoic acid, docosanoic acid, palmitoleic acid, oleic acid and erucic acid;
the compound-2 is one of 1- (2-hydroxyethyl) piperazine and 1- (4-hydroxyphenyl) piperazine;
the compound-3 is one of 3-chloropropanesulfonic acid sodium salt and 3-chloro-2-hydroxypropanesulfonic acid sodium salt;
(2) Preparation of high temperature stabilizers
Adding trimethyl borate, compound-4 and ethanol into a three-neck glass bottle provided with a stirrer, a spherical condenser tube and a thermometer, controlling the temperature at 50-80 ℃, reacting for 1-10 h, and distilling under reduced pressure at 60 ℃ to remove volatile components to obtain the compound; the mass ratio of the trimethyl borate to the compound-4 to the ethanol is 1 (0.2-0.7) to 1-6;
the compound-4 is one of ethylenediamine, 1, 3-propanediamine, 1, 4-butanediamine and 1, 6-hexanediamine;
(3) Preparation of fracturing fluid system
Adding tap water, sodium chloride, calcium chloride and a viscoelastic surfactant into a beaker provided with a stirrer, heating and stirring until all the surfactant is dissolved, adding a high-temperature stabilizer aqueous solution with the mass fraction of 20%, and uniformly stirring to obtain the water-soluble calcium phosphate; the mass ratio of tap water, sodium chloride, calcium chloride and viscoelastic surfactant is 1 (0.005-0.1) to 0.0001-0.02 to 0.002-0.04), and the mass ratio of viscoelastic surfactant to high-temperature stabilizer aqueous solution is 1 (0.002-0.25).
2. The method for preparing high temperature clean-resistant fracturing fluid as claimed in claim 1, wherein the mass ratio of compound-1 to compound-2 in the preparation of amidation product in step (1) is 1 (0.4-0.8), and the mass ratio of compound-2 to sodium fluoride is 1 (0.005-0.015).
3. The method for preparing the high-temperature resistant clean fracturing fluid as claimed in claim 1, wherein the reaction temperature in the preparation of the amidation product in the step (1) is 150-190 ℃ and the reaction time is 6-24 h.
4. The method for preparing high temperature resistant clean fracturing fluid as claimed in claim 1, wherein the mass ratio of amidation product, compound-3 and ethyl acetate in the preparation of viscoelastic surfactant in step (1) is 1 (0.45-1.2) to (2-6).
5. The preparation method of the high temperature resistant clean fracturing fluid as claimed in claim 1, wherein the reaction temperature in the preparation of the viscoelastic surfactant in the step (1) is 65-85 ℃ and the reaction time is 8-15 h.
6. The method for preparing the high temperature resistant clean fracturing fluid of claim 1, wherein the mass ratio of the trimethyl borate, the compound-4 and the ethanol in the step (2) is 1 (0.2-0.55) to 1-5.
7. The preparation method of the high temperature resistant clean fracturing fluid as claimed in claim 1, wherein the reaction temperature in the step (2) is 65-80 ℃ and the reaction time is 2-6 h.
8. The method for preparing high temperature resistant clean fracturing fluid of claim 1, wherein the mass ratio of tap water, sodium chloride, calcium chloride and viscoelastic surfactant in step (3) is 1 (0.01-0.05): (0.001-0.01): 0.004-0.025), and the mass ratio of viscoelastic surfactant to high temperature stabilizer aqueous solution is 1 (0.005-0.15).
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| US7125825B2 (en) * | 2003-04-25 | 2006-10-24 | Tomah Products, Inc. | Amidoamine salt-based viscosifying agents and methods of use |
| US7981845B2 (en) * | 2008-08-29 | 2011-07-19 | Schlumberger Technology Corporation | Partially neutralized polyhydroxy acids for well treatments |
| WO2010048091A2 (en) * | 2008-10-21 | 2010-04-29 | Bj Services Company | Boron crosslinkers for fracturing fluids with appreciably lower polymer loading and related methods and compositions |
| CN110776897B (en) * | 2019-11-20 | 2021-09-14 | 中国海洋石油集团有限公司 | Surfactant for low-permeability reservoir development and preparation method thereof |
| CN111205846A (en) * | 2020-01-17 | 2020-05-29 | 中国石油大学(华东) | Preparation method of viscoelastic surfactant for low-permeability reservoir development |
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| CN105080424A (en) * | 2015-09-02 | 2015-11-25 | 西南石油大学 | Cationic viscoelastic surfactant and preparation and application thereof |
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