CN110343220B - Retarding additive, preparation method thereof and retarding acid - Google Patents

Retarding additive, preparation method thereof and retarding acid Download PDF

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CN110343220B
CN110343220B CN201910682446.XA CN201910682446A CN110343220B CN 110343220 B CN110343220 B CN 110343220B CN 201910682446 A CN201910682446 A CN 201910682446A CN 110343220 B CN110343220 B CN 110343220B
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retarding
admixture
acid
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monomer
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CN110343220A (en
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全红平
陈中豪
黄志宇
吴洋
段文猛
王金玉
戴姗姗
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Southwest Petroleum University
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
    • C08F283/06—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
    • C08F283/065—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals on to unsaturated polyethers, polyoxymethylenes or polyacetals
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • 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
    • C09K8/60—Compositions for stimulating production by acting on the underground formation
    • C09K8/62—Compositions for forming crevices or fractures
    • C09K8/72—Eroding chemicals, e.g. acids
    • C09K8/74—Eroding chemicals, e.g. acids combined with additives added for specific purposes
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • 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
    • 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
    • C09K8/88—Compositions based on water or polar solvents containing organic compounds macromolecular compounds
    • C09K8/882—Compositions based on water or polar solvents containing organic compounds macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds

Abstract

The invention discloses a retarding admixture, a preparation method thereof and a retarding acid, wherein the retarding admixture is obtained by polymerizing monomers; the monomer consists of octadecyl methacrylate, allyl polyoxyethylene ether and acrylamide; the retarding admixture has good retarding effect in sandstone and carbonate rock, can be used for deep acidizing, has low viscosity, is favorable for flowback, has good thermal stability and strong temperature resistance, has good compatibility with other acidizing working additives, and does not have the phenomenon of precipitation and delamination.

Description

Retarding additive, preparation method thereof and retarding acid
Technical Field
The invention relates to the technical field of petrochemical industry, in particular to a retarding additive, a preparation method thereof and retarding acid.
Background
Acidification is one of the important stimulation measures for hydrocarbon reservoirs. It is a production-increasing measure for removing the pollution near the bottom of production well and injection well by using acid liquor, recovering the permeability of stratum or corroding the rock cement of stratum to raise the permeability of stratum. The method aims to relieve the damage to the stratum nearby a well hole in the processes of drilling, well completion, well workover, augmented injection and the like by using acid, and dredge a fluid seepage channel, thereby recovering and improving the productivity of the oil-gas well.
In the acidification construction, the conventional acid liquid used, such as hydrochloric acid and earth acid, acidifies limestone and sandstone strata, because the reaction speed of acid and rock is high, the action distance of acid is short, the blockage of the near-well stratum can only be eliminated, the aim of dredging deep stratum channels to increase the yield can not be achieved, even the near-well zone is over-acidified easily, karst cave or sand production is caused, the stratum permeability is damaged, and the yield increasing effect of an oil well and the water well increasing injection effect are seriously influenced. Therefore, formation deep acidizing must be performed using retarded acids to improve the acidizing effect. The retarding acid mainly comprises gelling acid, emulsifying acid, active acid, foaming acid and the like.
Gelled acids, also known as viscosifying acids, refer to acids that have been increased in viscosity by the addition of additives such as viscosifying agents. The gelled acid is a high-molecular acid liquid, and the gelling agent mainly comprises celluloses, acrylamides, biopolymers and the like. Its advantage is high effect to prevent H + Thereby reducing the reaction rate of the acid rock; but has the defects of high viscosity, difficult injection into stratum, sensitive shearing property, difficult gel breaking in residual acid, easy secondary damage to reservoir stratum and the like.
The emulsifying acid is an oil-in-acid type emulsion prepared by mixing oil and acid according to a certain proportion under the action of an emulsifier and a co-emulsifier, and the emulsion with the oil as an external phase is generally used. After the emulsified acid enters the stratum, the oil phase separates the acid liquid from the rock, and therefore the reaction of the acid liquid and the rock is delayed. The emulsified acid mainly takes oil as an external phase, an oil film is formed on the surface of a rock through the emulsion, and the acid liquid cannot directly contact with the rock wall and can react only by penetrating through an oil film interface to achieve the effect of retarding. The emulsified acid has small filtration loss and high viscosity, is suitable for fracture acidizing and can form long and wide cracks. However, the emulsified acid has the disadvantages of high construction friction resistance, high construction pressure, low discharge capacity and high cost.
The active acid is also called chemical retarded acid, which means that a surfactant is added into the acid liquor, and the action mechanism of the active acid is that the surfactant is adsorbed on the wall surface of a stratum fracture, so that the effect of delaying the reaction speed of acid rock is achieved. The active acid has the defect of poor control of filtration loss, so the active acid is mainly suitable for low-temperature dolomite formations with acid rock reaction speed controlled by the surface, and can be used for medium-temperature dolomite reservoirs by combining with a multi-stage alternative injection technology.
The foam acid is air, N 2 Or CO 2 By waiting for the aeration or gasification of a foaming system for the formation of acidAnd (4) a layered acidification process. The foam acid is composed of acid liquor, gas, foaming agent, foam stabilizer, water-soluble polymer and the like. The foam acid has the advantages of low liquid content, high apparent viscosity, small filtration loss, capability of effectively slowing down the reaction rate of acid rock, quick flowback and the like, but the stability of the foam acid is reduced under the condition of high temperature, the filtration loss of the acid liquor is increased, and the acid retarding effect is influenced.
Disclosure of Invention
In view of the above, the application provides a retarding admixture, a preparation method thereof and a retarding acid, which have high purity; the retarding admixture has good retarding effect in sandstone and carbonate rock, can be used for deep acidizing, has low viscosity, is favorable for flowback, has good thermal stability and strong temperature resistance, has good compatibility with other acidizing working additives, and cannot generate precipitation and delamination.
In order to solve the technical problems, the technical scheme provided by the application is that the retarding additive is obtained by polymerizing monomers; the monomer consists of octadecyl methacrylate, allyl polyoxyethylene ether and acrylamide.
Preferably, the retarding admixture is obtained by emulsion polymerization of the monomer.
Preferably, the monomer consists of 0.3-0.5% of octadecyl methacrylate, 0.9-1.0% of allyl polyoxyethylene ether and 98.5-98.8% of acrylamide in molar percentage.
Preferably, the retarding admixture is a compound represented by the formula (I):
Figure BDA0002145243580000031
wherein x is 98.5-98.8%, y is 0.9-1.0%, w is 0.3-0.5%, and n is 20-25%.
The invention also provides a preparation method of the retarding admixture, which comprises the following steps: carrying out polymerization reaction on the monomer under the action of an initiator to obtain the retarding additive; the monomer consists of octadecyl methacrylate, allyl polyoxyethylene ether and acrylamide.
Preferably, the monomer consists of 0.3-0.5% of octadecyl methacrylate, 0.9-1.0% of allyl polyoxyethylene ether and 98.5-98.8% of acrylamide in molar percentage.
Preferably, the preparation method specifically comprises the following steps: carrying out emulsion polymerization reaction on the monomer under the action of an initiator and an emulsifier to obtain the retarding admixture; the monomer consists of octadecyl methacrylate, allyl polyoxyethylene ether and acrylamide.
Preferably, the emulsifier is polyoxyethylene octyl phenol ether-10.
Preferably, the preparation method specifically comprises the following steps: mixing a monomer, an emulsifier, an initiator and water, and carrying out emulsion polymerization reaction to obtain the slow admixture; the dosage of the emulsifier is 6.0-8.0 wt% of the total mass of water.
Preferably, the initiator accounts for 0.2-0.3 wt% of the total mass of the monomers.
Preferably, the initiator azobisisobutyramidine hydrochloride.
Preferably, the emulsion polymerization reaction temperature is 50-55 ℃, and the reaction time is 6-7 h.
Preferably, the preparation method specifically comprises the following steps: mixing a monomer, an emulsifier, an initiator and water, carrying out emulsion polymerization reaction to obtain a gel transparent product, washing the gel transparent product for 3-5 times by using absolute ethyl alcohol until precipitation occurs, and drying the gel transparent product in an oven at the temperature of 50 ℃ for 24 hours to obtain the slow admixture.
The invention also provides a retarding acid which comprises the retarding additive or the retarding additive prepared by the preparation method.
Compared with the prior art, the detailed description of the application is as follows:
the invention provides a retarding admixture, a preparation method thereof and a retarding acid, wherein the retarding admixture is obtained by polymerizing monomers; the monomer consists of octadecyl methacrylate, allyl polyoxyethylene ether and acrylamide. Compared with the prior art, the retarding additive is a low-viscosity adsorption type acid liquor retarding additive, has low viscosity, good fluidity in acid liquor, easy injection and no obvious tackifying phenomenon, has the advantages of easy flowback and reduction of secondary damage to a reservoir, and is beneficial to acidification treatment of low-permeability and ultra-low-permeability reservoirs. The retarded acid added with the retarding admixture has good retarding effect in sandstone and carbonate rock, can be used for deep acidizing treatment, has moderate viscosity of an acid liquid system, and is beneficial to flowback. The slow admixture can hydrolyze and desorb from the surface of rock at the later stage, and has small secondary damage. The retarding admixture has good thermal stability, strong temperature resistance, good compatibility with other acidification working additives and no precipitation and delamination.
The retarding admixture has the advantages that the molecular weight of the polymer is effectively controlled by the appropriate initiator addition amount, and the good acid liquor retarding performance and low viscosity capability are met; adding emulsifier to carry out emulsion polymerization reaction, and the reaction is complete and the product purity is high. The retarding admixture adopts proper monomer proportion, so that precipitation is prevented; the polyoxyethylene ether long-chain branch in the allyl polyoxyethylene ether monomer structure has the functions of volume repulsion and electrostatic repulsion, and can increase the rigidity of the main chain, so that the main chain is not easy to curl or tangle and extends in conformation in a solution; the octadecyl methacrylate provides a hydrophobic chain for the polymerization product, and plays a role of a hydrophobic barrier; the acrylamide has good polymerizability, wide sources and low cost.
Drawings
FIG. 1 is a thermogravimetric analysis of the retarding admixture of the present invention;
FIG. 2 is an infrared spectrum of the retarding admixture of the present invention.
Detailed Description
In order to make those skilled in the art better understand the technical solution of the present invention, the following detailed description of the present invention is provided with reference to specific embodiments.
The invention provides a retarding admixture which is obtained by polymerizing monomers; the monomer consists of octadecyl methacrylate, allyl polyoxyethylene ether and acrylamide.
Preferably, the retarding admixture is obtained by emulsion polymerization of the monomer.
Preferably, the monomer consists of 0.3-0.5% of octadecyl methacrylate, 0.9-1.0% of allyl polyoxyethylene ether and 98.5-98.8% of acrylamide in molar percentage.
Preferably, the retarding admixture is a compound represented by the formula (I):
Figure BDA0002145243580000051
wherein x is 98.5-98.8%, y is 0.9-1.0%, w is 0.3-0.5%, and n is 20-25%.
The invention also provides a preparation method of the retarding admixture, which comprises the following steps: carrying out polymerization reaction on the monomer under the action of an initiator to obtain the retarding additive; the monomer consists of octadecyl methacrylate, allyl polyoxyethylene ether and acrylamide.
Preferably, the monomer consists of 0.3-0.5% of octadecyl methacrylate, 0.9-1.0% of allyl polyoxyethylene ether and 98.5-98.8% of acrylamide in percentage by mole.
Preferably, the preparation method specifically comprises the following steps: carrying out emulsion polymerization reaction on the monomer under the action of an initiator and an emulsifier to obtain the retarding admixture; the monomer consists of octadecyl methacrylate, allyl polyoxyethylene ether and acrylamide.
Preferably, the emulsifier is polyoxyethylene octyl phenol ether-10.
Preferably, the preparation method specifically comprises the following steps: mixing a monomer, an emulsifier, an initiator and water, and carrying out emulsion polymerization reaction to obtain the slow admixture; the dosage of the emulsifier is 6.0-8.0 wt% of the total mass of water.
Preferably, the initiator accounts for 0.2-0.3 wt% of the total mass of the monomers; the initiator azobisisobutyramidine hydrochloride.
Preferably, the emulsion polymerization reaction temperature is 50-55 ℃, and the reaction time is 6-7 h.
Preferably, the preparation method specifically comprises the following steps: mixing a monomer, an emulsifier, an initiator and water, carrying out emulsion polymerization reaction to obtain a gel transparent product, washing the gel transparent product for 3-5 times by using absolute ethyl alcohol until precipitation occurs, and drying the gel transparent product in an oven at the temperature of 50 ℃ for 24 hours to obtain the slow admixture.
The invention also provides a retarding acid which comprises the retarding additive or the retarding additive prepared by the preparation method.
The reagents used in the following examples are all commercially available.
Retarding admixture and preparation method thereof
Adding Octadecyl Methacrylate (OM), Allyl Polyoxyethylene Ether (APEG) and Acrylamide (AM) into a silk-mouth reagent bottle with the volume of 100 mL; then adding 26.93g of deionized water and an emulsifier OP-10 to prepare a solution with the monomer mass concentration of 15%, stirring and dissolving, and adding an initiator azo-bis-isobutyramidine hydrochloride; and finally, uniformly mixing the solutions, reacting for 6-7 hours at the temperature of 50-55 ℃ to obtain a gel transparent product, washing for 3-5 times by using absolute ethyl alcohol until precipitation occurs, and drying for 24 hours in an oven at the temperature of 50 ℃ to obtain the slow-speed admixture.
The retarding admixture is a compound shown as a formula (I):
Figure BDA0002145243580000061
wherein x is 98.5-98.8%, y is 0.9-1.0%, w is 0.3-0.5%, and n is 20-25%.
Secondly, optimizing the preparation conditions of the retarding admixture and evaluating the effect
2.1 the method is adopted to prepare the retarding admixture by changing the monomer ratio, the addition of the initiator and the addition of the emulsifier, and the specific ratio, the addition, the product purity and the thermal property of the product are shown in tables 1 and 2.
TABLE 1
Figure BDA0002145243580000071
TABLE 2
Figure BDA0002145243580000072
Figure BDA0002145243580000081
2.2 the retarding effect of the prepared retarding admixture is evaluated. 2.2.1 retarding Effect in sandstone
The retarding admixture in the amount shown in Table 3 is added into 100 parts of earth acid to dissolve completely to obtain retarding acid.
In order to evaluate the retarding performance of the retarding admixture in sandstone, a static test core corrosion method in a SY/T5886-. The process is as follows: firstly, placing equal amount of blank earth acid (12 wt% HCl + 3wt% HF) and prepared retarded acid in each identical plastic beaker, putting the beakers into a constant-temperature water bath kettle at the temperature of 100 ℃, and adding equal amount of sandstone cuttings after the temperature of each retarded acid is constant. And (3) washing the residues with distilled water until the filtrate is neutral after different reaction times, drying the residues at 105 ℃ to constant weight, and calculating the corrosion rate and the slow rate of the rock core, wherein the results are shown in Table 3.
TABLE 3
Figure BDA0002145243580000082
As can be seen from Table 3, the earth acid solution system added with the retarding additive of the present invention has better acid solution retarding effect compared with the blank earth acid.
2.2.2 retarding Effect in carbonate rock
The parts of the retarding admixtures shown in Table 4 were added to 100 parts of 15% hydrochloric acid, respectively, and completely dissolved to obtain retarding acids.
In order to evaluate the retarding performance of the retarding admixture in carbonate rocks, cubic carbonate rock samples of 2mm multiplied by 2mm are selected and calculatedThe surface area is taken out and weighed, and the mixture is placed in a constant temperature drying oven to be dried for a certain time. According to 1cm 2 And (3) pouring the equivalent blank hydrochloric acid and the retarded acid into a reaction beaker corresponding to 20ml of acid liquor, putting the reaction beaker into a constant-temperature water bath kettle at the temperature of 100 ℃, and adding the equivalent carbonate rock sample after the temperatures of the two acid liquors are constant. And (3) washing the rock sample after reaction with distilled water at different times, drying the rock sample at 105 ℃ to constant weight, and calculating the corrosion rate and the slow rate of the rock sample, wherein the results are shown in Table 4.
TABLE 4
Figure BDA0002145243580000091
As can be seen from Table 4, the hydrochloric acid solution added with the retarding admixture of the present invention is proved to have a better retarding effect.
Third, measuring intrinsic viscosity
The hair growth was measured by Shimadzu Rid-20A Gel Permeation Chromatograph (GPC) at 35 deg.C
The weight average molecular weight (Mw) and number average molecular weight (Mn), and the molecular distribution of the accelerator admixture.
TABLE 5
Retarding admixture Mw Mn Mw/Mn Mz
Example 1 891140 427474 2.08 1384150
Example 8 886746 426856 2.07 1382987
Example 9 891018 425655 2.09 1386672
As can be seen from Table 5, the retarding admixture of the present invention has a moderate molecular weight.
Fourthly, measuring the thermal stability
Thermogravimetric analysis was carried out on the retarding admixture of example 1, and the results are shown in FIG. 1.
As can be seen from the figure, the constant weight is carbonized at high temperature (above 400 ℃), and the retarding admixture provided by the invention has good thermal stability and strong temperature resistance.
Fifth, the structural characterization of the retarding admixture of the invention
The infrared absorption spectrum of the retarding admixture obtained in example 1 was measured by an infrared spectrometer, and the infrared absorption spectrum thereof was as shown in FIG. 2. As can be seen from FIG. 2, 3410cm -1 Is the N-H bond stretching vibration peak; 2912cm -1 And 2847cm -1 Methyl and methylene stretching vibration peaks; 1350cm -1 C ═ O stretching vibration peak for ester group; 1670cm -1 C ═ O stretching vibration peak of amide group; 1100cm -1 The ether bond stretching vibration peak is shown. In addition, there is no characteristic absorption peak of carbon-carbon double bond in the figure, which indicates that the synthesized product does not contain unpolymerized monomer. As can be seen from the above analysis, the copolymer is divided intoThe daughter strands carry initially designed molecular groups, from which it is concluded that the target product structure is consistent with the design.
The above is only a preferred embodiment of the present invention, and it should be noted that the above preferred embodiment should not be considered as limiting the present invention, and the protection scope of the present invention should be subject to the scope defined by the claims. It will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the spirit and scope of the invention, and should be considered to be within the scope of the invention.

Claims (7)

1. A retarding admixture, characterized by being obtained by polymerizing monomers; the monomer comprises, by mole percent, 0.3-0.5% of octadecyl methacrylate, 0.9-1.0% of allyl polyoxyethylene ether and 98.5-98.8% of acrylamide; the retarding admixture is a compound shown as a formula (I):
Figure 932827DEST_PATH_IMAGE001
（I）；
wherein x = 98.5-98.8%, y = 0.9-1.0%, w = 0.3-0.5%, and n = 20-25.
2. The retarding admixture according to claim 1, wherein the retarding admixture is obtained by emulsion polymerization of the monomers.
3. A preparation method of a retarding admixture is characterized by comprising the following steps: carrying out polymerization reaction on the monomer under the action of an initiator to obtain the retarding additive; the monomer comprises, by mole percent, 0.3-0.5% of octadecyl methacrylate, 0.9-1.0% of allyl polyoxyethylene ether and 98.5-98.8% of acrylamide.
4. The preparation method according to claim 3, characterized in that the preparation method specifically comprises: carrying out emulsion polymerization reaction on the monomer under the action of an initiator and an emulsifier to obtain the retarding admixture; the monomer consists of octadecyl methacrylate, allyl polyoxyethylene ether and acrylamide.
5. The preparation method according to claim 4, wherein the preparation method specifically comprises: mixing a monomer, an emulsifier, an initiator and water, and carrying out emulsion polymerization reaction to obtain the slow admixture; the dosage of the emulsifier is 6.0-8.0 wt% of the total mass of water.
6. The method according to claim 3, wherein the amount of the initiator is 0.2 to 0.3wt% based on the total mass of the monomers.
7. An accelerating admixture, characterized in that the accelerating admixture comprises the accelerating admixture of any one of claims 1 to 2 or the accelerating admixture prepared by the preparation method of any one of claims 3 to 6.
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US4892916A (en) * 1984-08-15 1990-01-09 Allied Colloids Limited Polymeric thickeners and their production
CN103194202A (en) * 2013-04-01 2013-07-10 西南石油大学 Adsorptive acid liquor retarding admixture and preparation method thereof
CN105001849A (en) * 2015-07-02 2015-10-28 西南石油大学 Hydrophobically associated type cation acid solution retardant and preparation method thereof
CN106928408A (en) * 2017-03-01 2017-07-07 西南石油大学 A kind of low viscosity acidifying retardant, its preparation method and tempered spline

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Publication number Priority date Publication date Assignee Title
US4892916A (en) * 1984-08-15 1990-01-09 Allied Colloids Limited Polymeric thickeners and their production
CN103194202A (en) * 2013-04-01 2013-07-10 西南石油大学 Adsorptive acid liquor retarding admixture and preparation method thereof
CN105001849A (en) * 2015-07-02 2015-10-28 西南石油大学 Hydrophobically associated type cation acid solution retardant and preparation method thereof
CN106928408A (en) * 2017-03-01 2017-07-07 西南石油大学 A kind of low viscosity acidifying retardant, its preparation method and tempered spline

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