CN116751573B - Petroleum nanometer blocking remover and preparation method thereof - Google Patents

Petroleum nanometer blocking remover and preparation method thereof Download PDF

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CN116751573B
CN116751573B CN202311050195.6A CN202311050195A CN116751573B CN 116751573 B CN116751573 B CN 116751573B CN 202311050195 A CN202311050195 A CN 202311050195A CN 116751573 B CN116751573 B CN 116751573B
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nano
agent
petroleum
silicon dioxide
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CN116751573A (en
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张冬梅
于瀚博
孙一僮
尹婷婷
于涛
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Daqing Kexun Oilfield Technical Service Co ltd
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Daqing Kexun Oilfield Technical Service Co ltd
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    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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    • C09K8/00Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
    • C09K8/52Compositions for preventing, limiting or eliminating depositions, e.g. for cleaning
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K8/00Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
    • C09K8/52Compositions for preventing, limiting or eliminating depositions, e.g. for cleaning
    • C09K8/524Compositions for preventing, limiting or eliminating depositions, e.g. for cleaning organic depositions, e.g. paraffins or asphaltenes
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K8/00Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
    • C09K8/52Compositions for preventing, limiting or eliminating depositions, e.g. for cleaning
    • C09K8/528Compositions for preventing, limiting or eliminating depositions, e.g. for cleaning inorganic depositions, e.g. sulfates or carbonates
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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Abstract

The invention relates to the technical field of petroleum nano blocking remover, and in particular discloses a petroleum nano blocking remover and a preparation method thereof, wherein the petroleum nano blocking remover comprises the following raw materials in parts by weight: 5-10 parts of sorbitan tristearate, 4-8 parts of triethanolamine, 3-5 parts of polyoxyethylene ether, 8-12 parts of coupling modified whisker double modifier, 6-10 parts of nano silicon dioxide modifier, 4-6 parts of hydrochloric acid, 3-5 parts of sodium dodecyl benzene sulfonate and 30-35 parts of deionized water. The nano blocking remover adopts the mutual coordination optimization among sorbitan tristearate, triethanolamine and polyoxyethylene ether, provides effective blocking removal efficiency for the treatment of organic polymers, improves the blocking removal efficiency of inorganic scales through the mutual coordination among hydrochloric acid and sodium dodecyl benzene sulfonate, and can bi-directionally coordinate the treatment efficiency of the organic polymers and the inorganic scales by adding the coupling modified whisker double-adjusting agent to optimize the coordination performance of the organic polymers and the inorganic scales.

Description

Petroleum nanometer blocking remover and preparation method thereof
Technical Field
The invention relates to the technical field of nano blocking remover, in particular to a petroleum nano blocking remover and a preparation method thereof.
Background
In the development and production process of the oil field, various technological processes such as drilling, oil gas exploitation and the like adopt a large number of chemical products, and mainly comprise mineral substances, natural materials, organic matters, inorganic matters, high polymer materials and the like. With the injection of chemicals, the near-well hydrocarbon reservoir is blocked to different degrees due to the nature of the reservoir and the influence of many factors in the development process, and the oil well stratum is subjected to a large amount of bacterial generation and high polymer deposition, so that stratum holes are blocked, and therefore, the plugging remover is required to treat the near-well hydrocarbon reservoir.
The blocking remover adopted in the prior art is mostly acid substances, can remove the blocking on inorganic scale, but has poor treatment efficiency on organic polymer, the blocking remover is difficult to coordinate and improve the blocking removal efficiency on inorganic scale and organic polymer, meanwhile, the stability of the product is poor, the blocking removal efficiency is poor under the conditions of acid corrosion and high temperature, and the service efficiency of the product is limited.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a petroleum nano blocking remover and a preparation method thereof, so as to solve the problems in the prior art.
The invention solves the technical problems by adopting the following technical scheme:
the invention provides a petroleum nano blocking remover which comprises the following raw materials in parts by weight:
5-10 parts of sorbitan tristearate, 4-8 parts of triethanolamine, 3-5 parts of polyoxyethylene ether, 8-12 parts of coupling modified whisker double modifier, 6-10 parts of nano silicon dioxide modifier, 4-6 parts of hydrochloric acid, 3-5 parts of sodium dodecyl benzene sulfonate, 2-5 parts of ethylene diamine tetraacetic acid and 30-35 parts of deionized water.
Preferably, the petroleum nano blocking remover comprises the following raw materials in parts by weight:
7.5 parts of sorbitan tristearate, 6 parts of triethanolamine, 4 parts of polyoxyethylene ether, 10 parts of coupling modified whisker double-regulating agent, 8 parts of nano silicon dioxide modifier, 5 parts of hydrochloric acid, 4 parts of sodium dodecyl benzene sulfonate, 3.5 parts of ethylene diamine tetraacetic acid and 32.5 parts of deionized water.
Preferably, the preparation method of the coupling modified whisker double dispensing agent comprises the following steps:
s01: 3-5 parts of silane coupling agent KH560, 5-7 parts of chitosan solution with mass fraction of 5-8% and 2-4 parts of lanthanum sulfate solution are stirred and mixed uniformly to obtain coupling complex-mixing base solution;
s02: immersing the aluminum borate whisker into yttrium nitrate solution according to the weight ratio of 1:5, carrying out ultrasonic treatment for 10-20 min, wherein the ultrasonic power is 350-450W, and carrying out suction filtration and drying after ultrasonic treatment to obtain an aluminum borate whisker impregnant;
s03: the aluminum borate whisker impregnant and the nano agent liquid are mixed according to the weight ratio of (5-7): 2, sending the mixture into a ball mill for ball milling treatment, wherein the ball milling rotating speed is 1000-1500 r/min, ball milling is carried out for 1-2 h, and after ball milling, water washing and drying are carried out to obtain a nano agent modified aluminum borate whisker body;
s04: stirring and uniformly mixing the nano agent modified aluminum borate whisker body and the coupling complex adjusting base solution according to the weight ratio of 2:5 to obtain the coupling modified whisker double adjusting agent.
Preferably, the mass fraction of the lanthanum sulfate solution is 5-10%; the mass fraction of the yttrium nitrate solution is 2-5%.
Preferably, the preparation method of the nano agent liquid comprises the following steps:
carrying out heat treatment on bentonite at 210-230 ℃ for 10-15 min, then cooling to 55-60 ℃ at the speed of 2-5 ℃/min, uniformly stirring in a sodium hydroxide solution, washing with water, and drying to obtain a bentonite modifier;
and sequentially adding 6-10 parts of bentonite modifier, 3-5 parts of silica sol and 1-3 parts of sodium lignin sulfonate into 15-20 parts of sulfuric acid solution with mass fraction of 5% and uniformly stirring to obtain the nano agent liquid.
Preferably, the mass fraction of the sodium hydroxide solution is 6-8%.
Preferably, the preparation method of the nano silicon dioxide modifier comprises the following steps:
s01: calcining the nano silicon dioxide at 150-160 ℃ for 15-20 min, and cooling after calcining to obtain calcined nano silicon dioxide;
s02: placing hydroxyapatite into a sodium alginate aqueous solution with the mass fraction of 10% and the total amount of 5 times of the hydroxyapatite, then adding a phosphate buffer solution with the total amount of 10-15% of the hydroxyapatite, uniformly stirring, washing with water, and drying to obtain a hydroxyapatite agent;
s03: 10-15 parts of calcined nano silicon dioxide, 4-7 parts of hydroxyapatite agent, 2-4 parts of sodium carboxymethylcellulose, 1-3 parts of stearic acid are added into 20-25 parts of deionized water, and the mixture is stirred fully, washed and dried to obtain the nano silicon dioxide modifier.
Preferably, the pH value of the phosphoric acid buffer solution is 4.5-5.5.
The invention also provides a preparation method of the petroleum nano blocking remover, which comprises the following steps:
adding the coupling modified whisker double-regulating agent and the nano silicon dioxide modifier into deionized water, then adding hydrochloric acid, sodium dodecyl benzene sulfonate and ethylene diamine tetraacetic acid dipotassium, uniformly stirring, then adding sorbitan tristearate, triethanolamine and polyoxyethylene ether, stirring for reaction treatment, and obtaining the petroleum nano blocking remover.
Preferably, the stirring reaction temperature is 46-48 ℃, the stirring rotation speed is 550-750 r/min, and the stirring time is 1-2 h.
Compared with the prior art, the invention has the following beneficial effects:
the nano blocking remover provided by the invention adopts mutual coordination optimization among sorbitan tristearate, triethanolamine and polyoxyethylene ether, provides effective blocking removal efficiency for the treatment of organic polymers, improves the blocking removal efficiency of inorganic scales through mutual coordination among hydrochloric acid, sodium dodecyl benzene sulfonate and dipotassium ethylenediamine tetraacetate, and improves the treatment efficiency of organic polymers and inorganic scales through bidirectional coordination of the added coupling modified whisker double-agent, so that the coordination performance of the two is optimized, the mutual coordination of the added nano silicon dioxide modifier and the coupling modified whisker double-agent is realized, the mutual coordination is realized, the treatment efficiency of the organic polymers and the inorganic scales is improved, and meanwhile, the acid mist resistance and the high temperature resistance stability of the product are improved;
the coupling modified whisker double-adjusting agent adopts silane coupling agent KH560, chitosan solution and lanthanum sulfate solution to be blended and matched as base solution, so that the interfacial property of a system and the activity degree between raw materials can be optimized, the aluminum borate whisker is treated by yttrium nitrate solution, the activity degree of the whisker is optimized, meanwhile, the nano agent solution is subjected to ball milling treatment, and the nano agent solution is matched with the whisker to cooperate together, so that the dispersibility of the whisker is enhanced, the stability of the system is optimized, and the acid corrosion resistance and the high temperature resistance of the system are improved; the nanometer agent liquid adopts bentonite to carry out heat treatment, then carries out cooling treatment and dispersing in sodium hydroxide solution, optimizes the interlayer spacing of the bentonite and the dispersity thereof, is beneficial to interpenetration of the interlayer spacing of the bentonite, optimizes the stability of the system, simultaneously carries out ball milling modification on the aluminum borate whisker impregnant by matching with the nanometer agent liquid formed by matching with silica sol, sodium lignin sulfonate and sulfuric acid solution, and coordinates to improve the whisker, the obtained nanometer agent modified aluminum borate whisker can better co-disperse the coupling and re-adjusting base liquid into the system, thereby better improving the interfacial property of the system, optimizing the co-adjustment blocking efficiency of organic polymers and inorganic scales, and further improving the acid corrosion resistance and high temperature resistance stability of the product;
the nano silicon dioxide modifier adopts nano silicon dioxide to be calcined and heat treated, so that the activity of the nano silicon dioxide modifier is optimized, meanwhile, the hydroxyapatite is treated by sodium alginate aqueous solution and phosphoric acid buffer solution, the optimized hydroxyapatite agent is better coordinated to improve the calcined nano silicon dioxide, and the prepared nano silicon dioxide modifier is better coordinated and synergistic with the coupling modified whisker double-adjustment agent through the coordination of the nano silicon dioxide and the modified whisker double-adjustment agent, so that the performance of the product is further improved.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and fully with reference to the accompanying drawings, in which it is evident that the embodiments described are only some, but not all embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The petroleum nano blocking remover comprises the following raw materials in parts by weight:
5-10 parts of sorbitan tristearate, 4-8 parts of triethanolamine, 3-5 parts of polyoxyethylene ether, 8-12 parts of coupling modified whisker double modifier, 6-10 parts of nano silicon dioxide modifier, 4-6 parts of hydrochloric acid, 3-5 parts of sodium dodecyl benzene sulfonate, 2-5 parts of ethylene diamine tetraacetic acid and 30-35 parts of deionized water.
The petroleum nano blocking remover comprises the following raw materials in parts by weight:
7.5 parts of sorbitan tristearate, 6 parts of triethanolamine, 4 parts of polyoxyethylene ether, 10 parts of coupling modified whisker double-regulating agent, 8 parts of nano silicon dioxide modifier, 5 parts of hydrochloric acid, 4 parts of sodium dodecyl benzene sulfonate, 3.5 parts of ethylene diamine tetraacetic acid and 32.5 parts of deionized water.
The preparation method of the coupling modified whisker double-regulating agent comprises the following steps:
s01: 3-5 parts of silane coupling agent KH560, 5-7 parts of chitosan solution with mass fraction of 5-8% and 2-4 parts of lanthanum sulfate solution are stirred and mixed uniformly to obtain coupling complex-mixing base solution;
s02: immersing the aluminum borate whisker into yttrium nitrate solution according to the weight ratio of 1:5, carrying out ultrasonic treatment for 10-20 min, wherein the ultrasonic power is 350-450W, and carrying out suction filtration and drying after ultrasonic treatment to obtain an aluminum borate whisker impregnant;
s03: the aluminum borate whisker impregnant and the nano agent liquid are mixed according to the weight ratio of (5-7): 2, sending the mixture into a ball mill for ball milling treatment, wherein the ball milling rotating speed is 1000-1500 r/min, ball milling is carried out for 1-2 h, and after ball milling, water washing and drying are carried out to obtain a nano agent modified aluminum borate whisker body;
s04: stirring and uniformly mixing the nano agent modified aluminum borate whisker body and the coupling complex adjusting base solution according to the weight ratio of 2:5 to obtain the coupling modified whisker double adjusting agent.
The mass fraction of the lanthanum sulfate solution in the embodiment is 5-10%; the mass fraction of the yttrium nitrate solution is 2-5%.
The preparation method of the nano agent liquid in the embodiment comprises the following steps:
carrying out heat treatment on bentonite at 210-230 ℃ for 10-15 min, then cooling to 55-60 ℃ at the speed of 2-5 ℃/min, uniformly stirring in a sodium hydroxide solution, washing with water, and drying to obtain a bentonite modifier;
and sequentially adding 6-10 parts of bentonite modifier, 3-5 parts of silica sol and 1-3 parts of sodium lignin sulfonate into 15-20 parts of sulfuric acid solution with mass fraction of 5% and uniformly stirring to obtain the nano agent liquid.
The mass fraction of the sodium hydroxide solution in the embodiment is 6-8%.
The preparation method of the nano silicon dioxide modifier in the embodiment comprises the following steps:
s01: calcining the nano silicon dioxide at 150-160 ℃ for 15-20 min, and cooling after calcining to obtain calcined nano silicon dioxide;
s02: placing hydroxyapatite into a sodium alginate aqueous solution with the mass fraction of 10% and the total amount of 5 times of the hydroxyapatite, then adding a phosphate buffer solution with the total amount of 10-15% of the hydroxyapatite, uniformly stirring, washing with water, and drying to obtain a hydroxyapatite agent;
s03: 10-15 parts of calcined nano silicon dioxide, 4-7 parts of hydroxyapatite agent, 2-4 parts of sodium carboxymethylcellulose, 1-3 parts of stearic acid are added into 20-25 parts of deionized water, and the mixture is stirred fully, washed and dried to obtain the nano silicon dioxide modifier.
The pH value of the phosphate buffer solution of the embodiment is 4.5-5.5.
The preparation method of the petroleum nano blocking remover comprises the following steps:
adding the coupling modified whisker double-regulating agent and the nano silicon dioxide modifier into deionized water, then adding hydrochloric acid, sodium dodecyl benzene sulfonate and ethylene diamine tetraacetic acid dipotassium, uniformly stirring, then adding sorbitan tristearate, triethanolamine and polyoxyethylene ether, stirring and reacting, and obtaining the petroleum nano blocking remover.
The stirring reaction temperature is 46-48 ℃, the stirring rotation speed is 550-750 r/min, and the stirring time is 1-2 h.
Example 1.
The petroleum nano blocking remover comprises the following raw materials in parts by weight:
5 parts of sorbitan tristearate, 4 parts of triethanolamine, 3 parts of polyoxyethylene ether, 8 parts of coupling modified whisker double-regulating agent, 6 parts of nano silicon dioxide modifier, 4 parts of hydrochloric acid, 3 parts of sodium dodecyl benzene sulfonate, 2 parts of ethylene diamine tetraacetic acid dipotassium and 30 parts of deionized water.
The preparation method of the coupling modified whisker double-regulating agent comprises the following steps:
s01: 3 parts of silane coupling agent KH560, 5 parts of chitosan solution with mass fraction of 5% and 2 parts of lanthanum sulfate solution are stirred and mixed uniformly to obtain coupling complex-mixing base solution;
s02: immersing the aluminum borate whisker into yttrium nitrate solution according to the weight ratio of 1:5, carrying out ultrasonic treatment for 10min with ultrasonic power of 350W, carrying out suction filtration and drying after ultrasonic treatment is finished, and obtaining an aluminum borate whisker impregnant;
s03: the aluminum borate whisker impregnant and the nano agent liquid are mixed according to the weight ratio of 5:2, feeding the mixture into a ball mill for ball milling treatment, wherein the ball milling rotating speed is 1000r/min, ball milling is carried out for 1h, and after ball milling is finished, water washing and drying are carried out, so as to obtain a nano agent modified aluminum borate whisker body;
s04: stirring and uniformly mixing the nano agent modified aluminum borate whisker body and the coupling complex adjusting base solution according to the weight ratio of 2:5 to obtain the coupling modified whisker double adjusting agent.
The mass fraction of the lanthanum sulfate solution of this example was 5%; the mass fraction of the yttrium nitrate solution is 2%.
The preparation method of the nano agent liquid in the embodiment comprises the following steps:
heat-treating bentonite at 210 ℃ for 10min, then cooling to 55 ℃ at the speed of 2 ℃/min, uniformly stirring in a sodium hydroxide solution, washing with water, and drying to obtain a bentonite modifier;
and sequentially adding 6 parts of bentonite modifier, 3 parts of silica sol and 1 part of sodium lignin sulfonate into 15 parts of sulfuric acid solution with mass fraction of 5% and stirring uniformly to obtain nano agent solution.
The mass fraction of the sodium hydroxide solution of this example was 6%.
The preparation method of the nano silicon dioxide modifier in the embodiment comprises the following steps:
s01: calcining the nano silicon dioxide at 150 ℃ for 15min, and cooling after calcining to obtain calcined nano silicon dioxide;
s02: placing hydroxyapatite into a sodium alginate aqueous solution with the mass fraction of 10% and the total amount of 5 times of the hydroxyapatite, then adding a phosphoric acid buffer solution with the total amount of 10% of the hydroxyapatite, uniformly stirring, washing with water, and drying to obtain a hydroxyapatite agent;
s03:10 parts of calcined nano silicon dioxide, 4 parts of hydroxyapatite agent, 2 parts of sodium carboxymethylcellulose and 1 part of stearic acid are added into 20 parts of deionized water, and the mixture is fully stirred, washed and dried to obtain the nano silicon dioxide modifier.
The pH of the phosphate buffer solution of this example was 4.5.
The preparation method of the petroleum nano blocking remover comprises the following steps:
adding the coupling modified whisker double-regulating agent and the nano silicon dioxide modifier into deionized water, then adding hydrochloric acid, sodium dodecyl benzene sulfonate and ethylene diamine tetraacetic acid dipotassium, uniformly stirring, then adding sorbitan tristearate, triethanolamine and polyoxyethylene ether, stirring and reacting, and obtaining the petroleum nano blocking remover.
The stirring reaction temperature in this example was 46℃and the stirring speed was 550r/min, and the stirring time was 1h.
Example 2.
The petroleum nano blocking remover comprises the following raw materials in parts by weight:
10 parts of sorbitan tristearate, 8 parts of triethanolamine, 5 parts of polyoxyethylene ether, 12 parts of coupling modified whisker double-regulating agent, 10 parts of nano silicon dioxide modifier, 6 parts of hydrochloric acid, 5 parts of sodium dodecyl benzene sulfonate, 5 parts of ethylene diamine tetraacetic acid dipotassium and 35 parts of deionized water.
The preparation method of the coupling modified whisker double-regulating agent comprises the following steps:
s01: uniformly stirring and mixing 5 parts of silane coupling agent KH560, 7 parts of 8% chitosan solution and 4 parts of lanthanum sulfate solution to obtain coupling complex-preparation base solution;
s02: immersing the aluminum borate whisker into yttrium nitrate solution according to the weight ratio of 1:5, carrying out ultrasonic treatment for 20min, wherein the ultrasonic power is 450W, and carrying out suction filtration and drying after ultrasonic treatment to obtain an aluminum borate whisker impregnant;
s03: the aluminum borate whisker impregnant and the nano agent liquid are mixed according to the weight ratio of 7:2, sending the mixture into a ball mill for ball milling treatment, wherein the ball milling rotating speed is 1500r/min, ball milling is carried out for 2 hours, and after ball milling is finished, water washing and drying are carried out, so as to obtain a nano agent modified aluminum borate whisker body;
s04: stirring and uniformly mixing the nano agent modified aluminum borate whisker body and the coupling complex adjusting base solution according to the weight ratio of 2:5 to obtain the coupling modified whisker double adjusting agent.
The mass fraction of the lanthanum sulfate solution of this example was 10%; the mass fraction of the yttrium nitrate solution is 5%.
The preparation method of the nano agent liquid in the embodiment comprises the following steps:
heat-treating bentonite at 230 ℃ for 15min, then cooling to 60 ℃ at a speed of 5 ℃/min, uniformly stirring in a sodium hydroxide solution, washing with water, and drying to obtain a bentonite modifier;
sequentially adding 10 parts of bentonite modifier, 5 parts of silica sol and 3 parts of sodium lignin sulfonate into 20 parts of sulfuric acid solution with mass fraction of 5%, and uniformly stirring to obtain nano agent solution.
The mass fraction of the sodium hydroxide solution of this example was 8%.
The preparation method of the nano silicon dioxide modifier in the embodiment comprises the following steps:
s01: calcining the nano silicon dioxide at 160 ℃ for 20min, and cooling after calcining to obtain calcined nano silicon dioxide;
s02: placing hydroxyapatite in sodium alginate aqueous solution with the mass fraction of 10% and the total amount of 5 times of the hydroxyapatite, then adding phosphoric acid buffer solution with the total amount of 15% of the hydroxyapatite, uniformly stirring, washing with water, and drying to obtain a hydroxyapatite agent;
s03:15 parts of calcined nano silicon dioxide, 7 parts of hydroxyapatite agent, 4 parts of sodium carboxymethylcellulose and 3 parts of stearic acid are added into 25 parts of deionized water, and the mixture is fully stirred, washed and dried to obtain the nano silicon dioxide modifier.
The pH of the phosphate buffer solution of this example was 5.5.
The preparation method of the petroleum nano blocking remover comprises the following steps:
adding the coupling modified whisker double-regulating agent and the nano silicon dioxide modifier into deionized water, then adding hydrochloric acid, sodium dodecyl benzene sulfonate and ethylene diamine tetraacetic acid dipotassium, uniformly stirring, then adding sorbitan tristearate, triethanolamine and polyoxyethylene ether, stirring and reacting, and obtaining the petroleum nano blocking remover.
The stirring reaction temperature in this example was 48℃and the stirring speed was 750r/min, and the stirring time was 2 hours.
Example 3.
The petroleum nano blocking remover comprises the following raw materials in parts by weight:
7.5 parts of sorbitan tristearate, 6 parts of triethanolamine, 4 parts of polyoxyethylene ether, 10 parts of coupling modified whisker double-regulating agent, 8 parts of nano silicon dioxide modifier, 5 parts of hydrochloric acid, 4 parts of sodium dodecyl benzene sulfonate, 3.5 parts of ethylene diamine tetraacetic acid and 32.5 parts of deionized water.
The preparation method of the coupling modified whisker double-regulating agent comprises the following steps:
s01: uniformly stirring and mixing 4 parts of silane coupling agent KH560, 6 parts of chitosan solution with the mass fraction of 6.5% and 3 parts of lanthanum sulfate solution to obtain coupling complex-mixing base solution;
s02: immersing the aluminum borate whisker into yttrium nitrate solution according to the weight ratio of 1:5, carrying out ultrasonic treatment for 15min, wherein the ultrasonic power is 400W, and carrying out suction filtration and drying after ultrasonic treatment to obtain an aluminum borate whisker impregnant;
s03: the aluminum borate whisker impregnant and the nano agent liquid are mixed according to the weight ratio of 3:1, feeding the mixture into a ball mill for ball milling treatment, wherein the ball milling rotating speed is 1250r/min, ball milling is carried out for 1.5 hours, and the mixture is washed and dried to obtain a nano agent modified aluminum borate whisker body;
s04: stirring and uniformly mixing the nano agent modified aluminum borate whisker body and the coupling complex adjusting base solution according to the weight ratio of 2:5 to obtain the coupling modified whisker double adjusting agent.
The mass fraction of the lanthanum sulfate solution of this example was 7.5%; the mass fraction of the yttrium nitrate solution is 3.5%.
The preparation method of the nano agent liquid in the embodiment comprises the following steps:
heat-treating bentonite at 220 ℃ for 12min, then cooling to 57.5 ℃ at the speed of 3.5 ℃/min, uniformly stirring in sodium hydroxide solution, washing with water, and drying to obtain a bentonite modifier;
8 parts of bentonite modifier, 4 parts of silica sol and 2 parts of sodium lignin sulfonate are sequentially added into 17.5 parts of sulfuric acid solution with mass fraction of 5% and uniformly stirred, so as to obtain nano agent liquid.
The mass fraction of the sodium hydroxide solution of this example was 7%.
The preparation method of the nano silicon dioxide modifier in the embodiment comprises the following steps:
s01: calcining the nano silicon dioxide at 155 ℃ for 17.5min, and cooling after calcining to obtain calcined nano silicon dioxide;
s02: placing hydroxyapatite in sodium alginate aqueous solution with the mass fraction of 10% and the total amount of 5 times of the hydroxyapatite, then adding phosphate buffer solution with the total amount of 12.5% of the hydroxyapatite, uniformly stirring, washing with water, and drying to obtain a hydroxyapatite agent;
s03:12.5 parts of calcined nano silicon dioxide, 5.5 parts of hydroxyapatite agent, 3 parts of sodium carboxymethyl cellulose and 2 parts of stearic acid are added into 22.5 parts of deionized water, and the mixture is fully stirred, washed and dried to obtain the nano silicon dioxide modifier.
The pH of the phosphate buffer solution of this example was 5.0.
The preparation method of the petroleum nano blocking remover comprises the following steps:
adding the coupling modified whisker double-regulating agent and the nano silicon dioxide modifier into deionized water, then adding hydrochloric acid, sodium dodecyl benzene sulfonate and ethylene diamine tetraacetic acid dipotassium, uniformly stirring, then adding sorbitan tristearate, triethanolamine and polyoxyethylene ether, stirring and reacting, and obtaining the petroleum nano blocking remover.
The stirring reaction temperature in this example was 47℃and the stirring speed was 600r/min, and the stirring time was 1.5 hours.
Comparative example 1.
The difference from example 3 is that no coupling modification whisker two-pass agent is added.
Comparative example 2.
The difference from example 3 is that the aluminum borate whisker impregnant is replaced by aluminum borate whisker in the preparation method of the coupling modified whisker double dispense.
Comparative example 3.
The difference from example 3 is that the coupling complex-adjusting base solution is replaced by deionized water in the preparation method of the coupling modified whisker double-adjusting agent.
Comparative example 4.
The difference from example 3 is that no nano-additive solution is added in the preparation method of the coupling modified whisker double dispense.
Comparative example 5.
The difference from example 3 is that bentonite modifier is replaced by bentonite in the preparation of nano agent liquid.
Comparative example 6.
The difference from example 3 is that no silica sol or sodium lignin sulfonate is added in the preparation of the nano agent solution.
Comparative example 7.
The difference from example 3 is that no nanosilica modifier is added.
Comparative example 8.
The difference from example 3 is that no hydroxyapatite agent is added in the preparation of the nano silica modifier.
Comparative example 9.
The difference from example 3 is that the nanosilica modifier is replaced with nanosilica.
Performance tests are carried out on the test products of the examples 1-3 and the comparative examples 1-9;
degradation rate of organic polymer gel = viscosity before organic polymer gel degradation-viscosity after organic polymer gel degradation/viscosity before organic polymer gel degradation;
mixing magnesium carbonate, calcium sulfate and marble according to a weight ratio of 1:1:1 to form inorganic scale, and then carrying out corrosion rate test by adopting the test products of examples 1-3 and comparative examples 1-9; testing the ratio of the test product to the organic polymer gel to the inorganic scale at a ratio of 1:10; placing the test products of examples 1-3 and comparative examples 1-9 under the condition of 2% hydrochloric acid mist for 6 hours, and then placing the test products at 65 ℃ for 12 hours; testing the stability of acid corrosion resistance and high temperature resistance;
as can be seen from comparative examples 1 to 9 and examples 1 to 3;
the product of the embodiment 3 has excellent organic polymer gel and inorganic scale treatment efficiency, the treatment effects of the organic polymer gel and the inorganic scale can be improved in a coordinated manner, and meanwhile, the product has excellent treatment stability under the conditions of acid corrosion resistance and high temperature resistance;
from comparative examples 1-6 and example 3, the inorganic scale and organic gel treatment rate of the product are obviously reduced without adding the coupling modified whisker double-regulating agent, meanwhile, in the preparation method of the coupling modified whisker double-regulating agent, the aluminum borate whisker impregnant is replaced by aluminum borate whisker, the coupling complex-regulating base solution is replaced by deionized water, no nano-additive solution is added, the bentonite modifier is replaced by bentonite in the nano-additive solution preparation, no silica sol and sodium lignin sulfonate are added in the nano-additive solution preparation, and the performance of the product is prone to deterioration;
meanwhile, the nano-agent liquid is not added, the performance change of the product is obvious under the acid corrosion and high temperature resistant conditions, and the use of the nano-agent liquid has obvious improvement effect on the acid corrosion and high temperature resistant performance of the product;
meanwhile, the preparation methods of the nano agent liquid are different, the preparation methods of the coupling complex-mixing base liquid and the treatment of the aluminum borate whisker impregnant are different, the performance effect of the product is prone to be poor, and only the coupling modified whisker double-mixing agent prepared by the method is adopted, so that the performance effect of the product is most obvious;
from the comparison example 1, the comparison example 7 and the example 3, one of the coupling modification whisker double-adjusting agent and the nano silicon dioxide modifier is not added, the performance of the product has obvious worsening trend, and the product has the most obvious performance effect by adopting the cooperation of the coupling modification whisker double-adjusting agent and the nano silicon dioxide modifier;
as shown in comparative examples 7-9, the preparation of the nano silicon dioxide modifier is not added with the hydroxyapatite agent, the nano silicon dioxide modifier is replaced by nano silicon dioxide, the performance of the product is prone to be deteriorated, and only the nano silicon dioxide modifier prepared by the method has the most obvious performance effect.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present disclosure describes embodiments, not every embodiment is provided with a separate embodiment, and that this description is provided for clarity only, and that the disclosure is not limited to the embodiments described in detail below, and that the embodiments described in the examples may be combined as appropriate to form other embodiments that will be apparent to those skilled in the art.

Claims (7)

1. The petroleum nano blocking remover is characterized by comprising the following raw materials in parts by weight:
5-10 parts of sorbitan tristearate, 4-8 parts of triethanolamine, 3-5 parts of polyoxyethylene ether, 8-12 parts of coupling modified whisker double modifier, 6-10 parts of nano silicon dioxide modifier, 4-6 parts of hydrochloric acid, 3-5 parts of sodium dodecyl benzene sulfonate, 2-5 parts of ethylene diamine tetraacetic acid and 30-35 parts of deionized water;
the preparation method of the coupling modified whisker double-dispensing agent comprises the following steps:
s01: 3-5 parts of silane coupling agent KH560, 5-7 parts of chitosan solution with mass fraction of 5-8% and 2-4 parts of lanthanum sulfate solution are stirred and mixed uniformly to obtain coupling complex-mixing base solution;
s02: immersing the aluminum borate whisker into yttrium nitrate solution according to the weight ratio of 1:5, carrying out ultrasonic treatment for 10-20 min, wherein the ultrasonic power is 350-450W, and carrying out suction filtration and drying after ultrasonic treatment to obtain an aluminum borate whisker impregnant;
s03: the aluminum borate whisker impregnant and the nano agent liquid are mixed according to the weight ratio of (5-7): 2, sending the mixture into a ball mill for ball milling treatment, wherein the ball milling rotating speed is 1000-1500 r/min, ball milling is carried out for 1-2 h, and after ball milling, water washing and drying are carried out to obtain a nano agent modified aluminum borate whisker body;
s04: stirring and uniformly mixing the nano agent modified aluminum borate whisker body and the coupling complex adjusting base solution according to the weight ratio of 2:5 to obtain a coupling modified whisker double adjusting agent;
the preparation method of the nano agent liquid comprises the following steps:
carrying out heat treatment on bentonite at 210-230 ℃ for 10-15 min, then cooling to 55-60 ℃ at the speed of 2-5 ℃/min, uniformly stirring in a sodium hydroxide solution, washing with water, and drying to obtain a bentonite modifier;
sequentially adding 6-10 parts of bentonite modifier, 3-5 parts of silica sol and 1-3 parts of sodium lignin sulfonate into 15-20 parts of sulfuric acid solution with mass fraction of 5%, and uniformly stirring to obtain nano agent liquid;
the preparation method of the nano silicon dioxide modifier comprises the following steps:
s01: calcining the nano silicon dioxide at 150-160 ℃ for 15-20 min, and cooling after calcining to obtain calcined nano silicon dioxide;
s02: placing hydroxyapatite into a sodium alginate aqueous solution with the mass fraction of 10% and the total amount of 5 times of the hydroxyapatite, then adding a phosphate buffer solution with the total amount of 10-15% of the hydroxyapatite, uniformly stirring, washing with water, and drying to obtain a hydroxyapatite agent;
s03: 10-15 parts of calcined nano silicon dioxide, 4-7 parts of hydroxyapatite agent, 2-4 parts of sodium carboxymethylcellulose, 1-3 parts of stearic acid are added into 20-25 parts of deionized water, and the mixture is stirred fully, washed and dried to obtain the nano silicon dioxide modifier.
2. The petroleum nano blocking remover according to claim 1, wherein the petroleum nano blocking remover comprises the following raw materials in parts by weight:
7.5 parts of sorbitan tristearate, 6 parts of triethanolamine, 4 parts of polyoxyethylene ether, 10 parts of coupling modified whisker double-regulating agent, 8 parts of nano silicon dioxide modifier, 5 parts of hydrochloric acid, 4 parts of sodium dodecyl benzene sulfonate, 3.5 parts of ethylene diamine tetraacetic acid and 32.5 parts of deionized water.
3. The petroleum nano blocking remover according to claim 1, wherein the mass fraction of the lanthanum sulfate solution is 5-10%; the mass fraction of the yttrium nitrate solution is 2-5%.
4. The petroleum nano blocking remover according to claim 1, wherein the mass fraction of the sodium hydroxide solution is 6-8%.
5. The petroleum nano blocking remover according to claim 1, wherein the pH value of the phosphoric acid buffer solution is 4.5-5.5.
6. A method for preparing the petroleum nano blocking remover according to any one of claims 1-5, which is characterized by comprising the following steps:
adding the coupling modified whisker double-regulating agent and the nano silicon dioxide modifier into deionized water, then adding hydrochloric acid, sodium dodecyl benzene sulfonate and ethylene diamine tetraacetic acid dipotassium, uniformly stirring, then adding sorbitan tristearate, triethanolamine and polyoxyethylene ether, stirring for reaction treatment, and obtaining the petroleum nano blocking remover after stirring.
7. The method for preparing the petroleum nano blocking remover according to claim 6, wherein the stirring reaction temperature is 46-48 ℃, the stirring rotation speed is 550-750 r/min, and the stirring time is 1-2 h.
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