CN110105507B - Nano aluminum complex, preparation method and application thereof - Google Patents
Nano aluminum complex, preparation method and application thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
- C02F1/56—Macromolecular compounds
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- 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
- C08F251/00—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof
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- C09K8/02—Well-drilling compositions
- C09K8/03—Specific additives for general use in well-drilling compositions
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C09K2208/00—Aspects relating to compositions of drilling or well treatment fluids
- C09K2208/12—Swell inhibition, i.e. using additives to drilling or well treatment fluids for inhibiting clay or shale swelling or disintegrating
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Abstract
The invention provides a nano aluminum complex, a preparation method and application thereof, wherein the nano aluminum complex is prepared by carrying out dispersion polymerization reaction on aluminum salt, humic acid, modified starch, acrylamide, complexing agent-ethylene diamine tetraacetic acid and initiator in an alcohol-water mixed solvent, wherein the mass percentage of each reactant is as follows: 10-20% of aluminum salt, 10-25% of humic acid, 20-35% of modified starch, 5-15% of acrylamide, 1-5% of complexing agent-ethylene diamine tetraacetic acid, 0.05-0.3% of initiator and 20-35% of alcohol-water mixed solvent. The invention provides a nano aluminum complex and a preparation method thereof, the process is simple and efficient, the comprehensive performance is excellent, the temperature and salt resistance is strong, the current strict environmental protection requirements can be met, and the prepared nano aluminum complex has multiple purposes, not only can be used as the main component of drilling fluid and completion fluid in oil field exploitation, but also can be used as a flocculating agent in the paper making industry and the water treatment industry.
Description
Technical Field
The invention belongs to the technical field of chemical additives, and particularly relates to a nano aluminum complex, a preparation method and application thereof.
Background
One of the most difficult problems and serious downhole complications frequently encountered in drilling engineering is borehole instability, which seriously affects the acquisition of geological data, drilling speed, drilling quality and cost. For part of new exploration areas, the target layer cannot be drilled due to borehole wall instability, so that exploration and development speed is delayed, and economic benefit is influenced. Borehole instability can occur in the stratum drilled during the drilling process, such as shale, sandy or silty mudstone, fluid rock, sandstone, argillaceous sandstone or silty sandstone, magma rock and the like. In addition, with the development of the drilling industry, the requirements on the temperature resistance and the salt resistance of the drilling fluid treatment agent are higher and higher, and the requirements on reservoir protection and the like are more and more prominent.
The method solves the problem of borehole wall instability, needs to improve the inhibition and plugging performance of the drilling fluid, and reduces the filtration loss of the drilling fluid. The plugging performance is improved, the filtration loss is reduced, the invasion of a liquid phase or a solid phase in the drilling fluid into a reservoir/stratum can be effectively reduced, the damage to the reservoir is prevented, the contact of the liquid phase and rock debris or the stratum is reduced, the inhibition performance can directly act on stratum rock strata or drill cuttings, the liquid phase is prevented from hydrating and dispersing the drill cuttings, and therefore the instability of a well wall is prevented. The current drilling fluid inhibitors include inorganic salts, synthetic polymers, humic acids, and asphalts. The inorganic salt and the synthetic polymer have the best inhibiting effect, but the damage to the rheological property and the filtration loss of the drilling fluid is serious, the humic acid and the asphalt have excellent temperature resistance and obvious filtration loss reducing effect, but the inhibiting performance is limited, and the asphalt product has the problems that the fluorescence is not easy to degrade, the environment pollution is caused, and the like.
An aluminum complex inhibitor is developed in the application of the drilling fluid with strong inhibition of aluminum complex sylvite (Guojinghua, Tianfeng, Zhangming and the like, drilling fluid and completion fluid, 2004, 21 (3): 23-24), has good inhibition, but can achieve good effect of stabilizing the well wall only by being matched with inorganic salt. A novel aluminum-based anti-collapse agent is developed in the research and development of the novel aluminum-based anti-collapse agent and an anti-collapse action mechanism (Qieusong, Zhang Shifeng, Weian and the like, Petroleum institute, 2014, 35(4):754 and 758), is formed by complexing humic acid and aluminum salt, has the effect of delaying pore pressure transmission, and has no evaluation on the filtration loss reduction performance and the inhibition performance. Therefore, the well wall stabilizing product with good inhibition performance, capability of effectively reducing the filtration loss and improving the plugging property, excellent comprehensive performance without changing the rheological property of the drilling fluid and the like needs to be further researched.
Therefore, it is necessary to invent a nano aluminum complex, a preparation method and an application thereof to solve the above problems.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a nano aluminum complex, a preparation method and application thereof, wherein the nano aluminum complex has the advantages of simple preparation process, excellent comprehensive performance and strong temperature and salt resistance, and can meet the current strict environmental protection requirement.
In order to achieve the above purposes, the invention adopts the technical scheme that:
the nano aluminum complex is prepared by carrying out dispersion polymerization reaction on aluminum salt, humic acid, modified starch, acrylamide, complexing agent-ethylene diamine tetraacetic acid and initiator in an alcohol-water mixed solvent, wherein the mass percent of each reactant is as follows: 10-20% of aluminum salt, 10-25% of humic acid, 20-35% of modified starch, 5-15% of acrylamide, 1-5% of complexing agent-ethylene diamine tetraacetic acid, 0.05-0.3% of initiator and 20-35% of alcohol-water mixed solvent.
Further, the aluminum salt is composed of at least one of aluminum sulfate, aluminum chloride and aluminum potassium sulfate.
Further, the initiator is selected from any one group of sodium bisulfite-ammonium persulfate, sodium bisulfite-potassium persulfate or sodium metabisulfite.
Further, the alcohol-water mixed solvent is a mixture composed of distilled water, methanol and isopropanol, and the mass percentages of the alcohol-water mixed solvent are 20-30% of distilled water, 30-50% of methanol and 30-40% of isopropanol.
The other technical scheme adopted by the invention is as follows: a method for preparing a nano aluminum complex, the method comprising the steps of:
(1) adding an alcohol-water mixed solvent into a reaction kettle, adding humic acid while stirring, adding sodium hydroxide to adjust the pH value to 11, and stirring for 30min to dissolve the humic acid;
(2) adding modified starch, acrylamide and aluminum salt into the mixture obtained in the step (1), stirring and mixing uniformly, adding an initiator and complexing agent-ethylenediamine tetraacetic acid, and stirring for 2-5 hours at 40-60 ℃ under the protection of nitrogen for dispersion polymerization;
(3) and after the reaction is finished, carrying out suction filtration separation, and drying to obtain the nano aluminum complex.
Further, the mass percentages of the reactants in the preparation process are respectively as follows:
10-20% of aluminum salt, 10-25% of humic acid, 20-35% of modified starch, 5-15% of acrylamide, 1-5% of complexing agent-ethylene diamine tetraacetic acid, 0.05-0.3% of initiator and 20-35% of alcohol-water mixed solvent.
The other technical scheme adopted by the invention is as follows: the application of the nano aluminum complex can be used as a main component of drilling fluid and completion fluid in oilfield exploitation.
The other technical scheme adopted by the invention is as follows: the application of the nano aluminum complex can be used as a flocculating agent in the papermaking industry.
The other technical scheme adopted by the invention is as follows: the application of the nano aluminum complex can be used as a flocculating agent in the water treatment industry.
The invention has the advantages of simple manufacturing process, excellent comprehensive performance and strong temperature and salt resistance, and can meet the current strict environmental protection requirement.
Drawings
Fig. 1 is a schematic flow chart of an embodiment of the method.
Detailed Description
In order to make the technical problems solved, the technical solutions adopted, and the technical effects achieved by the present invention clearer, the technical solutions of the embodiments of the present invention will be further described in detail with reference to the accompanying drawings. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
The nano aluminum complex is prepared by carrying out dispersion polymerization reaction on aluminum salt, humic acid, modified starch, acrylamide, complexing agent-ethylene diamine tetraacetic acid and initiator in an alcohol-water mixed solvent, wherein the mass percent of each reactant is as follows: 10-20% of aluminum salt, 10-25% of humic acid, 20-35% of modified starch, 5-15% of acrylamide, 1-5% of complexing agent-ethylene diamine tetraacetic acid, 0.05-0.3% of initiator and 20-35% of alcohol-water mixed solvent.
The aluminum salt is composed of at least one of aluminum sulfate, aluminum chloride and aluminum potassium sulfate.
The initiator is selected from any one group of sodium bisulfite-ammonium persulfate, sodium bisulfite-potassium persulfate or sodium metabisulfite.
The alcohol-water mixed solvent is a mixture consisting of distilled water, methanol and isopropanol, and the mass percentages of the alcohol-water mixed solvent are 20-30% of distilled water, 30-50% of methanol and 30-40% of isopropanol.
The novel nano aluminum complex provided by the invention is a novel multifunctional material, is subjected to molecular structure design and synthesis process design, and is prepared by firstly generating humic acid-starch-acrylamide graft copolymer by a dispersion polymerization process and then performing complexation reaction by using metal ion aluminum. Due to the amphoteric characteristic in the presence of aluminum ions, the aluminum complex can be dissolved in drilling fluid (pH 9-10) under alkaline conditions, nano-scale precipitates are generated when drilling the surface of acidic rock debris or formation water (pH 5-6), and the aluminum complex can invade into the pore throat of the formation, effectively reduce the permeability of shale and block microcracks. Combines the good temperature resistance of humic acid and the excellent salt resistance of starch and polyacrylamide, can effectively reduce the filtration loss under the high-temperature and high-salt environment, and prevents the filtration loss from being reducedThe filtrate enters the formation. AL3+The ion is the same as Na+、K+Similarly, clay minerals (with negative electricity) can be electrically neutralized, and a double electric layer is compressed and diffused, so that shale expansion and dispersion are weakened; novel nano aluminum complex positively charged group AL3+The clay is inserted between crystal layers of clay through electrostatic action and attracts the crystal layers, so that the hydration expansion of clay and shale is inhibited; the adsorption capacity of the Na is higher than that of Na in common inorganic salt inhibitor+、K+Strong and is more difficult to be replaced, can effectively compress the double electric layers on the surface of the clay, and further inhibits the hydration expansion and dispersion of the clay. The excellent dispersibility of the humic acid is combined with the gel protection property of the starch and the acrylamide, so that the rheological property of the drilling fluid can be effectively adjusted.
Referring to fig. 1, fig. 1 is a schematic flow chart of an embodiment of the method of the present invention.
A preparation method of a nano aluminum complex comprises the following steps:
step 101: adding the alcohol-water mixed solvent into a reaction kettle, adding humic acid while stirring, adding sodium hydroxide to adjust the pH value to 11, and stirring for 30min to dissolve the humic acid.
Step 102: adding modified starch, acrylamide and aluminum salt into the mixture obtained in the step (1), stirring and mixing uniformly, adding an initiator and complexing agent-ethylenediamine tetraacetic acid, and stirring for 2-5 hours at 40-60 ℃ under the protection of nitrogen for dispersion polymerization.
Step 103: and after the reaction is finished, carrying out suction filtration separation, and drying to obtain the nano aluminum complex.
It is emphasized that the mass percentages of the reactants are as follows: 10-20% of aluminum salt, 10-25% of humic acid, 20-35% of modified starch, 5-15% of acrylamide, 1-5% of complexing agent-ethylene diamine tetraacetic acid, 0.05-0.3% of initiator and 20-35% of alcohol-water mixed solvent.
Example 1
(1) Adding 4.4kg of distilled water, 10.6kg of methanol and 7.0kg of isopropanol into a reaction kettle, uniformly mixing, adding 20kg of humic acid while stirring, adding sodium hydroxide to adjust the pH value to 11, and stirring for 30min to dissolve the humic acid.
(2) Then adding 33kg of modified starch, 10kg of acrylamide and 12kg of aluminum sulfate into the mixture obtained in the step (1), stirring and mixing uniformly, and then adding 0.05kg of sodium bisulfite, 0.05kg of ammonium persulfate and 2.9kg of ethylene diamine tetraacetic acid. Stirring at 40 ℃ for 4 hours under nitrogen protection.
(3) After the reaction is finished, carrying out suction filtration separation and drying to obtain the product.
Example 2
(1) Adding 6.5kg of distilled water, 10.4kg of methanol and 9.1kg of isopropanol into a reaction kettle, uniformly mixing, adding 23kg of humic acid while stirring, adding sodium hydroxide to adjust the pH value to 11, and stirring for 30min to dissolve the humic acid.
(2) Then 20kg of modified starch, 13kg of acrylamide and 14kg of aluminum sulfate were added to (1), and stirred and mixed uniformly, and then 0.04kg of sodium bisulfite, 0.04kg of potassium persulfate and 3.92kg of ethylenediaminetetraacetic acid were added. The mixture was stirred at 50 ℃ for 3.5 hours under nitrogen.
(3) After the reaction is finished, carrying out suction filtration separation and drying to obtain the product.
Example 3
(1) Adding 9.9kg of distilled water, 10.9kg of methanol and 12.2kg of isopropanol into a reaction kettle, uniformly mixing, adding 12kg of humic acid while stirring, adding sodium hydroxide to adjust the pH value to 11, and stirring for 30min to dissolve the humic acid.
(2) Then 27kg of modified starch, 7kg of acrylamide and 19kg of aluminum sulfate are added into the mixture (1), the mixture is stirred and mixed evenly, and then 0.2kg of sodium metabisulfite and 1.8kg of ethylene diamine tetraacetic acid are added. The mixture was stirred at 60 ℃ for 3.0 hours under nitrogen.
(3) After the reaction is finished, carrying out suction filtration separation and drying to obtain the product.
And evaluating the performance of the drilling fluid of the prepared novel nano aluminum complex.
TABLE 1 Performance index of novel Nano-aluminum complexes
The analysis of the data shows that the novel nano aluminum complex provided by the invention has good comprehensive performance and outstanding temperature resistance and salt resistance.
Different from the prior art, the preparation method of the nano aluminum complex provided by the invention adopts a special dispersion polymerization process, the reactants are subjected to polymerization reaction in a special solvent, the reactants can be subjected to free radical dispersion copolymerization reaction in the special solvent, the interparticle agglomeration phenomenon is eliminated, the polymer particles with narrow molecular weight distribution, uniform particle size, nano-scale size and special morphology are prepared, the grafting efficiency is high, the chemical stability of the generated complex product is obviously improved, and the thermal stability is improved. In addition, the method also has the advantages of less side reaction, mild reaction condition, simple and convenient process operation, low production energy consumption and the like.
The application of the nano aluminum complex can be used as a main component of drilling fluid and completion fluid in oilfield exploitation.
The nano aluminum complex can be used as a flocculating agent in the papermaking industry.
The nano aluminum complex can be used as a flocculating agent in the water treatment industry.
Different from the prior art, the nano aluminum complex resists temperature of 160 ℃, resists saturated salt, is nontoxic and has no fluorescence. The composite flocculant can be used as a fluid loss additive, a plugging agent and a flow pattern regulator in water-based drilling/completion fluids, as a pulp flocculant in the papermaking industry, as a flocculant in the water treatment industry and the like.
It will be understood by those skilled in the art that the nano aluminum complex, the preparation method and the application thereof are not limited to the examples described in the embodiment, and the above detailed description is only for the purpose of illustrating the present invention and is not intended to limit the present invention. Other embodiments will be apparent to those skilled in the art from the following detailed description, which is intended to cover all modifications, equivalents, and alternatives falling within the spirit and scope of the invention as defined by the appended claims.
Claims (7)
1. A nano aluminum complex is characterized in that the nano aluminum complex is prepared by carrying out dispersion polymerization reaction on aluminum salt, humic acid, modified starch, acrylamide, complexing agent-ethylene diamine tetraacetic acid and initiator in an alcohol-water mixed solvent, and adding sodium hydroxide to adjust the pH value;
the mass percent of each reactant is as follows: 10-20% of aluminum salt, 10-25% of humic acid, 20-35% of modified starch, 5-15% of acrylamide, 1-5% of complexing agent-ethylene diamine tetraacetic acid, 0.05-0.3% of initiator and 20-35% of alcohol-water mixed solvent.
2. The nano-aluminum complex according to claim 1, wherein the aluminum salt is composed of at least one of aluminum sulfate, aluminum chloride and aluminum potassium sulfate.
3. The nano aluminum complex as claimed in claim 1, wherein the initiator is selected from any one of sodium bisulfite-ammonium persulfate, sodium bisulfite-potassium persulfate or sodium metabisulfite.
4. The nano aluminum complex as claimed in claim 1, wherein the alcohol-water mixed solvent is a mixture of distilled water, methanol and isopropanol, and each of the mass percentages is 20-30% of distilled water, 30-50% of methanol and 30-40% of isopropanol.
5. The method for preparing nano aluminum complex according to any one of claims 1 to 4, wherein the method comprises the following steps:
(1) adding an alcohol-water mixed solvent into a reaction kettle, adding humic acid while stirring, adding sodium hydroxide to adjust the pH value to 11, and stirring for 30min to dissolve the humic acid;
(2) adding modified starch, acrylamide and aluminum salt into the mixture obtained in the step (1), stirring and mixing uniformly, adding an initiator and complexing agent-ethylenediamine tetraacetic acid, and stirring for 2-5 hours at 40-60 ℃ under the protection of nitrogen for dispersion polymerization;
(3) and after the reaction is finished, carrying out suction filtration separation, and drying to obtain the nano aluminum complex.
6. The method for preparing the nano aluminum complex as claimed in claim 5, wherein the mass percentages of the reactants in the preparation process are respectively as follows:
10-20% of aluminum salt, 10-25% of humic acid, 20-35% of modified starch, 5-15% of acrylamide, 1-5% of complexing agent-ethylene diamine tetraacetic acid, 0.05-0.3% of initiator and 20-35% of alcohol-water mixed solvent.
7. The use of the nano aluminum complex according to any one of claims 1 to 4, wherein the nano aluminum complex is used as a main component of drilling fluid and completion fluid in oilfield exploitation.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4719021A (en) * | 1984-11-28 | 1988-01-12 | Sun Drilling Products Corporation | Shale-stabilizing drilling fluids and method for producing same |
| CN104650826A (en) * | 2013-11-21 | 2015-05-27 | 中国石油大学(华东) | Aluminum-based anti-collapse agent for drilling fluid |
| CN104830288A (en) * | 2015-04-27 | 2015-08-12 | 北京中科天启油气技术有限公司 | Borehole stabilizer for drilling fluid, preparation method and applications thereof |
| CN108728064A (en) * | 2017-04-25 | 2018-11-02 | 中国石油化工股份有限公司 | A kind of drilling fluid aluminium base closure inorganic agent and preparation method thereof |
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2019
- 2019-04-16 CN CN201910303912.9A patent/CN110105507B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4719021A (en) * | 1984-11-28 | 1988-01-12 | Sun Drilling Products Corporation | Shale-stabilizing drilling fluids and method for producing same |
| CN104650826A (en) * | 2013-11-21 | 2015-05-27 | 中国石油大学(华东) | Aluminum-based anti-collapse agent for drilling fluid |
| CN104830288A (en) * | 2015-04-27 | 2015-08-12 | 北京中科天启油气技术有限公司 | Borehole stabilizer for drilling fluid, preparation method and applications thereof |
| CN108728064A (en) * | 2017-04-25 | 2018-11-02 | 中国石油化工股份有限公司 | A kind of drilling fluid aluminium base closure inorganic agent and preparation method thereof |
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