CN112625664B - Nano plugging agent for drilling fluid and preparation method thereof - Google Patents
Nano plugging agent for drilling fluid and preparation method thereof Download PDFInfo
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- CN112625664B CN112625664B CN202011560314.9A CN202011560314A CN112625664B CN 112625664 B CN112625664 B CN 112625664B CN 202011560314 A CN202011560314 A CN 202011560314A CN 112625664 B CN112625664 B CN 112625664B
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- 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
- C09K8/42—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells
- C09K8/46—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells containing inorganic binders, e.g. Portland cement
- C09K8/467—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells containing inorganic binders, e.g. Portland cement containing additives for specific purposes
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4833—Polyethers containing oxyethylene units
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/61—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
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- 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
- C09K8/02—Well-drilling compositions
- C09K8/03—Specific additives for general use in well-drilling compositions
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- 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
- C09K8/42—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells
- C09K8/426—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells for plugging
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Abstract
The invention discloses a nano plugging agent for drilling fluid and a preparation method thereof, wherein the plugging agent comprises 8-10 parts by weight of fumed silica 8-10 parts, 15-20 parts by weight of amino silicone oil, 5-10 parts by weight of polyethylene glycol-400, 0.5-1 part by weight of toluene-2, 4-diisocyanate, 2-5 parts by weight of SPAN-80 and 75-105 parts by weight of water; the preparation method comprises the following steps of sequentially carrying out incomplete esterification reaction on fumed silica and amino silicone oil, reacting polyethylene glycol-400 and toluene diisocyanate to obtain polyurethane, mixing the two intermediate products for reaction to generate a mixture of fumed silica, amino silicone oil modified polyurethane and amino silicone oil ester, and finally adding SPAN-80 and water for uniform emulsification to obtain the polyurethane; the nano plugging agent for the drilling fluid has the advantages of improving the hydrophobicity, effectively avoiding the agglomeration of the conventional silicon dioxide at high temperature and having strong plugging capability.
Description
Technical Field
The invention relates to the technical field of petroleum and natural gas, in particular to a nano plugging agent for drilling fluid and a preparation method thereof.
Background
For hard brittle and breakable strata with bedding and microcrack development, the invasion of drilling fluid filtrate can destroy the mechanical stability of the strata, particularly, the hydraulic pressure is transmitted through the microcracks to cause the instability of a well wall, so the plugging performance of the drilling fluid is also an important index for drilling exploration and development. At present, drilling fluid has been sufficiently researched for plugging conventional pore throats, but with the development of exploration and development towards unconventional resources such as shale gas, shale oil and the like, the plugging of nano-scale pore throat cracks is more and more emphasized.
Disclosure of Invention
The invention aims to provide a nano plugging agent for drilling fluid, which can effectively plug nano pore throats, reduce the seepage of drilling fluid to a stratum in a drilling process and ensure the stability of the stratum.
The invention also aims to provide a preparation method of the nano plugging agent for the drilling fluid.
Therefore, the technical scheme of the invention is as follows:
the nano plugging agent for the drilling fluid comprises, by weight, 8-10 parts of fumed silica, 15-20 parts of amino silicone oil, 5-10 parts of polyethylene glycol-400, 0.5-1 part of toluene-2, 4-diisocyanate, 2-5 parts of SPAN-80 and 75-105 parts of water.
Preferably, the weight ratio of polyethylene glycol-400 to toluene-2, 4-diisocyanate is 10: 1.
A preparation method of the nano plugging agent for the drilling fluid comprises the following steps:
s1, mixing and stirring the fumed silica and the amino silicone oil uniformly in a reactor to obtain a mixed reactant;
s2, slowly heating the mixed reactant to 320 ℃, reacting for 2 hours under the stirring condition, and then cooling to room temperature to obtain an intermediate 1;
in the steps S1 and S2, the intermediate 1 is a product of incomplete esterification reaction of fumed silica and amino silicone oil at high temperature, and is a mixture of amino silicone oil ester and part of unreacted amino silicone oil; the esterification reaction product is physically mixed, so that the retention plugging capability can be improved, and the filtration loss and plugging effects can be improved;
s3, uniformly stirring polyethylene glycol-400 and toluene-2, 4-diisocyanate at 5 ℃, and then heating to 70 ℃ to react for 2h to obtain an intermediate 2;
in step S3, the intermediate 2 is polyurethane formed by condensation reaction of hydroxyl groups at two ends of polyethylene glycol-400 with two-NCO on toluene-2, 4-diisocyanate, respectively; the polyurethane can play a role in hydrophobic film formation in drilling fluid, namely a hydrophobic film is formed on a stratum, and film formation plugging is realized;
s4, slowly adding the intermediate 1 prepared in the step S2 into the intermediate 2, and continuously reacting for 3 hours at constant temperature of 70 ℃ to obtain an intermediate 3;
at this step S4, the condensation reaction at step S3 is not yet completely reacted but is already completed for the most part, and at this time, the intermediate 1 is added thereto, so that the amino group of the amino silicone oil unreacted in the intermediate 1 reacts with the hydroxyl group of the free state at the end side of polyethylene glycol-400, to produce a small amount of amino silicone oil-modified polyurethane; the amino silicone oil modified polyurethane also has a hydrophobic film forming effect and strong viscosity, and the hydrophobicity of the polyurethane is further improved;
s5, adding SPAN-80 and water into the intermediate 3, stirring until the emulsification is uniform, forming stable oil-in-water emulsion, and improving the action aging of the product in the drilling fluid to obtain the nano plugging agent for the drilling fluid.
Compared with the prior art, the nano plugging agent for the drilling fluid consists of a mixture of fumed silica, amino silicone oil modified polyurethane and amino silicone oil ester; compared with the conventional silicon dioxide, the hydrophobicity of the silicon dioxide can be effectively improved by modifying the silicon dioxide by amino silicone oil, the conventional silicon dioxide is prevented from agglomerating at high temperature, and the amino silicone oil contains a part of amino groups, so that the reactivity with fumed silica can be improved; in addition, the amino silicone oil modified polyurethane in the mixture is a paste, and compared with conventional silicone oil, the amino silicone oil modified polyurethane has stronger retention capacity in pore throats, and is matched with surface-modified silicon dioxide to improve the plugging capacity; meanwhile, the amino silicone oil modified polyurethane has certain soft elasticity, can effectively improve the composite effect of the amino silicone oil modified polyurethane, the fumed silica and the amino silicone oil ester, and improves the plugging effect.
Detailed Description
The present invention will be further described with reference to the following examples, which are not intended to limit the invention in any way. In the following examples and comparative examples, each component was purchased from a commercially available product.
Example 1
A preparation method of the nano plugging agent for the drilling fluid comprises the following steps:
s1, mixing and stirring 8 parts by weight of fumed silica and 15 parts by weight of amino silicone oil uniformly in a reactor to obtain a mixed reactant;
s2, slowly heating the mixed reactant to 320 ℃, reacting for 2 hours under the stirring condition, and then cooling to room temperature to obtain an intermediate 1;
s3, stirring 5 parts by weight of polyethylene glycol-400 and 0.5 part by weight of toluene-2, 4-diisocyanate uniformly at 5 ℃, and then heating to 70 ℃ for reaction for 2 hours to obtain an intermediate 2;
s4, slowly adding the intermediate 1 prepared in the step S2 into the intermediate 2, and continuously reacting for 3 hours at constant temperature of 70 ℃ to obtain an intermediate 3;
s5, adding 2 parts by weight of SPAN-80 and 75 parts by weight of water into the intermediate 3, and stirring until the mixture is emulsified uniformly to obtain the nano plugging agent for the drilling fluid.
Example 2
A preparation method of the nano plugging agent for the drilling fluid comprises the following steps:
s1, mixing and stirring 10 parts by weight of fumed silica and 20 parts by weight of amino silicone oil uniformly in a reactor to obtain a mixed reactant;
s2, slowly heating the mixed reactant to 320 ℃, reacting for 2 hours under the stirring condition, and then cooling to room temperature to obtain an intermediate 1;
s3, stirring 10 parts by weight of polyethylene glycol-400 and 1 part by weight of toluene-2, 4-diisocyanate uniformly at 5 ℃, and then heating to 70 ℃ for reaction for 2 hours to obtain an intermediate 2;
s4, slowly adding the intermediate 1 prepared in the step S2 into the intermediate 2, and continuously reacting for 3 hours at constant temperature of 70 ℃ to obtain an intermediate 3;
s5, adding 5 parts by weight of SPAN-80 and 105 parts by weight of water into the intermediate 3, and stirring until the mixture is emulsified uniformly to obtain the nano plugging agent for the drilling fluid.
Example 3
A preparation method of the nano plugging agent for the drilling fluid comprises the following steps:
s1, mixing and stirring 9 parts by weight of fumed silica and 18 parts by weight of amino silicone oil uniformly in a reactor to obtain a mixed reactant;
s2, slowly heating the mixed reactant to 320 ℃, reacting for 2 hours under the stirring condition, and then cooling to room temperature to obtain an intermediate 1;
s3, stirring 8 parts by weight of polyethylene glycol-400 and 0.8 part by weight of toluene-2, 4-diisocyanate uniformly at 5 ℃, and then heating to 70 ℃ for reaction for 2 hours to obtain an intermediate 2;
s4, slowly adding the intermediate 1 prepared in the step S2 into the intermediate 2, and continuously reacting for 3 hours at constant temperature of 70 ℃ to obtain an intermediate 3;
s5, adding 4 parts by weight of SPAN-80 and 95 parts by weight of water into the intermediate 3, and stirring until the mixture is emulsified uniformly to obtain the nano plugging agent for the drilling fluid.
Comparative example 1
A preparation method of the nano plugging agent for the drilling fluid comprises the following steps:
s1, mixing and stirring 10 parts by weight of fumed silica and 20 parts by weight of amino silicone oil uniformly in a reactor to obtain a mixed reactant;
s2, adding 5 parts by weight of SPAN-80 and 65 parts by weight of water into the mixed reactant, and stirring until the mixture is emulsified uniformly to obtain the nano plugging agent for the drilling fluid.
Comparative example 2
A preparation method of the nano plugging agent for the drilling fluid comprises the following steps:
s1, mixing and stirring 8 parts by weight of fumed silica and 15 parts by weight of amino silicone oil uniformly in a reactor to obtain a mixed reactant;
s2, slowly heating the mixed reactant to 100 ℃, reacting for 2 hours under the stirring condition, and then cooling to room temperature to obtain an intermediate 1;
s3, stirring 5 parts by weight of polyethylene glycol-400 and 0.5 part by weight of toluene-2, 4-diisocyanate uniformly at 5 ℃, and then heating to 70 ℃ for reaction for 2 hours to obtain an intermediate 2;
s4, slowly adding the intermediate 1 prepared in the step S2 into the intermediate 2, and continuously reacting for 3 hours at constant temperature of 70 ℃ to obtain an intermediate 3;
s5, adding 2 parts by weight of SPAN-80 and 75 parts by weight of water into the intermediate 3, and stirring until the mixture is emulsified uniformly to obtain the nano plugging agent for the drilling fluid.
Comparative example 3
A preparation method of the nano plugging agent for the drilling fluid comprises the following steps:
s1, stirring 5 parts by weight of polyethylene glycol-400 and 0.5 part by weight of toluene-2, 4-diisocyanate uniformly at 5 ℃, and then heating to 70 ℃ for reaction for 2 hours to obtain an intermediate 1;
s2, slowly adding 15 parts by weight of amino silicone oil into the intermediate 1, and keeping the temperature of 70 ℃ to continue reacting for 3 hours at constant temperature to obtain an intermediate 2;
and S3, adding 2 parts by weight of SPAN-80 and 75 parts by weight of water into the intermediate 2, and stirring until the mixture is emulsified uniformly to obtain the nano plugging agent for the drilling fluid.
And (3) performance testing:
referring to GB16783.1-2014 oil and gas industry drilling fluid field test first part: water-based drilling fluid, the viscosity, fluid loss reduction and plugging performance of the nano plugging agents prepared in examples 1 to 3 and comparative examples 1 to 3 were evaluated in 6 wt.% bentonite-based slurry. Wherein the plugging filtration loss is measured by an OFI plugging filtration loss instrument under the test conditions of 150 ℃, 21MPa of pressure, 170-55 of type of filter disc, 3 mu m of pore diameter and 400mD of permeability. The test sample is prepared by adding 3 wt.% of nano plugging agent for drilling fluid into 6 wt.% of bentonite-based slurry. The test results are shown in table 1 below.
Table 1:
from the test results in table 1, it can be seen that the nano plugging agent prepared in examples 1 to 3 shows good fluid loss reduction effect when the addition amount of the nano plugging agent is 3 wt.% in 6 wt.% bentonite-based slurry, and has no substantial viscosity effect, and after curing for 16 hours at 150 ℃, the nano plugging agent still maintains good fluid loss reduction and plugging effects, and shows good temperature resistance. In contrast, the comparative example 1 is only the physical mixing of the fumed silica and the amino silicone oil, so that the filtration loss is reduced, and the plugging effect is obviously weakened; in the comparative example 2, the reaction temperature in the step 2 is not enough, so that the esterification reaction degree of the fumed silica and the amino silicone oil is not high, and the filtration loss and plugging effects are weakened; and the gas-phase white carbon black is not added in the comparative example 3, so that the micro-nano hard material in the plugging agent is insufficient, and the plugging effect is obviously weakened.
Claims (3)
1. The preparation method of the nano plugging agent for the drilling fluid is characterized in that the nano plugging agent for the drilling fluid comprises 8-10 parts of fumed silica, 15-20 parts of amino silicone oil, 5-10 parts of polyethylene glycol-400, 0.5-1 part of toluene-2, 4-diisocyanate, 2-5 parts of SPAN-80 and 75-105 parts of water in parts by weight;
the preparation method comprises the following steps:
s1, mixing and stirring the fumed silica and the amino silicone oil uniformly in a reactor to obtain a mixed reactant;
s2, slowly heating the mixed reactant to 320 ℃, reacting for 2 hours under the stirring condition, and then cooling to room temperature to obtain an intermediate 1;
s3, uniformly stirring polyethylene glycol-400 and toluene-2, 4-diisocyanate at 5 ℃, and then heating to 70 ℃ to react for 2h to obtain an intermediate 2;
s4, slowly adding the intermediate 1 prepared in the step S2 into the intermediate 2, and continuously reacting for 3 hours at constant temperature of 70 ℃ to obtain an intermediate 3;
s5, adding SPAN-80 and water into the intermediate 3, and stirring until the emulsification is uniform to obtain the nano plugging agent for the drilling fluid.
2. The preparation method of the nano plugging agent for the drilling fluid, according to claim 1, is characterized in that the weight ratio of the polyethylene glycol-400 to the toluene-2, 4-diisocyanate is 10: 1.
3. The nano plugging agent for the drilling fluid prepared by the preparation method of the nano plugging agent for the drilling fluid according to claim 1 or 2.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102504518A (en) * | 2011-11-09 | 2012-06-20 | 温州大学 | Method for preparing nano silicon dioxide/aqueous polyurethane hybrid material |
| CN105567199A (en) * | 2014-10-15 | 2016-05-11 | 中国石油化工股份有限公司 | Hydrophobic nano silica emulsified water plugging agent and preparation method and application thereof |
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| US20120065341A1 (en) * | 2010-09-10 | 2012-03-15 | Basf Se | Silicon dioxide dispersions |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102504518A (en) * | 2011-11-09 | 2012-06-20 | 温州大学 | Method for preparing nano silicon dioxide/aqueous polyurethane hybrid material |
| CN105567199A (en) * | 2014-10-15 | 2016-05-11 | 中国石油化工股份有限公司 | Hydrophobic nano silica emulsified water plugging agent and preparation method and application thereof |
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