CN102603985A - High-temperature-resistant while-drilling plugging agent and preparation method thereof - Google Patents
High-temperature-resistant while-drilling plugging agent and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a high-temperature-resistant while-drilling plugging agent and a preparation method thereof and belongs to the technical field of oil field chemical drilling fluid treating agents. The method comprises the following steps: preparing a stable emulsion from an oil soluble monomer A, an oil soluble crosslinking agent B, an azo-type initiator, an organic hydroperoxide and water in the presence of an emulsifier, and polymerizing the stable emulsion to obtain a powder M; and swelling the powder M by use of a swelling agent, adding a water soluble monomer C, a water soluble crosslinking agent D and a reductive initiator into the swelled powder M, and polymerizing the mixture at the room temperature to obtain the high-temperature-resistant while-drilling plugging agent. The high-temperature-resistant while-drilling plugging agent is in a powder shape, has relatively high temperature resistance, can resist the temperature up to 180 DEG C, and can be used for performing while-drilling plugging on deep wells and supper deep wells. The while-drilling plugging agent can be used for quickly effectively plugging the permeability leak, the micro order crack and gap leak, avoiding the repeated leak, participating in the formation of a filter cake, keeping the stability of a well wall and obviously reducing the drilling filler loss and the pollution to a reservoir, has no influence on the rheological property of the drilling fluid and has the advantages of good compatibility with various drilling fluid systems and relatively good combination property.
Description
Technical field
The present invention relates to a kind of high temperature resistance drill-feeding plugging agent and preparation method thereof, belong to oilfield chemistry additive for drilling fluid technical field.
Background technology
Leak-proof leak-stopping in drilling process is one of theme of well borer author's research always, and leakage usually can cause the generation of a series of down hole problems such as bit freezing, blowout, well slough, is seriously restricting the raising of drilling speed.Leakage in the reservoir drilling process also has negative impact to reservoir protection; It generally is " anti-blocking laying equal stress on " to the technology that Slot Handling adopted both at home and abroad; Aspect leak stopping, generally adopt bridge joint leak stopping, the leak stopping of shear-thickening liquid, high absorbency material leak stopping, liquid sleeve pipe etc. to be suitable for perviousness and fractured leakage; Hide pipe sealing drop ply, gel leak stopping and some traditional blocking methods with bore hole and be applicable to cave leakage.Domestic and international existing uniaxial pressure encapsulant, bridge joint plugging agent, high dehydration plugging agent, the leak stopping of diesel oil bentonite cement, barite plug leak stopping, gel and resin plugging agent, grout plugging agent and their composite use tackle permeability loss, and the leak stopping success ratio reaches more than 90%.
Above-mentioned prior art and employed plugging agent do not belong to the lost circulation additive category basically, and plugging agent need stop to creep into capable leak stopping before getting into drop ply, prolong the activity duration, slow down drilling speed, and therefore, drill-feeding plugging agent is suggested and obtains broad research.But it is composite that the research of existing drill-feeding plugging agent mainly concentrates on the mixing of multiple material; Product cut size is bigger; Like patent 200410037657.1 is that its particle median size is 80～20 orders with the composite drill-feeding plugging agent that forms of vegetable fibre, limestone powder and oil-soluble resin; Patent 200810115975.3 is combined into shell powder, limestone powder and three kinds of components of OSR, and its main ingredient particulate median size is 100 orders; With bore 801 plugging agents with more than 10 kind of composite forming of macromolecular compound such as Chinese bandoline wood, humic acids, CMC 99.5 (a kind of research of novel well drilling leak-proof sealing agent and application. drilling fluid and well finishing liquid, 2006,23 (3): 42-44).The polymer class drill-feeding plugging agent is also arranged, but all be the water-absorbing resin that adopts aqueous solution polymerization to obtain, product needed is further dry, could use after the granulation, because the restriction of equipment, product cut size can't reach below the micron order, and the temperature resistance scarce capacity.As patent 200910216732.3 be with hydroscopic high-molecular resin as drill-feeding plugging agent, it is 2～3 kms that this agent is suitable for the stratum scope, in 120 ℃ of the bottom temperatures; The drill-feeding plugging agent of patent 200810224440.X is that the compound other materials of water-absorbing resin that adopts aqueous solution polymerization to obtain is prepared from; Patent 20091026736.1 is a kind of water-absorbing resin drill-feeding plugging agents that adopt aqueous solution polymerization to be prepared from.
Though certain effect has been used and obtained to existing drill-feeding plugging agent at the scene; But owing to deepening continuously of hydrocarbon resources exploitation; The deep-well ultra deep well is on the increase; Existing drill-feeding plugging agent is difficult to satisfy the leakage on HTHP stratum in harsh day by day field requirement, especially the deep-well ultra deep well does not still have effective solution.And see that from the characteristic of absorbent ground the passage that forms seepage all is the hole and the microfracture of rock, its radial dimension be that micron is above to a millimeter grade following rank, and the particle size of drill-feeding plugging agent must be complementary with the aperture and just can reach plugging effect preferably.
Summary of the invention
The objective of the invention is to the leakage problem that exists in the present drilling process, provide a kind of can lost circulation additive, do not influence mud property and can reduce filter loss, temperature resistance can reach 180 ℃, the significant high temperature resistance drill-feeding plugging agent of pressure-bearing plugging effect.
Another object of the present invention provides a kind of preparation method of drill-feeding plugging agent, and the drill-feeding plugging agent that this method is prepared is the controlled microspheroidal powder-product of particle diameter, can directly be used for lost circulation additive, and is easy to use, is easy to promote.
The present invention realizes through following technical proposals:
The present invention is mixed with stable emulsion by the molten monomer A of oil, the molten crosslinking agent B of oil, azo-initiator and organic hydroperoxide class initiator and water under the effect of emulsifying agent, behind polymerization reaction take place, obtain powder M; With M with the swelling agent swelling after, add water-soluble monomer C, water-soluble linking agent D and a reduction type initiator, polymerization at room temperature can obtain the high temperature resistance drill-feeding plugging agent after accomplishing.
The molten monomer A of above-mentioned oil is one or both in vinylbenzene, Bing Xisuandingzhi, the TEB 3K;
It is 1 that above-mentioned oil dissolves crosslinking agent B, the 4-Vinylstyrene;
Above-mentioned azo-initiator is a kind of in Diisopropyl azodicarboxylate, the ABVN;
Above-mentioned organic hydroperoxide class initiator is a kind of in cumyl hydroperoxide, the t-butyl hydrogen peroxide;
Mentioned emulsifier is a kind of in cetyl trimethylammonium bromide, the sodium lauryl sulphate;
Above-mentioned swelling agent is a kind of in n-Octanol, the normal hexane;
Above-mentioned water-soluble monomer C is at least a in vinylformic acid, acrylic amide, the 2-acrylamido-2-methyl propane sulfonic acid;
Above-mentioned water-soluble linking agent D is N, N-DMAA, N, a kind of in the N-diethylammonium acrylic amide;
Above-mentioned reduction class initiator is a kind of in ferrous sulfate, the Sodium Pyrosulfite;
Wherein, dissolving monomer A, the molten crosslinking agent B of oil, azo-initiator and organic hydroperoxide class initiator is 10: 0.5～2: 0.2～0.8: 0.3～1 by mass ratio.
The preparation method of high temperature resistance drill-feeding plugging agent may further comprise the steps:
1. oil being dissolved monomer A, oil, to dissolve crosslinking agent B, azo-initiator and organic hydroperoxide class initiator be 10: 0.5～2: 0.2～0.8: 0.3～1 to mix by mass ratio, and it is for use to form disperse phase;
2. emulsifying agent is mixed with 1.0～2.0g/100mL H
2The aqueous solution of O is for use as external phase;
3. the disperse phase that 1. step is obtained is added dropwise in the external phase that 2. step obtain; Be configured to 60～80% concentrated emulsion; Obtain powder M at 40～60 ℃ of following polymerization 6～8h, and take by weighing the swelling agent that quality is powder M0.4～0.6 times, it is for use to join among the powder M swelling 2～5h;
4. be that the water-soluble monomer C of powder M5～15% is for use with the aqueous solution that is mixedly configured into 10～20% with 0.5～1 times water-soluble linking agent D of water-soluble monomer C quality with quality;
5. it is for use quality to be that the inorganic reduction class initiator of water-soluble monomer C10～25% is configured to 3.6～25% the aqueous solution;
6. the powder M after the swelling that 3. step is obtained adds in the step aqueous solution 4., under whipped state, adds the step aqueous solution 5., and polyase 13 under the room temperature～5min afterreaction finishes, and the collection product obtains the high temperature resistance drill-feeding plugging agent.
Drill-feeding plugging agent of the present invention is a powdery product, has higher temperature resistance, and temperature resistance can reach 180 ℃, can be used for the lost circulation additive of deep-well ultra deep well; For the leakage effectively shutoff fast of permeability loss, micron order crack and hole, avoid the repeatability leakage; Can participate in filter cake and form, keep wellbore stability; Can significantly reduce drilling fluid filtration, reduce reservoir pollution; Do not influence the rheological of drilling fluid, excellent compatibility is arranged, show better comprehensive performance with various drilling fluid systems.
Description of drawings:
Fig. 1 is the microscopic pattern figure of the present invention under sem.
Embodiment:
Embodiment 1:
The cetyl trimethylammonium bromide of 0.3g is dissolved in the 30mL water; Dissolve the mixed solution of the cumyl hydroperoxide initiator of the Diisopropyl azodicarboxylate initiator of the Vinylstyrene of the vinylbenzene of adding 70g, 3.5g, 3.0g and 3.6g under lasting whipped state afterwards fully; Treat after the reinforced formation emulsion that finishes system to be warmed up to 50 ℃; After obtaining powder behind the polymerization 8h, take by weighing the 10.0g powder and join in the 5.0g n-Octanol; Then the acrylic amide of 1.5g and N ' the N-methylene-bisacrylamide of 1.0g are dissolved in the aqueous solution of 15.0mL; Join by in the PS powder of n-Octanol swelling 2h; After mixing; Under whipped state, add the 5.0mL aqueous solution of 0.20g ferrous sulfate, the 3min internal reaction is accomplished, and obtains the high temperature resistance drill-feeding plugging agent.
Embodiment 2:
The cetyl trimethylammonium bromide of 0.3g is dissolved in the 30mL water; Dissolve the mixed solution of the cumyl hydroperoxide initiator of the Diisopropyl azodicarboxylate initiator of the Vinylstyrene of the vinylbenzene of adding 70g, 7.0g, 3.0g and 3.6g under lasting whipped state afterwards fully; Treat after the reinforced formation emulsion that finishes system to be warmed up to 55 ℃; After obtaining powder behind the polymerase 17 h, take by weighing the 10.0g powder and join in the 6.0g n-Octanol; Then the acrylic amide of 1.5g and N ' the N-methylene-bisacrylamide of 1.0g are dissolved in the aqueous solution of 15.0mL; Join by in the PS powder of n-Octanol swelling 5h; After mixing; Under whipped state, add the 5.0mL aqueous solution of 0.20g ferrous sulfate, the 3min internal reaction is accomplished, and obtains the high temperature resistance drill-feeding plugging agent.
Embodiment 3～7: step is identical with embodiment 1, reactant and as shown in table 1 with scale:
Table 1 a high temperature resistance drill-feeding plugging agent and preparation method thereof embodiment
Surperficial metal spraying after the drill-feeding plugging agent drying that embodiment 1,2,3,4 is obtained is observed its microscopic pattern and is respectively a among Fig. 1, b, c, d under sem.Can be known that by Fig. 1 the high temperature resistance drill-feeding plugging agent particle diameter that the present invention obtains is a micron order, particle diameter distributes between 2～25 μ m; Consumption through adjusting the molten linking agent D of oil can obtain the different high temperature resistance drill-feeding plugging agent of particle diameter, and meets water and oily all abilities volume expanding, can be used in the microfracture and the hole of shutoff relative broad range.
The high temperature resistance drill-feeding plugging agent that embodiment 3 reactions are obtained adds in the 4% fresh water base slurry; Behind 180 ℃ of high temperature ageing 16h of high temperature roller stove; Under the room temperature with six fast rotary viscosity design determining drilling fluid rheologies; Measure filter loss with the drilling fluid filter press, measure wastage with the husky bed of 40～60 orders, the result is as shown in table 2.
Table 2 high temperature resistance drill-feeding plugging agent is performance in 4% fresh water base slurry
| Prescription | AV(mPa·s) | PV(mPa·s) | YP(Pa) | FL(mL) | Wastage (ml) |
| The base slurry | 4.0 | 3.5 | 0.5 | 27.2 | 400 |
| Base slurry+1% drill-feeding plugging agent | 5.5 | 4.5 | 1.0 | 13.2 | 38 |
Can be known that by present embodiment and table 2 in 4% fresh water base slurry, add the present invention's 1% high temperature resistance drill-feeding plugging agent, temperature resistance can reach 180 ℃, its leakproof ability obviously strengthens, and filter loss obviously reduces, and the system rheological changes little, can be used for the lost circulation additive of high-temperature stratum.
Claims (11)
1. a high temperature resistance drill-feeding plugging agent is characterized in that: under the effect of emulsifying agent, be mixed with stable emulsion by the molten monomer A of oil, the molten crosslinking agent B of oil, azo-initiator and organic hydroperoxide class initiator and water, behind polymerization reaction take place, obtain powder M; With powder M with the swelling agent swelling after, add water-soluble monomer C, water-soluble linking agent D and a reduction type initiator, polymerization at room temperature can obtain the high temperature resistance drill-feeding plugging agent after accomplishing.
2. a kind of high temperature resistance drill-feeding plugging agent according to claim 1 is characterized in that: the molten monomer A of oil is one or both in vinylbenzene, Bing Xisuandingzhi, the TEB 3K.
3. a kind of high temperature resistance drill-feeding plugging agent according to claim 1 and 2 is characterized in that: it is 1 that oil dissolves crosslinking agent B, the 4-Vinylstyrene.
4. a kind of high temperature resistance drill-feeding plugging agent according to claim 1 is characterized in that: azo-initiator is a kind of in Diisopropyl azodicarboxylate, the ABVN.
5. a kind of high temperature resistance drill-feeding plugging agent according to claim 1 and 2 is characterized in that: organic hydroperoxide class initiator is cumyl hydroperoxide or t-butyl hydrogen peroxide.
6. a kind of high temperature resistance drill-feeding plugging agent according to claim 1 and 2 is characterized in that: emulsifying agent is cetyl trimethylammonium bromide or sodium lauryl sulphate.
7. a kind of high temperature resistance drill-feeding plugging agent according to claim 1 and 2 is characterized in that: swelling agent is n-Octanol or normal hexane.
8. a kind of high temperature resistance drill-feeding plugging agent according to claim 1 and 2 is characterized in that: water-soluble monomer C is any one or its combination in vinylformic acid, acrylic amide, the 2-acrylamido-2-methyl propane sulfonic acid.
9. a kind of high temperature resistance drill-feeding plugging agent according to claim 1 is characterized in that: water-soluble linking agent D is N, N-DMAA, N, a kind of in the N-diethylammonium acrylic amide.
10. a kind of high temperature resistance drill-feeding plugging agent according to claim 1 and 2 is characterized in that: reduction type initiator is a kind of in ferrous sulfate, the Sodium Pyrosulfite.
11. the preparation method of a high temperature resistance drill-feeding plugging agent is characterized in that may further comprise the steps:
1. oil being dissolved monomer A, the molten crosslinking agent B of oil, azo-initiator and organic hydroperoxide class initiator is that 10:0.5 ~ 2:0.2 ~ 0.8:0.3 ~ 1 mixes by mass ratio, and it is for use to form disperse phase;
2. emulsifying agent is mixed with 1.0 ~ 2.0g/100mL H
2The aqueous solution of O is for use as external phase;
3. the disperse phase that 1. step is obtained is added dropwise in the external phase that 2. step obtain; Be configured to 60 ~ 80% concentrated emulsion; Obtain powder M at 40 ~ 60 ℃ of following polymerization 6 ~ 8h, and take by weighing the swelling agent that quality is powder M0.4 ~ 0.6 times, it is for use to join among the powder M swelling 2 ~ 5h;
4. be the water-soluble monomer C of powder M5 ~ 15% with quality, be mixedly configured into 10 ~ 20% the aqueous solution with 0.5 ~ 1 times water-soluble linking agent D of water-soluble monomer C quality for use;
5. it is for use quality to be that the inorganic reduction class initiator of water-soluble monomer C10 ~ 25% is configured to 3.6 ~ 25% the aqueous solution;
6. the powder M after the swelling that 3. step is obtained adds in the step aqueous solution 4., under whipped state, adds the step aqueous solution 5., and polyase 13 under the room temperature ~ 5min afterreaction finishes, and the collection product obtains the high temperature resistance drill-feeding plugging agent.
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| CN103387824A (en) * | 2013-08-09 | 2013-11-13 | 卫辉市化工有限公司 | Method for preparing plugging agent for well drilling |
| CN104194750A (en) * | 2014-07-30 | 2014-12-10 | 中国石油天然气集团公司 | Nanometer blocking agent for oil-based drilling fluid and preparation method of nanometer blocking agent |
| CN104403058A (en) * | 2014-10-31 | 2015-03-11 | 中国石油化工集团公司 | Latex plugging agent for drilling fluid and preparation method thereof |
| CN104418965A (en) * | 2013-08-27 | 2015-03-18 | 中国石油化工股份有限公司 | Preparation method of self-healing agent for oil well cement, well cementation self-healing cement slurry and application |
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| CN113388378A (en) * | 2020-03-13 | 2021-09-14 | 中石化南京化工研究院有限公司 | Novel slow-expansion plugging material and preparation method thereof |
| CN113388378B (en) * | 2020-03-13 | 2023-01-31 | 中石化南京化工研究院有限公司 | Novel slow expansion plugging material and preparation method thereof |
| CN115746197A (en) * | 2021-09-02 | 2023-03-07 | 中石化石油工程技术服务有限公司 | Double-crosslinked polymer microsphere plugging agent for oil-based drilling fluid and preparation method thereof |
| CN114181345A (en) * | 2021-11-05 | 2022-03-15 | 中国石油天然气集团有限公司 | Plugging agent, preparation method and application thereof, and drilling fluid |
| CN114524899A (en) * | 2022-02-28 | 2022-05-24 | 中国地质大学（北京） | Acrylate base fluid, preparation method thereof, plugging agent and application thereof |
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Application publication date: 20120725 |