CN105114032A - Method of plugging leak of medium-depth well via cross-linked polymer gel plugging agent - Google Patents
Method of plugging leak of medium-depth well via cross-linked polymer gel plugging agent Download PDFInfo
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Abstract
The invention relates to a method of plugging a leak of a medium-depth well via cross-linked polymer gel plugging agent. Raw materials include, by weight, 120 parts of refined cotton sodium salt solution, 75-85 parts of acrylamide, 13-17 parts of ammonium persulfate, 2-5 parts of ceric sulfate, 4 parts of beta-D-mannuronic acid (M), 1-1.5 parts of ammonium dihydrogen phosphate, 100 parts of composite Portland cement mortar, 150-200 parts of mixed microfiber. A water-cement ratio of the composite Portland cement mortar is 0.44. The plugging agent is obtained by adding the acrylamide, ammonium persulfate granules, ceric sulfate granules, the beta-D-mannuronic acid (M), the composite Portland cement mortar, the mixed microfiber and the ammonium dihydrogen phosphate in order into the refined cotton sodium salt solution and mixing them well; the plugging agent is delivered to a leak layer; a pressure test is run after mud replacement is performed in a drill pipe; if bottom hole pressure rises, borehole mud replacement is performed after standing and pressure holding; after standing and pressure holding for 12 hours, a leak plugging pressure-bearing test is run; if pump pressure is normal, drilling is continued. The method allows reliable leak plugging and resistance to high temperature and pressure.
Description
Technical field
The present invention relates to a kind of method adopting cross-linked polymer gel sealing agent to carry out middle-deep well leak stopping, belong to petroleum drilling technology field.
Background technology
Leakage is the technical barrier often run in drilling process, especially high temperature leakage can cause a large amount of losses of drilling fluid, cause the rising of drilling cost, bottom pressure can be caused to change simultaneously, bring out the generation of the complex accident such as borehole well instability, well slough, well kick, blowout, seriously govern the raising of bit speed.
At present when high-temperature stratum leakage section met by oil drilling brill, owing to lacking the leakage stopping technology of high temperature resistance, the conventional sealing agent leak stopping of general employing.What domestic process high temperature leakage generally adopted is bridge joint leak stopping, and bridge joint leak stopping has economy, easy to use, the advantage of construction safety, can solve the partial loss that caused by hole and crack and leakage is returned in mistake.The bridge joint loss circulation material of domestic use is roughly divided into three classes: hard fruit shell class, fibrous material and lamellar material.In Process of Leaking Stoppage, any class material is used alone, its effect is all limited, only have above-mentioned three class materials with rational ratio and grating compound use, just can receive due effect, but along with deepening continuously of creeping into, the temperature on leakage stratum is also in continuous rising, be immersed in hard fruit shell class material in mud and plant fiber material as walnut shell, hazelnut shell, cotton seed hulls and sawdust etc., high temperature in well, under the condition of high pressure and alkali corrosion, As time goes on, these materials are by slowly deliquescing, corrosion, even some material can be burnt, bridge joint intensity is caused sharply to decline, be easy to cause leak stopping failure or secondary leakage, fundamentally cannot solve a difficult problem for high temperature leak stopping.
Well depth is that 4000 ~ 5000m is called middle-deep well, and downhole temperature is usually at 120 DEG C ~ 140 DEG C.Although the stoppage engineering that conventional blocking method is oil drilling has played effect, but there is shortcoming or deficiency simultaneously, high-temperature resistance is low, period of validity is short, leak stopping efficiency is poor, loss circulation material consumption is large, plugging time is long, high temperature deep well and geothermal well leak stopping safety factor poor, easily there is down hole problem, these shortcomings directly affect the probing development process of high temperature well and geothermal well, therefore traditional high temperature loss circulation material far from can meet the leak stopping demand of growing deep-well Holes of Complicated Wells, therefore it is very necessary for studying a kind of high temperature deep well high temperature resistance sealing agent.
Summary of the invention
The object of the invention is to, overcome problems of the prior art, provide a kind of method adopting cross-linked polymer gel sealing agent to carry out middle-deep well leak stopping, leak stopping is reliable, and high temperature resistance, anti-pressure ability are strong.
For solving above technical problem, a kind of method adopting cross-linked polymer gel sealing agent to carry out middle-deep well leak stopping of the present invention, in turn include the following steps: (1) prepare raw material by following component and weight content, purified cotton sodium salt solution: 120 parts, acrylamide: (75 ~ 85) part, ammonium persulfate: (13 ~ 17) part, cerous sulfate: (2 ~ 5) part, beta-D-mannuronic acid (M): 4 parts, ammonium dihydrogen phosphate (ADP): (1 ~ 1.5) part, Composite portland cement slurry: 100 parts and mix type microfibre: (150 ~ 200) part; The water/binder ratio of described Composite portland cement slurry is 0.44; (2) in purified cotton sodium salt solution, add acrylamide, carry out high-speed stirred with the rotating speed of 400r/min and within 10 minutes, make both fully mixing, then carry out moderate-speed mixer with the rotating speed of 300r/min, be heated to 60 DEG C while moderate-speed mixer and keep constant temperature; (3) continue to pass into nitrogen in step product (2) and reaction vessel, pass into nitrogen and at remaining on constant temperature 60 DEG C, slowly add ammonium persulfate particle at maintenance moderate-speed mixer after 3 minutes, reaction is until after particle disappears, continue back flow reaction 1.5 hours; (4) temperature be increased to 80 DEG C and keep constant temperature, under maintenance moderate-speed mixer, slowly add cerous sulfate particle, then the charge door of off-response container, promote the charge of nitrogen, keep the pressure in reaction vessel to be 1.3MPa, back flow reaction more than 3 hours, until reactant presents white emulsion shape, obtains cross-linked polymer gel; Detect the molecular weight of described cross-linked polymer gel more than 4,000,000; (5), under the state keeping moderate-speed mixer, in above-mentioned cross-linked polymer gel, slowly add beta-D-mannuronic acid (M), continue moderate-speed mixer after adding 10 minutes, and adjust ph is 7 ~ 7.5; (6) in step product (5), add Composite portland cement slurry and mix type microfibre, moderate-speed mixer more than 15 minutes is until mix; (7) in step product (6), add ammonium dihydrogen phosphate (ADP), moderate-speed mixer 10 minutes, obtain middle-deep well cross-linked polymer gel sealing agent; (8) continue moderate-speed mixer after 10 minutes, start drilling fluid pump by above-mentioned middle-deep well cross-linked polymer gel sealing agent through Drill-pipe conveyed to drop ply, drilling fluid pump delivery is 1.5m3/min, and continus convergence 60 ~ 90m3; (9) continue to adopt drilling fluid pump to carry drilling fluid in drilling rod, until the middle-deep well cross-linked polymer gel sealing agent in drilling rod is all replaced with drilling fluid, then close drilling fluid pump and carry out leaving standstill the leak stopping 60 minutes that builds the pressure; (10) reopen drilling fluid pump and carry out pressure testing, if do not occur after pressure testing, bottom pressure rises, then repeat step after closing drilling fluid pump (1) extremely (9); (11) if occur after pressure testing, bottom pressure rises, then close drilling fluid pump and continue standing building the pressure 20 minutes, and then startup drilling fluid pump, and control drilling fluid pump delivery is 0.2 ~ 0.3m3/min, middle-deep well cross-linked polymer gel sealing agent between well and drilling rod is all replaced with drilling fluid, and after drilling fluid returns out from well head, closedown drilling fluid pump proceeds to leave standstill and builds the pressure 12 hours; Leave standstill the 12 hours periods that build the pressure every 30 minutes, supplement a drilling fluid to down-hole, again return out stopping from well head to drilling fluid; (12) open drilling fluid pump and carry out the test of leak stopping pressure-bearing, when normal value before the pump pressure of drilling fluid pump returns to leakage, proceed operation of drilling.
Relative to prior art, the present invention achieves following beneficial effect: 1. purified cotton sodium salt provides the cellulose of cross-linking reaction, and acrylamide plays bridge formation suction-operated, cellulose is flocculated, is cross-linked with each other.Ammonium persulfate causes cross-linking reaction, makes fiber destarch simultaneously; Before adding ammonium persulfate, pass into nitrogen, guarantee reaction environment anaerobic, avoid cellulose to rise in cross-linking process sticky, affect the molecular weight of final cross-linking products; Back flow reaction 1.5h guarantees under the effect of cross-linking reaction initator, and purified cotton fibre element builds bridge that adsorbing acrylamide is full cross-linked, copolyreaction with can provide, and makes cellulose molecular chain elongated, and molecular weight sharp increase.Cerous sulfate further between cellulose initiated and acrylamide, cellulose and acrylamide be by between ammonium persulfate copolymerzation with cross-linking product and mutual grafting between cellulose and copolymerzation with cross-linking reactant, make the molecular weight of the high molecular polymer of generation larger, strand has more side chain, there is provided more side chain for forming gel after formation under the effect of thixotropic agent, the gel strength of formation is higher.Reaction mechanism is:
。2. the molecular weight of cross-linked polymer gel illustrate more than 4,000,000 crosslinked, copolymerization, graft reaction very abundant, for the intensity forming " block wall " is given security.3. after adding beta-D-mannuronic acid (M) in cross-linked polymer gel, the amide groups in the sodium ion of beta-D-mannuronic acid (M) and cross-linked polymer gel exchanges, and carries out ionic compartmentation at carboxyl position, thus gelling reaction occurs, and forms blob of viscose.Beta-D-mannuronic acid (M) viscosity when pH reduces can increase, and there is viscosity thixotropic, have certain alkali resistance when pH is 6.7, and when pH is 7 ~ 7.5, the blob of viscose of formation has better shear thinning behavior, for pumping provides advantage.4. Composite portland cement slurry can provide intensity and the anti-pressure ability of blob of viscose; After cross-linked polymer gel gelling, if wherein do not have enough bridge particles, the blob of viscose intensity of formation only can reach 1 ~ 2MPa, can not meet the pressurization sealing requirement of middle-deep well; Mix the effect that type microfibre can play bridge particle, synthetic fibers and natural fiber is adopted to be cross-linked to form the net high-polymer polymer of mutual winding, under the high-temperature condition of down-hole, high molecular polymerization frozen glue slowly starts gelling, after complete gelation, the intensity forming blob of viscose can reach 15MPa, the high temperature of more than 140 DEG C can be resisted, the leak stopping needs of the middle-deep well of well depth 4000 ~ 5000m can be met.The adding proportion mixing type microfibre in the present invention makes sealing agent have the highest intensity, if continue to improve the weight ratio mixing type microfibre, can disturb the chemical crosslinking effect of gel chemistries material on the contrary, can reduce the bearing capacity of its leak stopping on the contrary.5. the ammonium dihydrogen phosphate (ADP) of ratio of the present invention is added, gelling can be controlled in suitable time range, both ensured before gelling, sealing agent can be pumped to drop ply, replacing in drilling rod and well can be completed again starch before gelling, there is gelling in time after sealing agent can also be made to arrive drop ply, make leak stopping slurries stop living at drop ply.6. adopt discharge capacity to be 1.5m3/min during pumping sealing agent, both avoid the excessive formation fracture that leakage occurs that causes of discharge capacity to expand further under huge discharge, drop ply of all can being made a gift to someone by sealing agent before initial set again; For the situation of most of little leakage and middle leakage, play the glue time in conjunction with gelling leak stopping, carry 60 ~ 90m3 the most appropriate at every turn.7., after sealing agent conveying drop ply, first adopt drilling fluid to complete replacing in drilling rod and starch, then enter standing building the pressure, prevent cross-linked polymer gel from drilling rod, gelling occurring, the central duct of blocking drilling rod.8. pressure testing not now bottom pressure rising, illustrates leak stopping failure, needs again to carry out leak stopping; Occur after pressure testing that bottom pressure rises, explanation leak stopping success, need to leave standstill and build the pressure 20 minutes, after making the rising 1 ~ 2MPa of drop ply blob of viscose intensity, then complete well for slurry, prevent well by drilling rod locking, the displacement control of drilling fluid pump is at 0.2 ~ 0.3m3/min, prevent from the excessive blob of viscose just formed drop ply of discharge capacity from being formed to impact and fragmentation, produce adverse influence, cause leak stopping failure.9. well is for after slurry completes, and continues to leave standstill to build the pressure 12 hours, waits for that blob of viscose reaches predetermined intensity, then carries out pressure-bearing test, when the pump pressure of drilling fluid pump returns to the normal value before leakage, illustrates that leak stopping completely successfully, can proceed operation of drilling.
As preferred version of the present invention, step (1) in raw material components and weight content as follows, purified cotton sodium salt solution: 120 parts, acrylamide: 75 parts, ammonium persulfate: 13 parts, cerous sulfate: 2 parts, beta-D-mannuronic acid (M): 4 parts, ammonium dihydrogen phosphate (ADP): 1 part, Composite portland cement slurry: 100 parts and mix type microfibre: 150 parts.
As preferred version of the present invention, step (1) in raw material components and weight content as follows, purified cotton sodium salt solution: 120 parts, acrylamide: 80 parts, ammonium persulfate: 15 parts, cerous sulfate: 3 parts, beta-D-mannuronic acid (M): 4 parts, ammonium dihydrogen phosphate (ADP): 1.2 parts, Composite portland cement slurry: 100 parts and mix type microfibre: 180 parts.
As preferred version of the present invention, step (1) in raw material components and weight content as follows, purified cotton sodium salt solution: 120 parts, acrylamide: 85 parts, ammonium persulfate: 17 parts, cerous sulfate: 5 parts, beta-D-mannuronic acid (M): 4 parts, ammonium dihydrogen phosphate (ADP): 1.5 parts, Composite portland cement slurry: 100 parts and mix type microfibre: 200 parts.
As preferred version of the present invention, the preparation method of described purified cotton sodium salt is as follows: 1. prepare the cotton fiber degree of polymerization be 12000 ~ 14000 purified cotton and concentration expressed in percentage by weight be the sodium hydroxide solution of 17.5 ~ 18%, the weight ratio of purified cotton and sodium hydroxide solution is 5:2; 2. purified cotton is dropped in sodium hydroxide solution, stir at 60 DEG C and react more than 1.5 hours, until present uniform white suspension emulsion, obtain purified cotton sodium salt just solution; 3. carry out ultrasonic micro-vibration 30 minutes to the first solution of purified cotton sodium salt, obtain purified cotton sodium salt solution, supersonic frequency is 20kHz ~ 30kHz, and ultrasonication intensity is 2.0W/cm2 ~ 3.0W/cm2.Purified cotton and NaOH react and generate purified cotton sodium salt, and what make purified cotton inside obtains abundant moistening expansion, improves the reactivity of purified cotton, is conducive to further cross-linking reaction.Ultrasonic process can improve the molecule link Zhi Chengdu of purified cotton sodium salt, for follow-up to provide with crosslinking agent more meets Zhi Duan.Reaction mechanism is:
。
As preferred version of the present invention, described in mix type microfibre and evenly mixed by calcium carbonate crystal whisker and organic microfiber and form, the mixing ratio of described calcium carbonate crystal whisker and organic microfiber is 0.8:1.Calcium carbonate crystal whisker and organic microfiber are dispersed in cross-linked polymer gel, are cross-linked to form with the high molecular polymer in cross-linked polymer gel the net high-polymer polymer be mutually wound around.Calcium carbonate crystal whisker provides physical supporting role for forming " block wall ", and its intensity is significantly promoted; Organic microfiber and calcium carbonate crystal whisker are wound around mutually, for " block wall " formed provides physical supporting role, its intensity are significantly promoted; Meanwhile, " block wall " is added by intensity when deforming under strata pressure effect.
As the further preferred version of the present invention, the length of described calcium carbonate crystal whisker 20 ~ 30 μm, diameter 0.5 ~ 1 μm, pH value 9.0 ~ 9.5, modulus of elasticity is 410 ~ 710GPa and tensile strength is not less than 2.058GPa; Described organic microfiber is made up of polyester fiber and polypropylene fibre, and the weight of polyester fiber and polypropylene fibre is 7:3; The diameter of described polyester fiber 20 ~ 25 μm, length 6 ~ 9mm, elongation at break >=15%, tensile strength >=960MPa and modulus of elasticity >=9000MPa; The length of described polypropylene fibre is 10 ~ 20mm, filament number≤2.2dtex, tensile strength >=660MPa, modulus of elasticity >=350MPa.Polypropylene fibre can improve the intensity of " block wall ", improves " block wall " rebound performance after compressive deformation.Polyester fiber can improve the anti-fatigue performance of " block wall ", cracking resistance and high temperature stability performance, effectively can improve the tension of " block wall ", resistance to compression, anti-shearing and impact strength, makes up the deficiency of polypropylene fibre in heat-resisting and ageing-resistant.
As the further preferred version of the present invention, described polyester fiber and polypropylene fibre all soak 3 hours at 60 DEG C in hydrophilic finishing agent.Due to polyester fiber and polypropylene fibre compound with regular structure but hydrophily is poor, be difficult to be uniformly dispersed in cross-linked polymer gel, hydrophilic finishing agent is adopted to carry out surface modification treatment to polyester fiber and polypropylene fibre, its hydrophilicity can be improved, be conducive to them dispersed in polymer gel, make " block wall " structure and the even intensity of formation.
Detailed description of the invention
Embodiment one
A kind of method adopting cross-linked polymer gel sealing agent to carry out middle-deep well leak stopping of the present invention, in turn includes the following steps:
(1) following component and weight content prepare raw material, purified cotton sodium salt solution: 120 parts, acrylamide: 75 parts, ammonium persulfate: 13 parts, cerous sulfate: 2 parts, beta-D-mannuronic acid (M): 4 parts, ammonium dihydrogen phosphate (ADP): 1 part, Composite portland cement slurry: 100 parts and mix type microfibre: 150 parts; The water/binder ratio of described Composite portland cement slurry is 0.44;
(2) add acrylamide in purified cotton sodium salt solution, carry out high-speed stirred with the rotating speed of 400r/min and within 10 minutes, make both fully mixing, then carry out moderate-speed mixer with the rotating speed of 300r/min, be heated to 60 DEG C while moderate-speed mixer and keep constant temperature;
(3) continue to pass into nitrogen in step product (2) and reaction vessel, pass into nitrogen and at remaining on constant temperature 60 DEG C, slowly add ammonium persulfate particle at maintenance moderate-speed mixer after 3 minutes, reaction is until after particle disappears, continue back flow reaction 1.5 hours;
(4) temperature be increased to 80 DEG C and keep constant temperature, under maintenance moderate-speed mixer, slowly add cerous sulfate particle, then the charge door of off-response container, promote the charge of nitrogen, keep the pressure in reaction vessel to be 1.3MPa, back flow reaction 3 hours, until reactant presents white emulsion shape, obtains cross-linked polymer gel; Detect the molecular weight of described cross-linked polymer gel more than 4,000,000;
(5), under the state keeping moderate-speed mixer, in above-mentioned cross-linked polymer gel, slowly add beta-D-mannuronic acid (M), continue moderate-speed mixer after adding 10 minutes, and adjust ph is 7;
(6) in step product (5), add Composite portland cement slurry and mix type microfibre, moderate-speed mixer more than 15 minutes is until mix;
(7) in step product (6), add ammonium dihydrogen phosphate (ADP), moderate-speed mixer 10 minutes, obtain middle-deep well cross-linked polymer gel sealing agent;
(8) continue moderate-speed mixer after 10 minutes, start drilling fluid pump by above-mentioned middle-deep well cross-linked polymer gel sealing agent through Drill-pipe conveyed to drop ply, drilling fluid pump delivery is 1.5m3/min, and continus convergence 60m3;
(9) continue to adopt drilling fluid pump to carry drilling fluid in drilling rod, until the middle-deep well cross-linked polymer gel sealing agent in drilling rod is all replaced with drilling fluid, then close drilling fluid pump and carry out leaving standstill the leak stopping 60 minutes that builds the pressure;
(10) reopen drilling fluid pump and carry out pressure testing, if do not occur after pressure testing, bottom pressure rises, then repeat step after closing drilling fluid pump (1) extremely (9);
(11) if occur after pressure testing, bottom pressure rises, then close drilling fluid pump and continue standing building the pressure 20 minutes, and then startup drilling fluid pump, and control drilling fluid pump delivery is 0.2m3/min, middle-deep well cross-linked polymer gel sealing agent between well and drilling rod is all replaced with drilling fluid, and after drilling fluid returns out from well head, closedown drilling fluid pump proceeds to leave standstill and builds the pressure 12 hours; Leave standstill the 12 hours periods that build the pressure every 30 minutes, supplement a drilling fluid to down-hole, again return out stopping from well head to drilling fluid;
(12) open drilling fluid pump and carry out the test of leak stopping pressure-bearing, when normal value before the pump pressure of drilling fluid pump returns to leakage, proceed operation of drilling.
Embodiment two
A kind of method adopting cross-linked polymer gel sealing agent to carry out middle-deep well leak stopping of the present invention, in turn includes the following steps:
(1) following component and weight content prepare raw material, purified cotton sodium salt solution: 120 parts, acrylamide: 80 parts, ammonium persulfate: 15 parts, cerous sulfate: 3 parts, beta-D-mannuronic acid (M): 4 parts, ammonium dihydrogen phosphate (ADP): 1.2 parts, Composite portland cement slurry: 100 parts and mix type microfibre: 180 parts; The water/binder ratio of described Composite portland cement slurry is 0.44;
(2) add acrylamide in purified cotton sodium salt solution, carry out high-speed stirred with the rotating speed of 400r/min and within 10 minutes, make both fully mixing, then carry out moderate-speed mixer with the rotating speed of 300r/min, be heated to 60 DEG C while moderate-speed mixer and keep constant temperature;
(3) continue to pass into nitrogen in step product (2) and reaction vessel, pass into nitrogen and at remaining on constant temperature 60 DEG C, slowly add ammonium persulfate particle at maintenance moderate-speed mixer after 3 minutes, reaction is until after particle disappears, continue back flow reaction 1.5 hours;
(4) temperature be increased to 80 DEG C and keep constant temperature, under maintenance moderate-speed mixer, slowly add cerous sulfate particle, then the charge door of off-response container, promote the charge of nitrogen, keep the pressure in reaction vessel to be 1.3MPa, back flow reaction 3.5 hours, until reactant presents white emulsion shape, obtains cross-linked polymer gel; Detect the molecular weight of described cross-linked polymer gel more than 4,000,000;
(5), under the state keeping moderate-speed mixer, in above-mentioned cross-linked polymer gel, slowly add beta-D-mannuronic acid (M), continue moderate-speed mixer after adding 10 minutes, and adjust ph is 7.5;
(6) in step product (5), add Composite portland cement slurry and mix type microfibre, moderate-speed mixer more than 15 minutes is until mix;
(7) in step product (6), add ammonium dihydrogen phosphate (ADP), moderate-speed mixer 10 minutes, obtain middle-deep well cross-linked polymer gel sealing agent;
(8) continue moderate-speed mixer after 10 minutes, start drilling fluid pump by above-mentioned middle-deep well cross-linked polymer gel sealing agent through Drill-pipe conveyed to drop ply, drilling fluid pump delivery is 1.5m3/min, and continus convergence 70m3;
(9) continue to adopt drilling fluid pump to carry drilling fluid in drilling rod, until the middle-deep well cross-linked polymer gel sealing agent in drilling rod is all replaced with drilling fluid, then close drilling fluid pump and carry out leaving standstill the leak stopping 60 minutes that builds the pressure;
(10) reopen drilling fluid pump and carry out pressure testing, if do not occur after pressure testing, bottom pressure rises, then repeat step after closing drilling fluid pump (1) extremely (9);
(11) if occur after pressure testing, bottom pressure rises, then close drilling fluid pump and continue standing building the pressure 20 minutes, and then startup drilling fluid pump, and control drilling fluid pump delivery is 0.25m3/min, middle-deep well cross-linked polymer gel sealing agent between well and drilling rod is all replaced with drilling fluid, and after drilling fluid returns out from well head, closedown drilling fluid pump proceeds to leave standstill and builds the pressure 12 hours; Leave standstill the 12 hours periods that build the pressure every 30 minutes, supplement a drilling fluid to down-hole, again return out stopping from well head to drilling fluid;
(12) open drilling fluid pump and carry out the test of leak stopping pressure-bearing, when normal value before the pump pressure of drilling fluid pump returns to leakage, proceed operation of drilling.
Embodiment three
A kind of method adopting cross-linked polymer gel sealing agent to carry out middle-deep well leak stopping of the present invention, in turn includes the following steps:
(1) following component and weight content prepare raw material, purified cotton sodium salt solution: 120 parts, acrylamide: 85 parts, ammonium persulfate: 17 parts, cerous sulfate: 5 parts, beta-D-mannuronic acid (M): 4 parts, ammonium dihydrogen phosphate (ADP): 1.5 parts, Composite portland cement slurry: 100 parts and mix type microfibre: 200 parts; The water/binder ratio of described Composite portland cement slurry is 0.44;
(2) add acrylamide in purified cotton sodium salt solution, carry out high-speed stirred with the rotating speed of 400r/min and within 10 minutes, make both fully mixing, then carry out moderate-speed mixer with the rotating speed of 300r/min, be heated to 60 DEG C while moderate-speed mixer and keep constant temperature;
(3) continue to pass into nitrogen in step product (2) and reaction vessel, pass into nitrogen and at remaining on constant temperature 60 DEG C, slowly add ammonium persulfate particle at maintenance moderate-speed mixer after 3 minutes, reaction is until after particle disappears, continue back flow reaction 1.5 hours;
(4) temperature be increased to 80 DEG C and keep constant temperature, under maintenance moderate-speed mixer, slowly add cerous sulfate particle, then the charge door of off-response container, promote the charge of nitrogen, keep the pressure in reaction vessel to be 1.3MPa, back flow reaction 3.5 hours, until reactant presents white emulsion shape, obtains cross-linked polymer gel; Detect the molecular weight of described cross-linked polymer gel more than 4,000,000;
(5), under the state keeping moderate-speed mixer, in above-mentioned cross-linked polymer gel, slowly add beta-D-mannuronic acid (M), continue moderate-speed mixer after adding 10 minutes, and adjust ph 7.5;
(6) in step product (5), add Composite portland cement slurry and mix type microfibre, moderate-speed mixer more than 15 minutes is until mix;
(7) in step product (6), add ammonium dihydrogen phosphate (ADP), moderate-speed mixer 10 minutes, obtain middle-deep well cross-linked polymer gel sealing agent;
(8) continue moderate-speed mixer after 10 minutes, start drilling fluid pump by above-mentioned middle-deep well cross-linked polymer gel sealing agent through Drill-pipe conveyed to drop ply, drilling fluid pump delivery is 1.5m3/min, and continus convergence 90m3;
(9) continue to adopt drilling fluid pump to carry drilling fluid in drilling rod, until the middle-deep well cross-linked polymer gel sealing agent in drilling rod is all replaced with drilling fluid, then close drilling fluid pump and carry out leaving standstill the leak stopping 60 minutes that builds the pressure;
(10) reopen drilling fluid pump and carry out pressure testing, if do not occur after pressure testing, bottom pressure rises, then repeat step after closing drilling fluid pump (1) extremely (9);
(11) if occur after pressure testing, bottom pressure rises, then close drilling fluid pump and continue standing building the pressure 20 minutes, and then startup drilling fluid pump, and control drilling fluid pump delivery is 0.3m3/min, middle-deep well cross-linked polymer gel sealing agent between well and drilling rod is all replaced with drilling fluid, and after drilling fluid returns out from well head, closedown drilling fluid pump proceeds to leave standstill and builds the pressure 12 hours; Leave standstill the 12 hours periods that build the pressure every 30 minutes, supplement a drilling fluid to down-hole, again return out stopping from well head to drilling fluid;
(12) open drilling fluid pump and carry out the test of leak stopping pressure-bearing, when normal value before the pump pressure of drilling fluid pump returns to leakage, proceed operation of drilling.
One, initial set, final setting time test are carried out to the sealing agent of the embodiment of the present invention two
Standard with reference to GB/T50080-2002 is tested sealing agent initial set at different temperatures and final setting time, and the initial set of record sealing agent and final setting time are as table 1.
Table 1
。
As can be seen from Table 1, at 30 DEG C, the sealing agent initial setting time can reach 135 minutes, and final setting time can reach 420 minutes, but along with the raising of temperature, gelling time shortens fast.When wherein reaching 60 DEG C, the initial setting time is 21 minutes, and when reaching 120 DEG C, the initial setting time is only 3min, substantially belongs to and has started glue instantaneously, but becomes steady higher than final setting time after 60 DEG C.
Two, slit formation plugging test is carried out to the sealing agent of the embodiment of the present invention one to embodiment three
Test is pressed SY/T5840-2007 " People's Republic of China's oil and gas industry standard well liquid bridge joint loss circulation material Experimental Method in Laboratory " and is performed.With the DLM-01 type sealing Analog Device that Bohai Sea drilling project institute produces, can heat to 150 DEG C, can 7.0MPa be forced into.Select vertical slit die plate, thickness 5mm, stitches high 50mm, and stitching wide is 3mm.
The sealing agent heating-up temperature of embodiment one is 80 DEG C, the sealing agent heating-up temperature of embodiment two is 120 DEG C, the sealing agent heating-up temperature of embodiment three is 140 DEG C, sealing agent 2000mL of the present invention is injected in test chamber, sealing agent enters rapidly template gap and flows out from the lower part outlet of device, record sealing agent stops the delivery time, and be blocking time, result of the test gathers as following table 2.
Table 2
。
After above shutoff success, leave standstill 4 hours respectively, then pour into clear water, then embodiment one is still heated to 80 DEG C and keeps constant temperature, and embodiment two is still heated to 120 DEG C and keeps constant temperature, embodiment three is still heated to 140 DEG C and keeps constant temperature, carry out plugging test under being forced into different pressures, under each pressure, maintain 300 seconds, observe leakage situation, judge plugging effect, result of the test is as shown in table 3.
Table 3
。
Three, osmosis type plugging test is carried out to the sealing agent of the embodiment of the present invention one to embodiment three
Test is pressed SY/T5840-2007 " People's Republic of China's oil and gas industry standard well liquid bridge joint loss circulation material Experimental Method in Laboratory " and is performed.With the DLM-01 type sealing Analog Device that Bohai Sea drilling project institute produces, the filter area 2289mm2 of casting bed, casting bed thickness 35mm.
The sealing agent heating-up temperature of embodiment one is 80 DEG C, the sealing agent heating-up temperature of embodiment two is 120 DEG C, the sealing agent heating-up temperature of embodiment three is 140 DEG C, sealing agent 2000mL of the present invention is injected in test chamber, sealing agent enters casting bed rapidly and flows out from the lower part outlet of device, record sealing agent stops the delivery time, and be blocking time, result of the test gathers as shown in table 4 below.
Table 4
。
Embodiment three does not have sealing agent to flow out at 140 DEG C, and sealing agent infiltrates casting bed 3/4 and is shutoff success.
After above shutoff success, leave standstill 4 hours respectively, then pour into clear water, then embodiment one is still heated to 80 DEG C and keeps constant temperature, and embodiment two is still heated to 120 DEG C and keeps constant temperature, embodiment three is still heated to 140 DEG C and keeps constant temperature, carry out plugging test under being forced into different pressures, under each pressure, maintain 300 seconds, observe leakage situation, judge plugging effect, result of the test is as shown in table 5.
Table 5
。
Four, ultimate compressive ability test is carried out to the blob of viscose that the sealing agent of the embodiment of the present invention two is formed
The sealing agent getting the embodiment of the present invention two is gelling 4 hours and 12 hours respectively at 140 DEG C, carries out mechanical pressurization respectively to the blob of viscose obtained, and tests to cause its structure and to be badly deformed loose force value.Result of the test is as shown in table 6.
Table 6
。
Can find out, along with the increase of gelling time, the blob of viscose compressive strength of formation increases, the highest can resistance to compression 15MPa.
The present invention purified cotton used be evenly loose, without the White Flocculus of the impurity such as wood chip, bamboo bits, silt, greasy dirt, metal object.Its raw material is cotton linter, and main chemical compositions is cellulose, lignin and hemicellulose.It is made up of carbon, hydrogen, oxygen three kinds of elements, the mass ratio of its composition: carbon 44.4%, hydrogen 6.17%, oxygen 49.39%.The general formula of purified cotton is: (C6H1005) n, n represents the cellulosic degree of polymerization, and the degree of polymerization is generally 12000 ~ 14000.
It is the Composite portland cement (P.C) that Beijing Jinyu cement Trade Co., Ltd. produces that Composite portland cement of the present invention starches Composite portland cement used.
The present invention's hydrophilic finishing agent used is the TD-5512 type durable hydrophilic finishing agent that Shenzhen Tianding Fine Chemical Engineering Manufacturing Co., Ltd produces.
The foregoing is only the better possible embodiments of the present invention, non-ly therefore limit to scope of patent protection of the present invention.In addition to the implementation, the present invention can also have other embodiments.All employings are equal to the technical scheme of replacement or equivalent transformation formation, all drop in the protection domain of application claims.The technical characteristic that the present invention does not describe to the greatest extent can pass through or adopt existing techniques in realizing, does not repeat them here.
Claims (8)
1. adopt cross-linked polymer gel sealing agent to carry out a method for middle-deep well leak stopping, it is characterized in that, in turn include the following steps:
(1) prepare raw material by following component and weight content, purified cotton sodium salt solution: 120 parts, acrylamide: (75 ~ 85) part, ammonium persulfate: (13 ~ 17) part, cerous sulfate: (2 ~ 5) part, beta-D-mannuronic acid (M): 4 parts, ammonium dihydrogen phosphate (ADP): (1 ~ 1.5) part, Composite portland cement slurry: 100 parts and mix type microfibre: (150 ~ 200) part; The water/binder ratio of described Composite portland cement slurry is 0.44;
(2) in purified cotton sodium salt solution, add acrylamide, carry out high-speed stirred with the rotating speed of 400r/min and within 10 minutes, make both fully mixing, then carry out moderate-speed mixer with the rotating speed of 300r/min, be heated to 60 DEG C while moderate-speed mixer and keep constant temperature;
(3) continue to pass into nitrogen in step product (2) and reaction vessel, pass into nitrogen and at remaining on constant temperature 60 DEG C, slowly add ammonium persulfate particle at maintenance moderate-speed mixer after 3 minutes, reaction is until after particle disappears, continue back flow reaction 1.5 hours;
(4) temperature be increased to 80 DEG C and keep constant temperature, under maintenance moderate-speed mixer, slowly add cerous sulfate particle, then the charge door of off-response container, promote the charge of nitrogen, keep the pressure in reaction vessel to be 1.3MPa, back flow reaction more than 3 hours, until reactant presents white emulsion shape, obtains cross-linked polymer gel; Detect the molecular weight of described cross-linked polymer gel more than 4,000,000;
(5), under the state keeping moderate-speed mixer, in above-mentioned cross-linked polymer gel, slowly add beta-D-mannuronic acid (M), continue moderate-speed mixer after adding 10 minutes, and adjust ph is 7 ~ 7.5;
(6) in step product (5), add Composite portland cement slurry and mix type microfibre, moderate-speed mixer more than 15 minutes is until mix;
(7) in step product (6), add ammonium dihydrogen phosphate (ADP), moderate-speed mixer 10 minutes, obtain middle-deep well cross-linked polymer gel sealing agent;
(8) continue moderate-speed mixer after 10 minutes, start drilling fluid pump by above-mentioned middle-deep well cross-linked polymer gel sealing agent through Drill-pipe conveyed to drop ply, drilling fluid pump delivery is 1.5m3/min, and continus convergence 60 ~ 90m3;
(9) continue to adopt drilling fluid pump to carry drilling fluid in drilling rod, until the middle-deep well cross-linked polymer gel sealing agent in drilling rod is all replaced with drilling fluid, then close drilling fluid pump and carry out leaving standstill the leak stopping 60 minutes that builds the pressure;
(10) reopen drilling fluid pump and carry out pressure testing, if do not occur after pressure testing, bottom pressure rises, then repeat step after closing drilling fluid pump (1) extremely (9);
(11) if occur after pressure testing, bottom pressure rises, then close drilling fluid pump and continue standing building the pressure 20 minutes, and then startup drilling fluid pump, and control drilling fluid pump delivery is 0.2 ~ 0.3m3/min, middle-deep well cross-linked polymer gel sealing agent between well and drilling rod is all replaced with drilling fluid, and after drilling fluid returns out from well head, closedown drilling fluid pump proceeds to leave standstill and builds the pressure 12 hours; Leave standstill the 12 hours periods that build the pressure every 30 minutes, supplement a drilling fluid to down-hole, again return out stopping from well head to drilling fluid;
(12) open drilling fluid pump and carry out the test of leak stopping pressure-bearing, when normal value before the pump pressure of drilling fluid pump returns to leakage, proceed operation of drilling.
2. employing cross-linked polymer gel sealing agent according to claim 1 carries out the method for middle-deep well leak stopping, it is characterized in that, step (1) in raw material components and weight content as follows, purified cotton sodium salt solution: 120 parts, acrylamide: 75 parts, ammonium persulfate: 13 parts, cerous sulfate: 2 parts, beta-D-mannuronic acid (M): 4 parts, ammonium dihydrogen phosphate (ADP): 1 part, Composite portland cement slurry: 100 parts and mix type microfibre: 150 parts.
3. employing cross-linked polymer gel sealing agent according to claim 1 carries out the method for middle-deep well leak stopping, it is characterized in that, step (1) in raw material components and weight content as follows, purified cotton sodium salt solution: 120 parts, acrylamide: 80 parts, ammonium persulfate: 15 parts, cerous sulfate: 3 parts, beta-D-mannuronic acid (M): 4 parts, ammonium dihydrogen phosphate (ADP): 1.2 parts, Composite portland cement slurry: 100 parts and mix type microfibre: 180 parts.
4. employing cross-linked polymer gel sealing agent according to claim 1 carries out the method for middle-deep well leak stopping, it is characterized in that, step (1) in raw material components and weight content as follows, purified cotton sodium salt solution: 120 parts, acrylamide: 85 parts, ammonium persulfate: 17 parts, cerous sulfate: 5 parts, beta-D-mannuronic acid (M): 4 parts, ammonium dihydrogen phosphate (ADP): 1.5 parts, Composite portland cement slurry: 100 parts and mix type microfibre: 200 parts.
5. employing cross-linked polymer gel sealing agent according to claim 1 carries out the method for middle-deep well leak stopping, it is characterized in that, the preparation method of described purified cotton sodium salt is as follows: 1. prepare the cotton fiber degree of polymerization be 12000 ~ 14000 purified cotton and concentration expressed in percentage by weight be the sodium hydroxide solution of 17.5 ~ 18%, the weight ratio of purified cotton and sodium hydroxide solution is 5:2; 2. purified cotton is dropped in sodium hydroxide solution, stir at 60 DEG C and react more than 1.5 hours, until present uniform white suspension emulsion, obtain purified cotton sodium salt just solution; 3. carry out ultrasonic micro-vibration 30 minutes to the first solution of purified cotton sodium salt, obtain purified cotton sodium salt solution, supersonic frequency is 20kHz ~ 30kHz, and ultrasonication intensity is 2.0W/cm2 ~ 3.0W/cm2.
6. employing cross-linked polymer gel sealing agent according to claim 1 carries out the method for middle-deep well leak stopping, it is characterized in that, the described type microfibre that mixes evenly is mixed by calcium carbonate crystal whisker and organic microfiber and forms, and the mixing ratio of calcium carbonate crystal whisker and organic microfiber is 0.8:1.
7. employing cross-linked polymer gel sealing agent according to claim 6 carries out the method for middle-deep well leak stopping, it is characterized in that, the length of described calcium carbonate crystal whisker 20 ~ 30 μm, diameter 0.5 ~ 1 μm, pH value 9.0 ~ 9.5, modulus of elasticity is 410 ~ 710GPa and tensile strength is not less than 2.058GPa; Described organic microfiber is made up of polyester fiber and polypropylene fibre, and the weight of polyester fiber and polypropylene fibre is 7:3; The diameter of described polyester fiber 20 ~ 25 μm, length 6 ~ 9mm, elongation at break >=15%, tensile strength >=960MPa and modulus of elasticity >=9000MPa; The length of described polypropylene fibre is 10 ~ 20mm, filament number≤2.2dtex, tensile strength >=660MPa, modulus of elasticity >=350MPa.
8. employing cross-linked polymer gel sealing agent according to claim 6 carries out the method for middle-deep well leak stopping, it is characterized in that, described polyester fiber and polypropylene fibre all soak 3 hours at 60 DEG C in hydrophilic finishing agent.
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