CN106590559A - Thickened oil thermal production channel blocking nano-composite gel - Google Patents
Thickened oil thermal production channel blocking nano-composite gel Download PDFInfo
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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
- C09K8/50—Compositions for plastering borehole walls, i.e. compositions for temporary consolidation of borehole walls
- C09K8/504—Compositions based on water or polar solvents
- C09K8/506—Compositions based on water or polar solvents containing organic compounds
- C09K8/508—Compositions based on water or polar solvents containing organic compounds macromolecular compounds
- C09K8/512—Compositions based on water or polar solvents containing organic compounds macromolecular compounds containing cross-linking agents
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- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/58—Compositions for enhanced recovery methods for obtaining hydrocarbons, i.e. for improving the mobility of the oil, e.g. displacing fluids
- C09K8/592—Compositions used in combination with generated heat, e.g. by steam injection
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- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/60—Compositions for stimulating production by acting on the underground formation
- C09K8/84—Compositions based on water or polar solvents
- C09K8/86—Compositions based on water or polar solvents containing organic compounds
- C09K8/88—Compositions based on water or polar solvents containing organic compounds macromolecular compounds
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Abstract
The invention provides thickened oil thermal production channel blocking nano-composite gel. The gel comprises, by weight, 0.4-0.5 part of a main agent, 0.1-0.3 part of an organic chromium cross-linking agent, 0.1-0.5 part of an inorganic chromium cross-linking agent, 1-1.5 parts of a reinforcer, 0.2-0.4 part of a stabilizer, 0.1-0.5 part of a dehydration inhibitor and the balance water, wherein the sum of the weight parts of the components is 100. The main agent refers to partially hydrolyzed polyacrylamide. The organic chromium cross-linking agent refers to malonic acid chromium. The inorganic chromium cross-linking agent is sodium bichromate, and the ratio of the sodium bichromate to sodium sulfite is 1:1-3. The reinforcer is silica soil nano particles, and the ratio of the silica soil nano particles to amino silane is 2-5:1. The stabilizer is thiourea. The dehydration inhibitor is one or a combination of polyphosphates and phosphoro-amidate. The ratio of the polyphosphates to the phosphoro-amidate is 1-4:1 during combination. According to the thickened oil thermal production channel blocking nano-composite gel provided by the invention, the gel forming temperature can be selected to be 50-180 DEG C, the gel forming time is adjustable within the range of 12-60h, gel strength is high, viscoelasticity is good, temperature resistance water-holding power is high, no dehydration phenomenon happens after ageing for 3 months under the temperature condition of 180 DEG C, and steam channeling caused in the thickened oil thermal production process can be blocked selectively.
Description
Technical field
The present invention relates to a kind of envelope alters agent, the specifically nano combined frozen glue of heavy oil thermal recovery fleeing proof.
Background technology
With using being allowed to increasingly in short supply, the exploitation of viscous crude can then alleviate high-quality stone with utilizing for a large amount of exploitations of petroleum resources
The scarcity of oily resource.The density of viscous crude is big, and viscosity high fluidity is poor, and exploitation difficulty is high, is mainly exploited using thermal recovery mode at present
Viscous crude, conventional thermal process has steam soak and steam drive etc..For different viscous crude resources, by core intersection, heterogeneous body
Property etc. geologic(al) factor impact, and injection steam and formation fluid between compatibility impact, easily send out in the middle and late stage of thermal recovery
Raw channeling phenomenon.Especially when thermal recovery round increases, offtake pattern Encryption Well becomes apparent from away from reduction, channeling phenomenon, reduces steaming
The utilization ratio of vapour, Heavy Oil Thermal Recovery Effect is deteriorated.Therefore, developing effective thermal recovery envelope, to alter agent extremely urgent.
Existing thermal recovery envelope alters agent mainly grain-type water shutoff agent, cement mortar class blocking agent, high temperature foam blocking agent, emulsified asphalt envelope
Alter the types such as agent, alkali lignin/tannic extract gel plugging agent.In order to solve the poor (granular pattern of selective shut-off effect that above-mentioned blocking agent is present
Blocking agent, cement mortar class blocking agent), high temperature auxiliary agent lack (high temperature foam blocking agent), preparation condition complicated (emulsified asphalt envelope alters agent), into
The problems such as glue temperature too high (alkali lignin/tannic extract gel plugging agent), the high temperature gel plugging agent of acrylamide polymer type and its compound
Envelope is altered agent and has been come out.Chinese invention patent application prospectus CN104629697A discloses a kind of heatproof frozen glue, each group
Point mass percent is：Acrylamide/acrylyl oxy-ethyl-trimethyl salmiac copolymer 0.3%～0.5%, sodium tripolyphosphate
Or/and amido methylenephosphonic acid sodium 0.1%～0.5%, phenol 0.05%～0.15%, paraformaldehyde 0.05%～0.1%, thiourea
0.2%～0.4%, sodium malonate or/and sodium D-isoascorbate 0.05%～0.2%, balance of water, each component sum is
100%.The frozen glue gelation time is adjustable between 15～54h, at 160 DEG C aging 180 days without dehydration shrinkage phenomenon, but this
It is bright to have used aldehyde crosslinking agent, could plastic in high temperature.Chinese invention patent application prospectus CN104277802A is disclosed
A kind of high temperature resistant pluralgel envelope alters agent and preparation method thereof, and weight portion includes：The water of 85-90 parts, 0.1 part -0.5 part of height
Molecular polypropylene amide, 0.2 part -0.5 part of polyalcohols retarder regulator, 1 part -1.5 parts 30% mineral acid and 8
The water-soluble silicate of -15 parts of part, closure of the water-soluble silicate that the invention is used to steam and crude oil does not have selectivity, because
And stand in channel is altered to steam and oil flow channel is respectively provided with ponding, so as to cause blocking agent also can reduce while channeling is blocked
Crude output.
The content of the invention
The invention aims to provide heavy oil thermal recovery fleeing proof nano combined frozen glue, gelling temperature wide ranges are sealed to channeling
Stifled to have selectivity, retention ability is strong, and channeling closure can be carried out in 180 DEG C of reservoir media, is not dehydrated within aging 3 months.
For achieving the above object, the technical solution used in the present invention is：
The nano combined frozen glue of heavy oil thermal recovery fleeing proof, the frozen glue by 0.4 part～0.5 part of host, 0.1 part of organic chrome cross linker～
0.3 part, 0.1 part～0.5 part of inorganic chromium cross linker, 1 part～1.5 parts of hardening agent, 0.2 part～0.4 part of stabilizer, dehydration inhibitor
0.1 part～0.5 part, excess water composition, consumption is weight portion, and the weight portion sum of said components is 100；The host is part
Hydrolyzed polyacrylamide, the organic chrome cross linker is malonic acid chromium, and the inorganic chromium cross linker is attached most importance to sodium chromate：Sodium sulfite
=1:1～3, the hardening agent is Ludox nanoparticle：Amino silane=2～5:1, the stabilizer is reducing substanceses sulfur
Urea, the dehydration inhibitor is one of polyphosphate and amino phosphonates do or combines, polyphosphate during combination：Aminophosphonic acid
Salt=1～4:1.
In above-mentioned technical proposal, the frozen glue is by 0.5 part of host, 0.1 part～0.3 part of organic chrome cross linker, inorganic chromium
0.1 part～0.5 part of cross-linking agent, 1 part～1.2 parts of hardening agent, 0.2 part～0.4 part of stabilizer, dehydration inhibitor 0.1 part～0.2
Part, excess water composition, consumption is weight portion, and weight portion sum is 100.
In above-mentioned technical proposal, the frozen glue is by 0.5 part of host, 0.2 part～0.3 part of organic chrome cross linker, inorganic chromium
It is 0.1 part～0.4 part of cross-linking agent, 1.08 parts～1.2 parts of hardening agent, 0.2 part～0.4 part of stabilizer, 0.1 part of dehydration inhibitor, remaining
Amount water composition, consumption is weight portion, and weight portion sum is 100.
In above-mentioned technical proposal, the frozen glue is by 0.5 part of host, 0.3 part of organic chrome cross linker, inorganic chromium cross linker
0.1 part, 1.2 parts of hardening agent, 0.4 part of stabilizer, 0.1 part of dehydration inhibitor, excess water composition, consumption is weight portion, weight portion
Sum is 100.
In above-mentioned technical proposal, the frozen glue is by 0.5 part of host, 0.1 part of organic chrome cross linker, inorganic chromium cross linker
0.4 part, 1.0 parts of hardening agent, 0.3 part of stabilizer, 0.2 part of dehydration inhibitor, excess water composition, consumption is weight portion, weight portion
Sum is 100.
In above-mentioned technical proposal, the frozen glue is by 0.4 part of host, 0.1 part of organic chrome cross linker, inorganic chromium cross linker
0.4 part, 1.5 parts of hardening agent, 0.3 part of stabilizer, 0.4 part of dehydration inhibitor, excess water composition, consumption is weight portion, weight portion
Sum is 100.
In above-mentioned technical proposal, the partially hydrolyzed polyacrylamide (PHPA) be PAMA, the anion
Partially hydrolyzed polyacrylamide (PHPA) relative molecular mass is 600 × 104～1200 × 104, degree of hydrolysis is 10%～30%.
In above-mentioned technical proposal, the particle diameter of the Ludox nanoparticle is 10～25nm.
The preparation method that above-mentioned envelope alters agent is as follows：
1st, partially hydrolyzed polyacrylamide (PHPA) is fully dissolved in tap water, it is standby；By proportioning by organic chrome cross linker, nothing
Machine chromium cross linker, hardening agent, stabilizer, dehydration inhibitor and excess water mixing and stirring；By the mixing of above two solution
Stirs the plastic liquid that obtain.
2nd, will be placed in ampoule bottle into glue, with alcohol blast burner sintering seal, be placed in the baking oven of uniform temperature it is aging i.e.
Above-mentioned frozen glue is obtained, gelling temperature is optional 50 DEG C～180 DEG C, the different gelation time of different gelling temperature correspondences is final to cause
Gelation time is adjustable between 12～60h.
Compared with prior art, beneficial effects of the present invention are：
1st, optional wide temperature range during frozen glue plastic of the invention, without the need for the plastic in high temperature, while corresponding frozen glue into
The glue time is adjustable, and without the need for preheating to stratum, process is simple during thickened oil recovery, efficiency high, frozen glue can not only be used near wellbore zone
Sealing agent, the deep profile controlling in remote well area is can be used for again.
2nd, the nano-pore of whole Gel Formation homogenization intersects interpenetrating structure, and good stability, intensity is high, heatproof moisture holding capacity
By force, can in 180 DEG C of reservoir media aging 3 months not syneresis.
3rd, effect of the frozen glue to the selective closure of channeling, will not block oil flow channel, it is ensured that heavy oil production.
Specific embodiment
It is easy to more clearly understand the present invention, now specific embodiments of the present invention is explained in detail, but this
Bright protection domain is not limited to this.
The nano combined frozen glue of heavy oil thermal recovery fleeing proof of the present invention, is a kind of super steady frozen glue of nano particle reinforced polymer, should
Frozen glue is by 0.4 part～0.5 part of host, 0.1 part～0.3 part of organic chrome cross linker, 0.1 part～0.5 part of inorganic chromium cross linker, reinforcing
1 part～1.5 parts of agent, 0.2 part～0.4 part of stabilizer, 0.1 part～0.5 part of dehydration inhibitor, excess water composition, consumption is weight
Part, the weight portion sum of said components is 100；The host is partially hydrolyzed polyacrylamide (PHPA), and the organic chrome cross linker is
Malonic acid chromium, the inorganic chromium cross linker is attached most importance to sodium chromate：Sodium sulfite=1:1～3, the hardening agent is Ludox nanoparticle
Son：Amino silane=2～5:1, the stabilizer is reducing substanceses thiourea, and the dehydration inhibitor is polyphosphate and ammonia
One of base phosphonate or combination, polyphosphate during combination：Amino phosphonates do=1～4:1.
The frozen glue is by 0.5 part of host, 0.1 part～0.3 part of organic chrome cross linker, inorganic chromium cross linker 0.1 part～0.5
Part, 1 part～1.2 parts of hardening agent, 0.2 part～0.4 part of stabilizer, 0.1 part～0.2 part of dehydration inhibitor, excess water composition, consumption
For weight portion, weight portion sum is 100.
The frozen glue is by 0.5 part of host, 0.2 part～0.3 part of organic chrome cross linker, inorganic chromium cross linker 0.1 part～0.4
Part, 1.08 parts～1.2 parts of hardening agent, 0.2 part～0.4 part of stabilizer, 0.1 part of dehydration inhibitor, excess water composition, consumption is attached most importance to
Amount part, weight portion sum is 100.
The frozen glue by 0.5 part of host, 0.3 part of organic chrome cross linker, 0.1 part of inorganic chromium cross linker, 1.2 parts of hardening agent,
0.4 part of stabilizer, 0.1 part of dehydration inhibitor, excess water composition, consumption is weight portion, and weight portion sum is 100.
The frozen glue by 0.5 part of host, 0.1 part of organic chrome cross linker, 0.4 part of inorganic chromium cross linker, 1.0 parts of hardening agent,
0.3 part of stabilizer, 0.2 part of dehydration inhibitor, excess water composition, consumption is weight portion, and weight portion sum is 100.
The frozen glue by 0.4 part of host, 0.1 part of organic chrome cross linker, 0.4 part of inorganic chromium cross linker, 1.5 parts of hardening agent,
0.3 part of stabilizer, 0.4 part of dehydration inhibitor, excess water composition, consumption is weight portion, and weight portion sum is 100.
The partially hydrolyzed polyacrylamide (PHPA) be PAMA, the anionicsite hydrolyzed polyacrylamide
Relative molecular mass is 600 × 104～1200 × 104, degree of hydrolysis is 10%～30%.
The particle diameter of the Ludox nanoparticle is 10～25nm.
The action principle of key component and addition reason are as follows in the technical proposal for solving the technical problem of the invention
It is described：
1st, host used in the present invention is partially hydrolyzed polyacrylamide (PHPA), and for PAMA, after hydrolysis
Carboxyl can be cross-linked to form network structure with the chromium ion in malonic acid chromium；The hardening agent Ludox nanoparticle that the present invention is used
Can be coupled together with hardening agent amino silane, formed fish network structure, the structure so with partially hydrolyzed polyacrylamide (PHPA)-chromium
The cross-meshed of formation is constituted intersects interpenetrating structure, and final obtained gel strength is high, viscoelasticity is good.
2nd, the present invention used by hardening agent particle diameter be 10-25nm, the presence of the Ludox nanoparticle of the particle size range,
So that the nano/micron pore structure of network non-generic frozen glue for nano-pore structure of compound frozen glue, grid is distributed more homogeneous
Change, gel structure stability is higher；In addition, Ludox nanoparticle surface carries substantial amounts of hydroxyl, with excellent hydrophilic energy
Power so that frozen glue has the effect of higher moisture holding capacity and selective shut-off channeling, frozen glue is difficult syneresis, at high temperature
It is more stable.
3rd, the cross-linking agent that the present invention is used is chromium cross linker, different from organic phenolic crosslinkers high temperature plastic characteristic, and chromium is handed over
Connection agent has excellent gel-forming property at a temperature of common oil reservoir, and final obtained frozen glue is in initial low middle temperature reservoir temperature
Plastic by lower, without the need for reinjecting into glue to stratum preheating, the optional wide ranges of gelling temperature are 50 DEG C～180 DEG C.
4th, dehydration inhibitor polyphosphate used in the present invention or/and amino phosphonates do can be suppressed by complexing
Chromium polynuclear hydroxy bridge complex ion is formed so that gelation time is adjustable between 12～60h；In addition, dehydration inhibitor can also by with
The weak crosslinking of partially hydrolyzed polyacrylamide (PHPA) amide groups improves frozen glue stability so that frozen glue does not take off for aging 3 months at 180 DEG C
Water.
Embodiment 1：
0.05 part of sodium dichromate, 0.05 part of sodium sulfite, 0.3 part of malonic acid chromium, 1 part of silicon are added in 47.9 parts of tap waters
Colloidal sol nanoparticle, 0.2 part of amino silane, 0.4 part of thiourea, 0.1 part of polyphosphate, stir so as to fully dissolving, then
The partially hydrolyzed polyacrylamide (PHPA) that the mass concentration that 50 parts are prepared with tap water is 1% is mixed with above-mentioned solution, is stirred,
Obtain the present invention into glue.Into glue, the gelation time at 50 DEG C is 60h for this, and the gel strength of acquisition (breaks through vacuum
Method is measured) it is 0.077MPa, aging 3 months no dehydrating phenomenas at 180 DEG C.
With the nano combined frozen glue of heavy oil thermal recovery fleeing proof obtained above as object of study, illustrated by physical simulation experiment
The thermal recovery envelope alters shut-off capacity of the frozen glue to steam.The fill out sand tube permeability of this test is 2468mD, and porosity is
38.23%, physical simulation experiment is carried out in three steps.The first step is just to yearn for inject in fill out sand tube 180 DEG C with the flow velocity of 2ml/min
Water vapour, survey its balance pressure, according to Darcy formula calculate permeability k1.Second step is reverse with the flow velocity of 0.5ml/min
The frozen glue of injection 0.5PV is replaced into glue, the clear water for being subsequently injected into 0.25PV, then fill out sand tube is placed into 60h at 50 DEG C.The
Three steps are, with the water vapour of positive 180 DEG C injected in fill out sand tube of the flow velocity of 2ml/min, to survey its balance pressure, calculate infiltration
Rate k2.Finally press formula E=(k1-k2)/k1× 100%, it is calculated frozen glue sealing ratiod E=95.9%.
Embodiment 2：
Add in 48.02 parts of tap waters 0.1 part of sodium dichromate, 0.3 part of sodium sulfite, 0.2 part of malonic acid chromium, 0.9 part
Ludox nanoparticle, 0.18 part of amino silane, 0.2 part of thiourea, 0.1 part of amino phosphonates do, stir so as to fully molten
Solution, then the partially hydrolyzed polyacrylamide (PHPA) that the mass concentration that 50 parts are prepared with tap water is 1% is mixed with above-mentioned solution, stir
Uniformly, that is, obtain the present invention into glue.Into glue, the gelation time at 60 DEG C is 56h for this, and the gel strength of acquisition is
0.081MPa, aging 3 months no dehydrating phenomenas at 180 DEG C.
With the nano combined frozen glue of heavy oil thermal recovery fleeing proof obtained above as object of study, illustrated by physical simulation experiment
The thermal recovery envelope alters shut-off capacity of the frozen glue to steam.The fill out sand tube permeability of this test is 2396mD, and porosity is
36.29%, physical simulation experiment is carried out in three steps.The first step is just to yearn for inject in fill out sand tube 180 DEG C with the flow velocity of 2ml/min
Water vapour, survey its balance pressure, according to Darcy formula calculate permeability k1.Second step is reverse with the flow velocity of 0.5ml/min
The frozen glue of injection 0.5PV is replaced into glue, the clear water for being subsequently injected into 0.25PV, then fill out sand tube is placed into 56h at 60 DEG C.The
Three steps are, with the water vapour of positive 180 DEG C injected in fill out sand tube of the flow velocity of 2ml/min, to survey its balance pressure, calculate infiltration
Rate k2.Finally press formula E=(k1-k2)/k1× 100%, it is calculated frozen glue sealing ratiod E=95.5%.
Embodiment 3：
Add in 47.97 parts of tap waters 0.2 part of sodium dichromate, 0.3 part of sodium sulfite, 0.1 part of malonic acid chromium, 0.9 part
Ludox nanoparticle, 0.18 part of amino silane, 0.2 part of thiourea, 0.15 part of polyphosphate, stir so as to fully molten
Solution, then the partially hydrolyzed polyacrylamide (PHPA) that the mass concentration that 50 parts are prepared with tap water is 1% is mixed with above-mentioned solution, stir
Uniformly, that is, obtain the present invention into glue.Into glue, the gelation time at 70 DEG C is 49h for this, and the gel strength of acquisition is
0.078MPa, aging 3 months no dehydrating phenomenas at 180 DEG C.
With the nano combined frozen glue of heavy oil thermal recovery fleeing proof obtained above as object of study, illustrated by physical simulation experiment
The thermal recovery envelope alters shut-off capacity of the frozen glue to steam.The fill out sand tube permeability of this test is 2445mD, and porosity is
38.11%, physical simulation experiment is carried out in three steps.The first step is just to yearn for inject in fill out sand tube 180 DEG C with the flow velocity of 2ml/min
Water vapour, survey its balance pressure, according to Darcy formula calculate permeability k1.Second step is reverse with the flow velocity of 0.5ml/min
The frozen glue of injection 0.5PV is replaced into glue, the clear water for being subsequently injected into 0.25PV, then fill out sand tube is placed into 49h at 70 DEG C.The
Three steps are, with the water vapour of positive 180 DEG C injected in fill out sand tube of the flow velocity of 2ml/min, to survey its balance pressure, calculate infiltration
Rate k2.Finally press formula E=(k1-k2)/k1× 100%, it is calculated frozen glue sealing ratiod E=95.0%.
Embodiment 4：
0.15 part of sodium dichromate, 0.25 part of sodium sulfite, 0.1 part of malonic acid chromium, 0.8 part of silicon are added in 48 parts of tap waters
Colloidal sol nanoparticle, 0.2 part of amino silane, 0.3 part of thiourea, 0.2 part of polyphosphate, stir so as to fully dissolving, then
The partially hydrolyzed polyacrylamide (PHPA) that the mass concentration that 50 parts are prepared with tap water is 1% is mixed with above-mentioned solution, is stirred,
Obtain the present invention into glue.Into glue, the gelation time at 100 DEG C is 28h for this, and the gel strength of acquisition is 0.076MPa,
Aging 3 months no dehydrating phenomenas at 180 DEG C.
With the nano combined frozen glue of heavy oil thermal recovery fleeing proof obtained above as object of study, illustrated by physical simulation experiment
The thermal recovery envelope alters shut-off capacity of the frozen glue to steam.The fill out sand tube permeability of this test is 2493mD, and porosity is
38.74%, physical simulation experiment is carried out in three steps.The first step is just to yearn for inject in fill out sand tube 180 DEG C with the flow velocity of 2ml/min
Water vapour, survey its balance pressure, according to Darcy formula calculate permeability k1.Second step is reverse with the flow velocity of 0.5ml/min
The frozen glue of injection 0.5PV is replaced into glue, the clear water for being subsequently injected into 0.25PV, then fill out sand tube is placed into 28h at 100 DEG C.
3rd step is, with the water vapour of positive 180 DEG C injected in fill out sand tube of the flow velocity of 2ml/min, to survey its balance pressure, and calculating is oozed
Saturating rate k2.Finally press formula E=(k1-k2)/k1× 100%, it is calculated frozen glue sealing ratiod E=92.9%.
Embodiment 5：
Add in 47.95 parts of tap waters 0.15 part of sodium dichromate, 0.25 part of sodium sulfite, 0.1 part of malonic acid chromium, 0.8
Part Ludox nanoparticle, 0.2 part of amino silane, 0.3 part of thiourea, 0.2 part of polyphosphate, 0.05 part of amino phosphonates do, stir
Mix uniform so as to fully dissolving, then by partially hydrolyzed polyacrylamide (PHPA) that the mass concentration that 50 parts are prepared with tap water is 0.9%
Mix with above-mentioned solution, stir, that is, obtain the present invention into glue.Into glue, the gelation time at 130 DEG C is 22h for this,
The gel strength of acquisition is 0.074MPa, aging 3 months no dehydrating phenomenas at 180 DEG C.
With the nano combined frozen glue of heavy oil thermal recovery fleeing proof obtained above as object of study, illustrated by physical simulation experiment
The thermal recovery envelope alters shut-off capacity of the frozen glue to steam.The fill out sand tube permeability of this test is 2361mD, and porosity is 36.03
Part, physical simulation experiment is carried out in three steps.The first step is just to yearn for the water that 180 DEG C are injected in fill out sand tube with the flow velocity of 2ml/min
Steam, surveys its balance pressure, and according to Darcy formula permeability k is calculated1.Second step is with the flow velocity inverse injection of 0.5ml/min
The frozen glue of 0.5PV is replaced into glue, the clear water for being subsequently injected into 0.25PV, then fill out sand tube is placed into 22h at 130 DEG C.3rd
Step is, with the water vapour of positive 180 DEG C injected in fill out sand tube of the flow velocity of 2ml/min, to survey its balance pressure, calculates permeability
k2.Finally press formula E=(k1-k2)/k1× 100%, it is calculated frozen glue sealing ratiod E=90.4%.
Embodiment 6：
0.15 part of sodium dichromate, 0.25 part of sodium sulfite, 0.1 part of malonic acid chromium, 1 part of silicon are added in 47.3 parts of tap waters
Colloidal sol nanoparticle, 0.5 part of amino silane, 0.3 part of thiourea, 0.25 part of polyphosphate, 0.25 part of amino phosphonates do, stirring is equal
It is even so as to fully dissolving, then by the mass concentration that 50 parts are prepared with tap water be 0.8% partially hydrolyzed polyacrylamide (PHPA) with it is upper
State solution mixing, stir, that is, obtain the present invention into glue.Into glue, the gelation time at 180 DEG C is 12h for this, is obtained
Gel strength be 0.071MPa, at 180 DEG C aging 3 months without dehydrating phenomena.
With the nano combined frozen glue of heavy oil thermal recovery fleeing proof obtained above as object of study, illustrated by physical simulation experiment
The thermal recovery envelope alters shut-off capacity of the frozen glue to steam.The fill out sand tube permeability of this test is 2402mD, and porosity is 37.79
Part, physical simulation experiment is carried out in three steps.The first step is just to yearn for the water that 180 DEG C are injected in fill out sand tube with the flow velocity of 2ml/min
Steam, surveys its balance pressure, and according to Darcy formula permeability k is calculated1.Second step is with the flow velocity inverse injection of 0.5ml/min
The frozen glue of 0.5PV is replaced into glue, the clear water for being subsequently injected into 0.25PV, then fill out sand tube is placed into 12h at 180 DEG C.3rd
Step is, with the water vapour of positive 180 DEG C injected in fill out sand tube of the flow velocity of 2ml/min, to survey its balance pressure, calculates permeability
k2.Finally press formula E=(k1-k2)/k1 × 100%, is calculated frozen glue sealing ratiod E=85.1%.
Embodiment 1 to the nano combined frozen glue each group distribution ratio of heavy oil thermal recovery fleeing proof and Gel Properties parameter of embodiment 6 are converged
Always as shown in rear table.
Table 1
As seen from the above table, the nano combined frozen glue of heavy oil thermal recovery fleeing proof of the invention is by 0.4 part of partially hydrolyzed polyacrylamide (PHPA)
～0.5 part；0.1 part～0.3 part of malonic acid chromium；0.1 part～0.5 part of sodium dichromate and sodium sulfite, wherein sodium dichromate：Sulfurous
Sour sodium=1:1～3；Ludox nanoparticle and 1 part～1.5 parts of amino silane, wherein Ludox nanoparticle：Amino silane=
2～5:1；0.2 part～0.4 part of thiourea；0.1 part～0.5 part of polyphosphate or/and amino phosphonates do, wherein poly during combination
Phosphate：Amino phosphonates do=1～4:1st, excess water composition, consumption is weight portion, and the weight portion sum of said components is 100.
Gelling temperature is optional 50 DEG C～180 DEG C, and the optional 12～60h of gelation time, gel strength is above 0.07Mpa, by force
Degree is higher.The nano combined frozen glue of heavy oil thermal recovery fleeing proof of the present invention is altered with stronger closure during heavy crude heat extraction to steam
Ability, sealing ratiod is all higher than 85%；Frozen glue of the present invention is alternative to be blocked channeling and not to block oil channel, can effectively be blocked
Steamchanneling, and then increase heavy crude heat extraction recovery ratio.
Other are unspecified to belong to prior art.
Claims (8)
1. the nano combined frozen glue of heavy oil thermal recovery fleeing proof, it is characterised in that：The frozen glue is handed over by 0.4 part～0.5 part of host, organic chromium
0.1 part～0.3 part of agent of connection, 0.1 part～0.5 part of inorganic chromium cross linker, 1 part～1.5 parts of hardening agent, stabilizer 0.2 part～0.4
Part, 0.1 part～0.5 part of dehydration inhibitor, excess water composition, consumption is weight portion, and the weight portion sum of said components is 100；
The host is partially hydrolyzed polyacrylamide (PHPA), and the organic chrome cross linker is malonic acid chromium, and the inorganic chromium cross linker is attached most importance to
Sodium chromate：Sodium sulfite=1:1～3, the hardening agent is Ludox nanoparticle：Amino silane=2～5:1, it is described stable
Agent is thiourea, and the dehydration inhibitor is one of polyphosphate and amino phosphonates do or combines, polyphosphate during combination：Ammonia
Base phosphonate=1～4:1.
2. the nano combined frozen glue of heavy oil thermal recovery fleeing proof according to claim 1, it is characterised in that：The frozen glue is by host
0.5 part, it is 0.1 part～0.3 part of organic chrome cross linker, 0.1 part～0.5 part of inorganic chromium cross linker, 1 part～1.2 parts of hardening agent, stable
0.2 part～0.4 part of agent, 0.1 part～0.2 part of dehydration inhibitor, excess water composition, consumption is weight portion, and weight portion sum is
100。
3. the nano combined frozen glue of heavy oil thermal recovery fleeing proof according to claim 1, it is characterised in that：The frozen glue is by host
0.5 part, 0.2 part～0.3 part of organic chrome cross linker, 0.1 part～0.4 part of inorganic chromium cross linker, 1.08 parts～1.2 parts of hardening agent,
0.2 part～0.4 part of stabilizer, 0.1 part of dehydration inhibitor, excess water composition, consumption is weight portion, and weight portion sum is 100.
4. the nano combined frozen glue of heavy oil thermal recovery fleeing proof according to claim 1, it is characterised in that：The frozen glue is by host
0.5 part, 0.3 part of organic chrome cross linker, 0.1 part of inorganic chromium cross linker, 1.2 parts of hardening agent, 0.4 part of stabilizer, dehydration inhibitor
0.1 part, excess water composition, consumption is weight portion, and weight portion sum is 100.
5. the nano combined frozen glue of heavy oil thermal recovery fleeing proof according to claim 1, it is characterised in that：The frozen glue is by host
0.5 part, 0.1 part of organic chrome cross linker, 0.4 part of inorganic chromium cross linker, 1.0 parts of hardening agent, 0.3 part of stabilizer, dehydration inhibitor
0.2 part, excess water composition, consumption is weight portion, and weight portion sum is 100.
6. the nano combined frozen glue of heavy oil thermal recovery fleeing proof according to claim 1, it is characterised in that：The frozen glue is by host
0.4 part, 0.1 part of organic chrome cross linker, 0.4 part of inorganic chromium cross linker, 1.5 parts of hardening agent, 0.3 part of stabilizer, dehydration inhibitor
0.4 part, excess water composition, consumption is weight portion, and weight portion sum is 100.
7. the nano combined frozen glue of heavy oil thermal recovery fleeing proof according to any one of claim 1～6, it is characterised in that：It is described
Partially hydrolyzed polyacrylamide (PHPA) is PAMA, the anionicsite hydrolyzed polyacrylamide relative molecular mass
For 600 × 104～1200 × 104, degree of hydrolysis is 10%～30%.
8. the nano combined frozen glue of heavy oil thermal recovery fleeing proof according to any one of claim 1～6, it is characterised in that：It is described
The particle diameter of Ludox nanoparticle is 10～25nm.
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