CN103013485B - Modified resin sand consolidation agent as well as preparation method and application thereof - Google Patents
Modified resin sand consolidation agent as well as preparation method and application thereof Download PDFInfo
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- CN103013485B CN103013485B CN201210537053.8A CN201210537053A CN103013485B CN 103013485 B CN103013485 B CN 103013485B CN 201210537053 A CN201210537053 A CN 201210537053A CN 103013485 B CN103013485 B CN 103013485B
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Abstract
The invention relates to a modified resin sand consolidation agent as well as a preparation method and an application of the modified resin sand consolidation agent. The sand consolidation agent mainly consists of epoxy resin as a main agent, 6.0-7.0% of a curing agent, 15% of a softener, 20-22% of a diluent, 2% of a coupling agent and 10% of glass fiber; and the dosages of the other components expect the epoxy resin is weighed by 100% of the epoxy resin in percentage by weight. The preparation comprises that the modified resin sand consolidation agent is used for preventing and curing sand production in oil wells. The application method comprises the steps of: pre-treating the stratum by using pre-cleaning fluid, then pouring the sand consolidation agent from an oil tube, and finally replacing the sand consolidation agent to the deep of the stratum by using replacement pore-broadening liquid. The formula of the sand consolidation agent disclosed by the invention can solve the problem of influence of sand production in oil wells on the production and is suitable for different sand grains.
Description
Technical field
The invention relates to a kind of modified resin sand-fixing agent and preparation method thereof and application.
Background technology
Gaosheng oil field thunder man block shakes out type mainly based on stratum fine sand, particle diameter at about 0.1mm, most of oil well mud extraction matter fine silt.Analyzed by sand sampling, measure median particle size and be respectively 0.15mm and 0.18mm.The measure such as sand-preventing pump, sand control screen, earth formation deep sand control of current employing, all effectively can not prevent and treat shale fine silt, often causes holddown or is blocked by well screen, cannot ensure that oil well is normally produced, the effective exploitation of serious restriction block.
Need to research and develop new sand control technique, to solve the difficult problem that sand production impact is produced.
Summary of the invention
One object of the present invention is to provide a kind of modified resin sand-fixing agent, and described sand-fixing agent can solve the problem that sand production impact is produced, and is applicable to the different particle diameters that shakes out.
Another object of the present invention is to the preparation method that above-mentioned modified resin sand-fixing agent is provided.
The third object of the present invention is the purposes providing above-mentioned modified resin sand-fixing agent.
The fourth object of the present invention is the using method providing above-mentioned modified resin sand-fixing agent.
For reaching above-mentioned purpose, on the one hand, the invention provides a kind of modified resin sand-fixing agent: described sand-fixation agent is prepared from primarily of following composition: epoxy resin is host, hardener dose is 6.0% ~ 7.0%; Tenderizer consumption is 15%; Thinner consumption is 20 ~ 22%; Coupling agent consumption is 2%; Glass fibre consumption is 10%; The per-cent consumption of other compositions except epoxy resin is in epoxy resin for 100%, and described per-cent is weight percentage.
According to specific embodiment of the present invention, in the present invention, preferred described hardener dose is 6.4%.
Each percentage composition consumption of the present invention all in epoxy resin for 100%, such as hardener dose is 6.0% ~ 7.0%, should be understood to that hardener dose is weight epoxy 6.0% ~ 7.0%.Other compositions by that analogy.
Described epoxy resin, solidifying agent, tenderizer, thinner, coupling agent and glass fibre can be any applicable epoxy resin, solidifying agent, tenderizer, thinner, coupling agent and fiber in association area in prior art.Those skilled in the art, after reading specification sheets of the present invention, in conjunction with the prior art that himself is grasped, can select rational mentioned reagent.
And the present invention preferably adopts: epoxy resin is the epoxy resin of epoxy equivalent (weight) 185 ~ 200g/eq, oxirane value 0.48 ~ 0.54eq/mg, viscosity 10000 ~ 25000PaS/25 DEG C; Solidifying agent is quadrol; Tenderizer is dibutylester; Thinner is acetone; Coupling agent is silane coupling agent.
The present invention can also preferred coupling agent be γ-(2,3-epoxy third oxygen) propyl trimethoxy silicane further.
Described epoxy resin is more preferably the linear epoxy resin of dihydroxyphenyl propane (two (4-hydroxy phenyl) propane of 2,2-) and epoxy chloropropane polycondensation synthesis in alkaline medium.
Described epoxy resin can more preferably E-51 epoxy resin;
Be for example the E-51 epoxy resin that Hangzhou Wu Huigang tackiness agent company limited produces.
Wherein said E-51 epoxy resin dawn known to those skilled in the art, E-51 is wherein the concrete epoxy resin model in this area, also can be called 618 epoxy resin.
Dibutylester molecular formula is wherein C
16h
220
4, structural formula is as follows:
Coupling agent is silane coupling agent γ-(2,3-epoxy third oxygen) propyl trimethoxy silicane, i.e. coupling agent KH-560.
Gordian technique of the present invention is the modification of epoxy resin.Because of epoxy resin and solidifying agent mix and blend solidify after product, fragility is large, and ultimate compression strength is little, will add tenderizer carry out modification to it.Take epoxy resin as host, change the consumption of solidifying agent, consumption is between 6.0%-7.0%, thinner consumption is 20 ~ 22%, tenderizer consumption be 15% and coupling agent consumption be 2% mixing and stirring, put into 60 DEG C, 75 DEG C water-bath constant temperature, observe it and just consolidate the time (using glass stick Pick Wire, until do not have wire drawing).Consider the factors such as on-site construction time, when the consumption of solidifying agent is between 6.1% ~ 6.5%, set time, about 2 hours, can meet site operation substantially.
When thinner consumption is 22%, better effect can be reached.
In the system of sand-fixing agent, simple epoxy resin does not have use value.Appropriate solidifying agent must be added in use, make epoxy molecule be cross-linked into cancellated macromole, form three dimensional structure.Epoxy resin is the tackiness agent that a kind of viscosity ratio is larger.During preparation sand-fixing agent, need to add thinner, when stirring sand-fixing agent, each component of sand-fixing agent can be made to contact fully, be also easier to when sand-fixing agent injects stratum simultaneously.The induration fragility that epoxy resin and solidifying agent generate is large, and ultimate compression strength is little, adds tenderizer and induration fragility is diminished, and elasticity increases, but the consumption of tenderizer is also too much unsuitable, otherwise there will be can not completely crued phenomenon.The group of coupling agent one end can with the silanol radical reaction on reservoir sand surface, be condensed into silica chain, thus form firmly Chemical bond; The other end group then produces avidity with epoxy resin, thus reservoir sand and epoxy resin are organically combined.The glass fibre added serves the effect being similar to reinforced concrete, and in sand body, random distribution defines tridimensional network, and the reticulated structure of the cementing formation of glass fibre, significantly enhances the intensity of sand block layer; Fine silt can be gathered into larger fine silt combination by glass fibre simultaneously, blocks fine silt and enters pit shaft.
Glass fibre of the present invention also can be preferably milled glass fiber;
Alkali free glass fibre can also be preferably;
Can also more preferably alkali-free milled glass fiber again.
According to sand-fixing agent of the present invention, preferred described glass fibre length is 2 ~ 3mm, and diameter is 20 μm.
Epoxy resin as sand-fixing agent has network molecular structure, and the strong polar group in molecule and the polar group of sand grains have affinity interaction, can produce physical adsorption, to sand grain surface migration and strong adhesion at sand grain surface.Polymerization reaction take place under the effect of solidifying agent, makes it to solidify to form high strength induration at short notice.Reaming liquid by time the low molecular compound in sand-fixing agent is taken away, ensure that consolidation thing has certain perviousness.
The selection of what the present invention was the most key is mentioned component, the record that those skilled in the art are above-mentioned according to the present invention, mentioned component is selected to carry out modification to epoxy resin, and concrete modified-reaction can with reference to the method for modifying of prior art loop-like epoxy resins, the primary goal of the invention of the present invention can be realized, obtain a kind of modified resin sand-fixing agent of good performance, and the present invention is in order to further improve the performance of described sand-fixing agent, further discloses a kind of preferred preparation method as described below.
On the other hand, the invention provides the preparation method of above-mentioned modified resin sand-fixing agent, comprising: extracting epoxy resin, be heated to 40 ~ 50 DEG C, add thinner, fully stir; Add tenderizer and coupling agent successively again, fully stir; Add solidifying agent, stir rapidly; Finally under agitation add glass fibre, stir and both obtain.
In the present invention's preparation, extracting epoxy resin is heated to 40 ~ 50 DEG C and can makes to react more efficient, abundant, and the present invention is preferably heated to epoxy resin viscosity further and is less than 5000mPa.s.
Another aspect, the invention provides the purposes of above-mentioned modified resin sand-fixing agent, and described modified resin sand-fixing agent is used for the control of sand production.
According to specific embodiment of the invention scheme, the particle diameter of preferred sand is 0.05mm ~ 0.22mm.
Adopt conventional chemical consolidated sand for particle diameter shaking out of 0.1mm at present, after usual intensity there will be greatly consolidation, rate of permeation is too low, causes production capacity to reduce; Still there is the problem of shaking out in the little meeting of intensity.
Glass fibre distributes and defines tridimensional network in sand body.The reticulated structure of the cementing formation of glass fibre, significantly enhances the intensity of sand block layer; Simultaneously fine silt can be gathered into larger combination by glass fibre, thus blocks fine silt to greatest extent and enter pit shaft.
Again on the one hand, the invention provides the using method of above-mentioned modified resin sand-fixing agent, described using method comprises: use preposition scavenging solution pre-treatment stratum, the sand-fixing agent described in then injecting from oil pipe, finally uses replacement reaming liquid to be replaced by sand-fixing agent and needs stratum to be processed.In the method, the prior art that the selection of described preposition scavenging solution and the operation on pre-treatment stratum, the selection replacing reaming liquid and replacement operation all can refer to affiliated field is carried out.
Described pre-treatment such as this area are generally to be injected preposition scavenging solution, can then inject described sand-fixing agent, sequential production after injecting scavenging solution.
According to specific embodiment of the invention scheme, preferred described preposition scavenging solution consumption is preferably 2 ~ 3PV.
According to specific embodiment of the invention scheme, preferred described sand-fixing agent consumption is 1PV.
According to specific embodiment of the invention scheme, preferred described preposition scavenging solution is salt solution, diesel oil or 2% Varion CDG-K (BS-12 tensio-active agent) solution.
Wherein be more preferably 2% Varion CDG-K solution.
According to specific embodiment of the invention scheme, preferred described replacement reaming liquid is salt solution or diesel oil.
Wherein more preferably described replacement reaming liquid is diesel oil.
According to specific embodiment of the invention scheme, preferred described replacement reaming liquid consumption is 0.5 ~ 1PV
According to specific embodiment of the invention scheme, preferably also inject expansion-resisting agent when injecting preposition scavenging solution.The selection of the concrete kind of described expansion-resisting agent can be carried out with reference to the prior art in affiliated field.
Wherein more preferably described expansion-resisting agent consumption is 2 ~ 3 times of formation pore volume.
After being injected by sand-fixing agent of the present invention, within usual 72 hours, solidification can be completed.
In sum, the invention provides a kind of modified resin sand-fixing agent and preparation method thereof and use this sand-fixing agent to carry out the method for solid sand.The advantage of sand-fixing agent of the present invention compared with currently available products is: (1) is applicable to shale fine silt, and sand control particle diameter is greater than 0.05mm; (2) consolidation strength is large, and formation injury is little, and the ultimate compression strength of sample can reach about 7.2MPa, and water surveys rate of permeation about 550 × 10
-3μm
2left and right; (3) sand-fixing agent first time admittedly at 75 DEG C is controlled, and system is water-fast, crude oil, acid energy are good.
Embodiment
Describe the beneficial effect of implementation process of the present invention and generation below by way of specific embodiment in detail, be intended to help reader to understand essence of the present invention and feature better, not as can the restriction of practical range to this case.
Embodiment 1
The composition of the modified resin sand-fixing agent of the present embodiment and preparation:
Host: E-51 epoxy resin (epoxy equivalent (weight) 185 ~ 200g/eq that Hangzhou Wu Huigang tackiness agent company limited produces; Oxirane value 0.48 ~ 0.54eq/mg; Viscosity 10000 ~ 25000PaS/25 DEG C), 100 weight parts;
Solidifying agent: quadrol, 6.4 weight parts;
Tenderizer: dibutylester, 15 weight parts;
Thinner: acetone, 22 weight parts;
Silane coupling agent: γ-(2,3-epoxy third oxygen) propyl trimethoxy silicane, 2 weight parts.
Glass fibre: length is 2 ~ 3mm, and diameter is about 20 μm, 10 weight parts;
By above-mentioned host epoxy resin, be heated to mobility and improve, add thinner, fully stir; Add tenderizer and coupling agent successively again, fully stir; Add solidifying agent, stir rapidly; And under agitation add glass fibre, stir both modified resin sand-fixing agent of the present invention.
The using method of the present embodiment sand-fixing agent: first use preposition scavenging solution (2% Varion CDG-K solution) pre-treatment stratum, then inject sand-fixing agent from oil pipe, finally use replacement reaming liquid (diesel oil) that sand-fixing agent is replaced to depths, stratum.
This formula sand-fixing agent carries out processing simulation experiment on oil-sand, and the induration obtained has higher ultimate compression strength and rate of permeation, and at 75 DEG C, Hou Gu is after 72 hours, and the ultimate compression strength of consolidation sample can reach about 7.2MPa, and water surveys rate of permeation about 550 × 10
-3μm
2left and right; Can stop when injecting the consumption of 1PV the sand grains being greater than 0.05mm, sand block effectiveness comparison is good; Sand-fixing agent system is water-fast, crude oil, acid energy are good, can meet onsite application requirement.
The current down-hole of thunder 22-9 well is sand-preventing pump, and pump detection period is 7 days, and shake out speed 18m/d, and type of shaking out is shale fine silt.This well measure production fluid day before yesterday 5.5t, day produce oil 1.6t, moisture 76%.June 16 has carried out resin sand consolidation, injects sand-fixing agent 30t altogether.Average day production fluid 6.2t after measure, day produce oil 2.1t, validity period reaches 94 days, and measure effectively extends pump detection period.
Test example 1
Sand control capability is whether this sand control agent can be applied to an on-the-spot major criterion and performance assessment criteria, therefore examines it with following experiment.
A, the experiment of simulation promotion thunder man block loaded in the Glass tubing of Φ 25mm*100mm with sand, hole plug compacting is carried at two ends secretly, calculates the quartz sand net weight loaded;
B, find time, saturation water, calculates PV number;
The sand-fixing agent (embodiment 1) that c, injection 1PV prepare, solidifies 72 hours in the water bath with thermostatic control of 75 DEG C;
D, the rock sample that consolidation is good is put in core holding unit, before rock core, puts into the steel pipe of Φ 25mm*25mm, in steel pipe, load experiment sand, add confined pressure;
Whether e, use clear water displacement 250ml (1ml/min), analyze in filtrate containing sand and size composition;
Whether the formation oil displacement 250ml (0.5ml/min) of f, use Gaosheng oil field, analyze in filtrate containing sand and size composition.
Filter sand performance measurement laboratory experiment, experimental result is in table 1.
Table 1 filter sand performance measurement experimental data table
Can being found out by simulating lab test, first use clear water displacement, then use the same consolidation sample of mother oil displacement, in filtrate, not find sand grains, illustrating that this sand-fixing agent can block the sand grains of 0.05mm when injecting the consumption of 1PV, sand block successful.
Test example 2
This test example has investigated sand-fixing agent set time of the present invention and oil resistant, water-fast and acidproof performance.
1. with reference to the feed composition of embodiment 1, take epoxy resin as host, change the consumption of solidifying agent, consumption is between 6.0% ~ 7.0%, thinner consumption is 20%, tenderizer consumption be 15% and coupling agent consumption be 2% mixing and stirring, put into 60 DEG C, 75 DEG C water-bath constant temperature, observe it and just consolidate the time (using glass stick Pick Wire, until do not have wire drawing).Experimental result is in table 2.
Table 2 hardener dose and set time relation
Along with the increase of hardener dose, set time shortens.No matter at 60 DEG C or at the temperature of 75 DEG C, this formula series can be solidified, but there is difference set time.When temperature is 75 DEG C, hardener dose between 6.0% ~ 7.0%, when not adding reservoir sand set time at 40 minutes within the scope of 150 minutes; When temperature is 60 DEG C, hardener dose is between 6.0% ~ 7.0%, and when not adding reservoir sand, set time was at 60 minutes to 200 minutes.
2. after the chemical stability of sand-fixing agent is related to sand control validity period length and other measure operations can be carried out.Therefore, it is quite necessary for carrying out chemical stability evaluation to it.Experiment adopts diesel oil, local water, acid, alkali at 25 DEG C, soak the sand-fixation agent that consolidation rock core carrys out Evaluation operation example 1, and experimental result is in table 3.
The experimental result of soaking in table 3 medium
Induration has good oil-proofness, water tolerance and acid resistance; In NaOH solution, have the small particle that corrosion is fallen at the bottom of beaker, highly basic has corrosion to induration, and the alkali resistance of sand-fixing agent system is poor.
Test example 3
In fill out sand tube, inject the sand-fixing agent (embodiment 1) of 1PV, solidify 72 hours in the water bath with thermostatic control of 75 DEG C.After 72 hours, the ultimate compression strength of induration is 7.60MPa, and it is 520.87 × 10 that water surveys rate of permeation
-3μm
2.
Claims (15)
1. a modified resin sand-fixing agent, is characterized in that, described sand-fixation agent is prepared from primarily of following composition: epoxy resin is host, and hardener dose is 6.0% ~ 7.0%; Tenderizer consumption is 15%; Thinner consumption is 20 ~ 22%; Coupling agent consumption is 2%; Glass fibre consumption is 10%; The per-cent consumption of other compositions except epoxy resin is in epoxy resin for 100%, and described per-cent is weight percentage; Wherein, epoxy resin is the epoxy resin of epoxy equivalent (weight) 185 ~ 200g/eq, oxirane value 0.48 ~ 0.54eq/mg, viscosity 10000 ~ 25000PaS/25 DEG C; Solidifying agent is quadrol; Tenderizer is dibutylester; Thinner is acetone; Coupling agent is silane coupling agent γ-(2,3-epoxy third oxygen) propyl trimethoxy silicane.
2. sand-fixing agent according to claim 1, is characterized in that, described hardener dose 6.4%.
3. sand-fixing agent according to claim 1, is characterized in that, epoxy resin is E-51 epoxy resin.
4. sand-fixing agent according to claim 1, is characterized in that, described glass fibre length is 2 ~ 3mm, and diameter is 20 μm.
5. the preparation method of sand-fixing agent described in claim 1-4 any one, is characterized in that, described preparation method comprises: extracting epoxy resin, is heated to 40 ~ 50 DEG C, adds thinner, fully stir; Add tenderizer and coupling agent successively again, fully stir; Add solidifying agent, stir rapidly; Finally under agitation add glass fibre, stir and get final product.
6. the application of sand-fixing agent described in claim 1-4 any one in sand production control.
7. application according to claim 6, is characterized in that, described oil well is the oil well of particle diameter 0.05mm ~ 0.22mm of shaking out.
8. a solid sand method, the method comprises: use preposition scavenging solution pre-treatment stratum, then injects the sand-fixing agent described in claim 1 or 2 from oil pipe, finally uses replacement reaming liquid to be replaced by sand-fixing agent and needs stratum to be processed.
9. method according to claim 8, is characterized in that, described sand-fixing agent consumption is 1PV.
10. method according to claim 8 or claim 9, it is characterized in that, described preposition scavenging solution is salt solution, diesel oil or 2% Varion CDG-K solution; Described preposition scavenging solution consumption is 2 ~ 3PV; Described replacement reaming liquid is salt solution or diesel oil; Described replacement reaming liquid consumption is 0.5-1PV.
11. methods according to claim 10, is characterized in that, described preposition scavenging solution is 2% Varion CDG-K solvent.
12. methods according to claim 10, is characterized in that, described replacement reaming liquid is diesel oil.
13. methods according to claim 10, is characterized in that, also inject expansion-resisting agent when injecting preposition scavenging solution.
14. methods according to claim 13, is characterized in that, described expansion-resisting agent is aluminum chloride.
15. methods according to claim 13, is characterized in that, described expansion-resisting agent consumption is 2 ~ 3 times of formation pore volume.
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| CN104723779A (en) * | 2013-12-19 | 2015-06-24 | 亿利资源集团有限公司 | Desert sand artware and preparation method thereof |
| CN104403651B (en) * | 2014-09-29 | 2017-06-30 | 赵辰 | A kind of preparation method of the high-strength oil well wet method anti-collapse particle of spherical solid sand |
| CN105331346A (en) * | 2015-11-18 | 2016-02-17 | 辽宁石油化工大学 | High-temperature-resistant composite epoxy resin sand consolidating agent and application thereof |
| CN106634918A (en) * | 2016-11-17 | 2017-05-10 | 中国石油天然气股份有限公司 | High-intensity modified resin sand consolidating agent |
| CN106753302A (en) * | 2016-12-02 | 2017-05-31 | 中国石油大学(华东) | Active washing oil sand-fixating agent and preparation method and application |
| CN106590562A (en) * | 2016-12-15 | 2017-04-26 | 中国石油大学(华东) | Active oil-washing sand consolidating agent and preparation method and application thereof |
| US10513915B2 (en) * | 2017-11-30 | 2019-12-24 | Saudi Arabian Oil Company | Consolidated material to equalize fluid flow into a wellbore |
| CN109321223B (en) * | 2018-10-30 | 2020-12-04 | 山东圣泉新材料股份有限公司 | Sand control agent, preparation method thereof and application of sand control agent in oil well sand control |
| CN109609111B (en) * | 2018-12-27 | 2021-04-06 | 长江大学 | Wood tar resin sand consolidation agent and preparation method and application thereof |
| CN109971484B (en) * | 2019-02-28 | 2021-04-09 | 伯森(烟台)环境工程技术有限公司 | High-molecular sand-fixing agent |
| CN111022011B (en) * | 2019-12-03 | 2022-03-18 | 中国石油化工股份有限公司 | Construction method of foamable resin sand consolidation agent for argillaceous fine silt oil reservoir |
| CN111154492B (en) * | 2020-01-17 | 2021-02-26 | 陕西科技大学 | Humic acid film-covering sand-fixing agent of phosphate system and using method thereof |
| CN111577215B (en) * | 2020-06-16 | 2022-04-05 | 青岛大地新能源技术研究院 | Sand control system combining high molecules and low-molecular polymers for fine silt |
| CN113445944B (en) * | 2021-06-25 | 2023-07-14 | 中国石油天然气股份有限公司 | Pollution-free sand prevention and yield increase method for oil well |
| CN113861988B (en) * | 2021-10-26 | 2022-06-10 | 华南理工大学 | Hyperbranched epoxy oligosiloxane sand-fixing material and preparation method and application thereof |
| CN115873587B (en) * | 2022-11-17 | 2024-01-23 | 中国石油天然气集团有限公司 | Composite chemical backflow-preventing additive and proppant backflow-preventing method |
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