CN105567199A - Hydrophobic nano silica emulsified water plugging agent and preparation method and application thereof - Google Patents
Hydrophobic nano silica emulsified water plugging agent and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a hydrophobic nano silica emulsified water plugging agent and a preparation method and an application thereof. The hydrophobic nano silica emulsified water plugging agent contains hydrophobic nano silica and ester with the structural formula of R1COOR2, with the total weight of the hydrophobic nano silica emulsified water plugging agent as a benchmark, the content of the hydrophobic nano silica is 0.5-20 wt%, and the content of the ester is 80-99.5 wt%, wherein R1 is C1-C20 alkyl group, and R2 is C1-C10 alkyl group. The hydrophobic nano silica emulsified water plugging agent is applied to crude oil, can obtain a uniform and stable emulsion with relatively high viscosity, and has relatively high plugging property; and moreover, the water plugging agent is simple in composition and is easily implemented in an oil field.
Description
Technical field
The present invention relates to a kind of hydrophobic nano-silica emulsification plugging agent and preparation method thereof and application, particularly, relate to a kind of hydrophobic nano-silica emulsification plugging agent for water plugging and profile controlling in oil development, with the method for this hydrophobic nano-silica emulsification plugging agent of preparation, and this hydrophobic nano-silica emulsification plugging agent carries out the application of water blockoff in oil well.
Background technology
In oilfield development process, water plugging and profile controlling is an important technical of " steady oil control water ".Current oilwell water shutoff agent mainly contains two large classes, and one is non-selective water-plugging, and two is selective water-plugging.Due to non-selective blocking agent non-selectivity, for the stratum of multilayer system exploitation, easily cause reservoir injury, have a strong impact on oil well productivity, and construction technology for plugging is complicated, operation is various, and operating cost is high.And conventional selective water-plugging is as limited in the selectivity such as polymkeric substance, foam, shut-off capacity is not strong, and water blockoff success ratio is not high yet.
Emulsified crude oil plugging agent forms high glutinous emulsion system after utilizing crude oil to meet emulsifying water, reaches the object of shutoff height infiltration circulation road, belongs to selective water-plugging.Emulsified crude oil plugging agent has good selectivity, forms viscosity higher water-in-oil emulsion when meeting water by emulsifying effect, blocking penetrating passage, and diluted when meeting crude oil, viscosity degradation, do not affect crude oil seepage flow passage.Emulsified crude oil plugging agent also has higher plugging strength simultaneously, and after emulsification of crude oil, viscosity can increase several times, reaches hundreds of mPas, and owing to there is kapillary " Jia Min " effect of water-oil interface in formation rock seam, emulsion plugging effect is improved further.
CN101824979A discloses a kind of emulsion process profile control and water shutoff method of thickened oil steam-stimulated well, is wherein injected with steam by high temperature resistance water-in-oil type emulsifier simultaneously or before well steam treatment of handling up, injects the heavy crude reservoir bottom through cyclic steam stimulation; Wherein, described high temperature resistance water-in-oil emulsifier mainly comprises HLB value and is less than the anionic of 6, cationic, non-ionic type or compound surfactant.Emulsifying agent in the method has stronger temperature resistant capability, but the steamed well be limited under worst hot case is implemented.
CN102061153 describes a kind of crude oil emulsifying agent for water plugging of oil well, and its raw material is dimethylamine, epoxy chloropropane and water.This emulsifying agent needs dimethylamine and epoxy chloropropane first to react, and the wayward easy impact of reaction process obtains quality and the implementation result of emulsifying agent.
CN102329600A discloses a kind of nanoparticle sealing channeling water shutoff agent for oil wells, containing calcium oxide, silicon oxide, aluminum oxide, ferric oxide, trolamine, KCl, Na
2siO
3, wilkinite, acetone and formaldehyde condensation products, feero-chromo-lignosulfonate and water, this plugging agent is by first by calcium oxide, silicon oxide, aluminum oxide, ferric oxide, Na
2siO
3, wilkinite and acetone and formaldehyde condensation products be first ground to grain diameter and reach 1-100nm, and be solution by trolamine, KCl, feero-chromo-lignosulfonate and water mixed dissolution, then the product of grinding and solution are mixed to get.The more complicated enforcement of the method composition is loaded down with trivial details, is unsuitable for actual use.
CN1704559A discloses a kind of high strength easy and dissolves nanometer blocking agent, is made up of nano silicon oxide, nano-sized iron oxide, nano-calcium carbonate, nano aluminium oxide, superfine cement and auxiliary agent.This agent composition complexity is unfavorable for practicing.
CN1760312A discloses a kind of water shut-off material of plant for oil field, comprising oven dry marine alga, polyether glycol, tolylene diisocyanate, natural rubber, silicon-dioxide, polyoxyethylene glycol (400), calcium carbonate (100 order) and rubber ingredients, this material require is by following explained hereafter: polyether glycol is added reactor and heat up 120 DEG C, vacuum hydro-extraction 30 minutes, be cooled to 50 DEG C afterwards, add tolylene diisocyanate and be warmed up to 85 DEG C, stir 2 hours, then 40 DEG C of dischargings are cooled to, for subsequent use as component A.By natural rubber and through pulverize be that 80 object marine algas, silicon-dioxide, polyoxyethylene glycol, calcium carbonate and rubber ingredients and component A mix, on glue pressing machine mixing evenly after, 120 DEG C of sulfurations 30 minutes, pulverizing through rubber crusher was 80 orders, is water shut-off material of plant for oil field.The method complexity is unsuitable for Water in Water Shutoff in Oil Field and uses.
As can be seen here, obtain that composition is simple, emulsion-stabilizing, easily application implementation plugging agent be still required for oil development.
Summary of the invention
The object of the invention is to obtain good emulsion stability and by more full-bodied plugging agent and the plugging agent overcoming prior art forms defect that is complicated and that not easily implement, providing a kind of hydrophobic nano-silica emulsification plugging agent and preparation method thereof and application.
To achieve these goals, the invention provides a kind of hydrophobic nano-silica emulsification plugging agent, this hydrophobic nano-silica emulsification plugging agent contains hydrophobic nano-silica and structural formula is R
1cOOR
2ester; With the gross weight of described hydrophobic nano-silica emulsification plugging agent for benchmark, the content of hydrophobic nano-silica is 0.5-20 % by weight, and the content of described ester is 80-99.5 % by weight, wherein R
1for the hydrocarbyl group of C1-C20, R
2for the hydrocarbyl group of C1-C10.
Present invention also offers the preparation method of hydrophobic nano-silica emulsification plugging agent provided by the invention, it is R that the method comprises hydrophobic nano-silica and structural formula
1cOOR
2ester mixing, the add-on of hydrophobic nano-silica and described ester makes in the hydrophobic nano-silica emulsification plugging agent obtained, with the gross weight of described hydrophobic nano-silica emulsification plugging agent for benchmark, the content of hydrophobic nano-silica is 0.5-20 % by weight, the content of described ester is 80-99.5 % by weight, wherein R
1for the hydrocarbyl group of C1-C20, R
2for the hydrocarbyl group of C1-C10.
Present invention also offers the application that hydrophobic nano-silica emulsification plugging agent provided by the invention carries out water blockoff in oil well, described hydrophobic nano-silica emulsification plugging agent, crude oil are mixed by weight for 0.01-0.1:1:0.4-2.4 with water.
Adopt hydrophobic nano-silica emulsification plugging agent provided by the invention, be applied in crude oil and can obtain uniform and stable and that viscosity is higher emulsion, there is higher plugging strength, and this plugging agent composition is simply easy to oil field enforcement.
Other features and advantages of the present invention are described in detail in embodiment part subsequently.
Embodiment
Below the specific embodiment of the present invention is described in detail.Should be understood that, embodiment described herein, only for instruction and explanation of the present invention, is not limited to the present invention.
The invention provides a kind of hydrophobic nano-silica emulsification plugging agent, this hydrophobic nano-silica emulsification plugging agent contains hydrophobic nano-silica and structural formula is R
1cOOR
2ester; With the gross weight of described hydrophobic nano-silica emulsification plugging agent for benchmark, the content of hydrophobic nano-silica is 0.5-20 % by weight, and the content of described ester is 80-99.5 % by weight, wherein R
1for the hydrocarbyl group of C1-C20, R
2for the hydrocarbyl group of C1-C10.
Hydrophobic nano-silica emulsification plugging agent composition provided by the invention is simple, the hydrophobic nano-silica particle wherein contained is the nano silicon modified with hydrophobic group, particle surface not only containing a large amount of oil loving hydrocarbyl group, and contains hydrophilic silica group, oh group.The present inventor finds under study for action, and this hydrophobic nano-silica is easy to be dispersed in water-oil interface and stops the coalescence of drop, has the effect of extraordinary stable water-oil interface.Compared with the common tensio-active agent with interfacial activity, hydrophobic nano-silica granular absorption forms the interfacial film of high strength on water-oil interface, makes emulsion have extraordinary stability and higher viscosity, can realize good plugging effect.In addition; select suitable ester compound can there is very strong interaction with hydrophilic, the lipophilic group of hydrophobic nano-silica particle surface; very easily be adsorbed on particle surface; after mixing with hydrophobic nano-silica particle; further enhance its emulsifying capacity, improve the stability of water-oil interface.
In the present invention, hydrophobic nano-silica and specific ester combine, under specifically forming content, when the hydrophobic nano-silica emulsification plugging agent being more conducive to obtaining is applied to crude oil, can good stability be obtained and have more full-bodied emulsion, better plugging effect can be realized.Preferably, with the gross weight of described hydrophobic nano-silica emulsification plugging agent for benchmark, the content of hydrophobic nano-silica is 2-10 % by weight, and the content of described ester is 90-98 % by weight.
According to the present invention, in the hydrophobic nano-silica emulsification plugging agent provided, as long as the selection of the median size of described hydrophobic nano-silica can be meet the stability and higher viscosity that make emulsion have.Under preferable case, the median size of described hydrophobic nano-silica is below 100nm; Preferably, the median size of described hydrophobic nano-silica is below 50nm; More preferably, the median size of described hydrophobic nano-silica is below 20nm.Described hydrophobic nano-silica can also be commercially available, the R106 (median size 7nm) of such as German Degussa (EVONIK-DEGUSSA), R202 (median size 14nm), R972 (median size 16nm), R974 (median size 12nm), U.S.'s Cabot (CABOT) TS-530 (median size 20nm), day Bender mountain (TOKUYAMA) DM-10 (median size 10nm).
According to the present invention, under preferable case, described hydrophobic nano-silica contains connection finishing group on the silicon atoms, and described finishing group is the alkyl of C1-C12; Preferably, described finishing group is the alkyl of C1-C3; More preferably, described finishing group is methyl.
According to the present invention, in the structure of described ester, preferably, R
1for the hydrocarbyl group of C10-C15, R
2for the hydrocarbyl group of C1-C3; More preferably, described ester is at least one in ethyl acetate, ethyl laurate, the positive butyl ester of laurostearic acid and the positive butyl ester of ester in the last of the ten Heavenly stems.Select above-mentioned ester, can have with hydrophobic nano-silica and better mutually rent, strengthen the emulsifying capacity of described hydrophobic nano-silica emulsification plugging agent, improve the stability of water-oil interface.
Present invention also offers the preparation method of hydrophobic nano-silica emulsification plugging agent provided by the invention, it is R that the method comprises hydrophobic nano-silica and structural formula
1cOOR
2ester mixing, the add-on of hydrophobic nano-silica and described ester makes in the hydrophobic nano-silica emulsification plugging agent obtained, with the gross weight of described hydrophobic nano-silica emulsification plugging agent for benchmark, the content of hydrophobic nano-silica is 0.5-20 % by weight, the content of described ester is 80-99.5 % by weight, wherein R
1for the hydrocarbyl group of C1-C20, R
2for the hydrocarbyl group of C1-C10.Preferably, with the gross weight of described hydrophobic nano-silica emulsification plugging agent for benchmark, the content of hydrophobic nano-silica is 2-10 % by weight, and the content of described ester is 90-98 % by weight.In the present invention, the hydrophobic nano-silica emulsification plugging agent provided not only forms simply, and can prepare easily, is convenient to realize in oil field using.
Present invention also offers the application that hydrophobic nano-silica emulsification plugging agent provided by the invention carries out water blockoff in oil well, described hydrophobic nano-silica emulsification plugging agent, crude oil are mixed by weight for 0.01-0.1:1:0.4-2.4 with water.
Below will be described the present invention by embodiment.
In following examples, the emulsion that stability of emulsion passes through to prepare is at 80 DEG C of constant-temperature enclosed standing 48h, and observing emulsion is emulsion-stabilizing without oily water separation, otherwise emulsion is unstable.
Emulsion viscosity adopts GB/T10247-2008 method to use the HakkeVT550 rotational viscosimeter of ThermoFisher company to record.
The tensio-active agent used in embodiment is all commercially available.
Embodiment 1
The present embodiment is for illustration of hydrophobic nano-silica emulsification plugging agent provided by the invention and application.
By hydrophobic nano-silica, (nano particle median size is about 10nm, finishing type is methyl, Sigma-Aldrich's product) mix with ester, be mixed with hydrophobic nano-silica emulsification plugging agent, wherein each ingredient names and content are in table 1.
This hydrophobic nano-silica emulsification plugging agent and crude oil (density is about 0.91g/mL, and 50 DEG C of viscositys are about 60mPas), water are acutely mixed to form emulsion by shaker mixer.Prepared emulsion is put into the constant-temperature enclosed standing 48h of 80 DEG C, baking oven, crude oil weight, water weight, plugging agent consumption and observe emulsion-stabilizing situation estimated viscosity the results are shown in Table 1.
Embodiment 2
The present embodiment is for illustration of hydrophobic nano-silica emulsification plugging agent provided by the invention and application.
According to the method for embodiment 1, concrete each ingredient names and content, crude oil weight, water weight, plugging agent consumption and observe emulsion-stabilizing situation and estimated viscosity the results are shown in Table 1.
Embodiment 3
The present embodiment is for illustration of hydrophobic nano-silica emulsification plugging agent provided by the invention and application.
According to the method for embodiment 1, concrete each ingredient names and content, crude oil weight, water weight, plugging agent consumption and observe emulsion-stabilizing situation and estimated viscosity the results are shown in Table 1.
Embodiment 4
The present embodiment is for illustration of hydrophobic nano-silica emulsification plugging agent provided by the invention and application.
According to the method for embodiment 1, concrete each ingredient names and content, crude oil weight, water weight, plugging agent consumption and observe emulsion-stabilizing situation and estimated viscosity the results are shown in Table 1.
Embodiment 5
The present embodiment is for illustration of hydrophobic nano-silica emulsification plugging agent provided by the invention and application.
According to the method for embodiment 1, concrete each ingredient names and content, crude oil weight, water weight, plugging agent consumption and observe emulsion-stabilizing situation and estimated viscosity the results are shown in Table 1.
Table 1
Comparative example 1
1g nonyl phenol polyethers (polymerization degree 10) and 10g crude oil (density is about 0.91g/mL, and 50 DEG C of viscositys are about 60mPas), 10g water are acutely mixed to form emulsion by shaker mixer.
Prepared emulsion is put into the constant-temperature enclosed standing 48h of 80 DEG C, baking oven, observe emulsion-stabilizing situation, estimated viscosity.The results are shown in Table 2.
Comparative example 2
According to the method for comparative example 1, unlike, substitute " nonyl phenol polyethers (polymerization degree 10) " with " tween 20 (polymerization degree 20) ".
The results are shown in Table 2.
Comparative example 3
According to the method for comparative example 1, unlike, substitute " nonyl phenol polyethers (polymerization degree 10) " with " dodecanol polyethers (polymerization degree 80) ".
The results are shown in Table 2.
Comparative example 4
According to the method for comparative example 1, unlike, substitute " nonyl phenol polyethers (polymerization degree 10) " with " cetyl trimethylammonium bromide ".
The results are shown in Table 2.
Comparative example 5
By 0.2g hydrophobic nano-silica, (nano particle median size is about 10nm, finishing type is methyl, Sigma-Aldrich's product) be acutely mixed to form emulsion with 10g crude oil (density is about 0.91g/mL, and 50 DEG C of viscositys are about 60mPas), 10g water by shaker mixer.
Prepared emulsion is put into the constant-temperature enclosed standing 48h of 80 DEG C, baking oven, observe emulsion-stabilizing situation, estimated viscosity.The results are shown in Table 2.
Comparative example 6
According to the method for comparative example 5, unlike, substitute " 0.2g hydrophobic nano-silica " with " 1g n-butyl acetate ".
The results are shown in Table 2.
Table 2
As can be seen from the result of embodiment 1-5 and comparative example 1-6, hydrophobic nano-silica emulsification plugging agent provided by the invention contains hydrophobic nano-silica and structural formula is R
1cOOR
2ester match, be applied in crude oil and can form stable emulsion, leave standstill 48h through 80 DEG C of constant temperature and do not occur oily water separation, and emulsion viscosity reaches more than 200mPas, higher plugging strength can be had.And not containing nano silicon in comparative example 1-4 and 6, being only tensio-active agent is that oil hydrosol prepared by emulsifying agent, cannot form stable emulsion; And comparative example 5 is only containing nano silicon, also stable emulsion cannot be formed.
Embodiment 6
In order to measure plugging agent actual water plugging effect in the earth formation, displacement of reservoir oil evaluating apparatus (Shandong CUP Shiyi Science and Technology Co., Ltd.) is adopted to carry out water plugging property evaluation.
Test(ing) medium is the fill out sand tube of diameter 25mm, length 200mm, and test temperature is 50 DEG C (fill out sand tube making method adopts SY/T6315-2006 5.4.2 to save described dry dress method).First in fill out sand tube, fill up 30-40 μm of quartz sand, fill out sand tube is placed in displacement of reservoir oil evaluating apparatus, constant temperature 4h under 50 DEG C of test temperatures, inject distilled water, by measuring injection pressure, flowing liquid flow relocity calculation obtains fill out sand tube rate of permeation (adopting SY/T5336-2006 6.3.2 to save described fluid homeostasis permeability determination method), and numerical value is designated as stifled front rate of permeation kw0; Then the plugging agent that injection embodiment 1 obtains makes it fill up fill out sand tube hole, constant temperature places 24h, inject distilled water, improve injection pressure gradually, injection pressure when the first drop of liquid flows out from fill out sand tube end is plugging strength, obtain fill out sand tube rate of permeation by mensuration injection pressure, flowing liquid flow relocity calculation, numerical value is designated as stifled rear rate of permeation kw1.
Water plugging rate E%=((kw0-kw1)/kw0) × 100% is obtained with stifled rear computing permeability before stifled
The results are shown in Table 3.
Comparative example 7
According to the method for embodiment 6, unlike, the plugging agent that the plugging agent alternate embodiment 1 obtained by comparative example 1 obtains.The results are shown in Table 2.
Comparative example 8
According to the method for embodiment 6, unlike, the plugging agent obtained by the plugging agent alternate embodiment 1 obtained according to patent CN102061153.
This plugging agent preparation method is: by 110g technical grade 40 % by weight concentration dimethylamine and 400g clear water mixed diluting, 78g epoxy chloropropane is divided into four parts, within every 2 hours, adds portion, after all adding, be cooled to room temperature, add 412g clear water again, obtain 1kg water blockoff emulsifying agent.By 3g water blockoff emulsifying agent and 97g viscosity be 630mPas, moisture 0.3% dewatered oil mix, stir, obtain plugging agent.
The results are shown in Table 3.
Table 3
| Numbering | Plugging strength/MPa | kw0/μm 2 | kw1/μm 2 | E/％ |
| Embodiment 6 | 1.2 | 3.172 | 0.027 | 99.16 |
| Comparative example 7 | 0.02 | 3.166 | 3.037 | 4.07 |
| Comparative example 8 | 0.03 | 3.162 | 2.963 | 6.29 |
Comparative example 7 and 8 due to formed stability of emulsion poor, inject after profit be separated rapidly, occur seepage channel, thus plugging strength is significantly lower than embodiment 6.Adopt hydrophobic nano-silica emulsification plugging agent provided by the invention, the liquid for plugging good stability formed, has higher plugging strength and water plugging rate.
Claims (10)
1. a hydrophobic nano-silica emulsification plugging agent, this hydrophobic nano-silica emulsification plugging agent contains hydrophobic nano-silica and structural formula is R
1cOOR
2ester; With the gross weight of described hydrophobic nano-silica emulsification plugging agent for benchmark, the content of hydrophobic nano-silica is 0.5-20 % by weight, and the content of described ester is 80-99.5 % by weight, wherein R
1for the hydrocarbyl group of C1-C20, R
2for the hydrocarbyl group of C1-C10.
2. hydrophobic nano-silica emulsification plugging agent according to claim 1, wherein, with the gross weight of described hydrophobic nano-silica emulsification plugging agent for benchmark, the content of hydrophobic nano-silica is 2-10 % by weight, and the content of described ester is 90-98 % by weight.
3. hydrophobic nano-silica emulsification plugging agent according to claim 1 and 2, wherein, described hydrophobic nano-silica contains connection finishing group on the silicon atoms, and described finishing group is the alkyl of C1-C12.
4. hydrophobic nano-silica emulsification plugging agent according to claim 3, wherein, described finishing group is the alkyl of C1-C3.
5. hydrophobic nano-silica emulsification plugging agent according to claim 4, wherein, described finishing group is methyl.
6. hydrophobic nano-silica emulsification plugging agent according to claim 1 and 2, wherein, R
1for the hydrocarbyl group of C1-C15, R
2for the hydrocarbyl group of C1-C4.
7. hydrophobic nano-silica emulsification plugging agent according to claim 6, wherein, described ester is at least one in ethyl acetate, ethyl laurate, the positive butyl ester of laurostearic acid and the positive butyl ester of ester in the last of the ten Heavenly stems.
8. the preparation method of the hydrophobic nano-silica emulsification plugging agent in claim 1-7 described in any one, it is R that the method comprises hydrophobic nano-silica and structural formula
1cOOR
2ester mixing, the add-on of hydrophobic nano-silica and described ester makes in the hydrophobic nano-silica emulsification plugging agent obtained, with the gross weight of described hydrophobic nano-silica emulsification plugging agent for benchmark, the content of hydrophobic nano-silica is 0.5-20 % by weight, the content of described ester is 80-99.5 % by weight, wherein R
1for the hydrocarbyl group of C1-C20, R
2for the hydrocarbyl group of C1-C10.
9. method according to claim 8, wherein, with the gross weight of described hydrophobic nano-silica emulsification plugging agent for benchmark, the content of hydrophobic nano-silica is 2-10 % by weight, and the content of described ester is 90-98 % by weight.
10. the hydrophobic nano-silica emulsification plugging agent in claim 1-7 described in any one carries out the application of water blockoff in oil well, described hydrophobic nano-silica emulsification plugging agent, crude oil is mixed by weight for 0.01-0.1:1:0.4-2.4 with water.
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Application publication date: 20160511 |