CN104402740B - Acidification diversion agent octadecylbutyldihydroxyethyl ammonium bromide and its preparation method and use - Google Patents
Acidification diversion agent octadecylbutyldihydroxyethyl ammonium bromide and its preparation method and use Download PDFInfo
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Abstract
The invention relates to an acidification diversion agent octadecylbutyldihydroxyethyl ammonium bromide and its preparation method and use. A two-step synthesis method of the acidification diversion agent octadecylbutyldihydroxyethyl ammonium bromide comprises that 1, diethanolamine and 1-bromobutane undergo a reaction in the presence of sodium bicarbonate as an assistant to produce N-tert-butyldiethanolamine, and 2, the N-tert-butyldiethanolamine and bromooctadecane undergo a reaction to produce the desired product. The invention also provides the use of the acidification diversion agent. A self-diversion acid adopting the acidification diversion agent as a main agent has a use temperature range of 40-60 DEG C. In acidification, the acidification diversion agent can realize automatic diversion, deep penetration and uniform and efficient acidification of stratum, has good adsorptivity, and can effectively reduce acid filtration loss. The acidification diversion agent can realize automatic gel breaking when contacting hydrocarbon after acidification, can be returned easily, and has no residue, no secondary damage and low toxicity.
Description
Technical field
The present invention relates to a kind of acidified diverting agent octadecyl butyl dihydroxy ethyl brometo de amonio and preparation method thereof and application, belong to technical field of petrochemical industry.
Background technology
Acidifying can remove pollution and the blocking of immediate vicinity of wellbore oil reservoir effectively, improves the connectedness of pit shaft and immediate vicinity of wellbore reservoir, increases oil well productivity.Minimum impedance concept is followed in the flowing of acid solution, and in acidization, acid solution preferentially enters the good reservoir of perviousness.In the reservoir that nonuniformity is stronger, major part acid solution enters middle and high pervious course, only has small part acid solution even not have acid solution to enter low permeability layer, this is not only difficult to realize reservoir homogeneous acidification, the object increasing oil well productivity, the nonuniformity of reservoir can be made on the contrary to strengthen further, strengthen exploitation difficulty.Therefore, adopt acid solution steering technique to realize homogeneous acidification reservoir, improve acidifying section, significant to well production increment.
According to steering mechanism, acid solution steering technique is generally divided into mechanical steering and chemistry diversion.Mechanical steering mainly comprises pkr and turns to and turn to particle, and mechanical steering technology is comparatively ripe, but complicated operation, expensive, and when turning to acidifying to the reservoir containing many little thin layers and crack, the turning efficiency of acid solution is poor; Compare mechanical steering technology, chemistry diversion technology has easy construction, feature that risk is low, chemistry diversion technology mainly comprises that particulate turns to, foam turns to, polymkeric substance turns to and turns to tensio-active agent, particulate steering technique easily causes secondary injury to reservoir, foam steering technique steering capability is limited, ooze in reservoir at height and easily cause leak-off, polymkeric substance steering technique still has number of polymers to remain in reservoir after the row of returning, and causes serious secondary injury to reservoir.
Viscoelastic surfactant steering technique has that technique is simple, turning efficiency good, the feature of slow filtrate reducing, is that the self-diverting acid of host has been widely used in the acidifying of Heterogeneous reservoir with viscoelastic surfactant.Such as, patent CN103086909A provides a kind of low damage agent for heterogeneous body fracture acid system, for erucicamide CAB, can realize automatically becoming sticky along with the carrying out of acid-rock reaction by the acid fluid system of its preparation, produce higher resistance to flow, realize the effective distribution of acid solution in reservoir, there is the filter loss reducing acid solution, increase the penetration range of acid solution, guarantee the feature that acid fluid system low damage effectively carries out; Patent CN102559168A has invented a kind of acid-sensitive variable-viscosity mixed surfactant, and tensio-active agent described in invention is mixed by quality 1:4 ~ 4:1 by sulphonate Gemini surfactant and alkyl glycoside nonionogenic tenside.The viscosity of mixed system is high, but after acid adding in system, viscosity declines rapidly.Acid sensitivity mixed surfactant system containing acid causes soltion viscosity to raise by the consumption of acid, having the feature of Automatic-searching low permeability interval, possessing low damage function, can realize homogeneous acidification, obtaining good acidizing effect when carrying out oil reservoir acidifying.Acid sensitivity mixed surfactant viscosity after acidifying containing acid is high, but understands automatic viscosity reduction after it contacts with crude oil or hydrocarbons, and viscosity, close to the viscosity of water, is easy to the row of returning.
Summary of the invention
Based on the deficiencies in the prior art, the invention provides a kind of acidified diverting agent octadecyl butyl dihydroxy ethyl brometo de amonio and preparation method.
The present invention also provides octadecyl butyl dihydroxy ethyl brometo de amonio as the application of acidified diverting agent.
The present invention also provides a kind of oil-gas field souring method.
The present invention also provides the self-diverting acid composition prepared for acidified diverting agent (host) with octadecyl butyl dihydroxy ethyl brometo de amonio.Effectively homogeneous acidification can be carried out to Heterogeneous reservoir with the self-diverting acid that octadecyl butyl dihydroxy ethyl brometo de amonio is prepared for acidified diverting agent (host).
Technical scheme of the present invention is as follows:
A kind of acidified diverting agent, it is characterized in that octadecyl butyl dihydroxy ethyl brometo de amonio.Molecular formula: C
26h
56o
2brN.Structural formula is as shown in the formula shown in I:
A preparation method for acidified diverting agent octadecyl butyl dihydroxy ethyl brometo de amonio, comprise two-step reaction, step is as follows:
(1) condensation reaction
Diethanolamine and bromination of n-butane press 1:1 mixed in molar ratio, add sodium bicarbonate and make auxiliary agent, and stirring and refluxing reaction 3-5h under 90-110 DEG C of constant temperature oil bath condition, underpressure distillation steams the water of generation, obtains N butyl diethanol amine.
In this step (1), setting-up point preferably 100 DEG C; The preferred 4h of reflux time;
(2) quaterisation
N butyl diethanol amine prepared by step (1) and bromo-octadecane are by 1:1 mixed in molar ratio, add sodium bicarbonate and make auxiliary agent, stirring and refluxing reaction 9-11h under 130-150 DEG C of constant temperature oil bath condition, underpressure distillation steams the water of generation, obtains octadecyl butyl dihydroxy ethyl brometo de amonio.
In this step (2), quaterisation temperature preferably 140 DEG C; Reaction times preferred 10h.
According to the present invention, the reaction formula of two-step reaction is as follows:
Step (1) reaction formula is as follows:
Step (2) reaction formula is as follows:
Preferred according to the present invention, add the hydrogen bromide that sodium bicarbonate auxiliary agent is conducive to removing dereaction generation in step (1), (2).Sodium bicarbonate in step (1): diethanolamine=1 ~ 1.5:1 mol ratio, sodium bicarbonate in step (2): bromo-octadecane=1 ~ 1.2:1 mol ratio.
Octadecyl butyl dihydroxy ethyl brometo de amonio of the present invention, as the application of acidified diverting agent, carries out homogeneous acidification to Heterogeneous reservoir.
According to the present invention, octadecyl butyl dihydroxy ethyl brometo de amonio is as the application of acidified diverting agent, it is the self-diverting acid prepared for host with octadecyl butyl dihydroxy ethyl brometo de amonio, wherein octadecyl butyl dihydroxy ethyl brometo de amonio consumption concentration in self-diverting acid is 6-8% mass ratio, and optimum amount is 6% mass ratio.
The use temperature scope of the self-diverting acid prepared by octadecyl butyl dihydroxy ethyl brometo de amonio is at 40-60 DEG C.
The self-diverting acid prepared by octadecyl butyl dihydroxy ethyl brometo de amonio can carry out homogeneous acidification to Heterogeneous reservoir effectively.
A kind of oil-gas field souring method, is characterized in that using octadecyl butyl dihydroxy ethyl brometo de amonio of the present invention as acidified diverting agent, the Oil/gas Well of oil-gas field to be carried out to the method for acidifying.
For a self-diverting acid for heterogeneous reservoir acidifying transformation, be made up of following mass percent component:
Acidified diverting agent octadecyl butyl dihydroxy ethyl brometo de amonio: 6-8%;
Turn to synergistic agent hydroxypropylguar gum: 0.3%-0.5%,
Organic borate cross-linker LGD (BOH)
6: 0.2%-0.4%,
Anti-swollenly press down sand agent Hydrin-dimethylamine: 2%-4%,
Cleanup additive three quaternary surfactant: 0.5%-1.5%,
Reverse wetting agent alcohol ether: 8%-12%, alcohol ether is made up of ethylene glycol and propylene glycol, mass ratio 0.75-1:1;
Hydrochloric acid: 6%-10% (in HCl);
All the other are water.
Preferred according to the present invention, the quality proportioning of described self-diverting acid is: acidified diverting agent octadecyl butyl dihydroxy ethyl brometo de amonio consumption concentration in self-diverting acid is 6-8%, synergistic agent hydroxypropylguar gum consumption concentration is turned to be 0.4%, linking agent organic boron LGD (BOH)
6consumption concentration is 0.3%, prevent that but swollen sand agent Hydrin-dimethylamine consumption concentration is 3%, cleanup additive three quaternary surfactant consumption concentration is 1%, reverse wetting agent alcohol ether consumption concentration is 10%, wherein alcohol ether is made up of ethylene glycol and propylene glycol 0.85:1, hydrochloric acid is 8%, and all the other are water.
Above-mentioned raw materials is well known materials, can be bought by market.
The present inventor studies and finds that octadecyl butyl dihydroxy ethyl brometo de amonio adaptive temperature scope is wide, just shows significant visco-elasticity when minimum temperature reaches 40 DEG C; Be interweaved between molecular layer, between plane micella branch during plastic, tangle into a three-dimensional network structure, and layer of structure sense is strong, as shown in Figure 1.Octadecyl butyl dihydroxy ethyl brometo de amonio product possesses good viscosity in residual acid system, and acid solution can be made to possess steering capability in the earth formation.
The self-diverting acid prepared for acidified diverting agent with octadecyl butyl dihydroxy ethyl brometo de amonio in acidization can auto-steering, deep penetrate, uniform high-efficiency ground acidifying strata, this acidified diverting agent excellent adsorption, effectively can reduce acid liquid loss, meet hydrocarbon after acidifying and automatically break glue, the easily row of returning, without residue, secondary injury, toxicity can not be caused low.
Accompanying drawing explanation
Fig. 1 is that octadecyl butyl dihydroxy ethyl brometo de amonio product S EM prepared by embodiment 1 observes plastic structure iron.
Fig. 2 is the octadecyl butyl dihydroxy ethyl brometo de amonio product that embodiment 1 obtains, thick white shape colloid.
Fig. 3 is the relation curve of residual acid system viscosity and octadecyl butyl dihydroxy ethyl brometo de amonio concentration.
Fig. 4 is the relation curve of residual acid system viscosity and residual acid system pH value.
Fig. 5 is the relation curve of residual acid system viscosity and temperature.
Fig. 6 is residual acid solution is 6wt%, 22wt%CaCl2, pH=5.4 in octadecyl butyl dihydroxy ethyl brometo de amonio concentration, residual acid solution system status under temperature 21 DEG C of conditions.
Fig. 7 is acidizing treatment graphic representation.
Embodiment
The main agents that embodiment adopts has diethanolamine (CP), bromination of n-butane (CP) and bromo-octadecane (CP) all purchased from Chemical Reagent Co., Ltd., Sinopharm Group.Hydrin-dimethylamine is purchased from Zibo three good fortune chemical development company limited.Hydroxypropylguar gum, linking agent organic boron LGD (BOH)
6be Dongying City and believe that Dehua work limited liability company product is sold, three quaternary surfactants are purchased from east, Ningbo Yongning Chemical Industry Science Co., Ltd.
Concentration in embodiment is mass percent concentration, except special instruction.
Embodiment 1: the preparation of octadecyl butyl dihydroxy ethyl brometo de amonio
(1) condensation reaction
Add to after getting 0.05mol diethanolamine and the mixing of 0.05mol bromination of n-butane in the there-necked flask of the 500mL of band condensation reflux unit, add 0.05mol sodium bicarbonate (hydrogen bromide for generating except dereaction) again, be placed in thermostatical oil bath, stirring and refluxing reaction 4h under 100 DEG C of conditions, underpressure distillation steams the water of generation, can obtain the deep yellow color liquid N butyl diethanol amine solution that intermediate product is slightly thick.
(2) quaterisation
Getting the tertiary amine that step is obtained by reacting adds in 500mL there-necked flask, add 0.05mol bromo-octadecane and 0.05mol sodium bicarbonate, be placed in thermostatical oil bath stirring and refluxing reaction 10h under 140 DEG C of conditions, underpressure distillation steams the water of generation, finally obtain white paste liquid, be octadecyl butyl dihydroxy ethyl brometo de amonio (see Fig. 2).
Embodiment 2, the octadecyl butyl dihydroxy ethyl brometo de amonio prepared by embodiment 1, the concentration preparing 5 groups of octadecyl butyl dihydroxy ethyl brometo de amonios is respectively the residual acid solution of 4%, 5%, 6%, 7%, 8%, and method is as follows:
(1) get 5 clean beakers (specification is 200mL), in 5 beakers, add distilled water 74g, 73g, 72g, 71g, 70g respectively successively;
(2) 5 groups of CaCl are taken under room temperature respectively
2solid, often organizes 22g, adds 5 respectively and fills in the beaker of distilled water, is stirred to evenly; Add octadecyl butyl dihydroxy ethyl brometo de amonio under room temperature respectively, often group 4g, 5g, 6g, 7g, 8g respectively, is stirred to evenly;
(3) add hydrochloric acid respectively in above-mentioned 5 groups of solution, the pH value of 5 groups of solution is adjusted to 5.4, the concentration of obtained octadecyl butyl dihydroxy ethyl brometo de amonio is the residual acid solution of 4%, 5%, 6%, 7%, 8%;
Above-mentioned 5 groups of residual acid solution CaCl
2concentration is 22%, pH value 5.4, and octadecyl butyl dihydroxy ethyl brometo de amonio concentration is respectively 4%, 5%, 6%, 7%, 8%, and under 60 DEG C of conditions, measure its viscosity respectively, measurement result is in table 1 and Fig. 3.
At 60 DEG C, table 1, residual acid solution viscosity is with the data sheet of octadecyl butyl dihydroxy ethyl brometo de amonio change in concentration
| Concentration/% | 4 | 5 | 6 | 7 | 8 |
| Viscosity/mPas | 54.3 | 62.0 | 523.1 | 704.5 | 796.7 |
As can be seen from table 1 and Fig. 3, along with the rising of octadecyl butyl dihydroxy ethyl brometo de amonio concentration, the viscosity of residual acid system is also increased significantly.When concentration is less, the viscosity of residual acid system is less than 100mPas, this is because now octadecyl butyl dihydroxy ethyl brometo de amonio concentration is near micelle-forming concentration, mainly form globular micelle in system, viscosity is lower; When octadecyl butyl dihydroxy ethyl brometo de amonio concentration reaches 6%, system viscosity increases rapidly, can reach 523.1mPas, then along with the continuation of concentration increases, residual acid system viscosity also continues to increase, and now in system, acidified diverting agent molecule forms cylindrical micellar, causes viscosity significantly to improve.Can determine that the working concentration of octadecyl butyl dihydroxy ethyl brometo de amonio should be greater than 6% by experimental data and analysis, consider cost factor, determine that working concentration is 6-8%, optimum amount is 6%.
Embodiment 3, the octadecyl butyl dihydroxy ethyl brometo de amonio prepared by embodiment 1, prepare 4 groups of pH value and be respectively 4,5,6,7 residual acid solutions, method is as follows:
(1) get 4 clean beakers (specification is 200mL), in each beaker, add 72g distilled water respectively;
(2) 4 groups of CaCl are taken under room temperature respectively
2solid, often organizes 22g, adds 4 respectively and fills in the beaker of distilled water, is stirred to evenly; Add octadecyl butyl dihydroxy ethyl brometo de amonio respectively, often organize 6g, be stirred to evenly;
(3) add hydrochloric acid respectively in above-mentioned 4 groups of solution, solution ph is transferred to 4,5,6,7 respectively.
Above-mentioned 4 groups of residual acid solution CaCl
2concentration is 22%, and octadecyl butyl dihydroxy ethyl brometo de amonio concentration is 6%, and pH value is respectively 4,5,6,7, under 60 DEG C of conditions, measure its viscosity respectively, and measurement result is in table 2 and Fig. 4.
The data sheet that at 60 DEG C, table 2, residual acid solution viscosity changes with pH value
| pH | 4 | 5 | 6 | 7 |
| Viscosity/mPas | 376.2 | 520.0 | 525.7 | 560.5 |
As can be seen from table 2 and Fig. 4, along with system pH must increase, the viscosity of residual acid system also increases thereupon.As residual acid system pH>5, residual acid system viscosity can reach more than 500mPas, the instrument measuring residual acid system viscosity is selected to be Brookfield viscometer, because its rotor is easily subject to acid liquid corrosion, so experiment and undetermined pH<4 time residual acid system viscosity, as can be seen from Fig. 4 curvilinear trend, for fresh acid solution and pH value in 1 ~ 2 scope, its viscosity is lower than 100mPas, can determine as the self-diverting acid that diversion agent is prepared, to there is good steering qualities using octadecyl butyl dihydroxy ethyl brometo de amonio by experimental data and analysis.
Embodiment 4, the octadecyl butyl dihydroxy ethyl brometo de amonio prepared by embodiment 1, prepare 6 groups of residual acid solutions:
(1) get 6 clean beakers (specification is 200mL), in each beaker, add 72g distilled water respectively;
(2) 6 groups of CaCl are taken under room temperature respectively
2solid, often organizes 22g, adds 6 respectively and fills in the beaker of distilled water, is stirred to evenly; Add octadecyl butyl dihydroxy ethyl brometo de amonio under room temperature respectively, often organize 6g, be stirred to evenly;
(3) add hydrochloric acid respectively in above-mentioned 6 groups of solution under room temperature, the pH value of 6 groups of solution is adjusted to 5.4.
Above-mentioned 6 groups of residual acid solution CaCl
2concentration is 22%, pH=5.4, octadecyl butyl dihydroxy ethyl brometo de amonio concentration are 6%, respectively the viscosity of residual acid system at different temperatures, experimental result in table 3, Fig. 5.
The data sheet of the residual acid solution viscosity with temperature change of table 3
| Temperature/DEG C | 47.1 | 49.6 | 54.4 | 59.6 | 64.2 | 79.5 |
| Viscosity/mPas | 1003.0 | 879.2 | 589.5 | 538.3 | 64.0 | 79.2 |
As can be seen from table 3 and Fig. 5, along with the rising of temperature, the viscosity of residual acid solution reduces gradually.The instrument measuring viscosity is selected to be Brookfield viscometer, the peak viscosity that it can measure is 8000mPas, and when temperature is lower than 47.1 DEG C, the viscosity of residual acid system has exceeded the maximum useful range of viscometer, now soltion viscosity is very high, in the pasty state (see Fig. 6).When temperature is higher than 60 DEG C, residual acid system viscosity reduces rapidly, between 60 ~ 80mPas.Can determine that the use temperature scope of octadecyl butyl dihydroxy ethyl brometo de amonio is at 40 ~ 60 DEG C by experimental data and analysis.
Embodiment 5: self-diverting acid composition and application
(1) the octadecyl butyl dihydroxy ethyl brometo de amonio adopting embodiment 1 to prepare prepares self-diverting acid as acidified diverting agent, and mass percent is composed as follows:
Acidified diverting agent octadecyl butyl dihydroxy ethyl brometo de amonio 6%;
Turn to synergistic agent hydroxypropylguar gum 0.4%;
Linking agent organic boron LGD (BOH)
60.3%;
Anti-swollenly press down sand agent Hydrin-dimethylamine 3%;
Cleanup additive three quaternary surfactant 1%;
Reverse wetting agent alcohol ether concentration is 10%; Alcohol ether is made up of ethylene glycol and propylene glycol 0.85:1
Hydrochloric acid 8% (in HCl);
All the other are water.
During preparation self-diverting acidizing fluids, mass concentration is 30%-38% technical hydrochloric acid, and in the self-diverting acid prepared, the mass concentration of HCl is 8%.
(2) application of self-diverting acid:
By the self-diverting acid of the formulated in (1), and test in place will be carried out at the old 3 fault block X wells of Jiangsu Gaoyou Depression Chen Bao structure.This test pit adopts self-diverting acid metallization processes, design acid amount 38m
3, construction well section span 5m (2150.6-2155.6m), discharge capacity 0.28-0.35m
3/ min, operation pressure 17-20MPa.Acidizing treatment curve as shown in Figure 7.After acid solution enters stratum, starting stage displacement variation is little but pressure amplification is obvious, shows that the self-diverting acid viscosity entering high permeability zones increases sharply, forces follow-up fresh acid to turn to into hyposmosis district, turn to acidizing effect obvious.After construction, oilwell produced fluid amount brings up to the 21t/d after measure by 3t/d before measure, and de-plugging increases liquid Be very effective.
Claims (3)
1. a preparation method for acidified diverting agent octadecyl butyl dihydroxy ethyl brometo de amonio, comprise two-step reaction, step is as follows:
(1) condensation reaction
Diethanolamine and bromination of n-butane press 1:1 mixed in molar ratio, add sodium bicarbonate and make auxiliary agent, stirring and refluxing reaction 3-5h under 90-110 DEG C of constant temperature oil bath condition, and underpressure distillation steams the water of generation, obtains N butyl diethanol amine;
(2) quaterisation
N butyl diethanol amine prepared by step (1) and bromo-octadecane are by 1:1 mixed in molar ratio, add sodium bicarbonate and make auxiliary agent, stirring and refluxing reaction 9-11h under 130-150 DEG C of constant temperature oil bath condition, underpressure distillation steams the water of generation, obtains octadecyl butyl dihydroxy ethyl brometo de amonio.
2. the preparation method of octadecyl butyl dihydroxy ethyl brometo de amonio as claimed in claim 1, is characterized in that, in step (1), setting-up point is 100 DEG C; Reflux time 4h.
3. the preparation method of octadecyl butyl dihydroxy ethyl brometo de amonio as claimed in claim 1, is characterized in that, in step (2), quaterisation temperature is 140 DEG C; Reaction times 10h.
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| CN108384528B (en) * | 2018-03-12 | 2020-07-10 | 中国石油天然气股份有限公司 | Diverting agent for diverting and acidifying water injection well and preparation method thereof |
| CN109762543A (en) * | 2019-02-20 | 2019-05-17 | 中国石油大学(华东) | A kind of heat-resistant salt-resistant is from Tackified emulsion work-in-progress control diversion agent and preparation method thereof |
| CN110951475A (en) * | 2019-12-31 | 2020-04-03 | 西南石油大学 | Ultra-high temperature resistant low-viscosity low-corrosion emulsifier, emulsified acid system and preparation method thereof |
| CN111154478B (en) * | 2020-01-14 | 2022-11-01 | 中国石油天然气股份有限公司 | Filtrate reducer for enlarging effective action distance of acid liquor and preparation method and application thereof |
| CN113004883A (en) * | 2021-03-22 | 2021-06-22 | 郑州市新郑梅久实业有限公司 | Cleanup additive for fracturing and preparation method thereof |
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