CN1420153A - Aluminium citrate oil production additive and preparing process thereof - Google Patents
Aluminium citrate oil production additive and preparing process thereof Download PDFInfo
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Abstract
An aluminium citrate type additive for recovering petroleum has the formula of M0-2Al1-3C6H4-10O7N1-4X0.1-9, and is prepared through reaction of Al-containing aqueous solution with the aqueous solution containing radical of citric acid, adding alkaline substance or putting in ionic exchange resin for stabilizing and regulating pH value. Its advantages are high content of Al, excellent performance and high stability.
Description
Technical field
The present invention relates to oil recovery additive of a kind of Tiorco 677 type and preparation method thereof.
Background technology
In the oil production process, in order to improve the oil recovery yield, often need to add polyvalent metal ion, make polymkeric substance oil recovery injecting crosslinked, improved this polymer property.Just propose technology as far back as Needham in 1974 etc., studies show that, be detained resistance coefficient than using polymkeric substance to improve 6 times separately with multivalent metallic ion crosslinking PAM control mobility.The conclusion of Needham that Thomas etc. have used experiment confirm.Parmerswar etc. are research further, and the mechanism of permeability plugging proposed, he thinks two kinds of possibilities: a kind of is the delay of excess polymeric in core, this is created in the low zone of rate of permeation or polymer molecular size when very big with respect to the core aperture, and this explanation has obtained the support of the data that Vela etc. provides; Another kind is obstruction or crosslinked, because Al
3+Can be detained thereby be adsorbed onto the Al of rock stratum by the rock stratum intensive
3+With the interpolymer interaction that is detained, just produced crosslinkedly, formed obstruction.In fact these two kinds of mechanism are simultaneous.And in polymer molecular size during less than the effective pore radius, rock stratum, crosslinked or on the spot gel be the major cause that causes permeability plugging.
Operational polyvalent metal ion has Fe
3+, Fe
2+, Al
3+, Ti
4+, Zn
2+, Sn
4+, Ca
2+, Mg
2+, and Cr
3+One or more.At present commonly used have an Al
3+, Cr
3+Systematic studyes such as Seright the polymkeric substance of different systems/polyvalent metal ion distribution situation, these systems comprise Cr
3+/ CH
3COO
-/ HPAM, Cr
3+/ CH
3COO
-/ Resorcinol-formaldehyde, Cr
3+/ xanthan gum, Tiorco 677/HPAM etc.In the in Campable state NorthRainbow Ranch Unit oil field, adopt water drive to exploit out to be lower than 20% crude oil of reserves after because high osmotic pressure makes the water capacity easily penetrate oil reservoir, and produces very high water-oil ratio, cause the decline of injection pressure.Behind the using polymer gel, recovery ratio reaches 45% of crude oil reserves, improves petroleum production when wherein using Tiorco 677/PAM system and reaches 300,000 barrels, uses acetic acid acid chromium/PAM to improve petroleum production and reach 155,000 barrels.Hachanadel, S.m. etc. used the technology of polymer flooding and the summary that economy has been done system thereof in 15 years in the past to the Minnelsua oil field.
Gao, the PAM of different degree of hydrolysis such as H.W. and Cr
3+, Al
3+Gel carried out systematically research.The result shows, and Al
3+/ PAM system is compared, Cr
3+/ PAM has gelation rate and stronger gel-strength faster.And too fast gelation rate is undesirable in the deep layer water blockoff, and further studies show that: the gel with more weak gel-strength is by porous medium the time, its cross-linking part is under high shearing condition, can be destroyed, and under low shearing condition, can recover again, this characteristic is very favourable to the EOR technology.Mumallah, N.A. studies show that Cr
3+/ polymkeric substance is comparatively effective in high saliferous pool.
The compound of polyvalent metal ion or effectively complex compound or the use of inner complex form.The negatively charged ion of these complex compounds or inner complex is generally one or more in acetate moiety, itrile group nitrilotriacetic root, tartrate anion, citrate, tripolyphosphate, phosphate radical, metaphosphoric acid radical and the analogue.Complex compound or inner complex have postponed the generation and the gelation rate of polymer gelization.Because economy and use properties, Tiorco 677 are considered to best Al
3+The source, citrate can prevent Ca effectively simultaneously
2+, Mg
2+, comprise Al
3+Be precipitated out.
Comprehensive report both at home and abroad, Tiorco 677 is as the linking agent in the oil production, and production prices are low, and Al
3+All relatively good, easy to control with polymkeric substance gelation time and intensity, can form intramolecular colloidal dispersion system through suitable adjusting.But the hydrolysis under hot conditions of organoaluminum linking agent generates precipitation, very unstable, feasible linking agent Tiorco 677 is stable existence under low ph condition only, and Tiorco 677 is to the harsh requirement of envrionment conditions, make its technology of preparing become the difficult point and the focus of this area research, the industrialization of being unrealized so far of high-quality Tiorco 677 product has had a strong impact on its use in the oil field.
So-called Tiorco 677 is not meant the pure substance of Tiorco 677 or simple Tiorco 677, but a kind of composition is meant in the goods effective composition in oil recovery or other industry.
Patent USP3,762,476 disclose a kind of manufacture method of Tiorco 677, and this method is with Tai-Ace S 150 and Trisodium Citrate is dried mixes, and transports to the oil field then, is dispersed in and pumps into the rock stratum in the water.Owing to do not make the aluminum citrate solution method of stabilizing, mix the thing water-dispersion so have only to do before use.This method has several shortcomings: at first, the solids component dissolving is very slow.And usually can not dissolve fully, thereby do not dissolve hermetic unit and the moving parts that part can be corroded pump; Secondly, the pH value of solution is about 2.5, and this makes solution have corrodibility.In addition, because the use of Tai-Ace S 150 is introduced the rock stratum to sulfuric acid, when the sulfuric acid killing bacteria, generation has corrosive H
2S gas, and contaminate environment and crude oil;
Patent GB1,598,709 disclose the method for making of the aluminum citrate solution of preparation PH=4.1-4.2, and this solution is fit to leather industry, and for the intensified oil reduction technology, then acidity is too strong, and if during with NaOH adjusting pH value, most of Tiorco 677 will be precipitated out;
Patent USP3,200,136 and patent USP2,327, the technology that 815 pairs of preparations aluminum ion and citrate mol ratios are extremely rare Tiorco 677 of 1: 1 is studied, but because concentration is extremely rare, brought great inconvenience for transportation, storage and use, be not suitable for the needs of intensified oil reduction technology equally.
Many preparation methods about Tiorco 677 are successively abroad arranged, but up to 1996, the Julie E Smith of U.S. Tiorco company has invented breakthrough technology of preparing most, patent USP5,559,263 announce, use citric acid and aluminum chloride in the aqueous solution, can prepare aluminium content higher, be convenient to the dry powder form Tiorco 677 that stores and transport.Aluminium content is higher in the dry powder, can be used for secondary and tertiary oil recovery.
Summed up the manufacture method of Tiorco 677 in the past few decades in this patent, the outstanding contributions of this patent are to have illustrated the stable possibility of the aqueous solution or the dry powder of Tiorco 677.But aluminium content in the dry powder and the aluminium content in the solution all can't satisfy the requirement on the petroleum industry, and raw material is too harsh, and the aluminium content and the aluminium content in the solution that how to improve in the dry powder are the key points of dealing with problems.
Summary of the invention
The composition formula of the said Tiorco 677 type of the present invention oil recovery additive subtracts than being most:
M
0-2Al
1-3C
6H
4-10O
7N
1-4X
0.1-9
In the formula: M is sodium ion, potassium ion, calcium ion, barium ion, iron ion or ferrous ion;
X is chlorine, hydroxide radical, sulfate radical, nitrate radical or organic amine;
The mol ratio of aluminium and citrate is 0.5-3: 1.
Each component concentration (mass percent) is:
Aluminium: 8%-18%
NH
4 +： 3.2％-15.4％
C
6O
7： 31％-51％
Hydrogen: 2.8%-7.6%
X： 0.1％-46％
M： 0-12％
In order to obtain above-mentioned Tiorco 677 type oil recovery additive, the contriver at first reacts the aluminiferous aqueous solution and the aqueous solution that contains citrate ion, and then in reaction solution, add alkaline matter or reaction solution is inserted in the ion exchange resin, carry out stabilizing treatment, the potential of hydrogen of regulator solution can obtain said Tiorco 677 type oil recovery additive.Its preparation key step is as follows: the preparation of (1) solution:
Prepare the aqueous solution of aluminium salt and citric acid or its salt respectively, the concentration that makes the aqueous solution that contains citrate ion is concentration 0.33-2 times of the aluminiferous aqueous solution; (2) reaction
Above-mentioned preparation contain aluminum solutions under 20 ℃-100 ℃ and stirring condition, the above-mentioned aqueous solution that contains citrate ion is added drop-wise in the aluminiferous aqueous solution, reacted 0.5-10 hour, clarify until solution; Can drip the vitriol oil, concentrated hydrochloric acid or phosphoric acid in order to add fast response.(3) solution is stable
Alkaline reagents being added drop-wise to by in step (2) the gained solution, being 4.0-10.0 or will being inserted in the ion exchange resin by step (2) gained solution until the pH of solution value, is 4.0-10.0 until the pH of solution value, stirs and gets target product after 0.5-10 hour; Wherein: said aluminium salt is Aluminum chloride anhydrous, crystal aluminum chloride, polymerize aluminum chloride, sodium aluminate, potassium aluminate, aluminum nitrate, one or more in Tai-Ace S 150 and the aluminum bromide;
Said Citrate trianion is Trisodium Citrate and/or citric acid tri-amonia;
Said alkaline reagents is a sodium hydroxide, potassium hydroxide, hydrated barta, ammonium hydroxide, ammoniacal liquor, ammonia, sodium oxide, potassium oxide, sulfuric acid, hydrochloric acid, one or more in phosphoric acid and the ion exchange resin.
In addition, adopt the conventional drying method, as the solution of method dryings such as forced air drying method (temperature is at 15 ℃-200 ℃), crystallization process or spray method by the step 3 gained.Can obtain stable Tiorco 677 solid or crystal.
Compare with in the past Tiorco 677 solid, crystal or solution and synthetic method thereof, the invention has the advantages that:
1, the aluminium content height of Tiorco 677 solid of the present invention, crystal or solution, the high-content of solid or crystal are more than 18%, and the high-content of solution is more than 8%;
2, Tiorco 677 product of the present invention, can with polyacrylamide PAM, oil recovery polymer polymers such as partially hydrolyzed polyacrylamide HPAM are crosslinked, and delay cross linking, the retarded crosslinking system performance is good, helps improving the oil recovery yield;
3, the synthetic aluminum citrate solution can be directly as product among the present invention, or directly applies in the industrial circles such as oil recovery;
4, product of the present invention is convenient to transportation, can be at-40 ℃ of-200 ℃ of stable existences;
5, product performance of the present invention are stable, can stablize more than 2 years;
6, preparation process of the present invention is very simple, and is workable, is easy to suitability for industrialized production, and the energy save energy, and production cost is low.
Specific implementation method
By the following examples relevant details of the present invention is further elaborated.
Embodiment one
Place the reactor of 500ml to be made into the aqueous solution that aluminium composition is about 0.5mol/L in aluminum chloride, undissolved aluminum chloride is arranged in the solution, 80 ℃ and constantly stir under condition under, slowly drip and contain the aqueous solution that citric acid is about 0.25mol/L, undissolved aluminium salt in the solution, dissolving gradually is after dropwising, continue to stir about 0.5 hour, clarify until solution; The beginning dropping ammonia, at 1.4 o'clock, the adularescent precipitation produced in the pH value, disappear at 4.0 white precipitates up to the pH value of solution value, continue to stir about 4 hours, gained solution is behind Zeo-karb, the pH value of gained solution after the forced air drying, obtains milk yellow Tiorco 677 crystal 6.5.Aluminium content is 17.0% in the crystal.
Embodiment two
Place the reactor of 500ml to be made into the aqueous solution that aluminium composition is about 0.5mol/L polymerize aluminum chloride, undissolved polymerize aluminum chloride is arranged in the solution, 33 ℃ and constantly stir under condition under, slowly drip and contain the aqueous solution that citrate ion is about the 0.25mol/L citric acid tri-amonia, undissolved aluminium salt in the solution, dissolving gradually is after dropwising, continue to stir about 4.5 hours, clarify until solution; The beginning dropping sodium, continues to stir about 1.2 hours 4.6 up to the pH value of solution value, and gained solution obtains milk yellow Tiorco 677 powder behind recrystallization.Aluminium content is 15.7% in the powder.
Embodiment three
Place the reactor of 500ml to be made into the aqueous solution that aluminium composition is about 0.5mol/L in Tai-Ace S 150, undissolved Tai-Ace S 150 is arranged in the solution, 78 ℃ and constantly stir under condition under, slowly drip and contain the aqueous solution that citric acid is about 0.25mol/L, undissolved aluminium salt in the solution, dissolving gradually is after dropwising, continue to stir about 2 hours, clarify until solution; The beginning dropping ammonia, continues to stir about 3.2 hours 5.6 up to the pH value of solution value, and gained solution is through behind ion exchange resin, and the pH value of gained solution after the spraying drying, obtains milk yellow Tiorco 677 crystal 6.9.Aluminium content is 16.8% in the crystal.
Embodiment four
Place the reactor of 500ml to be made into the aqueous solution that aluminium composition is about 0.5mol/L polymerize aluminum chloride, undissolved aluminium salt is arranged in the solution, 86 ℃ and constantly stir under condition under, slowly drip and contain the aqueous solution that citrate is about 0.25mol/L, undissolved aluminium salt in the solution, dissolving gradually is after dropwising, continue to stir about 8 hours, clarify until solution; Gained solution is behind anionite-exchange resin, and the pH value of gained solution is 6.9.Aluminium content is 7.9% in the solution.
Embodiment five
To be made into the aqueous solution that aluminium composition is about 0.5mol/L as the reactor that aluminum chloride places 500ml to place, undissolved aluminium salt is arranged in the solution, 34 ℃ and constantly stir under condition under, slowly drip and contain the aqueous solution that citrate ion (as citric acid) is about 0.25mol/L, undissolved aluminium salt is arranged in the solution, and dissolving gradually is after dropwising, continue to stir about 2 hours, clarify until solution; Begin to feed ammonia,, continue to stir about 3.2 hours 8.3 up to the pH value of solution value, aluminium content is 6.1% in the gained solution solution.
Embodiment six is at 25 ℃,
The HPAM content of the aluminum chloride of the Al (III) of configuration PPM5000 is the aqueous solution of PPM5000, generates gel at once, and the gel dehydration;
The HPAM content of the Tiorco 677 (solid is chloride to be 15%) of the Al (III) of configuration PPM5000 is the aqueous solution of PPM5000, and along with the growth of time, viscosity increases gradually, and generates gel at 4-9 hour, and the gel dehydration;
The HPAM content of Tiorco 677 of the Al (III) of configuration PPM5000 is the aqueous solution of PPM5000, along with the growth viscosity of time increases gradually, and generates gel at the 32nd day, dehydration.
Embodiment seven is at 45 ℃
The HPAM content of the aluminum chloride of the Al (III) of configuration PPM5000 is the aqueous solution of PPM4000, generates gel at once, and the gel dehydration;
The HPAM content of the Tiorco 677 (solid is chloride to be 15%) of the Al (III) of configuration PPM5000 is the aqueous solution of PPM4000, and along with the growth of time, viscosity increases gradually, and generates gel in 4-9 hour, and the gel dehydration;
The HPAM content of the Tiorco 677 of the Al (III) of configuration PPM5000 is the aqueous solution of PPM4000, and along with the growth of time, viscosity increases gradually, and generates gel at the 38th day, not dehydration.
Embodiment eight is at 55 ℃
The HPAM content of the aluminum chloride of the Al (III) of configuration PPM3000 is the aqueous solution of PPM4000, generates gel at once, and the gel dehydration;
The HPAM content of the Tiorco 677 (solid is chloride to be 15%) of the Al (III) of configuration PPM3000 is the aqueous solution of PPM4000, and along with the growth of time, viscosity increases gradually, and generates gel at 3-7 hour, and the gel dehydration;
The HPAM content of the Tiorco 677 of the Al (III) of configuration PPM3000 is the aqueous solution of PPM4000, generates gel at the 30th day, not dehydration.
Embodiment nine is at 80 ℃
The HPAM content of the aluminum chloride of the Al (III) of configuration PPM2000 is the aqueous solution of PPM4000, generates gel at once, and gel dehydration, not dehydration;
The HPAM content of the Tiorco 677 (solid is chloride to be 15%) of the Al (III) of configuration PPM2000 is the aqueous solution of PPM4000, and along with the growth of time, viscosity increases gradually, and generates gel at 2-5 hour, and the gel dehydration;
The HPAM content of the Tiorco 677 of the Al (III) of configuration PPM2000 is the aqueous solution of PPM4000, and along with the growth of time, viscosity increases gradually, and generates gel the 3rd talent, gel dehydration in 3-4 days.
Embodiment ten is at 45 ℃
The HPAM content of the aluminum chloride of the Al (III) of configuration PPM1500 is the aqueous solution of PPM1000, generates gel at once, and the gel dehydration;
The HPAM content of the Tiorco 677 (solid is chloride to be 15%) of the Al (III) of configuration PPM1500 is the aqueous solution of PPM1000, and along with the growth of time, viscosity increases gradually, and generates gel at 4-20 hour, and the gel dehydration;
The HPAM content of the Tiorco 677 of the Al (III) of configuration PPM1500 is the aqueous solution of PPM1000, and along with the growth of time, viscosity increases gradually, and generates gel at the 28th day, not dehydration.
Claims (5)
1, a kind of Tiorco 677 type oil recovery additive is characterized in that described additive composition formula subtracts than being most:
M
0-2Al
1-3C
6H
4-10O
7N
1-4X
0.1-9In the formula: M is sodium ion, potassium ion, calcium ion, barium ion, iron ion or ferrous ion;
X is chlorine, hydroxide radical, sulfate radical, nitrate radical or organic amine;
The mol ratio of aluminium and citrate is 0.5-3: 1;
Each component concentration (mass percent) is:
Aluminium: 8%-18%
NH
4 +： 3.2％-15.4％
C
6O
7： 31％-51％
Hydrogen: 2.8%-7.6%
X： 0.1％-46％
M： 0-12％。
2, the described additive of preparation claim 1 is characterized in that described preparation method's key step is as follows:
(1) preparation of solution:
Prepare the aqueous solution of aluminium salt and citric acid or its salt respectively, the concentration that makes the aqueous solution that contains citrate ion is concentration 0.33-2 times of the aluminiferous aqueous solution;
(2) reaction
Above-mentioned preparation contain aluminum solutions under 20 ℃-100 ℃ and stirring condition, the above-mentioned aqueous solution that contains citrate ion is added drop-wise in the aluminiferous aqueous solution, reacted 0.5-10 hour;
(3) solution is stable
Alkaline reagents being added drop-wise to by in step (2) the gained solution, being 4.0-10.0 or will being inserted in the ion exchange resin by step (2) gained solution until the pH of solution value, is 4.0-10.0 until the pH of solution value, stirs and gets target product after 0.5-10 hour;
Wherein: said aluminium salt is Aluminum chloride anhydrous, crystal aluminum chloride, polymerize aluminum chloride, sodium aluminate, potassium aluminate, aluminum nitrate, one or more in Tai-Ace S 150 and the aluminum bromide; Said Citrate trianion is Trisodium Citrate and/or citric acid tri-amonia;
Said alkaline reagents is a sodium hydroxide, potassium hydroxide, hydrated barta, ammonium hydroxide, ammoniacal liquor, ammonia, sodium oxide, oxidation clock, sulfuric acid, hydrochloric acid, one or more in phosphoric acid and the ion exchange resin.
3, preparation method as claimed in claim 2 is characterized in that, in the step (2), adds the vitriol oil, concentrated hydrochloric acid or phosphoric acid in reaction system.
4, preparation method as claimed in claim 3 is characterized in that, wherein said aluminium salt is Aluminum chloride anhydrous, crystal aluminum chloride, polymerize aluminum chloride or Tai-Ace S 150.
5, preparation method as claimed in claim 4 is characterized in that, wherein said alkaline reagents is sodium hydroxide, ammoniacal liquor, ammonia or ion exchange resin.
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|---|---|---|---|
| CN 02151145 CN1420153A (en) | 2002-12-06 | 2002-12-06 | Aluminium citrate oil production additive and preparing process thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02151145 CN1420153A (en) | 2002-12-06 | 2002-12-06 | Aluminium citrate oil production additive and preparing process thereof |
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ID=4751931
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| CN102504292A (en) * | 2011-10-31 | 2012-06-20 | 扬州润达油田化学剂有限公司 | Organic cross linking system for polymer flooding and preparation method of cross linking agent |
| CN105712865A (en) * | 2014-12-02 | 2016-06-29 | 中国石油天然气股份有限公司 | Solid aluminum citrate cross-linking agent, preparation method and application thereof |
| CN107286917A (en) * | 2017-06-19 | 2017-10-24 | 中国地质大学（北京） | Retarded crosslinking gel diverting agent and preparation method thereof and composition and application |
| CN108456513A (en) * | 2017-02-20 | 2018-08-28 | 中国石油化工股份有限公司 | A kind of fracturing fluid organic aluminum crosslinker, preparation method and application |
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2002
- 2002-12-06 CN CN 02151145 patent/CN1420153A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102504292A (en) * | 2011-10-31 | 2012-06-20 | 扬州润达油田化学剂有限公司 | Organic cross linking system for polymer flooding and preparation method of cross linking agent |
| CN102504292B (en) * | 2011-10-31 | 2013-10-02 | 扬州润达油田化学剂有限公司 | Organic cross linking system for polymer flooding and preparation method of cross linking agent |
| CN105712865A (en) * | 2014-12-02 | 2016-06-29 | 中国石油天然气股份有限公司 | Solid aluminum citrate cross-linking agent, preparation method and application thereof |
| CN108456513A (en) * | 2017-02-20 | 2018-08-28 | 中国石油化工股份有限公司 | A kind of fracturing fluid organic aluminum crosslinker, preparation method and application |
| CN108456513B (en) * | 2017-02-20 | 2021-09-10 | 中国石油化工股份有限公司 | Organic aluminum crosslinking agent for fracturing fluid, preparation method and application |
| CN107286917A (en) * | 2017-06-19 | 2017-10-24 | 中国地质大学（北京） | Retarded crosslinking gel diverting agent and preparation method thereof and composition and application |
| CN110105938A (en) * | 2019-05-14 | 2019-08-09 | 中国石油大学(华东) | A kind of high intensity retarded crosslinking chromium gel and preparation method thereof |
| CN113234425A (en) * | 2021-04-09 | 2021-08-10 | 中国石油大学(华东) | Composite aluminum gel plugging agent for deep profile control of medium-low permeability oil reservoir and preparation method and application thereof |
| CN113234425B (en) * | 2021-04-09 | 2023-02-28 | 中国石油大学(华东) | Composite aluminum gel plugging agent for deep profile control of medium-low permeability oil reservoir and preparation method and application thereof |
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