CN103450872A - Authigenic acid system and its application - Google Patents
Authigenic acid system and its application Download PDFInfo
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Abstract
The invention relates to an authigenic acid system and its application. The authigenic acid contains ZX-339 and ZX-368 components, the mole ratio of n(ZX-339) to n(ZX-368) is 5:8. Under a reaction temperature of 70DEG C-100DEG C, 19%-21% hydrochloric acid can be produced. The ZX-339 is any one of allyl chloride, benzoyl chloride, and a chlorinated organic ammonium salt. The ZX-368 is any one of polydimethylaminobenzaldehyde and polyhexa aldehyde. A clean acid fracturing fluid system is employed to carry the authigenic acid system to deep stratum. During application, the authigenic acid is compounded from, by weight: 2% of ZX-19, 15-20% of hydrochloric acid, 2% of ZX-09, 1% of ZX-10, (12-18)% of ZX-339, (10-16)% of ZX-368, and the balance water. The corrosion ability of the authigenic acid is equivalent to 70%-74% of that of isoconcentration hydrochloric acid.
Description
Technical field
The present invention relates to a kind of spontaneous acid system and application thereof.Specifically a kind of acid solution body system and application thereof that is applicable to the deep acid fracturing of high temperature carbonate rock reservoir.
Background technology
In recent years, the exploitation of carbonate reservoir causes people's attention day by day.Carbonate reservoir generally has the characteristics such as hypotonic, that nonuniformity is strong, usually needs to transform and improve its production capacity by volume increase.Acid fracturing is one of well stimulation that carbonate reservoir is commonly used, its mechanism is: the use acid solution is carried out non-homogeneous etching to the wall of man-made fracture, making operation pressure remove rear crack wall can not be fully closed, thereby forms a flow passage with certain flow conductivity.The effect of acid fracturing transformation depends primarily on acid corrosion fracture and acid-etched fracture length.
Yet it is darker that carbonate reservoir generally buries, and reservoir temperature is higher, conventional acid solution can be reacted with rock and consume rapidly after being entered stratum, can't be penetrated into earth formation deep, and the acid-etched fracture length of generation is very limited, has restricted the effect of acid fracturing transformation.Therefore develop a kind ofly can slow down sour rock speed of response, deep penetrating acid fluid system is very necessary.
Have at present some and be applicable to the acid fluid system of carbonatite deep acid fracturing, as gel acid, emulsified acid, the acid that becomes sticky, surfactivity acid etc., they have slowed down sour rock speed of response by improving the modes such as acid liquid viscosity, minimizing acid and rock contact area, but, due to its various shortcomings, be subject to larger limitation on the scope of application.Such as gel acid and the acid that becomes sticky at high temperature still have speed of response faster with rock, penetration range is limited; Emulsified acid is difficult for preparation, and frictional resistance is higher, in deep-well, high pressure reservoir, uses difficulty large; Surfactivity acid cost is high, be difficult to preparation, should not promote the use of.Spontaneous acid is a kind of more satisfactory deep penetration acid, but the spontaneous acid system of current routine is mainly used in the sandstone reservoir acidifying; At present both at home and abroad also not for the spontaneous acid system of the maturation of carbonate reservoir.
Developed a kind of spontaneous acid system that is applicable to high temperature carbonate rock reservoir deep acid fracturing under this background.
Summary of the invention
The purpose of this invention is to provide a kind of spontaneous acidifying formula that is applicable to the carbonate reservoir acid fracturing, chemical reaction does not occur in this spontaneous acid formula on ground, do not there is at normal temperatures the corrosion ability, pump into behind stratum along with being heated by stratum, can react gradually and discharge hydrochloric acid, temperature is higher, and the time is longer, the hydrochloric acid generated is more, reaches the purpose to the transformation of high temperature carbonate rock reservoir deep; This spontaneous acid formula have cost low, prepare simple advantage, be convenient to promote the use of.
Ultimate principle: the chlorion in the organic chloride salt of basic metal or ammonium can generate hydrochloric acid under the initiator effects such as aldehyde, ketone, organic carboxyl acid, such as:
HCOOH+NH
4Cl→NH
4 ++HCOO
-+HCl
Poly-many aldehyde (ZX-368) that the reactant that the present invention selects is a kind of chlorination organic ammonium salt (ZX-339) and a kind of appropriate polymerization degree.At a certain temperature, these two kinds of materials mix and can react generation hydrochloric acid in water:
ZX-339+6ZX-368→C
6H
12NH
4 ++3H
++H
2O
Carried out by experiment formula optimization:
1. liquid ZX-339 and ZX-368 at room temperature react, undesirable; Select the ZX-368 of solid, can guarantee not react under room temperature.
2. it is limited that the ZX-368 of equivalent reacts the concentration of hydrochloric acid produced with ZX-339; Use excessive (ZX-368), can improve level of response, increase the hydrochloric acid productive rate.
3. take into account Cost Problems, finally determine that ZX-339 reacts best proportioning and is with ZX-368: n (ZX-339): n (ZX-368)=5:8; While using this proportioning, under 70 ° of C ~ 100 ° C of temperature of reaction, can produce 19% ~ 21% hydrochloric acid; This formulation cost and conventional acid are substantially suitable.
The indoor compound method of spontaneous acid: take a certain amount of solid ZX-339, be made into saturated or near saturated solution; Then the solid-state ZX-368 that adds wherein above-mentioned best proportional quantity, fully stir and get final product.For guaranteeing stability of suspension, sometimes also add wherein viscosifying agent.
Spontaneous sour field compounding method is shown in " embodiment ".
Spontaneous acid system performance:
1. the density of spontaneous acid system is 1.07 ~ 1.19g/cm
3, can generate the hydrochloric acid that concentration is 5% ~ 21%.
2. good with tensio-active agent ZX-19 compatibleness, also available ZX-19 carries out multiviscosisty to spontaneous acid.
(1) tensio-active agent ZX-19, can be well composite with 15 ~ 20% hydrochloric acid for forming the viscoelastic surfactant of gel, is selected from any one in benzene sulfonate, hydroxyethyl multi-alkylamine, methyl halogeno-amine.
(2) the spontaneous acid after the ZX-19 multiviscosisty can produce the hydrochloric acid of 20% left and right under 70 ° of C ~ 100 ° C, and hydrochloric acid is slowly to produce: reacting the effective salt acid concentration produced in 1 hour when 100 ° of C with landwaste is 9.5%, react 4 hours, the effective salt acid concentration of generation is 14%.The slow generation of hydrochloric acid is achieved the corrosion of deep reservoir.
3. the part hydrochloric acid generated can become hydrochloride and not participate in the corrosion rock with the black tropine complexing generated, and under 70 ° of C ~ 100 ° C, the actual concentration of hydrochloric acid reacted with rock is 14% ~ 16%; If temperature is higher, black tropine hydrochloride can decompose generation hydrochloric acid, and the effective salt acid concentration can be higher.
4. the clean acid fracturing liquid of spontaneous acid system and acidic group has good compatibility; Available clean acid fracturing liquid system is carried spontaneous acid and is arrived earth formation deep, realizes the relay-type acid fracturing.
(1) clean acid fracturing liquid system is comprised of ZX-19, hydrochloric acid, ZX-10, ZX-09 and water, and this composing system is simple, dosing convenient.
(2) ZX-10 in clean acid fracturing liquid system composition is that Fe stabilizer is selected from the EDTA tetra-na salt; ZX-09 is organic inhibitor, is selected from 16 mercaptan.
5. the local water that is 150000ppm～180000ppm by spontaneous acid with salinity mixes in the ratio of 1:2,1:1,2:1 respectively, places and produces without precipitation in 4 hours, illustrates that spontaneous acid and local water compatibleness are good.
6. the crude oil that is 0.85g/ml by spontaneous acid and density carries out the compatibleness experiment in 1:2,1:1,2:1 ratio respectively, and the average demulsification efficiency 99.36% of crude oil, illustrate that the compatibleness of spontaneous acid and crude oil is good.
7. experiment showed, with guar gum fracturing fluid, cross-linked acid, the acid that becomes sticky, gel acid, pure ether acid, the clean six kinds of common acid liquid system compatiblenesies of acid that turn to good.
The effect of invention
Respectively with the middle ancient times 7 well, the middle ancient times 8 well and Ha9Jing landwaste carry out the acid etching experiment, investigate the corrosion ability of spontaneous acid.The theoretical product of the spontaneous acid acid concentration of preparation is 15%.Under 100 ° of C, the reaction experimental result of 0.5 hour is in Table 1; The corrosion ability of visible spontaneous acid is equivalent to 70% ~ 74% of isoconcentration hydrochloric acid.Test and also show, if will extend in the reaction times, the corrosion ability of spontaneous acid also can correspondingly improve.
The spontaneous acid of table 1 and the contrast of hydrochloric acid acid etching ability experimental data
Annotate: the acid etching ability refers to that spontaneous acid etching landwaste ratio accounts for the per-cent of isoconcentration hydrochloric acid acid etching landwaste ratio relatively.
With the middle ancient times 7 the well rock core carry out sour rock reaction dynamics experiment, investigate the speed of response of spontaneous acid and rock.Experiment shows, spontaneous acidifying medicament is prefabricated into to liquid system, can produce the hydrochloric acid that concentration is higher, and sour rock speed of response is considerable: under the 500r/min rotating speed, during 70 ~ 140 ° of C of temperature, speed of response is not less than 2.9384E-04mol/cm
2.s; Speed of response raises and increases with temperature, and during 140 ° of C, acid rock speed of response maximum, be 1.3654E-03mol/cm
2.s.
Be mixed with the spontaneous acid of multiviscosisty with tensio-active agent ZX-19, investigate it and produce speed and the concentration of hydrochloric acid under differing temps.React the experimental result of 4 hours in Table 2; Visible temperature is higher, and the effective salt acid concentration of generation is higher.Find in addition: during 100 ° of C, reaction is 1 hour, produces hydrochloric acid total concn 18.86%, effective salt acid concentration 9.5%; React 4 hours, hydrochloric acid total concn 19.54%, the effective salt acid concentration is 14%, under hot conditions, spontaneous acid discharges H as seen
+speed comparatively slow.
The spontaneous acid of table 2 generates the concentration of hydrochloric acid under differing temps
| Temperature (° C) | Produce sour total concn (%) | Effective acid concentration (%) | Residual acid concentration () |
| 70 | 20.26 | 10.9 | 9.36 |
| 80 | 20.73 | 11.2 | 9.53 |
| 90 | 19.15 | 11.7 | 7.45 |
| 100 | 19.54 | 14.0 | 5.54 |
Experiment shows that this spontaneous acid system can produce the hydrochloric acid of enough concentration and formation rock is played to corrosion; Simultaneously, its ability that generates hydrochloric acid raises and strengthens with temperature, strengthens with the reaction times, can reach deep penetrating effect in the high temperature reservoir.
Embodiment
Spontaneous this formula of acidic group requires: n (ZX-339): n (ZX-368)=5:8
During practical application, may add other additive, but the basic proportioning of ZX-339 and ZX-368 is constant.Such as, prepare theoretical acid strength 8% ~ 12%, effectively during the spontaneous acid system of acid strength 5.24% ~ 7.24%, actual formula is: (12 ~ 18) %ZX-339+ (10 ~ 16) %ZX-368+2%ZX-19+2%ZX-09+1%ZX-10.
Be example with the clean acid fracturing liquid of spontaneous acid-acidic group, set forth on-the-spot dosing method.The pharmaceutical chemicals related to has ZX-19, ZX339, ZX-368, ZX-09(inhibiter), the ZX-10(Fe stabilizer) and HCl, wherein ZX-19, ZX-339 are very easily water-soluble pressed powder, ZX-368 is water-fast pressed powder, and ZX-09, ZX-10 and HCl are liquid.Field compounding method has two kinds of dry powder dosing and concentrated solution dosings.
Dosing method one: the dry powder dosing, take that to prepare the clean acid fracturing liquid complex liquid of 1000 milliliters of spontaneous acid-acidic groups be example.
Embodiment 1:
(1) add 500 milliliters of 18% hydrochloric acid in the clean beaker of 2000 milliliters, the complex acid water quality requirement is industrial clear water;
(2) add 2%EDTA tetra-na salt (ZX-09) and 1% inhibiter 16 mercaptan (ZX-10) by interior addition, power stirs;
(3) add 20 gram benzene sulfonate (ZX-19) tensio-active agent dry powder, power stirs;
(4) add 340 gram chlorination organic ammonium salt (ZX-339) dry powder and stir;
(5) add 325 grams gather dimethylaminobenzaldehyde (ZX-368) dry powder and stir.
Embodiment 2:
(1) add 500 milliliters of 15% hydrochloric acid in the clean beaker of 2000 milliliters, the complex acid water quality requirement is industrial clear water;
(2) add 2%EDTA tetra-na salt (ZX-09) and 1% inhibiter 16 mercaptan (ZX-10) by interior addition, power stirs;
(3) add 20 gram hydroxyethyl multi-alkylamine (ZX-19) tensio-active agent dry powder, stir;
(4) add 350 gram Benzoyl chloride (ZX-339) dry powder and stir;
(5) add poly-six aldehyde (ZX-368) dry powder of 325 grams and stir.
Embodiment 3:
(1) add 500 milliliters of 16% hydrochloric acid in the clean beaker of 2000 milliliters, the complex acid water quality requirement is industrial clear water;
(2) add 2%EDTA tetra-na salt (ZX-09) and 1% inhibiter 16 mercaptan (ZX-10) by interior addition, power stirs;
(3) add 20 gram methyl halogeno-amine (ZX-19) tensio-active agent dry powder, stir;
(4) add 350 gram chlorallylene (ZX-339) dry powder and stir;
(5) add 320 grams gather dimethylaminobenzaldehyde (ZX-368) dry powder and stir.
Dosing method two: concentrated solution dosing
Concentrated solution dosing: first ZX-339 is made to concentrated solution, ZX-368 is made to suspension with ZX-19, then dosing.
1, ZX-339 concentrated solution compound method, the preparation 200ml of take is example:
(1) add 100ml industry clear water in the beaker of 300ml;
(2) add in batches a kind of in 160 gram ZX-339(chlorallylenes, Benzoyl chloride, chlorination organic ammonium salt), power stirs;
(3) add a kind of in 2 gram ZX-19(benzene sulfonates, hydroxyethyl multi-alkylamine, methyl halogeno-amine), power stirs, and obtains the ZX-339 concentrated solution of 200ml;
2, ZX-368 and ZX-19 suspension preparation method, the preparation 200ml of take is example:
(1) add 100ml industry clear water in the beaker of 300ml;
(2) add in batches a kind of in the poly-dimethylaminobenzaldehyde of 140 gram ZX-368(and poly-six aldehyde), power stirs;
(3) add a kind of in 10 gram ZX-19(benzene sulfonates, hydroxyethyl multi-alkylamine, methyl halogeno-amine), power stirs, and obtains the ZX-368 concentrated solution of 200ml;
Concentrated solution dosing example: take that to prepare the clean acid fracturing liquid complex liquid of 1000 milliliters of spontaneous acid-acidic groups be example.
Embodiment 1.
(1) add 660 milliliters of 16% hydrochloric acid in the clean beaker of 2000 milliliters, the complex acid water quality requirement is industrial clear water;
(2) add 2%EDTA tetra-na salt (ZX-09) and 1% inhibiter 16 mercaptan (ZX-10) by interior addition, power stirs;
(3) add 8 kilograms of benzene sulfonate (ZX-19) dry powder and stir.
(4) add the poly-dimethylaminobenzaldehyde of the ZX-368(prepared) suspension 200ml, power stirs;
(5) add the ZX-339(chlorallylene prepared) concentrated solution 125ml, power stirs, and completes preparation;
Embodiment 2.
(1) add 660 milliliters of 18% hydrochloric acid in the clean beaker of 2000 milliliters, the complex acid water quality requirement is industrial clear water;
(2) add 2%EDTA tetra-na salt (ZX-09) and 1% inhibiter 16 mercaptan (ZX-10) by interior addition, power stirs;
(3) add 10 kilograms of hydroxyethyl multi-alkylamine (ZX-19) dry powder and stir.
(4) add poly-six aldehyde of the ZX-368(prepared) suspension 180ml, power stirs;
(5) add the ZX-339(chlorination organic ammonium salt prepared) concentrated solution 150ml, power stirs, and completes preparation;
On-the-spot dosing requires:
1, the amount of preparation of each component obtains by example sample magnification ratio according to scope of construction item.
2, use large discharge capacity impeller pump and jet-pump, the preparation that circulates, medicament adds the speed should be in the 30min/ tank.The circulation mixing time should, more than the 15min/ tank, guarantee that liquid mixing is even.
3, liquid can be constructed after preparing.Constructional method is identical with conventional acid fracturing: the spontaneous acid system prepared is pumped into to stratum according to certain infusion program and constructed.
Claims (2)
1. a spontaneous acid system; It is characterized in that: this spontaneous acid includes ZX-339 and ZX-368 composition, in molar ratio n (ZX-339): n (ZX-368)=5:8; Can produce 19% ~ 21% hydrochloric acid under 70 ° of C ~ 100 ° C of temperature of reaction;
Described ZX-339 is selected from any one material in chlorallylene, Benzoyl chloride, chlorination organic ammonium salt;
Described ZX-368 is selected from any one in poly-dimethylaminobenzaldehyde or poly-six aldehyde.
2. the application of a spontaneous acid system claimed in claim 1 is characterized in that: carry spontaneous acid system by clean acid fracturing liquid system and arrive earth formation deep, realize the relay-type acid fracturing; Clean acid fracturing liquid system is comprised of ZX-19, hydrochloric acid, ZX-10, ZX-09 and water; During application, by 2% multiviscosisty tensio-active agent ZX-19,15 ~ 20% hydrochloric acid, 2% organic inhibitor ZX-09 and 1% Fe stabilizer ZX-10 and (12 ~ 18) %ZX-339 and composite the forming of (10 ~ 16) %ZX-368, surplus is water by weight percentage;
Described multiviscosisty tensio-active agent ZX-19 is selected from any one in benzene sulfonate, hydroxyethyl multi-alkylamine, methyl halogeno-amine;
Described Fe stabilizer ZX-10 is selected from the EDTA tetra-na salt;
Described organic inhibitor ZX-09 is selected from 16 mercaptan.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103805159A (en) * | 2014-02-18 | 2014-05-21 | 中联煤层气有限责任公司 | Acid group viscoelastic fluid and preparation method thereof as well as oil and gas reservoir or coal seam treatment method |
| CN104975840A (en) * | 2015-06-18 | 2015-10-14 | 中国石油化工股份有限公司 | Self-born acid composite acid fracturing process for high-temperature deep well carbonate rock reservoir |
| WO2018108186A1 (en) * | 2016-12-15 | 2018-06-21 | 中国石油大学(华东) | Authigenic acid-induced tackifying control system having oil washing function and preparation method therefor |
| CN108384529A (en) * | 2018-05-08 | 2018-08-10 | 中联煤层气有限责任公司 | A kind of water-in-oil emulsion fluid, preparation method and oil exploitation method |
| CN106905194B (en) * | 2017-03-07 | 2018-10-19 | 四川格鑫拓科技有限公司 | A kind of multi-function rotating suitable for sandstone formation is to acid, thickening agent and preparation method thereof |
| CN110643344A (en) * | 2018-06-26 | 2020-01-03 | 中国石油化工股份有限公司 | Double-retarding emulsifying self-generated acid and preparation method thereof |
| CN114350343A (en) * | 2022-03-21 | 2022-04-15 | 中海油天津化工研究设计院有限公司 | Composite biological self-generated acid system for reservoir transformation |
| CN114737898A (en) * | 2022-03-29 | 2022-07-12 | 中国石油天然气股份有限公司西南油气田分公司 | Ultrahigh-temperature carbonate reservoir yield-increasing transformation method |
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Cited By (12)
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| CN103805159A (en) * | 2014-02-18 | 2014-05-21 | 中联煤层气有限责任公司 | Acid group viscoelastic fluid and preparation method thereof as well as oil and gas reservoir or coal seam treatment method |
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| WO2018108186A1 (en) * | 2016-12-15 | 2018-06-21 | 中国石油大学(华东) | Authigenic acid-induced tackifying control system having oil washing function and preparation method therefor |
| CN106905194B (en) * | 2017-03-07 | 2018-10-19 | 四川格鑫拓科技有限公司 | A kind of multi-function rotating suitable for sandstone formation is to acid, thickening agent and preparation method thereof |
| CN108384529A (en) * | 2018-05-08 | 2018-08-10 | 中联煤层气有限责任公司 | A kind of water-in-oil emulsion fluid, preparation method and oil exploitation method |
| CN110643344A (en) * | 2018-06-26 | 2020-01-03 | 中国石油化工股份有限公司 | Double-retarding emulsifying self-generated acid and preparation method thereof |
| CN110643344B (en) * | 2018-06-26 | 2021-11-02 | 中国石油化工股份有限公司 | Double-retarding emulsifying self-generated acid and preparation method thereof |
| CN114350343A (en) * | 2022-03-21 | 2022-04-15 | 中海油天津化工研究设计院有限公司 | Composite biological self-generated acid system for reservoir transformation |
| CN114737898A (en) * | 2022-03-29 | 2022-07-12 | 中国石油天然气股份有限公司西南油气田分公司 | Ultrahigh-temperature carbonate reservoir yield-increasing transformation method |
| CN114737898B (en) * | 2022-03-29 | 2024-03-19 | 中国石油天然气股份有限公司西南油气田分公司 | Ultrahigh-temperature carbonate reservoir yield increasing transformation method |
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