CN103450872B - A kind of spontaneous acid system and application thereof - Google Patents
A kind of spontaneous acid system and application thereof Download PDFInfo
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Abstract
The present invention relates to a kind of spontaneous acid system and application thereof; This spontaneous acid includes ZX-339 and ZX-368 composition, in molar ratio n (ZX-339): n (ZX-368)=5:8; The hydrochloric acid of 19% ~ 21% can be produced under temperature of reaction 70 ° of C ~ 100 ° C; ZX-339 is selected from any one material in chlorallylene, Benzoyl chloride, chlorination organic ammonium salt; ZX-368 be selected from poly-dimethylaminobenzaldehyde or poly-six aldehyde any one; Carry spontaneous acid system by clean acid fracturing liquid system and arrive earth formation deep; During application, formed with (10 ~ 16) %ZX-368 is composite by 2%ZX-19,15 ~ 20% hydrochloric acid, 2%ZX-09 and 1%ZX-10 and (12 ~ 18) %ZX-339 by weight percentage, surplus is water; The solution ration of this spontaneous acid is equivalent to 70% ~ 74% 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 sour liquid system and application thereof being applicable to the deep acid fracturing of high temperature carbonate rock reservoir.
Background technology
In recent years, the exploitation of carbonate reservoir causes the attention of people day by day.Carbonate reservoir generally has the features such as hypotonic, nonuniformity is strong, usually needs to improve its production capacity by storey increase design.Acid fracturing is one of well stimulation that carbonate reservoir is conventional, its mechanism is: use acid solution to carry out non-homogeneous etching to the wall of man-made fracture, making operation pressure remove rear crack wall can not be completely closed, thus forms the flow passage that has certain flow conductivity.The effect of acidfracturing treatment depends primarily on acid corrosion fracture and acid-etched fracture length.
But carbonate reservoir generally buries comparatively dark, reservoir temperature is higher, after conventional acid solution enters stratum can rapidly and rock react and consume, cannot be penetrated into earth formation deep, the acid-etched fracture length of generation is very limited, constrains the effect of acidfracturing treatment.Therefore one can slow down acid-rock reaction speed, deep penetrating acid fluid system is very necessary in development.
Have the acid fluid system that some are applicable to carbonatite deep acid fracturing at present, as gel acid, emulsified acid, the acid that becomes sticky, surfactivity acid etc., they slow down acid-rock reaction speed by improving the modes such as acid liquid viscosity, minimizing acid and rock contact area, but due to its various shortcoming, the scope of application receives larger limitation.Such as gel acid and the acid that becomes sticky at high temperature still have speed of response faster with rock, and penetration range is limited; Emulsified acid is not easily prepared, and frictional resistance is higher, in deep-well, high-pressure reservoir, use difficulty large; Surfactivity acid cost 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 sandstone reservoir acidifying; At present both at home and abroad also not used for the spontaneous acid system of the maturation of carbonate reservoir.
Have developed a kind of spontaneous acid system being applicable to high temperature carbonate rock reservoir deep acid fracturing in this context.
Summary of the invention
The object of this invention is to provide a kind of spontaneous sour chemical formulation being applicable to carbonate reservoir acid fracturing, chemical reaction is there is not in this spontaneous acid formula on ground, not there is solution ration at normal temperatures, heat along with by stratum after pumping into stratum, can react gradually and discharge hydrochloric acid, temperature is higher, and the time is longer, the hydrochloric acid generated is more, reaches the object 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
The reactant that the present invention selects is poly-many aldehyde (ZX-368) of 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
Carry out formula optimization by experiment:
1. namely liquid ZX-339 and ZX-368 at room temperature reacts, undesirable; Select the ZX-368 of solid, do not react under room temperature can be ensured.
2. the concentration of hydrochloric acid of ZX-368 and the ZX-339 reaction generation of equivalent is limited; Use excessive (ZX-368), can level of response be improved, increase hydrochloric acid productive rate.
3. take into account Cost Problems, finally determine that ZX-339 and ZX-368 reacts optimum proportioning and is: n (ZX-339): n (ZX-368)=5:8; When using this proportioning, the hydrochloric acid of 19% ~ 21% under temperature of reaction 70 ° of C ~ 100 ° C, can be produced; 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 add the solid-state ZX-368 of above-mentioned optimum proportioning amount wherein, fully stir.For ensureing stability of suspension, sometimes also add viscosifying agent wherein.
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, the hydrochloric acid that concentration is 5% ~ 21% can be generated.
2. good with tensio-active agent ZX-19 compatibleness, also can carry out multiviscosisty with ZX-19 to spontaneous acid.
(1) tensio-active agent ZX-19 is the viscoelastic surfactant that can form gel, can be well composite with 15 ~ 20% hydrochloric acid, is selected from any one in benzene sulfonate, hydroxyethyl multi-alkylamine, methyl halogeno-amine.
(2) the spontaneous acid after ZX-19 multiviscosisty can produce the hydrochloric acid of about 20% under 70 ° of C ~ 100 ° C, and hydrochloric acid slowly produces: when 100 ° of C and landwaste to react the effective salt acid concentration produced for 1 hour be 9.5%, react 4 hours, the effective salt acid concentration of generation is 14%.The slow generation of hydrochloric acid makes the corrosion of deep reservoir be achieved.
3. the part hydrochloric acid generated can become hydrochloride with the black tropine complexing generated and not participate in corrosion rock, 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 effective salt acid concentration can be higher.
4. spontaneous acid system and acidic group clean acid fracturing liquid good compatibility; Available clean acid fracturing liquid system is carried spontaneous acid and is arrived earth formation deep, realizes relay-type acid fracturing.
(1) clean acid fracturing liquid system is made up of ZX-19, hydrochloric acid, ZX-10, ZX-09 and water, and this system composition is simple, dosing is convenient.
(2) ZX-10 in clean acid fracturing liquid system composition is that Fe stabilizer is selected from EDTA tetra-na salt; ZX-09 is organic inhibitor, is selected from 16 mercaptan.
5. the local water being 150000ppm ~ 180000ppm by spontaneous acid and salinity mixes in the ratio of 1:2,1:1,2:1 respectively, place 4 hours without precipitation produce, illustrate spontaneous acid and local water compatibleness good.
6. the crude oil being 0.85g/ml by spontaneous acid and density carries out compatibleness experiment in 1:2,1:1,2:1 ratio respectively, and the average demulsification efficiency 99.36% of crude oil, illustrates that the compatibleness of spontaneous acid and crude oil is good.
7. experiment proves, good with guar gum fracturing fluid, cross-linked acid, the acid that becomes sticky, gel acid, alcohol ether acid, visco-elastic surfactant acid six kinds of common acid liquid system compatiblenesies.
The effect of invention
Respectively with the middle ancient times 7 well, the middle ancient times 8 well and the landwaste of Ha9Jing carry out acid etching experiment, investigate the solution ration of spontaneous acid.The spontaneous acid theoretical product acid concentration of preparation is 15%.The experimental result of 0.5 hour is reacted in table 1 under 100 ° of C; The solution ration of visible spontaneous acid is equivalent to 70% ~ 74% of isoconcentration hydrochloric acid.Experiment also shows, if will extend in the reaction times, the solution ration of spontaneous acid also can correspondingly improve.
The spontaneous acid of table 1 and hydrochloric acid acid etching capacity experimental Data Comparison
Note: 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.
Carry out acid-rock reaction dynamic experiment with well rock core in the middle ancient times 7, investigate the speed of response of spontaneous acid and rock.Experiment shows, spontaneous sour chemical agent is prefabricated into liquid system, can produces the hydrochloric acid that concentration is higher, and acid-rock reaction speed is considerable: under 500r/min rotating speed, and during temperature 70 ~ 140 ° of C, speed of response is not less than 2.9384E-04mol/cm
2.s; Speed of response raises with temperature and increases, and during 140 ° of C, acid-rock reaction speed is maximum, is 1.3654E-03mol/cm
2.s.
Be mixed with the spontaneous acid of multiviscosisty with tensio-active agent ZX-19, investigate its speed producing hydrochloric acid at different temperatures and concentration.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, react 1 hour, produce hydrochloric acid total concn 18.86%, effective salt acid concentration 9.5%; React 4 hours, hydrochloric acid total concn 19.54%, effective salt acid concentration is 14%, as seen under the high temperature conditions, and spontaneous acid release H
+speed comparatively slow.
The spontaneous acid of table 2 generates the concentration of hydrochloric acid at different temperatures
| 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 plays corrosion; Meanwhile, its ability generating hydrochloric acid raises with temperature and strengthens, and increases and strengthens, can reach deep penetrating effect in temperature reservoirs with the reaction times.
Embodiment
Spontaneous this recipe requirements of acidic group: n (ZX-339): n (ZX-368)=5:8
During practical application, other additive may be added, but the basic proportioning of ZX-339 and ZX-368 is constant.Such as, prepare theoretical acid strength 8% ~ 12%, during the spontaneous acid system of effective 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.
Cleaning acid fracturing liquid with spontaneous acid-acidic group is example, sets forth on-the-spot dosing method.The pharmaceutical chemicals related to has ZX-19, ZX339, ZX-368, ZX-09(inhibiter), 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 dry powder dosing and concentrated solution dosing two kinds.
Dosing method one: dry powder dosing, cleans acid fracturing liquid complex liquid to prepare 1000 milliliters of spontaneous acid-acidic groups.
Embodiment 1:
(1) in the beaker of clean 2000 milliliters, add the hydrochloric acid 500 milliliters of 18%, 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 grams of benzene sulfonate (ZX-19) tensio-active agent dry powder, power stirs;
(4) add 340 grams of chlorination organic ammonium salt (ZX-339) dry powder and stir;
(5) add 325 grams of poly-dimethylaminobenzaldehyde (ZX-368) dry powder and stir.
Embodiment 2:
(1) in the beaker of clean 2000 milliliters, add the hydrochloric acid 500 milliliters of 15%, 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 grams of hydroxyethyl multi-alkylamine (ZX-19) tensio-active agent dry powder, stir;
(4) add 350 grams of Benzoyl chloride (ZX-339) dry powder and stir;
(5) add 325 grams of poly-six aldehyde (ZX-368) dry powder and stir.
Embodiment 3:
(1) in the beaker of clean 2000 milliliters, add the hydrochloric acid 500 milliliters of 16%, 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 grams of methyl halogeno-amine (ZX-19) tensio-active agent dry powder, stir;
(4) add 350 grams of chlorallylene (ZX-339) dry powder and stir;
(5) add 320 grams of poly-dimethylaminobenzaldehyde (ZX-368) dry powder and stir.
Dosing method two: concentrated solution dosing
Concentrated solution dosing: first ZX-339 is made concentrated solution, makes suspension by ZX-368 ZX-19, then dosing.
1, ZX-339 concentrated solution compound method, to prepare 200ml:
(1) in the beaker of 300ml, add 100ml industry clear water;
(2) one in 160 grams of ZX-339(chlorallylenes, Benzoyl chloride, chlorination organic ammonium salt is added in batches), power stirs;
(3) one in 2 grams of ZX-19(benzene sulfonates, hydroxyethyl multi-alkylamine, methyl halogeno-amine is added), power stirs, and namely obtains the ZX-339 concentrated solution of 200ml;
2, ZX-368 and ZX-19 suspension preparation method, to prepare 200ml:
(1) in the beaker of 300ml, add 100ml industry clear water;
(2) one that 140 grams of ZX-368(gather dimethylaminobenzaldehyde and gather in six aldehyde is added in batches), power stirs;
(3) one in 10 grams of ZX-19(benzene sulfonates, hydroxyethyl multi-alkylamine, methyl halogeno-amine is added), power stirs, and namely obtains the ZX-368 concentrated solution of 200ml;
Concentrated solution dosing example: clean acid fracturing liquid complex liquid to prepare 1000 milliliters of spontaneous acid-acidic groups.
Embodiment 1.
(1) in the beaker of clean 2000 milliliters, add the hydrochloric acid 660 milliliters of 16%, 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 ZX-368(prepared and gather dimethylaminobenzaldehyde) suspension 200ml, power stirs;
(5) the ZX-339(chlorallylene prepared is added) concentrated solution 125ml, power stirs, and namely completes preparation;
Embodiment 2.
(1) in the beaker of clean 2000 milliliters, add the hydrochloric acid 660 milliliters of 18%, 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) poly-six aldehyde of the ZX-368(prepared are added) suspension 180ml, power stirs;
(5) the ZX-339(chlorination organic ammonium salt prepared is added) concentrated solution 150ml, power stirs, and namely 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 huge discharge impeller pump and jet-pump, carry out circulation preparation, medicament adds speed should within 30min/ tank.Circulation mixing time more than 15min/ tank, should ensure 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 stratum according to certain infusion program and constructs.
Claims (1)
1. an application for spontaneous acid system, 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;
Described ZX-339 is selected from any one material in chlorallylene, Benzoyl chloride, chlorination organic ammonium salt;
Described ZX-368 be selected from poly-dimethylaminobenzaldehyde or poly-six aldehyde any one;
The hydrochloric acid of 19% ~ 21% can be produced at temperature of reaction 70 DEG C ~ 100 DEG C;
Carry spontaneous acid system by clean acid fracturing liquid system and arrive earth formation deep, realize relay-type acid fracturing; Clean acid fracturing liquid system is made up of ZX-19, hydrochloric acid, ZX-10, ZX-09 and water; During application, formed with (10 ~ 16) %ZX-368 is composite by 2% viscosifying surfactant ZX-19,15 ~ 20% hydrochloric acid, 2% organic inhibitor ZX-09 and 1% Fe stabilizer ZX-10 and (12 ~ 18) %ZX-339 by weight percentage, surplus is water; Described viscosifying surfactant ZX-19 be selected from benzene sulfonate, hydroxyethyl multi-alkylamine, methyl halogeno-amine any one;
Described Fe stabilizer ZX-10 is selected from EDTA tetra-na salt;
Described organic inhibitor ZX-09 is selected from 16 mercaptan.
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