CN103666414B - Polyamide-based amine flow pattern regulator and preparation method thereof for mineral oil based drilling fluid - Google Patents
Polyamide-based amine flow pattern regulator and preparation method thereof for mineral oil based drilling fluid Download PDFInfo
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/02—Well-drilling compositions
- C09K8/03—Specific additives for general use in well-drilling compositions
- C09K8/035—Organic additives
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/02—Well-drilling compositions
- C09K8/32—Non-aqueous well-drilling compositions, e.g. oil-based
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Abstract
The invention discloses a kind of mineral oil based drilling fluid polyamide-based amine flow pattern regulator and preparation method thereof, this conditioning agent is under 120～160 DEG C of conditions, to carry out amidation process by dimer (fatty acid) yl and polyamine, then product is evenly mixed and made with solvent; In described dimer (fatty acid) yl, dimeric content is greater than 78wt%; Described polyamine is the homologue of the polyethylene polyamine that contains 2～5 amidos; In dimer (fatty acid) yl, in carboxyl and polyamine, the mol ratio of amido is 1:0.2～1.2. Preparation process is to complete in the reaction vessel that is connected with Dean-Stark receiver. This polyamide-based amine flow pattern regulator molecular weight is large, and active function groups is many, can form multiple spot absorption, be difficult to from organoclay surface desorption attached, at high temperature continuous and effective, stable performance. And its preparation process is simple, reaction condition is easy to control.
Description
Technical field
The present invention relates to a kind of oil and natural gas industry drilling fluid, particularly a kind of mineral oil based drilling wellPolyamide-based amine flow pattern regulator and preparation method thereof for liquid.
Background technology
Along with the development of modern drilling technology, lubricity is good, strong inhibition capability, right because it has for oil base drilling fluidThe little primary selection that waits premium properties to become various complex stratigraphic drillings of formation damage. But oil base drilling fluid is outstandingBuoyancy is poor, may form cutting bed, and therefore, suspending power is one of parameter determining oil base drilling fluid performance,Directly have influence on effect of hole cleaning, weighting material sedimentation, equivalent circulating density, pressure excitement and suction pressurePower etc. Only have suitable suspending power and keep it stable, could successfully drill Holes of Complicated Wells, especially deep waterThe well section that well, hp-ht well and ' Safe Density Windows are narrow.
Cut agent as glutinous the carrying of increasing of oil base drilling fluid in early days--organoclay is widely used. But, organoclay high temperatureEasily multiviscosisty, the service life of reducing oil base drilling fluid, reduce the solid content of oil base drilling fluid, pollutes hypotonicReservoir thoroughly. Along with the increasingly stringent of environmental protection requirement, low/to replace without mineral oil and the synthetic base oil of aromatic hydrocarbonsAfter diesel oil, conventional organoclay dispersion suspension performance in this class environmental protection base oil is lower, often needs higherThe organoclay of concentration, just can reach the effect of suspension weighting material and hole cleaning, through shaft bottom high temperature, makesBecome environment-friendly oil-based/synthetic base drilling fluid plastic viscosity to increase, rate of penetration reduces, at many cover pressure systemsIn bad ground, cause down-hole accident.
Research is in early days thought, improves the suspending power of drilling fluid by increasing Drilling Fluid Viscosity realization, and exploitationThe oil-soluble macromolecular materials such as butadiene-styrene rubber. Along with going deep into of industrial practice and scientific research, occurNew viewpoint is also progressively applied in oil drilling industry: in mineral oil and synthetic base drilling fluid, add oneThe oil-soluble polar organic matter matter of class low viscosity (low-molecular-weight), can significantly improve the gelling of organoclayBehavior, yield value, the low-shear rate viscosity etc. of raising system, oil base drilling fluid reaches the " fast of " low sticky height is cut "The weak gel of speed " state.
At present, domestic mineral oil based drilling liquid technology, in developing stage, has larger gap compared with abroad.In order to reach required suspension character, often add the organoclay of excessive concentrations, under the hot conditions of shaft bottom,Organoclay degree of scatter increases, and drilling fluid multiviscosisty is serious, and plastic viscosity is increased sharply; And for addressing this problem,In site operation, add polyalcohols, as ethylene glycol, glycerine and polyethylene glycol etc.; Ethers, as diethylene glycolAnd dimethyl ether; Little molecule amide-type, as the material such as formamide, acetamide. These small-molecule substances are at heightCan be attached from organoclay surface desorption under temperature, thus the jelling structure of minimizing drilling fluid.
Summary of the invention
The object of the present invention is to provide a kind of mineral oil based drilling fluid polyamide-based amine flow pattern regulator, itsMolecular weight is large, and active function groups is many, can form multiple spot absorption, be difficult to from organoclay surface desorption attached, at heightThe lower continuous and effective of temperature, stable performance.
Another object of the present invention is to provide a kind of mineral oil based drilling fluid polyamide-based amine flow pattern regulatorPreparation method, the method technical process is simple, can meticulous control reaction condition; Do not affecting result of usePrerequisite under adopt double solvents, reduce the use amount of polar solvent, reduce costs; And what finally make is poly-Product characteristics and the stable performance of amide groups amine flow pattern regulator.
For this reason, technical scheme of the present invention is:
Polyamide-based amine flow pattern regulator for a kind of mineral oil based drilling fluid, is existed by dimer (fatty acid) yl and polyamineUnder 120～160 DEG C of conditions, carry out amidation process, after having reacted, by the product making and solvent according to qualityMix and make than 0.5～1.5:1; In described dimer (fatty acid) yl, dimeric content is greater than 78wt%; InstituteState polyamine and be the homologue of the polyethylene polyamine that contains 2～5 amidos; In described dimer (fatty acid) yl carboxyl withIn polyamine, the mol ratio of amido is 1:0.2～1.2, preferably 1:0.4～0.8, more preferably 1:0.7; Described solventFor diethylene glycol monomethyl ether, diethylene glycol dimethyl ether, Dipropylene glycol mono-n-butyl Ether or DPG monomethylEther, or any one and the mixture of any ratio of mineral oil in these four kinds of materials.
Described dimer (fatty acid) yl is the mixed acid of monomer acids, dimer (fatty acid) yl and three polyglycerol fatty acids, wherein saidThe content of monomer acids is 2～22wt%, and the content of dimer (fatty acid) yl is 78%～98wt%, the containing of three polyglycerol fatty acidsAmount is 0～12wt%.
Described polyamine is for being ethylenediamine, diethylenetriamine, triethylene tetramine or TEPA.
The mass ratio that described amidation process makes product and solvent is 0.8～1.2:1, preferably 1:1.
Described mineral oil is 5# technical white oil, and described solvent is that glycol monomethyl ether and 5# technical white oil are with qualityThe double solvents mixing than 10～90:90～10; Preferably 30～80:70～20 of both mass ratioes, most preferably are60:40。
A preparation method for polyamide-based amine flow pattern regulator for mineral oil based drilling fluid, comprises the steps:
1) take respectively two taking the mol ratio of amido in carboxyl in dimer (fatty acid) yl and polyamine as 1:0.2～1.2Aggressiveness content is greater than dimer (fatty acid) yl and the polyamine of 78wt%;
2) material step 1) being taken is inserted in the reaction vessel that is connected with Dean-Stark receiver,Stir, 120～160 DEG C, be connected with under condition of nitrogen gas and react 1～3h, obtain just finished product; This step reaction temperature is preferredBe 140～160 DEG C, more preferably 150～155 DEG C.
3) described just finished product is mixed according to mass ratio 0.5～1.5:1 with solvent, obtain described mineral oilPolyamide-based amine flow pattern regulator for base drilling fluid; Wherein said solvent is diethylene glycol monomethyl ether, diethylGlycol dimethyl ether, Dipropylene glycol mono-n-butyl Ether or DPGME, or appointing in these four kinds of materialsAnticipate a kind of and mineral oil with arbitrarily than mixture.
Polyamide-based amine flow pattern regulator prepared by the present invention is that a class is by dimer (fatty acid) yl and multi-element organic amineNon-nylon material class polyamide materials prepared by condensation, the feature of condensation reaction has determined primary amine groups, secondary amineFunctional group is uniformly distributed in polymer molecule with amide groups isopolarity, and this class active function groups can be organicSoil surface forms multiple spot absorption, has strengthened the interaction of organoclay in nonpolar environment, has improved gellingCharacter, is difficult for desorption under high temperature, still can keep certain jelling structure at shaft bottom high temperature. In addition,In preparation method, the present invention is at the enterprising one-step optimization in the basis of the disclosed method of patent CN103012180A,Change two kinds of raw materials into by three kinds of raw materials, feed intake and change a step into and feed intake by two steps, change one into by two step pyroreactionsWalk pyroreaction, reduced the control difficulty of technical process, saved energy consumption, reduced labour intensity.
Detailed description of the invention
Mineral oil based drilling fluid of the present invention is mainly to be reacted by carboxylic acyloxy amination with polyamide-based amine flow pattern regulatorMake, the functional group of generation is mainly acid amides, generates water in course of reaction. But at aliphatic acid and polyamineIn course of reaction, can the higher cross-linking products of generating portion molecular weight. If the reaction time under hot conditionsLong, can there is part cross-linking reaction, but not affect the performance that makes product. If excessively crosslinked, thatCross-linking products is difficult to dissolve, disperse, and can not be applied.
In order to obtain the product of excellent performance, not only need to control the type of reactant, also need strict control insteadBetween seasonable.
Describe the present invention below in conjunction with embodiment.
Embodiment 1
With agitator, thermometer, logical nitrogen device (inert gas shielding is also carried steam) andWhat in the four-hole reactor of Dean-Stark receiver, to add by amido quantity and the ratio of carboxyl quantity be 0.4:1.0Diethylenetriamine and dimer (fatty acid) yl (78wt% dimeric dibasic acid, 10wt% monomer acids and 12wt% trimer acid), useConstant temperature oil bath is heated to 110 DEG C of reaction 0.5h, then is warming up to 150 DEG C, and reaction 3.0h obtains mineral oil of the present inventionPolyamide-based amine flow pattern regulator for base drilling fluid. By polyamide-based amine stream for the mineral oil based drilling fluid obtainingType conditioning agent mixes with mass ratio 1:1 with solvent, obtains product P AA-1; Wherein: solvent is mass ratioFor the dipropylene glycol monomethyl ether of 60:40 and the mixture of 5# technical white oil.
Embodiment 2
With agitator, thermometer, logical nitrogen device (inert gas shielding is also carried steam) andWhat in the four-hole reactor of Dean-Stark receiver, to add by amido quantity and the ratio of carboxyl quantity be 0.7:1.0Triethylene tetramine and dimer (fatty acid) yl (92wt% dimeric dibasic acid, 2.5% monomer acids and 5.5% trimer acid), use constant temperatureOil bath is heated to 110 DEG C of reaction 0.5h, then is warming up to 160 DEG C, and reaction 2.0h obtains mineral oil based of the present invention and borePolyamide-based amine flow pattern regulator for well liquid. The mineral oil based drilling fluid obtaining is adjusted by polyamide-based amine flow patternJoint agent mixes with mass ratio 1:1 with solvent, obtains product P AA-2; Wherein: solvent is that mass ratio isThe mixture of the dipropylene glycol monomethyl ether of 60:40 and 5# technical white oil.
Embodiment 3
With agitator, thermometer, logical nitrogen device (inert gas shielding is also carried steam) andWhat in the four-hole reactor of Dean-Stark receiver, to add by amido quantity and the ratio of carboxyl quantity be 0.8:1.0Triethylene tetramine and dimer (fatty acid) yl (98wt% dimeric dibasic acid and 2wt% monomer acids), be heated to constant temperature oil bath110 DEG C of reaction 0.5h, then be warming up to 160 DEG C, reaction 1.5h obtains mineral oil based drilling fluid polyamides of the present inventionAmido amine flow pattern regulator. By polyamide-based amine flow pattern regulator and solvent for the mineral oil based drilling fluid obtainingWith mass ratio, 1:1 mixes, and obtains product P AA-3; Wherein: solvent is that mass ratio is the dipropyl of 60:40The mixture of glycol monomethyl ether and 5# technical white oil.
Embodiment 4
With agitator, thermometer, logical nitrogen device (inert gas shielding is also carried steam) andWhat in the four-hole reactor of Dean-Stark receiver, to add by amido quantity and the ratio of carboxyl quantity be 0.8:1.0TEPA and dimer (fatty acid) yl (98wt% dimeric dibasic acid and 2wt% monomer acids), be heated to constant temperature oil bath110 DEG C of reaction 0.5h, then be warming up to 150 DEG C, reaction 1.5h obtains mineral oil based drilling fluid polyamides of the present inventionAmido amine flow pattern regulator. By polyamide-based amine flow pattern regulator and solvent for the mineral oil based drilling fluid obtainingWith mass ratio, 1:1 mixes, and obtains product P AA-4; Wherein: solvent is that mass ratio is the dipropyl of 60:40The mixture of glycol monomethyl ether and 5# technical white oil.
Embodiment 5
With agitator, thermometer, logical nitrogen device (inert gas shielding is also carried steam) andWhat in the four-hole reactor of Dean-Stark receiver, to add by amido quantity and the ratio of carboxyl quantity be 0.8:1.0Ethylenediamine and dimer (fatty acid) yl (98wt% dimeric dibasic acid and 2wt% monomer acids), be heated to 110 DEG C with constant temperature oil bathReaction 0.5h, then be warming up to 155 DEG C, reaction 1.5h obtains mineral oil based drilling fluid polyamide-based of the present inventionAmine flow pattern regulator. Use polyamide-based amine flow pattern regulator and solvent with matter the mineral oil based drilling fluid obtainingAmount mixes than 1:1, obtains product P AA-5; Wherein: solvent is that mass ratio is the DPG of 60:40The mixture of monomethyl ether and 5# technical white oil.
Note: described in embodiment, three kinds of dimer (fatty acid) yls are respectively dimer (fatty acid) yl (78wt% dimeric dibasic acid, 10wt%Monomer acids and 12wt% trimer acid), dimer (fatty acid) yl (92wt% dimeric dibasic acid, 2.5% monomer acids and 5.5% trimerizationAcid) and dimer (fatty acid) yl (98wt% dimeric dibasic acid and 2wt% monomer acids), its trade name is dimer (fatty acid) ylOr dimeric dibasic acid, be concrete content difference, in bracket, be concrete technical indicator.
Application experiment: preparation mineral oil based drilling fluid
Formula composition:
5# white oil: mineral oil based drilling fluid base oil;
Organobentonite: tackifier;
Calcium oxide: alkalinity control agent;
BZ-OFL-II: pitch class fluid loss additive;
PAA: the polyamide-based amine flow pattern regulator that the present invention makes;
SPAN-80: wetting agent;
Agstone: weighting material;
Barite: weighting material;
Layoutprocedure: SPAN-80, flow pattern regulator PAA are joined in 5# white oil to high-speed stirred5～10min, then adds organobentonite, calcium oxide, stirs 30～40min; Add fluid loss additive BZ-OFL-II stirs 15min, adds agstone and barite, stirs 40～60min.
According to the method described above, the polyamide-based amine flow pattern regulator preparation mineral oil that utilizes embodiment 1～3 to makeBase drilling fluid, as shown in table 1:
The polyamide-based amine flow pattern regulator preparation mineral oil based drilling fluid that table 1 utilizes embodiment 1～3 to make
| Component | Formula-1 | Formula-2 | Formula-3 |
| 5# white oil, mL | 400 | 400 | 400 |
| SPAN-80，g | 8 | 8 | 8 |
| PAA-1，g | 6 | — | — |
| PAA-3，g | — | 6 | — |
| PAA-5，g | — | — | 6 |
| Organoclay, g | 18 | 18 | 18 |
| Calcium oxide, g | 10 | 10 | 10 |
| BZ-OFL-II，g | 16 | 16 | 16 |
| Agstone, g | 170 | 170 | 170 |
| Barite, g | 150 | 150 | 150 |
As shown in table 2 by the fill a prescription performance of the full oil base drilling fluid that makes of table 1.
The performance of full oil base drilling fluid in table 2 table 1
Note: 1. rheological parameter probe temperature is 50 DEG C;
2. aging condition is 150 DEG C × 16h;
3. HTHP leak-off FLHTHPCondition is 150 DEG C, and pressure reduction is 3.5MPa.
4. Φ wherein600、Φ300、Φ200、Φ100、Φ6、Φ3Represent that respectively 600 revs/min, 300 revs/min, 200 turn/ point, the reading of 100 revs/min, 6 revs/min, 3 revs/min.
Above result shows, adds after polyamide-based amine flow pattern regulator, and complete the moving of oil base drilling fluid system cutsPower (YP), low-shear rate viscosity while turning (6 revs/min and 3/ point reading) all increase substantially, and mouldProperty viscosity (PV) is not subject to remarkable impact, and good with other inorganic agent compatibilities. At 150 DEG C of high temperatureAfter aging, the performance of the product of three kinds of different material proportion of composing has greatly changed, and wherein, contains amineIngressing after the full oil base drilling fluid system of the product P AA-3 that base and carboxyl ratio are 0.7:1.0 is aging, egressDifference is less, and the full oil base drilling fluid system that contains other two kinds of product P AA-1 and PAA-5 is ingressed, endCut difference larger, illustrate that product P AA-3 has preferably temperature stability, make full oil base drilling fluid system moreThe characteristic with " weak gel strength fast " and inductile viscosity, is conducive to improve bit speed and wellPurification efficiency.
Claims (10)
1. a polyamide-based amine flow pattern regulator for mineral oil based drilling fluid, is characterized in that: by two polyestersFat acid and polyamine carry out amidation process under 120～160 DEG C of conditions, after having reacted, by the product makingMix and make according to mass ratio 0.5～1.5:1 with solvent;
In described dimer (fatty acid) yl, dimeric content is greater than 78wt%;
Described polyamine is the homologue of the polyethylene polyamine that contains 2～5 amidos;
In described dimer (fatty acid) yl, in carboxyl and polyamine, the mol ratio of amido is 1:0.2～0.8;
Described solvent is diethylene glycol monomethyl ether, diethylene glycol dimethyl ether, Dipropylene glycol mono-n-butyl Ether or twoPropylene glycol monomethyl ether, or any one and the mixture of any ratio of mineral oil in these four kinds of materials.
2. polyamide-based amine flow pattern regulator for mineral oil based drilling fluid as claimed in claim 1, its featureBe: in described dimer (fatty acid) yl, in carboxyl and polyamine, the mol ratio of amido is 1:0.4～0.8.
3. polyamide-based amine flow pattern regulator for mineral oil based drilling fluid as claimed in claim 1, its featureBe: described dimer (fatty acid) yl is the mixed acid of monomer acids, dimer (fatty acid) yl and three polyglycerol fatty acids.
4. polyamide-based amine flow pattern regulator for mineral oil based drilling fluid as claimed in claim 3, its featureBe: the content of described monomer acids is 2～22wt%, the content of dimer (fatty acid) yl is 78%～98wt%, trimerizationThe content of aliphatic acid is 0～12wt%.
5. polyamide-based amine flow pattern regulator for mineral oil based drilling fluid as claimed in claim 1, its featureBe: described polyamine is for being ethylenediamine, diethylenetriamine, triethylene tetramine or TEPA.
6. polyamide-based amine flow pattern regulator for mineral oil based drilling fluid as claimed in claim 1, its featureBe: the mass ratio that described amidation process makes product and solvent is 0.8～1.2:1.
7. polyamide-based amine flow pattern regulator for mineral oil based drilling fluid as claimed in claim 1, its featureBe: described mineral oil is 5# technical white oil.
8. polyamide-based amine flow pattern regulator for mineral oil based drilling fluid as claimed in claim 7, its featureBe: described solvent is glycol monomethyl ether and answering that 5# technical white oil mixes with mass ratio 10～90:90～10Bonding solvent.
9. the preparation of polyamide-based amine flow pattern regulator for mineral oil based drilling fluid as described in claim 1Method, is characterized in that: comprise the steps:
1) take respectively two taking the mol ratio of amido in carboxyl in dimer (fatty acid) yl and polyamine as 1:0.2～0.8Aggressiveness content is greater than dimer (fatty acid) yl and the polyamine of 78wt%;
2) by step 1) material that takes inserts in the reaction vessel that is connected with Dean-Stark receiver,Stir, 120～160 DEG C, be connected with under condition of nitrogen gas and react 1～3h, obtain just finished product;
3) described just finished product is mixed according to mass ratio 0.5～1.5:1 with solvent, obtain described mineral oilPolyamide-based amine flow pattern regulator for base drilling fluid; Wherein said solvent is diethylene glycol monomethyl ether, diethylGlycol dimethyl ether, Dipropylene glycol mono-n-butyl Ether or DPGME, or appointing in these four kinds of materialsAnticipate a kind of and mineral oil with arbitrarily than mixture.
10. preparation method as claimed in claim 9, is characterized in that: step 2) reaction temperature be140～160℃。
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| CN109652030B (en) * | 2018-12-10 | 2020-03-31 | 中国石油大学(北京) | Flow pattern regulator and large-temperature-difference constant-rheology oil-based drilling fluid |
| CN110746944B (en) * | 2019-11-15 | 2021-11-09 | 中国石油集团渤海钻探工程有限公司 | Flow pattern regulator for synthetic base drilling fluid and preparation method thereof |
| CN113943422B (en) * | 2020-07-15 | 2022-11-01 | 中国石油天然气集团有限公司 | Flow pattern regulator and preparation method and application thereof |
| CN114436885A (en) * | 2020-11-03 | 2022-05-06 | 中石化石油工程技术服务有限公司 | Oil-based drilling fluid shear strength improving agent, preparation method thereof and high-density oil-based drilling fluid |
| CN116064003B (en) * | 2021-11-01 | 2024-07-02 | 中国石油化工股份有限公司 | Oil-based gas stagnation for well drilling and preparation method thereof |
| CN116410709A (en) * | 2021-12-31 | 2023-07-11 | 中国石油天然气集团有限公司 | Synthetic base drilling fluid with flat plate flow pattern characteristics and preparation method thereof |
| CN114316936B (en) * | 2022-03-15 | 2022-05-13 | 华睿致诚化学(山东)有限公司 | Bifunctional depolymerization scale dissolver for oil extraction, and preparation and application thereof |
| CN114907823A (en) * | 2022-06-09 | 2022-08-16 | 成都西油华巍科技有限公司 | High-temperature-resistant shear-promoting agent for oil-based drilling fluid, preparation method and compound shear-promoting agent |
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